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We have synthesized large chlorapatite [ClAp, Ca5(PO4)3Clx(OH)1 − x, where x = 1] single crystals using the molten salt method. We have corroborated that the hexagonal symmetry P63/m describes the crystal structure best, even though the crystals are synthetic and stoichiometric. Moreover, we have performed several thermal treatments on these ClAp crystals, generating new single crystals in the apatite system [Ca5(PO4)3Clx(OH)1 − x, where x ≤ 1], where the chloride anions (Cl) were systematically substituted by hydroxyl anions (OH). These new single crystals were methodically characterized by powder and single-crystal X-ray diffraction (SXRD), scanning electron microscopy (SEM), Fourier transform–IR spectroscopy (FT–IR), and energy-dispersive X-ray spectroscopy (EDS). We have discovered a previously unreported OH inclusion site substituting the Cl anion during the ion-exchanging process. Finally, we evaluated the atomic rearrangements of the other species involved in the structure. These movements are associated with ionic exchange, which can be justified from an energetic point of view. We also found a novel phase transformation at high temperature. When the crystals are heated over 1753 K the apatite system evolves to a less ordered monoclinic structure, in which the complete loss of the species in the anionic channel (Cl, OH) has been confirmed.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768112019520/zb5021sup1.cif
Contains datablocks global, h_room_needle, e_room_prism, c_room_prism, v_room, 1_low_needle, 2_low_prism, 3_low_prism, 4_low_needle, C_mono, E_mono, H_mono, G_mono, B_mono, D_mono, F_mono, A_mono, 1400l, 1400r, 1450l, 1450r, 1475l, 1475r, 1480l, 1480r, 1500l

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768112019520/zb5021h_room_needlesup2.fcf
Contains datablock h_room_needle

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768112019520/zb5021e_room_prismsup3.fcf
Contains datablock e_room_prism

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Structure factor file (CIF format) https://doi.org/10.1107/S0108768112019520/zb5021c_room_prismsup4.fcf
Contains datablock c_room_prism

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768112019520/zb5021v_roomsup5.fcf
Contains datablock v_room

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768112019520/zb50211_low_needlesup6.fcf
Contains datablock a_low_needle

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768112019520/zb50212_low_prismsup7.fcf
Contains datablock d_low_prism

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768112019520/zb50213_low_prismsup8.fcf
Contains datablock f_low_prism

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768112019520/zb50214_low_needlesup9.fcf
Contains datablock b_low_needle

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768112019520/zb5021C_monosup10.fcf
Contains datablock C_mono

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768112019520/zb5021E_monosup11.fcf
Contains datablock E_mono

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768112019520/zb5021H_monosup12.fcf
Contains datablock H_mono

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768112019520/zb5021G_monosup13.fcf
Contains datablock G_mono

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768112019520/zb5021B_monosup14.fcf
Contains datablock B_mono

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768112019520/zb5021D_monosup15.fcf
Contains datablock D_mono

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768112019520/zb5021F_monosup16.fcf
Contains datablock F_mono

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768112019520/zb5021A_monosup17.fcf
Contains datablock A_mono

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Structure factor file (CIF format) https://doi.org/10.1107/S0108768112019520/zb50211400lsup18.fcf
Contains datablock 1400l

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Structure factor file (CIF format) https://doi.org/10.1107/S0108768112019520/zb50211400rsup19.fcf
Contains datablock 1400r

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768112019520/zb50211450lsup20.fcf
Contains datablock 1450l

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768112019520/zb50211450rsup21.fcf
Contains datablock 1450r

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768112019520/zb50211475lsup22.fcf
Contains datablock 1475l

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768112019520/zb50211475rsup23.fcf
Contains datablock 1475r

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768112019520/zb50211480lsup24.fcf
Contains datablock 1480l

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768112019520/zb50211480rsup25.fcf
Contains datablock 1480r

fcf

Structure factor file (CIF format) https://doi.org/10.1107/S0108768112019520/zb50211500lsup26.fcf
Contains datablock 1500l

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S0108768112019520/zb5021sup27.pdf
Extra figures and tables

Computing details top

Data collection: APPEX2 (BRUKER AXS, 2005) for h_room_needle, e_room_prism, c_room_prism, v_room, 1_low_needle, 2_low_prism, 3_low_prism, C_mono, E_mono, H_mono, G_mono, B_mono, D_mono, F_mono, A_mono, 1400l, 1400r, 1450l, 1450r, 1475l, 1475r, 1480l, 1480r, 1500l. Cell refinement: APPEX2 (BRUKER AXS, 2005) for h_room_needle, e_room_prism, c_room_prism, v_room, 1_low_needle, 2_low_prism, 3_low_prism, C_mono, E_mono, H_mono, G_mono, B_mono, D_mono, F_mono, A_mono, 1400l, 1400r, 1450l, 1450r, 1475l, 1475r, 1480l, 1480r, 1500l. Data reduction: APPEX2 (BRUKER AXS, 2005) for h_room_needle, e_room_prism, c_room_prism, v_room, 1_low_needle, 2_low_prism, 3_low_prism, C_mono, E_mono, H_mono, G_mono, B_mono, D_mono, F_mono, A_mono, 1400l, 1400r, 1450l, 1450r, 1475l, 1475r, 1480l, 1480r, 1500l. Program(s) used to solve structure: SIR2004 (Giacovazzo et al., 2004) for h_room_needle, e_room_prism, c_room_prism, v_room, 1_low_needle, 2_low_prism, 3_low_prism, 4_low_needle, C_mono, E_mono, H_mono, G_mono, B_mono, D_mono, F_mono, A_mono, 1400l, 1400r, 1450l, 1450r, 1475l, 1475r, 1480l, 1480r; SIR97 (Giacovazzo et al.l, 1999) for 1500l. Program(s) used to refine structure: SHELXL97 (Sheldrick, 1997) for h_room_needle, e_room_prism, c_room_prism, v_room, 1_low_needle, 2_low_prism, 1500l; SHELXL97 (Sheldrick, 2008) for 3_low_prism, 4_low_needle, C_mono, E_mono, H_mono, G_mono, B_mono, D_mono, F_mono, A_mono, 1400l, 1400r, 1450l, 1450r, 1475l, 1475r, 1480l, 1480r. For all compounds, molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX publication routines (Farrugia, 1999).

(h_room_needle) chlorapatite top
Crystal data top
3(O4P)·Cl·5(Ca)Dx = 3.174 Mg m3
Mr = 520.76Mo Kα radiation, λ = 0.7107 Å
Trigonal, P63/mCell parameters from 1653 reflections
Hall symbol: -P 6cθ = 11.5–51.6°
a = 9.6452 (2) ŵ = 3.21 mm1
c = 6.7636 (2) ÅT = 293 K
V = 544.92 (2) Å3Needle, colourless
Z = 20.30 × 0.03 × 0.02 mm
F(000) = 516
Data collection top
BRUKER APPEX-II CCD
diffractometer
403 independent reflections
Radiation source: fine-focus sealed tube345 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.061
ω and phi scansθmax = 26.4°, θmin = 2.4°
Absorption correction: multi-scan
BRUKER SADABS
h = 120
Tmin = 0.802, Tmax = 1k = 012
12306 measured reflectionsl = 08
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.022Secondary atom site location: difference Fourier map
wR(F2) = 0.056 w = 1/[σ2(Fo2) + (0.0294P)2 + 0.4891P]
where P = (Fo2 + 2Fc2)/3
S = 1.08(Δ/σ)max < 0.001
403 reflectionsΔρmax = 0.56 e Å3
40 parametersΔρmin = 0.52 e Å3
Crystal data top
3(O4P)·Cl·5(Ca)Z = 2
Mr = 520.76Mo Kα radiation
Trigonal, P63/mµ = 3.21 mm1
a = 9.6452 (2) ÅT = 293 K
c = 6.7636 (2) Å0.30 × 0.03 × 0.02 mm
V = 544.92 (2) Å3
Data collection top
BRUKER APPEX-II CCD
diffractometer
403 independent reflections
Absorption correction: multi-scan
BRUKER SADABS
345 reflections with I > 2σ(I)
Tmin = 0.802, Tmax = 1Rint = 0.061
12306 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.02240 parameters
wR(F2) = 0.0560 restraints
S = 1.08Δρmax = 0.56 e Å3
403 reflectionsΔρmin = 0.52 e Å3
Special details top

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ca10.00429 (9)0.74406 (8)0.250.0093 (2)
Ca20.33330.66670.00352 (13)0.0092 (2)
P10.37486 (11)0.96745 (10)0.250.0057 (2)
O20.3433 (3)0.5079 (3)0.250.0122 (6)
O30.0865 (2)0.6467 (2)0.0674 (3)0.0170 (5)
O40.1273 (3)0.5923 (3)0.250.0124 (6)
Cl1010.4433 (4)0.0272 (9)0.5
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0112 (4)0.0110 (4)0.0073 (4)0.0067 (3)00
Ca20.0115 (3)0.0115 (3)0.0047 (5)0.00577 (16)00
P10.0055 (4)0.0048 (4)0.0063 (5)0.0021 (3)00
O20.0182 (13)0.0136 (13)0.0106 (14)0.0124 (11)00
O30.0131 (9)0.0275 (11)0.0137 (10)0.0126 (8)0.0040 (8)0.0128 (9)
O40.0106 (12)0.0080 (12)0.0181 (15)0.0042 (11)00
Cl10.0151 (6)0.0151 (6)0.051 (3)0.0075 (3)00
Geometric parameters (Å, º) top
Ca1—O42.300 (3)Ca2—P1vi3.2179 (8)
Ca1—O32.331 (2)Ca2—P1ix3.2179 (8)
Ca1—O3i2.331 (2)P1—O3iii1.5300 (19)
Ca1—O3ii2.543 (2)P1—O3ii1.5300 (19)
Ca1—O3iii2.543 (2)P1—O2x1.536 (3)
Ca1—Cl12.8120 (14)P1—O4ix1.544 (3)
Ca1—Cl1i2.8120 (14)P1—Ca2i3.2179 (8)
Ca1—O22.965 (3)P1—Ca1ix3.3915 (11)
Ca1—P13.1172 (11)O2—P1xi1.536 (3)
Ca1—Cl1iv3.2405 (18)O2—Ca2viii2.4052 (18)
Ca1—Cl1v3.2405 (18)O2—Ca2xii2.4052 (18)
Ca1—P1vi3.3915 (11)O3—P1xiii1.5300 (19)
Ca2—O2iii2.4052 (18)O3—Ca1xiii2.543 (2)
Ca2—O2vii2.4052 (18)O3—Ca2viii2.800 (2)
Ca2—O2viii2.4052 (18)O4—P1vi1.544 (3)
Ca2—O4ix2.4449 (18)O4—Ca2i2.4449 (18)
Ca2—O42.4449 (18)Cl1—Cl1iv0.767 (5)
Ca2—O4vi2.4449 (18)Cl1—Ca1x2.8120 (14)
Ca2—O3iii2.800 (2)Cl1—Ca1xi2.8120 (14)
Ca2—O3viii2.800 (2)Cl1—Ca1iv3.2405 (18)
Ca2—O3vii2.800 (2)Cl1—Ca1xiv3.2405 (18)
Ca2—P13.2179 (8)Cl1—Ca1xv3.2405 (18)
O4—Ca1—O387.32 (6)O2vii—Ca2—P188.66 (5)
O4—Ca1—O3i87.32 (6)O2viii—Ca2—P1165.91 (6)
O3—Ca1—O3i134.11 (11)O4ix—Ca2—P127.57 (6)
O4—Ca1—O3ii75.19 (7)O4—Ca2—P166.89 (6)
O3—Ca1—O3ii139.36 (8)O4vi—Ca2—P199.08 (5)
O3i—Ca1—O3ii82.20 (4)O3iii—Ca2—P128.38 (4)
O4—Ca1—O3iii75.19 (7)O3viii—Ca2—P1122.51 (5)
O3—Ca1—O3iii82.20 (4)O3vii—Ca2—P193.93 (4)
O3i—Ca1—O3iii139.36 (8)O2iii—Ca2—P1vi88.66 (5)
O3ii—Ca1—O3iii58.11 (9)O2vii—Ca2—P1vi165.91 (6)
O4—Ca1—Cl1142.90 (6)O2viii—Ca2—P1vi99.29 (6)
O3—Ca1—Cl1127.89 (7)O4ix—Ca2—P1vi99.08 (5)
O3i—Ca1—Cl175.99 (7)O4—Ca2—P1vi27.57 (6)
O3ii—Ca1—Cl169.93 (5)O4vi—Ca2—P1vi66.89 (6)
O3iii—Ca1—Cl196.23 (6)O3iii—Ca2—P1vi93.93 (4)
O4—Ca1—Cl1i142.90 (6)O3viii—Ca2—P1vi28.38 (4)
O3—Ca1—Cl1i75.99 (7)O3vii—Ca2—P1vi122.51 (5)
O3i—Ca1—Cl1i127.89 (7)P1—Ca2—P1vi94.25 (2)
O3ii—Ca1—Cl1i96.23 (6)O2iii—Ca2—P1ix165.91 (6)
O3iii—Ca1—Cl1i69.93 (5)O2vii—Ca2—P1ix99.29 (6)
Cl1—Ca1—Cl1i55.41 (10)O2viii—Ca2—P1ix88.66 (5)
O4—Ca1—O2104.83 (8)O4ix—Ca2—P1ix66.89 (6)
O3—Ca1—O268.77 (5)O4—Ca2—P1ix99.08 (5)
O3i—Ca1—O268.77 (5)O4vi—Ca2—P1ix27.57 (6)
O3ii—Ca1—O2150.87 (4)O3iii—Ca2—P1ix122.51 (5)
O3iii—Ca1—O2150.87 (4)O3viii—Ca2—P1ix93.93 (4)
Cl1—Ca1—O299.62 (5)O3vii—Ca2—P1ix28.38 (4)
Cl1i—Ca1—O299.62 (5)P1—Ca2—P1ix94.25 (2)
O4—Ca1—P170.23 (7)P1vi—Ca2—P1ix94.25 (2)
O3—Ca1—P1110.39 (5)O3iii—P1—O3ii107.65 (16)
O3i—Ca1—P1110.39 (5)O3iii—P1—O2x112.07 (9)
O3ii—Ca1—P129.17 (4)O3ii—P1—O2x112.07 (9)
O3iii—Ca1—P129.17 (4)O3iii—P1—O4ix106.75 (10)
Cl1—Ca1—P184.74 (2)O3ii—P1—O4ix106.75 (10)
Cl1i—Ca1—P184.74 (2)O2x—P1—O4ix111.24 (14)
O2—Ca1—P1175.06 (5)O3iii—P1—Ca154.12 (8)
O4—Ca1—Cl1iv133.80 (4)O3ii—P1—Ca154.12 (8)
O3—Ca1—Cl1iv138.67 (6)O2x—P1—Ca1136.37 (11)
O3i—Ca1—Cl1iv64.65 (6)O4ix—P1—Ca1112.39 (10)
O3ii—Ca1—Cl1iv65.63 (5)O3iii—P1—Ca260.45 (8)
O3iii—Ca1—Cl1iv102.07 (5)O3ii—P1—Ca2111.53 (8)
Cl1—Ca1—Cl1iv12.10 (9)O2x—P1—Ca2135.68 (7)
Cl1i—Ca1—Cl1iv67.509 (19)O4ix—P1—Ca247.12 (7)
O2—Ca1—Cl1iv98.34 (4)Ca1—P1—Ca278.11 (2)
P1—Ca1—Cl1iv85.44 (2)O3iii—P1—Ca2i111.53 (8)
O4—Ca1—Cl1v133.80 (4)O3ii—P1—Ca2i60.45 (8)
O3—Ca1—Cl1v64.65 (6)O2x—P1—Ca2i135.68 (7)
O3i—Ca1—Cl1v138.67 (6)O4ix—P1—Ca2i47.12 (7)
O3ii—Ca1—Cl1v102.07 (5)Ca1—P1—Ca2i78.11 (2)
O3iii—Ca1—Cl1v65.63 (5)Ca2—P1—Ca2i64.40 (3)
Cl1—Ca1—Cl1v67.509 (19)O3iii—P1—Ca1ix122.06 (9)
Cl1i—Ca1—Cl1v12.10 (9)O3ii—P1—Ca1ix122.06 (9)
O2—Ca1—Cl1v98.34 (4)O2x—P1—Ca1ix76.41 (10)
P1—Ca1—Cl1v85.44 (2)Ca1—P1—Ca1ix147.22 (3)
Cl1iv—Ca1—Cl1v79.60 (8)Ca2—P1—Ca1ix74.27 (2)
O4—Ca1—P1vi22.55 (6)Ca2i—P1—Ca1ix74.27 (2)
O3—Ca1—P1vi78.95 (5)O3iii—P1—Ca1x80.43 (8)
O3i—Ca1—P1vi78.95 (5)O3ii—P1—Ca1x80.43 (8)
O3ii—Ca1—P1vi94.85 (5)O2x—P1—Ca1x55.90 (10)
O3iii—Ca1—P1vi94.85 (5)O4ix—P1—Ca1x167.14 (10)
Cl1—Ca1—P1vi152.13 (5)Ca1—P1—Ca1x80.47 (3)
Cl1i—Ca1—P1vi152.13 (5)Ca2—P1—Ca1x140.83 (2)
O2—Ca1—P1vi82.28 (5)Ca2i—P1—Ca1x140.83 (2)
P1—Ca1—P1vi92.78 (3)Ca1ix—P1—Ca1x132.31 (3)
Cl1iv—Ca1—P1vi140.09 (4)P1xi—O2—Ca2viii133.38 (6)
Cl1v—Ca1—P1vi140.09 (4)P1xi—O2—Ca2xii133.38 (6)
O2iii—Ca2—O2vii77.25 (7)Ca2viii—O2—Ca2xii87.76 (9)
O2iii—Ca2—O2viii77.25 (7)P1xi—O2—Ca198.69 (12)
O2vii—Ca2—O2viii77.25 (7)Ca2viii—O2—Ca196.44 (7)
O2iii—Ca2—O4ix126.28 (8)Ca2xii—O2—Ca196.44 (7)
O2vii—Ca2—O4ix89.88 (6)P1xiii—O3—Ca1139.23 (11)
O2viii—Ca2—O4ix150.32 (8)P1xiii—O3—Ca1xiii96.71 (10)
O2iii—Ca2—O489.88 (6)Ca1—O3—Ca1xiii118.91 (8)
O2vii—Ca2—O4150.32 (8)P1xiii—O3—Ca2viii91.17 (9)
O2viii—Ca2—O4126.28 (8)Ca1—O3—Ca2viii102.85 (8)
O4ix—Ca2—O476.24 (7)Ca1xiii—O3—Ca2viii96.58 (6)
O2iii—Ca2—O4vi150.32 (8)P1vi—O4—Ca1122.62 (14)
O2vii—Ca2—O4vi126.28 (8)P1vi—O4—Ca2i105.31 (9)
O2viii—Ca2—O4vi89.88 (6)Ca1—O4—Ca2i114.55 (7)
O4ix—Ca2—O4vi76.24 (7)P1vi—O4—Ca2105.31 (9)
O4—Ca2—O4vi76.24 (7)Ca1—O4—Ca2114.55 (7)
O2iii—Ca2—O3iii70.91 (7)Ca2i—O4—Ca289.07 (9)
O2vii—Ca2—O3iii82.12 (7)Cl1iv—Cl1—Ca1x117.71 (5)
O2viii—Ca2—O3iii145.13 (7)Cl1iv—Cl1—Ca1117.71 (5)
O4ix—Ca2—O3iii55.62 (7)Ca1x—Cl1—Ca1100.12 (6)
O4—Ca2—O3iii68.36 (7)Cl1iv—Cl1—Ca1xi117.71 (5)
O4vi—Ca2—O3iii124.96 (7)Ca1x—Cl1—Ca1xi100.12 (6)
O2iii—Ca2—O3viii82.12 (7)Ca1—Cl1—Ca1xi100.12 (6)
O2vii—Ca2—O3viii145.13 (7)Cl1iv—Cl1—Ca1iv50.20 (4)
O2viii—Ca2—O3viii70.91 (7)Ca1x—Cl1—Ca1iv87.567 (16)
O4ix—Ca2—O3viii124.96 (7)Ca1—Cl1—Ca1iv167.90 (9)
O4—Ca2—O3viii55.62 (7)Ca1xi—Cl1—Ca1iv87.567 (16)
O4vi—Ca2—O3viii68.36 (7)Cl1iv—Cl1—Ca1xiv50.20 (4)
O3iii—Ca2—O3viii117.13 (3)Ca1x—Cl1—Ca1xiv87.567 (16)
O2iii—Ca2—O3vii145.13 (7)Ca1—Cl1—Ca1xiv87.567 (16)
O2vii—Ca2—O3vii70.91 (7)Ca1xi—Cl1—Ca1xiv167.90 (9)
O2viii—Ca2—O3vii82.12 (7)Ca1iv—Cl1—Ca1xiv83.42 (6)
O4ix—Ca2—O3vii68.36 (7)Cl1iv—Cl1—Ca1xv50.20 (4)
O4—Ca2—O3vii124.96 (7)Ca1x—Cl1—Ca1xv167.90 (9)
O4vi—Ca2—O3vii55.62 (7)Ca1—Cl1—Ca1xv87.567 (16)
O3iii—Ca2—O3vii117.13 (3)Ca1xi—Cl1—Ca1xv87.567 (16)
O3viii—Ca2—O3vii117.13 (3)Ca1iv—Cl1—Ca1xv83.42 (6)
O2iii—Ca2—P199.29 (6)Ca1xiv—Cl1—Ca1xv83.42 (6)
O4—Ca1—P1—O3iii94.97 (9)O3ii—Ca1—O2—Ca2viii130.34 (11)
O3—Ca1—P1—O3iii15.73 (8)O3iii—Ca1—O2—Ca2viii41.88 (16)
O3i—Ca1—P1—O3iii174.22 (13)Cl1—Ca1—O2—Ca2viii163.91 (7)
O3ii—Ca1—P1—O3iii170.05 (19)Cl1i—Ca1—O2—Ca2viii107.63 (7)
Cl1—Ca1—P1—O3iii112.86 (11)Cl1iv—Ca1—O2—Ca2viii176.09 (6)
Cl1i—Ca1—P1—O3iii57.19 (11)Cl1v—Ca1—O2—Ca2viii95.46 (6)
Cl1iv—Ca1—P1—O3iii124.98 (10)O4—Ca1—O2—Ca2xii44.23 (5)
Cl1v—Ca1—P1—O3iii45.07 (10)O3—Ca1—O2—Ca2xii125.32 (9)
P1vi—Ca1—P1—O3iii94.97 (9)O3i—Ca1—O2—Ca2xii36.86 (6)
O4—Ca1—P1—O3ii94.97 (9)O3ii—Ca1—O2—Ca2xii41.88 (16)
O3—Ca1—P1—O3ii174.22 (13)O3iii—Ca1—O2—Ca2xii130.34 (11)
O3i—Ca1—P1—O3ii15.73 (8)Cl1—Ca1—O2—Ca2xii107.63 (7)
O3iii—Ca1—P1—O3ii170.05 (19)Cl1i—Ca1—O2—Ca2xii163.91 (7)
Cl1—Ca1—P1—O3ii57.19 (11)Cl1iv—Ca1—O2—Ca2xii95.46 (6)
Cl1i—Ca1—P1—O3ii112.86 (11)Cl1v—Ca1—O2—Ca2xii176.09 (6)
Cl1iv—Ca1—P1—O3ii45.07 (10)P1vi—Ca1—O2—Ca2xii44.23 (5)
Cl1v—Ca1—P1—O3ii124.98 (10)O4—Ca1—O3—P1xiii31.9 (2)
P1vi—Ca1—P1—O3ii94.97 (9)O3i—Ca1—O3—P1xiii115.54 (17)
O4—Ca1—P1—O2x180O3ii—Ca1—O3—P1xiii31.5 (3)
O3—Ca1—P1—O2x100.76 (6)O3iii—Ca1—O3—P1xiii43.5 (2)
O3i—Ca1—P1—O2x100.76 (6)Cl1—Ca1—O3—P1xiii135.37 (16)
O3ii—Ca1—P1—O2x85.03 (9)Cl1i—Ca1—O3—P1xiii114.70 (19)
O3iii—Ca1—P1—O2x85.03 (9)O2—Ca1—O3—P1xiii138.9 (2)
Cl1—Ca1—P1—O2x27.83 (5)P1—Ca1—O3—P1xiii35.9 (2)
Cl1i—Ca1—P1—O2x27.83 (5)Cl1iv—Ca1—O3—P1xiii142.96 (15)
Cl1iv—Ca1—P1—O2x39.95 (4)Cl1v—Ca1—O3—P1xiii110.2 (2)
Cl1v—Ca1—P1—O2x39.95 (4)P1vi—Ca1—O3—P1xiii53.00 (18)
P1vi—Ca1—P1—O2x180O4—Ca1—O3—Ca1xiii179.55 (10)
O4—Ca1—P1—O4ix0O3i—Ca1—O3—Ca1xiii96.80 (14)
O3—Ca1—P1—O4ix79.24 (6)O3ii—Ca1—O3—Ca1xiii116.13 (6)
O3i—Ca1—P1—O4ix79.24 (6)O3iii—Ca1—O3—Ca1xiii104.14 (5)
O3ii—Ca1—P1—O4ix94.97 (9)Cl1—Ca1—O3—Ca1xiii12.29 (13)
O3iii—Ca1—P1—O4ix94.97 (9)Cl1i—Ca1—O3—Ca1xiii32.97 (8)
Cl1—Ca1—P1—O4ix152.17 (5)O2—Ca1—O3—Ca1xiii73.40 (9)
Cl1i—Ca1—P1—O4ix152.17 (5)P1—Ca1—O3—Ca1xiii111.80 (7)
Cl1iv—Ca1—P1—O4ix140.05 (4)Cl1iv—Ca1—O3—Ca1xiii4.70 (15)
Cl1v—Ca1—P1—O4ix140.05 (4)Cl1v—Ca1—O3—Ca1xiii37.47 (7)
P1vi—Ca1—P1—O4ix0P1vi—Ca1—O3—Ca1xiii159.34 (9)
O4—Ca1—P1—Ca232.994 (15)O4—Ca1—O3—Ca2viii75.36 (7)
O3—Ca1—P1—Ca246.25 (6)O3i—Ca1—O3—Ca2viii8.28 (16)
O3i—Ca1—P1—Ca2112.24 (6)O3ii—Ca1—O3—Ca2viii138.79 (11)
O3ii—Ca1—P1—Ca2127.97 (10)O3iii—Ca1—O3—Ca2viii150.78 (6)
O3iii—Ca1—P1—Ca261.98 (9)Cl1—Ca1—O3—Ca2viii117.38 (7)
Cl1—Ca1—P1—Ca2174.84 (5)Cl1i—Ca1—O3—Ca2viii138.05 (6)
Cl1i—Ca1—P1—Ca2119.17 (5)O2—Ca1—O3—Ca2viii31.68 (6)
Cl1iv—Ca1—P1—Ca2173.04 (4)P1—Ca1—O3—Ca2viii143.11 (4)
Cl1v—Ca1—P1—Ca2107.05 (4)Cl1iv—Ca1—O3—Ca2viii109.79 (8)
P1vi—Ca1—P1—Ca232.994 (15)Cl1v—Ca1—O3—Ca2viii142.55 (7)
O4—Ca1—P1—Ca2i32.994 (15)P1vi—Ca1—O3—Ca2viii54.25 (5)
O3—Ca1—P1—Ca2i112.24 (6)O3—Ca1—O4—P1vi67.21 (5)
O3i—Ca1—P1—Ca2i46.25 (6)O3i—Ca1—O4—P1vi67.21 (5)
O3ii—Ca1—P1—Ca2i61.98 (9)O3ii—Ca1—O4—P1vi149.85 (5)
O3iii—Ca1—P1—Ca2i127.97 (10)O3iii—Ca1—O4—P1vi149.85 (5)
Cl1—Ca1—P1—Ca2i119.17 (5)Cl1—Ca1—O4—P1vi129.57 (9)
Cl1i—Ca1—P1—Ca2i174.84 (5)Cl1i—Ca1—O4—P1vi129.57 (9)
Cl1iv—Ca1—P1—Ca2i107.05 (4)O2—Ca1—O4—P1vi0
Cl1v—Ca1—P1—Ca2i173.04 (4)P1—Ca1—O4—P1vi180
P1vi—Ca1—P1—Ca2i32.994 (15)Cl1iv—Ca1—O4—P1vi117.51 (7)
O4—Ca1—P1—Ca1ix0Cl1v—Ca1—O4—P1vi117.51 (7)
O3—Ca1—P1—Ca1ix79.24 (6)O3—Ca1—O4—Ca2i163.24 (9)
O3i—Ca1—P1—Ca1ix79.24 (6)O3i—Ca1—O4—Ca2i62.35 (9)
O3ii—Ca1—P1—Ca1ix94.97 (9)O3ii—Ca1—O4—Ca2i20.29 (8)
O3iii—Ca1—P1—Ca1ix94.97 (9)O3iii—Ca1—O4—Ca2i80.60 (9)
Cl1—Ca1—P1—Ca1ix152.17 (5)Cl1—Ca1—O4—Ca2i0.01 (15)
Cl1i—Ca1—P1—Ca1ix152.17 (5)Cl1i—Ca1—O4—Ca2i100.88 (7)
Cl1iv—Ca1—P1—Ca1ix140.05 (4)O2—Ca1—O4—Ca2i129.55 (7)
Cl1v—Ca1—P1—Ca1ix140.05 (4)P1—Ca1—O4—Ca2i50.45 (7)
P1vi—Ca1—P1—Ca1ix0Cl1iv—Ca1—O4—Ca2i12.04 (13)
O4—Ca1—P1—Ca1x180Cl1v—Ca1—O4—Ca2i112.94 (5)
O3—Ca1—P1—Ca1x100.76 (6)P1vi—Ca1—O4—Ca2i129.55 (7)
O3i—Ca1—P1—Ca1x100.76 (6)O3—Ca1—O4—Ca262.35 (9)
O3ii—Ca1—P1—Ca1x85.03 (9)O3i—Ca1—O4—Ca2163.24 (9)
O3iii—Ca1—P1—Ca1x85.03 (9)O3ii—Ca1—O4—Ca280.60 (9)
Cl1—Ca1—P1—Ca1x27.83 (5)O3iii—Ca1—O4—Ca220.29 (8)
Cl1i—Ca1—P1—Ca1x27.83 (5)Cl1—Ca1—O4—Ca2100.88 (7)
Cl1iv—Ca1—P1—Ca1x39.95 (4)Cl1i—Ca1—O4—Ca20.01 (15)
Cl1v—Ca1—P1—Ca1x39.95 (4)O2—Ca1—O4—Ca2129.55 (7)
P1vi—Ca1—P1—Ca1x180P1—Ca1—O4—Ca250.45 (7)
O2iii—Ca2—P1—O3iii1.06 (10)Cl1iv—Ca1—O4—Ca2112.94 (5)
O2vii—Ca2—P1—O3iii75.80 (10)Cl1v—Ca1—O4—Ca212.04 (13)
O2viii—Ca2—P1—O3iii73.5 (3)P1vi—Ca1—O4—Ca2129.55 (7)
O4ix—Ca2—P1—O3iii168.09 (13)O2iii—Ca2—O4—P1vi87.35 (10)
O4—Ca2—P1—O3iii86.92 (10)O2vii—Ca2—O4—P1vi150.65 (12)
O4vi—Ca2—P1—O3iii157.65 (10)O2viii—Ca2—O4—P1vi13.33 (13)
O3viii—Ca2—P1—O3iii87.59 (5)O4ix—Ca2—O4—P1vi145.08 (10)
O3vii—Ca2—P1—O3iii146.56 (10)O4vi—Ca2—O4—P1vi66.16 (13)
P1vi—Ca2—P1—O3iii90.40 (9)O3iii—Ca2—O4—P1vi156.80 (11)
P1ix—Ca2—P1—O3iii175.01 (9)O3viii—Ca2—O4—P1vi6.83 (7)
O2iii—Ca2—P1—O3ii97.62 (10)O3vii—Ca2—O4—P1vi94.47 (10)
O2vii—Ca2—P1—O3ii174.47 (11)P1—Ca2—O4—P1vi172.49 (10)
O2viii—Ca2—P1—O3ii172.2 (3)P1ix—Ca2—O4—P1vi81.72 (8)
O4ix—Ca2—P1—O3ii93.23 (13)O2iii—Ca2—O4—Ca150.33 (10)
O4—Ca2—P1—O3ii11.76 (10)O2vii—Ca2—O4—Ca112.97 (18)
O4vi—Ca2—P1—O3ii58.97 (11)O2viii—Ca2—O4—Ca1124.35 (9)
O3iii—Ca2—P1—O3ii98.68 (17)O4ix—Ca2—O4—Ca177.24 (13)
O3viii—Ca2—P1—O3ii11.09 (13)O4vi—Ca2—O4—Ca1156.16 (10)
O3vii—Ca2—P1—O3ii114.76 (10)O3iii—Ca2—O4—Ca119.13 (7)
P1vi—Ca2—P1—O3ii8.28 (9)O3viii—Ca2—O4—Ca1130.85 (10)
P1ix—Ca2—P1—O3ii86.31 (9)O3vii—Ca2—O4—Ca1127.86 (7)
O2iii—Ca2—P1—O2x93.22 (15)P1—Ca2—O4—Ca149.84 (7)
O2vii—Ca2—P1—O2x16.36 (17)P1vi—Ca2—O4—Ca1137.68 (14)
O2viii—Ca2—P1—O2x18.7 (2)P1ix—Ca2—O4—Ca1140.60 (7)
O4ix—Ca2—P1—O2x75.93 (15)O2iii—Ca2—O4—Ca2i167.03 (8)
O4—Ca2—P1—O2x179.08 (13)O2vii—Ca2—O4—Ca2i103.73 (13)
O4vi—Ca2—P1—O2x110.19 (13)O2viii—Ca2—O4—Ca2i118.95 (8)
O3iii—Ca2—P1—O2x92.16 (14)O3iii—Ca2—O4—Ca2i97.57 (7)
O3viii—Ca2—P1—O2x179.75 (12)O3viii—Ca2—O4—Ca2i112.45 (9)
O3vii—Ca2—P1—O2x54.40 (13)O3vii—Ca2—O4—Ca2i11.16 (11)
P1vi—Ca2—P1—O2x177.44 (12)P1—Ca2—O4—Ca2i66.87 (5)
P1ix—Ca2—P1—O2x82.85 (12)P1vi—Ca2—O4—Ca2i105.62 (11)
O2iii—Ca2—P1—O4ix169.15 (11)P1ix—Ca2—O4—Ca2i23.90 (6)
O2vii—Ca2—P1—O4ix92.29 (11)O4—Ca1—Cl1—Cl1iv46.01 (10)
O2viii—Ca2—P1—O4ix94.6 (3)O3—Ca1—Cl1—Cl1iv155.41 (7)
O4—Ca2—P1—O4ix104.99 (14)O3i—Ca1—Cl1—Cl1iv19.78 (5)
O4vi—Ca2—P1—O4ix34.26 (11)O3ii—Ca1—Cl1—Cl1iv66.91 (5)
O3iii—Ca2—P1—O4ix168.09 (13)O3iii—Ca1—Cl1—Cl1iv119.63 (4)
O3viii—Ca2—P1—O4ix104.32 (11)Cl1i—Ca1—Cl1—Cl1iv180.000 (2)
O3vii—Ca2—P1—O4ix21.53 (10)O2—Ca1—Cl1—Cl1iv84.89 (3)
P1vi—Ca2—P1—O4ix101.51 (9)P1—Ca1—Cl1—Cl1iv92.773 (12)
P1ix—Ca2—P1—O4ix6.92 (9)Cl1v—Ca1—Cl1—Cl1iv180.000 (2)
O2iii—Ca2—P1—Ca154.25 (5)P1vi—Ca1—Cl1—Cl1iv6.79 (7)
O2vii—Ca2—P1—Ca1131.10 (6)O4—Ca1—Cl1—Ca1x82.83 (13)
O2viii—Ca2—P1—Ca1128.8 (2)O3—Ca1—Cl1—Ca1x75.74 (7)
O4ix—Ca2—P1—Ca1136.60 (9)O3i—Ca1—Cl1—Ca1x148.63 (7)
O4—Ca2—P1—Ca131.61 (5)O3ii—Ca1—Cl1—Ca1x61.93 (6)
O4vi—Ca2—P1—Ca1102.34 (6)O3iii—Ca1—Cl1—Ca1x9.21 (7)
O3iii—Ca2—P1—Ca155.31 (9)Cl1i—Ca1—Cl1—Ca1x51.15 (5)
O3viii—Ca2—P1—Ca132.28 (5)O2—Ca1—Cl1—Ca1x146.26 (5)
O3vii—Ca2—P1—Ca1158.13 (4)P1—Ca1—Cl1—Ca1x36.07 (4)
P1vi—Ca2—P1—Ca135.088 (18)Cl1iv—Ca1—Cl1—Ca1x128.85 (5)
P1ix—Ca2—P1—Ca1129.677 (17)Cl1v—Ca1—Cl1—Ca1x51.15 (5)
O2iii—Ca2—P1—Ca2i136.63 (5)P1vi—Ca1—Cl1—Ca1x122.06 (9)
O2vii—Ca2—P1—Ca2i146.51 (6)O4—Ca1—Cl1—Ca1xi174.86 (9)
O2viii—Ca2—P1—Ca2i148.8 (2)O3—Ca1—Cl1—Ca1xi26.57 (9)
O4ix—Ca2—P1—Ca2i54.22 (9)O3i—Ca1—Cl1—Ca1xi109.06 (7)
O4—Ca2—P1—Ca2i50.77 (5)O3ii—Ca1—Cl1—Ca1xi164.24 (8)
O4vi—Ca2—P1—Ca2i19.95 (6)O3iii—Ca1—Cl1—Ca1xi111.52 (6)
O3iii—Ca2—P1—Ca2i137.69 (9)Cl1i—Ca1—Cl1—Ca1xi51.15 (5)
O3viii—Ca2—P1—Ca2i50.10 (5)O2—Ca1—Cl1—Ca1xi43.95 (6)
O3vii—Ca2—P1—Ca2i75.75 (4)P1—Ca1—Cl1—Ca1xi138.38 (5)
P1vi—Ca2—P1—Ca2i47.294 (12)Cl1iv—Ca1—Cl1—Ca1xi128.85 (5)
P1ix—Ca2—P1—Ca2i47.294 (12)Cl1v—Ca1—Cl1—Ca1xi51.15 (5)
O2iii—Ca2—P1—Ca1ix143.58 (5)P1vi—Ca1—Cl1—Ca1xi135.63 (8)
O2vii—Ca2—P1—Ca1ix66.73 (6)O4—Ca1—Cl1—Ca1iv46.01 (10)
O2viii—Ca2—P1—Ca1ix69.0 (2)O3—Ca1—Cl1—Ca1iv155.41 (7)
O4ix—Ca2—P1—Ca1ix25.56 (9)O3i—Ca1—Cl1—Ca1iv19.78 (5)
O4—Ca2—P1—Ca1ix130.55 (5)O3ii—Ca1—Cl1—Ca1iv66.91 (5)
O4vi—Ca2—P1—Ca1ix59.83 (6)O3iii—Ca1—Cl1—Ca1iv119.63 (4)
O3iii—Ca2—P1—Ca1ix142.53 (9)Cl1i—Ca1—Cl1—Ca1iv180.000 (2)
O3viii—Ca2—P1—Ca1ix129.88 (5)O2—Ca1—Cl1—Ca1iv84.89 (3)
O3vii—Ca2—P1—Ca1ix4.03 (4)P1—Ca1—Cl1—Ca1iv92.773 (12)
P1vi—Ca2—P1—Ca1ix127.077 (18)Cl1iv—Ca1—Cl1—Ca1iv0
P1ix—Ca2—P1—Ca1ix32.488 (17)Cl1v—Ca1—Cl1—Ca1iv180.000 (2)
O2iii—Ca2—P1—Ca1x4.00 (7)P1vi—Ca1—Cl1—Ca1iv6.79 (7)
O2vii—Ca2—P1—Ca1x72.86 (7)O4—Ca1—Cl1—Ca1xiv4.26 (12)
O2viii—Ca2—P1—Ca1x70.5 (2)O3—Ca1—Cl1—Ca1xiv162.83 (7)
O4ix—Ca2—P1—Ca1x165.15 (11)O3i—Ca1—Cl1—Ca1xiv61.54 (6)
O4—Ca2—P1—Ca1x89.86 (7)O3ii—Ca1—Cl1—Ca1xiv25.16 (5)
O4vi—Ca2—P1—Ca1x160.58 (7)O3iii—Ca1—Cl1—Ca1xiv77.88 (5)
O3iii—Ca2—P1—Ca1x2.94 (9)Cl1i—Ca1—Cl1—Ca1xiv138.25 (3)
O3viii—Ca2—P1—Ca1x90.53 (7)O2—Ca1—Cl1—Ca1xiv126.65 (3)
O3vii—Ca2—P1—Ca1x143.62 (6)P1—Ca1—Cl1—Ca1xiv51.02 (2)
P1vi—Ca2—P1—Ca1x93.33 (5)Cl1iv—Ca1—Cl1—Ca1xiv41.75 (3)
P1ix—Ca2—P1—Ca1x172.08 (5)Cl1v—Ca1—Cl1—Ca1xiv138.25 (3)
O4—Ca1—O2—P1xi180P1vi—Ca1—Cl1—Ca1xiv34.96 (8)
O3—Ca1—O2—P1xi98.91 (6)O4—Ca1—Cl1—Ca1xv87.76 (9)
O3i—Ca1—O2—P1xi98.91 (6)O3—Ca1—Cl1—Ca1xv113.66 (8)
O3ii—Ca1—O2—P1xi93.89 (13)O3i—Ca1—Cl1—Ca1xv21.97 (5)
O3iii—Ca1—O2—P1xi93.89 (13)O3ii—Ca1—Cl1—Ca1xv108.67 (6)
Cl1—Ca1—O2—P1xi28.14 (5)O3iii—Ca1—Cl1—Ca1xv161.39 (5)
Cl1i—Ca1—O2—P1xi28.14 (5)Cl1i—Ca1—Cl1—Ca1xv138.25 (3)
Cl1iv—Ca1—O2—P1xi40.31 (4)O2—Ca1—Cl1—Ca1xv43.14 (4)
Cl1v—Ca1—O2—P1xi40.31 (4)P1—Ca1—Cl1—Ca1xv134.53 (4)
O4—Ca1—O2—Ca2viii44.23 (5)Cl1iv—Ca1—Cl1—Ca1xv41.75 (3)
O3—Ca1—O2—Ca2viii36.86 (6)Cl1v—Ca1—Cl1—Ca1xv138.25 (3)
O3i—Ca1—O2—Ca2viii125.32 (9)P1vi—Ca1—Cl1—Ca1xv48.54 (7)
Symmetry codes: (i) x, y, z+1/2; (ii) xy+1, x+1, z+1/2; (iii) xy+1, x+1, z; (iv) x, y+2, z+1; (v) x, y+2, z1/2; (vi) y+1, xy+1, z; (vii) y, x+y, z; (viii) x, y+1, z; (ix) x+y, x+1, z; (x) y+1, xy+2, z; (xi) x+y1, x+1, z; (xii) x, y+1, z+1/2; (xiii) y1, x+y, z; (xiv) xy+1, x+1, z+1; (xv) y1, x+y, z+1.
(e_room_prism) chlorapatite top
Crystal data top
3(O4P)·Cl·5(Ca)Dx = 3.176 Mg m3
Mr = 520.76Mo Kα radiation, λ = 0.7107 Å
Trigonal, P63/mCell parameters from 1997 reflections
Hall symbol: -P 6cθ = 7.8–54.1°
a = 9.6434 (2) ŵ = 3.21 mm1
c = 6.7643 (2) ÅT = 293 K
V = 544.77 (2) Å3Prism, colourless
Z = 20.29 × 0.12 × 0.1 mm
F(000) = 516
Data collection top
BRUKER APPEX-II CCD
diffractometer
399 independent reflections
Radiation source: fine-focus sealed tube386 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.027
ω and phi scansθmax = 26.3°, θmin = 2.4°
Absorption correction: multi-scan
BRUKER SADABS
h = 1212
Tmin = 0.654, Tmax = 1k = 1212
11773 measured reflectionsl = 88
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.017 w = 1/[σ2(Fo2) + (0.024P)2 + 0.4799P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.046(Δ/σ)max < 0.001
S = 1.11Δρmax = 0.28 e Å3
399 reflectionsΔρmin = 0.42 e Å3
41 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.160 (7)
Crystal data top
3(O4P)·Cl·5(Ca)Z = 2
Mr = 520.76Mo Kα radiation
Trigonal, P63/mµ = 3.21 mm1
a = 9.6434 (2) ÅT = 293 K
c = 6.7643 (2) Å0.29 × 0.12 × 0.1 mm
V = 544.77 (2) Å3
Data collection top
BRUKER APPEX-II CCD
diffractometer
399 independent reflections
Absorption correction: multi-scan
BRUKER SADABS
386 reflections with I > 2σ(I)
Tmin = 0.654, Tmax = 1Rint = 0.027
11773 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.01741 parameters
wR(F2) = 0.0460 restraints
S = 1.11Δρmax = 0.28 e Å3
399 reflectionsΔρmin = 0.42 e Å3
Special details top

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ca10.00437 (6)0.74425 (6)0.250.0109 (2)
Ca20.33330.66670.00346 (9)0.0110 (2)
P10.37491 (7)0.96744 (7)0.250.0073 (2)
O20.3439 (2)0.5080 (2)0.250.0139 (4)
O30.08671 (15)0.64664 (17)0.0671 (2)0.0190 (3)
O40.1274 (2)0.5924 (2)0.250.0142 (4)
Cl1010.4441 (3)0.0259 (5)0.5
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0129 (3)0.0130 (3)0.0085 (3)0.0076 (2)00
Ca20.0131 (3)0.0131 (3)0.0067 (3)0.00653 (13)00
P10.0070 (3)0.0066 (3)0.0076 (3)0.0029 (2)00
O20.0201 (9)0.0149 (9)0.0132 (9)0.0136 (7)00
O30.0149 (6)0.0294 (7)0.0164 (7)0.0138 (6)0.0046 (5)0.0126 (6)
O40.0122 (8)0.0087 (8)0.0214 (10)0.0049 (7)00
Cl10.0160 (4)0.0160 (4)0.0458 (15)0.0080 (2)00
Geometric parameters (Å, º) top
Ca1—O42.2997 (17)Ca2—P1vi3.2167 (6)
Ca1—O32.3298 (13)Ca2—P1ix3.2167 (6)
Ca1—O3i2.3298 (13)P1—O3iii1.5321 (13)
Ca1—O3ii2.5418 (14)P1—O3ii1.5321 (13)
Ca1—O3iii2.5418 (14)P1—O2x1.5313 (17)
Ca1—Cl12.8125 (10)P1—O4ix1.5447 (17)
Ca1—Cl1i2.8125 (10)P1—Ca2i3.2167 (6)
Ca1—O22.9692 (19)P1—Ca1ix3.3916 (7)
Ca1—P13.1160 (7)O2—P1xi1.5313 (17)
Ca1—Cl1iv3.2353 (12)O2—Ca2viii2.4075 (12)
Ca1—Cl1v3.2353 (12)O2—Ca2xii2.4075 (12)
Ca1—P1vi3.3916 (7)O3—P1xiii1.5321 (13)
Ca2—O2iii2.4075 (12)O3—Ca1xiii2.5418 (13)
Ca2—O2vii2.4075 (12)O3—Ca2viii2.7975 (14)
Ca2—O2viii2.4075 (12)O4—P1vi1.5447 (17)
Ca2—O4ix2.4436 (12)O4—Ca2i2.4436 (12)
Ca2—O42.4436 (12)Cl1—Cl1iv0.756 (4)
Ca2—O4vi2.4436 (12)Cl1—Ca1x2.8125 (10)
Ca2—O3iii2.7975 (14)Cl1—Ca1xi2.8125 (10)
Ca2—O3viii2.7976 (14)Cl1—Ca1iv3.2353 (12)
Ca2—O3vii2.7975 (14)Cl1—Ca1xiv3.2353 (12)
Ca2—P13.2167 (6)Cl1—Ca1xv3.2353 (12)
O4—Ca1—O387.31 (4)O2vii—Ca2—P188.55 (4)
O4—Ca1—O3i87.31 (4)O2viii—Ca2—P1165.87 (4)
O3—Ca1—O3i133.95 (8)O4ix—Ca2—P127.59 (4)
O4—Ca1—O3ii75.14 (5)O4—Ca2—P166.87 (4)
O3—Ca1—O3ii139.47 (5)O4vi—Ca2—P199.09 (3)
O3i—Ca1—O3ii82.21 (3)O3iii—Ca2—P128.44 (3)
O4—Ca1—O3iii75.14 (5)O3viii—Ca2—P1122.57 (3)
O3—Ca1—O3iii82.21 (3)O3vii—Ca2—P193.93 (3)
O3i—Ca1—O3iii139.47 (5)O2iii—Ca2—P1vi88.55 (4)
O3ii—Ca1—O3iii58.23 (6)O2vii—Ca2—P1vi165.87 (4)
O4—Ca1—Cl1142.84 (4)O2viii—Ca2—P1vi99.35 (4)
O3—Ca1—Cl1128.01 (5)O4ix—Ca2—P1vi99.09 (4)
O3i—Ca1—Cl175.93 (5)O4—Ca2—P1vi27.59 (4)
O3ii—Ca1—Cl169.94 (3)O4vi—Ca2—P1vi66.87 (4)
O3iii—Ca1—Cl196.38 (4)O3iii—Ca2—P1vi93.93 (3)
O4—Ca1—Cl1i142.84 (4)O3viii—Ca2—P1vi28.44 (3)
O3—Ca1—Cl1i75.93 (5)O3vii—Ca2—P1vi122.57 (3)
O3i—Ca1—Cl1i128.01 (5)P1—Ca2—P1vi94.254 (14)
O3ii—Ca1—Cl1i96.38 (4)O2iii—Ca2—P1ix165.87 (4)
O3iii—Ca1—Cl1i69.94 (3)O2vii—Ca2—P1ix99.35 (4)
Cl1—Ca1—Cl1i55.63 (7)O2viii—Ca2—P1ix88.55 (4)
O4—Ca1—O2104.89 (6)O4ix—Ca2—P1ix66.87 (4)
O3—Ca1—O268.70 (4)O4—Ca2—P1ix99.09 (4)
O3i—Ca1—O268.70 (4)O4vi—Ca2—P1ix27.59 (4)
O3ii—Ca1—O2150.81 (3)O3iii—Ca2—P1ix122.57 (3)
O3iii—Ca1—O2150.81 (3)O3viii—Ca2—P1ix93.93 (3)
Cl1—Ca1—O299.55 (3)O3vii—Ca2—P1ix28.44 (3)
Cl1i—Ca1—O299.55 (3)P1—Ca2—P1ix94.254 (14)
O4—Ca1—P170.20 (5)P1vi—Ca2—P1ix94.254 (14)
O3—Ca1—P1110.46 (3)O3iii—P1—O3ii107.67 (11)
O3i—Ca1—P1110.46 (3)O3iii—P1—O2x112.15 (6)
O3ii—Ca1—P129.23 (3)O3ii—P1—O2x112.15 (6)
O3iii—Ca1—P129.23 (3)O3iii—P1—O4ix106.70 (7)
Cl1—Ca1—P184.784 (15)O3ii—P1—O4ix106.70 (7)
Cl1i—Ca1—P184.784 (15)O2x—P1—O4ix111.15 (10)
O2—Ca1—P1175.09 (4)O3iii—P1—Ca154.12 (5)
O4—Ca1—Cl1iv133.85 (3)O3ii—P1—Ca154.12 (5)
O3—Ca1—Cl1iv138.63 (4)O2x—P1—Ca1136.44 (8)
O3i—Ca1—Cl1iv64.76 (4)O4ix—P1—Ca1112.41 (7)
O3ii—Ca1—Cl1iv65.67 (3)O3iii—P1—Ca260.40 (6)
O3iii—Ca1—Cl1iv102.14 (4)O3ii—P1—Ca2111.49 (5)
Cl1—Ca1—Cl1iv11.93 (6)O2x—P1—Ca2135.62 (5)
Cl1i—Ca1—Cl1iv67.561 (12)O4ix—P1—Ca247.12 (4)
O2—Ca1—Cl1iv98.29 (3)Ca1—P1—Ca278.130 (14)
P1—Ca1—Cl1iv85.468 (13)O3iii—P1—Ca2i111.49 (5)
O4—Ca1—Cl1v133.85 (3)O3ii—P1—Ca2i60.40 (6)
O3—Ca1—Cl1v64.76 (4)O2x—P1—Ca2i135.62 (5)
O3i—Ca1—Cl1v138.63 (4)O4ix—P1—Ca2i47.12 (4)
O3ii—Ca1—Cl1v102.14 (4)Ca1—P1—Ca2i78.130 (14)
O3iii—Ca1—Cl1v65.67 (3)Ca2—P1—Ca2i64.39 (2)
Cl1—Ca1—Cl1v67.561 (12)O3iii—P1—Ca1ix122.02 (6)
Cl1i—Ca1—Cl1v11.93 (6)O3ii—P1—Ca1ix122.02 (6)
O2—Ca1—Cl1v98.29 (3)O2x—P1—Ca1ix76.32 (7)
P1—Ca1—Cl1v85.468 (13)Ca1—P1—Ca1ix147.24 (2)
Cl1iv—Ca1—Cl1v79.49 (5)Ca2—P1—Ca1ix74.265 (13)
O4—Ca1—P1vi22.56 (4)Ca2i—P1—Ca1ix74.265 (13)
O3—Ca1—P1vi78.91 (4)O3iii—P1—Ca1x80.46 (6)
O3i—Ca1—P1vi78.91 (4)O3ii—P1—Ca1x80.46 (6)
O3ii—Ca1—P1vi94.80 (4)O2x—P1—Ca1x56.03 (7)
O3iii—Ca1—P1vi94.80 (4)O4ix—P1—Ca1x167.18 (7)
Cl1—Ca1—P1vi152.02 (3)Ca1—P1—Ca1x80.41 (2)
Cl1i—Ca1—P1vi152.02 (3)Ca2—P1—Ca1x140.817 (14)
O2—Ca1—P1vi82.33 (4)Ca2i—P1—Ca1x140.817 (14)
P1—Ca1—P1vi92.76 (2)Ca1ix—P1—Ca1x132.35 (2)
Cl1iv—Ca1—P1vi140.15 (3)P1xi—O2—Ca2viii133.51 (4)
Cl1v—Ca1—P1vi140.15 (3)P1xi—O2—Ca2xii133.51 (4)
O2iii—Ca2—O2vii77.33 (5)Ca2viii—O2—Ca2xii87.65 (6)
O2iii—Ca2—O2viii77.33 (5)P1xi—O2—Ca198.65 (8)
O2vii—Ca2—O2viii77.33 (5)Ca2viii—O2—Ca196.30 (5)
O2iii—Ca2—O4ix126.37 (6)Ca2xii—O2—Ca196.30 (5)
O2vii—Ca2—O4ix89.80 (4)P1xiii—O3—Ca1139.18 (7)
O2viii—Ca2—O4ix150.18 (6)P1xiii—O3—Ca1xiii96.64 (6)
O2iii—Ca2—O489.80 (4)Ca1—O3—Ca1xiii118.93 (5)
O2vii—Ca2—O4150.18 (6)P1xiii—O3—Ca2viii91.16 (6)
O2viii—Ca2—O4126.37 (6)Ca1—O3—Ca2viii102.98 (5)
O4ix—Ca2—O476.24 (5)Ca1xiii—O3—Ca2viii96.65 (4)
O2iii—Ca2—O4vi150.18 (6)P1vi—O4—Ca1122.61 (9)
O2vii—Ca2—O4vi126.37 (6)P1vi—O4—Ca2i105.29 (6)
O2viii—Ca2—O4vi89.80 (4)Ca1—O4—Ca2i114.57 (5)
O4ix—Ca2—O4vi76.24 (5)P1vi—O4—Ca2105.29 (6)
O4—Ca2—O4vi76.24 (5)Ca1—O4—Ca2114.57 (5)
O2iii—Ca2—O3iii70.92 (5)Ca2i—O4—Ca289.08 (6)
O2vii—Ca2—O3iii81.98 (5)Cl1iv—Cl1—Ca1x117.81 (3)
O2viii—Ca2—O3iii145.15 (4)Cl1iv—Cl1—Ca1117.81 (3)
O4ix—Ca2—O3iii55.70 (5)Ca1x—Cl1—Ca199.99 (4)
O4—Ca2—O3iii68.34 (5)Cl1iv—Cl1—Ca1xi117.81 (3)
O4vi—Ca2—O3iii125.01 (4)Ca1x—Cl1—Ca1xi99.99 (4)
O2iii—Ca2—O3viii81.98 (5)Ca1—Cl1—Ca1xi99.99 (4)
O2vii—Ca2—O3viii145.15 (4)Cl1iv—Cl1—Ca1iv50.25 (3)
O2viii—Ca2—O3viii70.92 (5)Ca1x—Cl1—Ca1iv87.612 (11)
O4ix—Ca2—O3viii125.01 (4)Ca1—Cl1—Ca1iv168.07 (6)
O4—Ca2—O3viii55.70 (5)Ca1xi—Cl1—Ca1iv87.612 (11)
O4vi—Ca2—O3viii68.34 (5)Cl1iv—Cl1—Ca1xiv50.25 (2)
O3iii—Ca2—O3viii117.154 (17)Ca1x—Cl1—Ca1xiv87.612 (11)
O2iii—Ca2—O3vii145.15 (4)Ca1—Cl1—Ca1xiv87.612 (11)
O2vii—Ca2—O3vii70.92 (5)Ca1xi—Cl1—Ca1xiv168.07 (6)
O2viii—Ca2—O3vii81.98 (5)Ca1iv—Cl1—Ca1xiv83.50 (4)
O4ix—Ca2—O3vii68.34 (5)Cl1iv—Cl1—Ca1xv50.25 (3)
O4—Ca2—O3vii125.01 (4)Ca1x—Cl1—Ca1xv168.07 (6)
O4vi—Ca2—O3vii55.70 (5)Ca1—Cl1—Ca1xv87.612 (11)
O3iii—Ca2—O3vii117.154 (17)Ca1xi—Cl1—Ca1xv87.612 (11)
O3viii—Ca2—O3vii117.154 (16)Ca1iv—Cl1—Ca1xv83.50 (4)
O2iii—Ca2—P199.35 (4)Ca1xiv—Cl1—Ca1xv83.50 (4)
O4—Ca1—P1—O3iii94.90 (7)Cl1i—Ca1—O2—Ca2viii107.60 (5)
O3—Ca1—P1—O3iii15.70 (6)Cl1iv—Ca1—O2—Ca2viii176.09 (4)
O3i—Ca1—P1—O3iii174.09 (10)Cl1v—Ca1—O2—Ca2viii95.59 (4)
O3ii—Ca1—P1—O3iii170.21 (14)P1vi—Ca1—O2—Ca2viii44.16 (3)
Cl1—Ca1—P1—O3iii113.04 (8)O4—Ca1—O2—Ca2xii44.16 (3)
Cl1i—Ca1—P1—O3iii57.16 (7)O3—Ca1—O2—Ca2xii125.20 (6)
Cl1iv—Ca1—P1—O3iii125.00 (7)O3i—Ca1—O2—Ca2xii36.88 (4)
Cl1v—Ca1—P1—O3iii45.21 (7)O3ii—Ca1—O2—Ca2xii41.94 (11)
P1vi—Ca1—P1—O3iii94.90 (7)O3iii—Ca1—O2—Ca2xii130.26 (8)
O4—Ca1—P1—O3ii94.90 (7)Cl1—Ca1—O2—Ca2xii107.60 (5)
O3—Ca1—P1—O3ii174.09 (10)Cl1i—Ca1—O2—Ca2xii164.08 (5)
O3i—Ca1—P1—O3ii15.70 (6)Cl1iv—Ca1—O2—Ca2xii95.59 (4)
O3iii—Ca1—P1—O3ii170.21 (14)Cl1v—Ca1—O2—Ca2xii176.09 (4)
Cl1—Ca1—P1—O3ii57.16 (7)P1vi—Ca1—O2—Ca2xii44.16 (3)
Cl1i—Ca1—P1—O3ii113.04 (8)O4—Ca1—O3—P1xiii32.03 (14)
Cl1iv—Ca1—P1—O3ii45.21 (7)O3i—Ca1—O3—P1xiii115.69 (12)
Cl1v—Ca1—P1—O3ii125.00 (7)O3ii—Ca1—O3—P1xiii31.2 (2)
P1vi—Ca1—P1—O3ii94.90 (7)O3iii—Ca1—O3—P1xiii43.33 (16)
O4—Ca1—P1—O2x180Cl1—Ca1—O3—P1xiii135.36 (11)
O3—Ca1—P1—O2x100.81 (4)Cl1i—Ca1—O3—P1xiii114.51 (14)
O3i—Ca1—P1—O2x100.81 (4)O2—Ca1—O3—P1xiii139.16 (15)
O3ii—Ca1—P1—O2x85.10 (7)P1—Ca1—O3—P1xiii35.66 (14)
O3iii—Ca1—P1—O2x85.10 (7)Cl1iv—Ca1—O3—P1xiii142.88 (10)
Cl1—Ca1—P1—O2x27.94 (3)Cl1v—Ca1—O3—P1xiii110.05 (14)
Cl1i—Ca1—P1—O2x27.94 (3)P1vi—Ca1—O3—P1xiii53.15 (13)
Cl1iv—Ca1—P1—O2x39.90 (3)O4—Ca1—O3—Ca1xiii179.41 (7)
Cl1v—Ca1—P1—O2x39.90 (3)O3i—Ca1—O3—Ca1xiii96.93 (10)
P1vi—Ca1—P1—O2x180O3ii—Ca1—O3—Ca1xiii116.15 (4)
O4—Ca1—P1—O4ix0O3iii—Ca1—O3—Ca1xiii104.04 (4)
O3—Ca1—P1—O4ix79.19 (4)Cl1—Ca1—O3—Ca1xiii12.02 (9)
O3i—Ca1—P1—O4ix79.19 (4)Cl1i—Ca1—O3—Ca1xiii32.87 (5)
O3ii—Ca1—P1—O4ix94.90 (7)O2—Ca1—O3—Ca1xiii73.47 (6)
O3iii—Ca1—P1—O4ix94.90 (7)P1—Ca1—O3—Ca1xiii111.71 (5)
Cl1—Ca1—P1—O4ix152.06 (3)Cl1iv—Ca1—O3—Ca1xiii4.50 (10)
Cl1i—Ca1—P1—O4ix152.06 (3)Cl1v—Ca1—O3—Ca1xiii37.32 (5)
Cl1iv—Ca1—P1—O4ix140.10 (3)P1vi—Ca1—O3—Ca1xiii159.48 (6)
Cl1v—Ca1—P1—O4ix140.10 (3)O4—Ca1—O3—Ca2viii75.34 (5)
P1vi—Ca1—P1—O4ix0O3i—Ca1—O3—Ca2viii8.32 (11)
O3—Ca1—P1—Ca246.21 (4)O3ii—Ca1—O3—Ca2viii138.60 (8)
O3i—Ca1—P1—Ca2112.18 (4)O3iii—Ca1—O3—Ca2viii150.70 (4)
O3ii—Ca1—P1—Ca2127.88 (7)Cl1—Ca1—O3—Ca2viii117.27 (4)
O3iii—Ca1—P1—Ca261.91 (7)Cl1i—Ca1—O3—Ca2viii138.12 (4)
Cl1—Ca1—P1—Ca2174.95 (3)O2—Ca1—O3—Ca2viii31.79 (4)
Cl1i—Ca1—P1—Ca2119.07 (3)P1—Ca1—O3—Ca2viii143.04 (3)
Cl1iv—Ca1—P1—Ca2173.09 (3)Cl1iv—Ca1—O3—Ca2viii109.75 (6)
Cl1v—Ca1—P1—Ca2107.12 (3)Cl1v—Ca1—O3—Ca2viii142.58 (4)
O3—Ca1—P1—Ca2i112.18 (4)P1vi—Ca1—O3—Ca2viii54.22 (3)
O3i—Ca1—P1—Ca2i46.21 (4)O3—Ca1—O4—P1vi67.12 (4)
O3ii—Ca1—P1—Ca2i61.91 (7)O3i—Ca1—O4—P1vi67.12 (4)
O3iii—Ca1—P1—Ca2i127.88 (7)O3ii—Ca1—O4—P1vi149.77 (3)
Cl1—Ca1—P1—Ca2i119.07 (3)O3iii—Ca1—O4—P1vi149.77 (3)
Cl1i—Ca1—P1—Ca2i174.95 (3)Cl1—Ca1—O4—P1vi129.42 (6)
Cl1iv—Ca1—P1—Ca2i107.12 (3)Cl1i—Ca1—O4—P1vi129.42 (6)
Cl1v—Ca1—P1—Ca2i173.09 (3)O2—Ca1—O4—P1vi0
O4—Ca1—P1—Ca1ix0P1—Ca1—O4—P1vi180
O3—Ca1—P1—Ca1ix79.19 (4)Cl1iv—Ca1—O4—P1vi117.54 (5)
O3i—Ca1—P1—Ca1ix79.19 (4)Cl1v—Ca1—O4—P1vi117.54 (5)
O3ii—Ca1—P1—Ca1ix94.90 (7)O3—Ca1—O4—Ca2i163.34 (6)
O3iii—Ca1—P1—Ca1ix94.90 (7)O3i—Ca1—O4—Ca2i62.41 (6)
Cl1—Ca1—P1—Ca1ix152.06 (3)O3ii—Ca1—O4—Ca2i20.24 (5)
Cl1i—Ca1—P1—Ca1ix152.06 (3)O3iii—Ca1—O4—Ca2i80.69 (6)
Cl1iv—Ca1—P1—Ca1ix140.10 (3)Cl1—Ca1—O4—Ca2i0.12 (10)
Cl1v—Ca1—P1—Ca1ix140.10 (3)Cl1i—Ca1—O4—Ca2i101.04 (5)
P1vi—Ca1—P1—Ca1ix0O2—Ca1—O4—Ca2i129.54 (5)
O4—Ca1—P1—Ca1x180P1—Ca1—O4—Ca2i50.46 (5)
O3—Ca1—P1—Ca1x100.81 (4)Cl1iv—Ca1—O4—Ca2i11.99 (9)
O3i—Ca1—P1—Ca1x100.81 (4)Cl1v—Ca1—O4—Ca2i112.92 (3)
O3ii—Ca1—P1—Ca1x85.10 (7)P1vi—Ca1—O4—Ca2i129.54 (5)
O3iii—Ca1—P1—Ca1x85.10 (7)O3—Ca1—O4—Ca262.41 (6)
Cl1—Ca1—P1—Ca1x27.94 (3)O3i—Ca1—O4—Ca2163.34 (6)
Cl1i—Ca1—P1—Ca1x27.94 (3)O3ii—Ca1—O4—Ca280.69 (6)
Cl1iv—Ca1—P1—Ca1x39.90 (3)O3iii—Ca1—O4—Ca220.24 (5)
Cl1v—Ca1—P1—Ca1x39.90 (3)Cl1—Ca1—O4—Ca2101.04 (5)
P1vi—Ca1—P1—Ca1x180Cl1i—Ca1—O4—Ca20.12 (10)
O2iii—Ca2—P1—O3iii1.17 (7)O2—Ca1—O4—Ca2129.54 (5)
O2vii—Ca2—P1—O3iii75.74 (7)P1—Ca1—O4—Ca250.46 (5)
O2viii—Ca2—P1—O3iii73.98 (18)Cl1iv—Ca1—O4—Ca2112.92 (3)
O4ix—Ca2—P1—O3iii168.09 (9)Cl1v—Ca1—O4—Ca211.99 (9)
O4—Ca2—P1—O3iii86.91 (7)P1vi—Ca1—O4—Ca2129.54 (5)
O4vi—Ca2—P1—O3iii157.62 (7)O2iii—Ca2—O4—P1vi87.25 (7)
O3viii—Ca2—P1—O3iii87.58 (3)O2vii—Ca2—O4—P1vi150.69 (8)
O3vii—Ca2—P1—O3iii146.50 (7)O2viii—Ca2—O4—P1vi13.21 (9)
P1vi—Ca2—P1—O3iii90.39 (6)O4ix—Ca2—O4—P1vi145.06 (7)
P1ix—Ca2—P1—O3iii175.01 (6)O4vi—Ca2—O4—P1vi66.14 (9)
O2iii—Ca2—P1—O3ii97.54 (7)O3iii—Ca2—O4—P1vi156.74 (7)
O2vii—Ca2—P1—O3ii174.45 (8)O3viii—Ca2—O4—P1vi6.83 (5)
O2viii—Ca2—P1—O3ii172.69 (18)O3vii—Ca2—O4—P1vi94.51 (6)
O4ix—Ca2—P1—O3ii93.20 (9)P1—Ca2—O4—P1vi172.49 (7)
O4—Ca2—P1—O3ii11.80 (7)P1ix—Ca2—O4—P1vi81.73 (5)
O4vi—Ca2—P1—O3ii58.91 (7)O2iii—Ca2—O4—Ca150.41 (7)
O3iii—Ca2—P1—O3ii98.71 (11)O2vii—Ca2—O4—Ca113.03 (12)
O3viii—Ca2—P1—O3ii11.13 (9)O2viii—Ca2—O4—Ca1124.46 (7)
O3vii—Ca2—P1—O3ii114.79 (7)O4ix—Ca2—O4—Ca177.28 (9)
P1vi—Ca2—P1—O3ii8.32 (6)O4vi—Ca2—O4—Ca1156.20 (7)
P1ix—Ca2—P1—O3ii86.28 (6)O3iii—Ca2—O4—Ca119.08 (5)
O2iii—Ca2—P1—O2x93.43 (10)O3viii—Ca2—O4—Ca1130.83 (7)
O2vii—Ca2—P1—O2x16.52 (12)O3vii—Ca2—O4—Ca1127.83 (5)
O2viii—Ca2—P1—O2x18.29 (14)P1—Ca2—O4—Ca149.85 (5)
O4ix—Ca2—P1—O2x75.83 (10)P1vi—Ca2—O4—Ca1137.66 (9)
O4—Ca2—P1—O2x179.18 (9)P1ix—Ca2—O4—Ca1140.61 (5)
O4vi—Ca2—P1—O2x110.11 (9)O2iii—Ca2—O4—Ca2i167.15 (6)
O3iii—Ca2—P1—O2x92.26 (10)O2vii—Ca2—O4—Ca2i103.70 (9)
O3viii—Ca2—P1—O2x179.84 (9)O2viii—Ca2—O4—Ca2i118.81 (5)
O3vii—Ca2—P1—O2x54.24 (9)O4ix—Ca2—O4—Ca2i39.460 (15)
P1vi—Ca2—P1—O2x177.34 (8)O4vi—Ca2—O4—Ca2i39.460 (15)
P1ix—Ca2—P1—O2x82.75 (9)O3iii—Ca2—O4—Ca2i97.66 (5)
O2iii—Ca2—P1—O4ix169.26 (7)O3viii—Ca2—O4—Ca2i112.43 (6)
O2vii—Ca2—P1—O4ix92.35 (8)O3vii—Ca2—O4—Ca2i11.09 (7)
O2viii—Ca2—P1—O4ix94.11 (17)P1—Ca2—O4—Ca2i66.89 (3)
O4—Ca2—P1—O4ix105.00 (9)P1vi—Ca2—O4—Ca2i105.60 (8)
O4vi—Ca2—P1—O4ix34.29 (8)P1ix—Ca2—O4—Ca2i23.88 (5)
O3iii—Ca2—P1—O4ix168.09 (9)O4—Ca1—Cl1—Cl1iv45.89 (7)
O3viii—Ca2—P1—O4ix104.33 (7)O3—Ca1—Cl1—Cl1iv155.27 (5)
O3vii—Ca2—P1—O4ix21.59 (7)O3i—Ca1—Cl1—Cl1iv19.86 (4)
P1vi—Ca2—P1—O4ix101.52 (6)O3ii—Ca1—Cl1—Cl1iv66.86 (3)
P1ix—Ca2—P1—O4ix6.92 (6)O3iii—Ca1—Cl1—Cl1iv119.65 (3)
O2iii—Ca2—P1—Ca154.13 (4)Cl1i—Ca1—Cl1—Cl1iv180.0000 (10)
O2vii—Ca2—P1—Ca1131.04 (4)O2—Ca1—Cl1—Cl1iv84.909 (18)
O2viii—Ca2—P1—Ca1129.27 (17)P1—Ca1—Cl1—Cl1iv92.760 (8)
O4ix—Ca2—P1—Ca1136.62 (6)Cl1v—Ca1—Cl1—Cl1iv180.000 (2)
O4—Ca2—P1—Ca131.62 (3)P1vi—Ca1—Cl1—Cl1iv6.71 (5)
O4vi—Ca2—P1—Ca1102.33 (4)O4—Ca1—Cl1—Ca1x83.06 (9)
O3iii—Ca2—P1—Ca155.29 (6)O3—Ca1—Cl1—Ca1x75.78 (5)
O3viii—Ca2—P1—Ca132.28 (3)O3i—Ca1—Cl1—Ca1x148.81 (5)
O3vii—Ca2—P1—Ca1158.20 (3)O3ii—Ca1—Cl1—Ca1x62.09 (4)
P1vi—Ca2—P1—Ca135.097 (12)O3iii—Ca1—Cl1—Ca1x9.30 (4)
P1ix—Ca2—P1—Ca1129.693 (11)Cl1i—Ca1—Cl1—Ca1x51.06 (3)
O2iii—Ca2—P1—Ca2i136.52 (4)O2—Ca1—Cl1—Ca1x146.15 (3)
O2vii—Ca2—P1—Ca2i146.57 (4)P1—Ca1—Cl1—Ca1x36.18 (3)
O2viii—Ca2—P1—Ca2i148.33 (17)Cl1iv—Ca1—Cl1—Ca1x128.94 (3)
O4ix—Ca2—P1—Ca2i54.22 (6)Cl1v—Ca1—Cl1—Ca1x51.06 (3)
O4—Ca2—P1—Ca2i50.78 (3)P1vi—Ca1—Cl1—Ca1x122.24 (6)
O4vi—Ca2—P1—Ca2i19.93 (4)O4—Ca1—Cl1—Ca1xi174.83 (6)
O3iii—Ca2—P1—Ca2i137.69 (6)O3—Ca1—Cl1—Ca1xi26.33 (6)
O3viii—Ca2—P1—Ca2i50.11 (3)O3i—Ca1—Cl1—Ca1xi109.08 (4)
O3vii—Ca2—P1—Ca2i75.81 (3)O3ii—Ca1—Cl1—Ca1xi164.20 (5)
P1vi—Ca2—P1—Ca2i47.298 (8)O3iii—Ca1—Cl1—Ca1xi111.41 (4)
P1ix—Ca2—P1—Ca2i47.298 (8)Cl1i—Ca1—Cl1—Ca1xi51.06 (3)
O2iii—Ca2—P1—Ca1ix143.69 (4)O2—Ca1—Cl1—Ca1xi44.04 (4)
O2vii—Ca2—P1—Ca1ix66.78 (4)P1—Ca1—Cl1—Ca1xi138.29 (3)
O2viii—Ca2—P1—Ca1ix68.55 (17)Cl1iv—Ca1—Cl1—Ca1xi128.94 (3)
O4ix—Ca2—P1—Ca1ix25.56 (6)Cl1v—Ca1—Cl1—Ca1xi51.06 (3)
O4—Ca2—P1—Ca1ix130.56 (3)P1vi—Ca1—Cl1—Ca1xi135.65 (5)
O4vi—Ca2—P1—Ca1ix59.85 (4)O4—Ca1—Cl1—Ca1iv45.89 (7)
O3iii—Ca2—P1—Ca1ix142.53 (6)O3—Ca1—Cl1—Ca1iv155.27 (5)
O3viii—Ca2—P1—Ca1ix129.90 (3)O3i—Ca1—Cl1—Ca1iv19.86 (4)
O3vii—Ca2—P1—Ca1ix3.98 (3)O3ii—Ca1—Cl1—Ca1iv66.86 (3)
P1vi—Ca2—P1—Ca1ix127.080 (12)O3iii—Ca1—Cl1—Ca1iv119.65 (3)
P1ix—Ca2—P1—Ca1ix32.485 (11)Cl1i—Ca1—Cl1—Ca1iv180.0000 (10)
O2iii—Ca2—P1—Ca1x4.05 (5)O2—Ca1—Cl1—Ca1iv84.909 (18)
O2vii—Ca2—P1—Ca1x72.86 (5)P1—Ca1—Cl1—Ca1iv92.760 (8)
O2viii—Ca2—P1—Ca1x71.09 (17)Cl1iv—Ca1—Cl1—Ca1iv0
O4ix—Ca2—P1—Ca1x165.21 (7)Cl1v—Ca1—Cl1—Ca1iv180.0000 (10)
O4—Ca2—P1—Ca1x89.80 (4)P1vi—Ca1—Cl1—Ca1iv6.71 (5)
O4vi—Ca2—P1—Ca1x160.51 (5)O4—Ca1—Cl1—Ca1xiv4.09 (8)
O3iii—Ca2—P1—Ca1x2.88 (6)O3—Ca1—Cl1—Ca1xiv162.93 (5)
O3viii—Ca2—P1—Ca1x90.46 (4)O3i—Ca1—Cl1—Ca1xiv61.66 (4)
O3vii—Ca2—P1—Ca1x143.62 (4)O3ii—Ca1—Cl1—Ca1xiv25.06 (3)
P1vi—Ca2—P1—Ca1x93.28 (4)O3iii—Ca1—Cl1—Ca1xiv77.85 (4)
P1ix—Ca2—P1—Ca1x172.13 (3)Cl1i—Ca1—Cl1—Ca1xiv138.207 (19)
O4—Ca1—O2—P1xi180O2—Ca1—Cl1—Ca1xiv126.70 (2)
O3—Ca1—O2—P1xi98.96 (4)P1—Ca1—Cl1—Ca1xiv50.967 (17)
O3i—Ca1—O2—P1xi98.96 (4)Cl1iv—Ca1—Cl1—Ca1xiv41.79 (2)
O3ii—Ca1—O2—P1xi93.90 (9)Cl1v—Ca1—Cl1—Ca1xiv138.207 (19)
O3iii—Ca1—O2—P1xi93.90 (9)P1vi—Ca1—Cl1—Ca1xiv35.09 (5)
Cl1—Ca1—O2—P1xi28.24 (3)O4—Ca1—Cl1—Ca1xv87.68 (6)
Cl1i—Ca1—O2—P1xi28.24 (3)O3—Ca1—Cl1—Ca1xv113.48 (5)
Cl1iv—Ca1—O2—P1xi40.25 (3)O3i—Ca1—Cl1—Ca1xv21.93 (4)
Cl1v—Ca1—O2—P1xi40.25 (3)O3ii—Ca1—Cl1—Ca1xv108.65 (4)
P1vi—Ca1—O2—P1xi180O3iii—Ca1—Cl1—Ca1xv161.44 (3)
O4—Ca1—O2—Ca2viii44.16 (3)Cl1i—Ca1—Cl1—Ca1xv138.207 (19)
O3—Ca1—O2—Ca2viii36.88 (4)O2—Ca1—Cl1—Ca1xv43.12 (3)
O3i—Ca1—O2—Ca2viii125.20 (6)P1—Ca1—Cl1—Ca1xv134.55 (2)
O3ii—Ca1—O2—Ca2viii130.26 (8)Cl1iv—Ca1—Cl1—Ca1xv41.79 (2)
O3iii—Ca1—O2—Ca2viii41.94 (11)Cl1v—Ca1—Cl1—Ca1xv138.207 (19)
Cl1—Ca1—O2—Ca2viii164.08 (5)P1vi—Ca1—Cl1—Ca1xv48.50 (5)
Symmetry codes: (i) x, y, z+1/2; (ii) xy+1, x+1, z+1/2; (iii) xy+1, x+1, z; (iv) x, y+2, z+1; (v) x, y+2, z1/2; (vi) y+1, xy+1, z; (vii) y, x+y, z; (viii) x, y+1, z; (ix) x+y, x+1, z; (x) y+1, xy+2, z; (xi) x+y1, x+1, z; (xii) x, y+1, z+1/2; (xiii) y1, x+y, z; (xiv) xy+1, x+1, z+1; (xv) y1, x+y, z+1.
(c_room_prism) chlorapatite top
Crystal data top
3(O4P)·Cl·5(Ca)Dx = 3.176 Mg m3
Mr = 520.76Mo Kα radiation, λ = 0.7107 Å
Trigonal, P63/mCell parameters from 1653 reflections
Hall symbol: -P 6cθ = 11.5–51.6°
a = 9.6430 (2) ŵ = 3.21 mm1
c = 6.7620 (1) ÅT = 293 K
V = 544.54 (2) Å3Prism, colourless
Z = 20.25 × 0.12 × 0.05 mm
F(000) = 516
Data collection top
BRUKER APPEX-II CCD
diffractometer
403 independent reflections
Radiation source: fine-focus sealed tube398 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.015
ω and phi scansθmax = 26.4°, θmin = 2.4°
Absorption correction: multi-scan
BRUKER SADABS
h = 120
Tmin = 0.852, Tmax = 1k = 012
6423 measured reflectionsl = 08
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.017 w = 1/[σ2(Fo2) + (0.0183P)2 + 0.6752P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.045(Δ/σ)max < 0.001
S = 1.18Δρmax = 0.34 e Å3
403 reflectionsΔρmin = 0.35 e Å3
41 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.042 (3)
Crystal data top
3(O4P)·Cl·5(Ca)Z = 2
Mr = 520.76Mo Kα radiation
Trigonal, P63/mµ = 3.21 mm1
a = 9.6430 (2) ÅT = 293 K
c = 6.7620 (1) Å0.25 × 0.12 × 0.05 mm
V = 544.54 (2) Å3
Data collection top
BRUKER APPEX-II CCD
diffractometer
403 independent reflections
Absorption correction: multi-scan
BRUKER SADABS
398 reflections with I > 2σ(I)
Tmin = 0.852, Tmax = 1Rint = 0.015
6423 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.01741 parameters
wR(F2) = 0.0450 restraints
S = 1.18Δρmax = 0.34 e Å3
403 reflectionsΔρmin = 0.35 e Å3
Special details top

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ca10.00438 (6)0.74425 (6)0.250.0104 (2)
Ca20.33330.66670.00344 (9)0.0106 (2)
P10.37490 (8)0.96744 (7)0.250.0069 (2)
O20.3437 (2)0.5079 (2)0.250.0138 (4)
O30.08666 (16)0.64657 (18)0.0673 (2)0.0183 (4)
O40.1272 (2)0.5923 (2)0.250.0136 (4)
Cl1010.4437 (3)0.0267 (6)0.5
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0123 (3)0.0123 (3)0.0080 (3)0.0073 (2)00
Ca20.0128 (3)0.0128 (3)0.0061 (3)0.00640 (13)00
P10.0065 (3)0.0063 (3)0.0071 (3)0.0027 (3)00
O20.0201 (10)0.0155 (10)0.0122 (10)0.0137 (8)00
O30.0147 (6)0.0286 (8)0.0153 (8)0.0137 (6)0.0042 (6)0.0120 (6)
O40.0115 (9)0.0081 (9)0.0212 (11)0.0049 (7)00
Cl10.0154 (4)0.0154 (4)0.0491 (18)0.0077 (2)00
Geometric parameters (Å, º) top
Ca1—O42.2995 (19)Ca2—P1vi3.2167 (6)
Ca1—O32.3309 (14)Ca2—P1ix3.2167 (6)
Ca1—O3i2.3309 (14)P1—O3iii1.5305 (14)
Ca1—O3ii2.5420 (15)P1—O3ii1.5305 (14)
Ca1—O3iii2.5420 (15)P1—O2x1.5322 (19)
Ca1—Cl12.8113 (11)P1—O4ix1.5436 (19)
Ca1—Cl1i2.8113 (11)P1—Ca2i3.2167 (6)
Ca1—O22.969 (2)P1—Ca1ix3.3917 (8)
Ca1—P13.1158 (8)O2—P1xi1.5322 (19)
Ca1—Cl1iv3.2370 (13)O2—Ca2viii2.4071 (14)
Ca1—Cl1v3.2370 (13)O2—Ca2xii2.4071 (14)
Ca1—P1vi3.3917 (8)O3—P1xiii1.5305 (14)
Ca2—O2iii2.4071 (14)O3—Ca1xiii2.5420 (15)
Ca2—O2vii2.4071 (14)O3—Ca2viii2.7974 (15)
Ca2—O2viii2.4071 (14)O4—P1vi1.5436 (19)
Ca2—O4ix2.4445 (14)O4—Ca2i2.4445 (14)
Ca2—O42.4445 (14)Cl1—Cl1iv0.762 (4)
Ca2—O4vi2.4445 (14)Cl1—Ca1x2.8113 (11)
Ca2—O3iii2.7974 (15)Cl1—Ca1xi2.8113 (11)
Ca2—O3viii2.7974 (15)Cl1—Ca1iv3.2370 (13)
Ca2—O3vii2.7974 (15)Cl1—Ca1xiv3.2370 (13)
Ca2—P13.2167 (6)Cl1—Ca1xv3.2370 (13)
O4—Ca1—O387.27 (4)O2vii—Ca2—P188.57 (4)
O4—Ca1—O3i87.27 (4)O2viii—Ca2—P1165.87 (4)
O3—Ca1—O3i133.95 (8)O4ix—Ca2—P127.57 (4)
O4—Ca1—O3ii75.17 (5)O4—Ca2—P166.90 (4)
O3—Ca1—O3ii139.43 (6)O4vi—Ca2—P199.11 (4)
O3i—Ca1—O3ii82.23 (3)O3iii—Ca2—P128.40 (3)
O4—Ca1—O3iii75.17 (5)O3viii—Ca2—P1122.54 (3)
O3—Ca1—O3iii82.23 (3)O3vii—Ca2—P193.93 (3)
O3i—Ca1—O3iii139.43 (6)O2iii—Ca2—P1vi88.57 (4)
O3ii—Ca1—O3iii58.17 (6)O2vii—Ca2—P1vi165.87 (4)
O4—Ca1—Cl1142.90 (4)O2viii—Ca2—P1vi99.34 (4)
O3—Ca1—Cl1127.98 (5)O4ix—Ca2—P1vi99.11 (4)
O3i—Ca1—Cl175.99 (5)O4—Ca2—P1vi27.57 (4)
O3ii—Ca1—Cl169.97 (4)O4vi—Ca2—P1vi66.90 (4)
O3iii—Ca1—Cl196.34 (4)O3iii—Ca2—P1vi93.93 (3)
O4—Ca1—Cl1i142.90 (4)O3viii—Ca2—P1vi28.40 (3)
O3—Ca1—Cl1i75.99 (5)O3vii—Ca2—P1vi122.54 (3)
O3i—Ca1—Cl1i127.98 (5)P1—Ca2—P1vi94.258 (15)
O3ii—Ca1—Cl1i96.34 (4)O2iii—Ca2—P1ix165.87 (4)
O3iii—Ca1—Cl1i69.97 (4)O2vii—Ca2—P1ix99.34 (4)
Cl1—Ca1—Cl1i55.53 (7)O2viii—Ca2—P1ix88.57 (4)
O4—Ca1—O2104.84 (6)O4ix—Ca2—P1ix66.90 (4)
O3—Ca1—O268.71 (4)O4—Ca2—P1ix99.11 (4)
O3i—Ca1—O268.71 (4)O4vi—Ca2—P1ix27.57 (4)
O3ii—Ca1—O2150.84 (3)O3iii—Ca2—P1ix122.54 (3)
O3iii—Ca1—O2150.84 (3)O3viii—Ca2—P1ix93.93 (3)
Cl1—Ca1—O299.56 (3)O3vii—Ca2—P1ix28.40 (3)
Cl1i—Ca1—O299.56 (3)P1—Ca2—P1ix94.258 (15)
O4—Ca1—P170.24 (5)P1vi—Ca2—P1ix94.258 (15)
O3—Ca1—P1110.44 (4)O3iii—P1—O3ii107.68 (12)
O3i—Ca1—P1110.44 (4)O3iii—P1—O2x112.14 (7)
O3ii—Ca1—P129.20 (3)O3ii—P1—O2x112.14 (7)
O3iii—Ca1—P129.20 (3)O3iii—P1—O4ix106.71 (7)
Cl1—Ca1—P184.781 (16)O3ii—P1—O4ix106.71 (7)
Cl1i—Ca1—P184.781 (16)O2x—P1—O4ix111.13 (11)
O2—Ca1—P1175.08 (4)O3iii—P1—Ca154.13 (6)
O4—Ca1—Cl1iv133.84 (3)O3ii—P1—Ca154.13 (6)
O3—Ca1—Cl1iv138.68 (5)O2x—P1—Ca1136.43 (8)
O3i—Ca1—Cl1iv64.74 (5)O4ix—P1—Ca1112.44 (7)
O3ii—Ca1—Cl1iv65.68 (3)O3iii—P1—Ca260.39 (6)
O3iii—Ca1—Cl1iv102.14 (4)O3ii—P1—Ca2111.49 (6)
Cl1—Ca1—Cl1iv12.02 (6)O2x—P1—Ca2135.63 (5)
Cl1i—Ca1—Cl1iv67.549 (14)O4ix—P1—Ca247.14 (5)
O2—Ca1—Cl1iv98.30 (3)Ca1—P1—Ca278.129 (15)
P1—Ca1—Cl1iv85.469 (14)O3iii—P1—Ca2i111.49 (6)
O4—Ca1—Cl1v133.84 (3)O3ii—P1—Ca2i60.39 (6)
O3—Ca1—Cl1v64.74 (5)O2x—P1—Ca2i135.63 (5)
O3i—Ca1—Cl1v138.68 (5)O4ix—P1—Ca2i47.14 (5)
O3ii—Ca1—Cl1v102.14 (4)Ca1—P1—Ca2i78.129 (15)
O3iii—Ca1—Cl1v65.68 (3)Ca2—P1—Ca2i64.38 (2)
Cl1—Ca1—Cl1v67.549 (14)O3iii—P1—Ca1ix122.01 (6)
Cl1i—Ca1—Cl1v12.02 (6)O3ii—P1—Ca1ix122.01 (6)
O2—Ca1—Cl1v98.30 (3)O2x—P1—Ca1ix76.34 (8)
P1—Ca1—Cl1v85.469 (14)Ca1—P1—Ca1ix147.24 (2)
Cl1iv—Ca1—Cl1v79.56 (6)Ca2—P1—Ca1ix74.260 (14)
O4—Ca1—P1vi22.52 (5)Ca2i—P1—Ca1ix74.260 (14)
O3—Ca1—P1vi78.89 (4)O3iii—P1—Ca1x80.47 (6)
O3i—Ca1—P1vi78.89 (4)O3ii—P1—Ca1x80.47 (6)
O3ii—Ca1—P1vi94.80 (4)O2x—P1—Ca1x56.01 (8)
O3iii—Ca1—P1vi94.80 (4)O4ix—P1—Ca1x167.14 (8)
Cl1—Ca1—P1vi152.07 (4)Ca1—P1—Ca1x80.42 (2)
Cl1i—Ca1—P1vi152.07 (4)Ca2—P1—Ca1x140.821 (15)
O2—Ca1—P1vi82.31 (4)Ca2i—P1—Ca1x140.821 (15)
P1—Ca1—P1vi92.76 (2)Ca1ix—P1—Ca1x132.35 (2)
Cl1iv—Ca1—P1vi140.11 (3)P1xi—O2—Ca2viii133.48 (5)
Cl1v—Ca1—P1vi140.11 (3)P1xi—O2—Ca2xii133.48 (5)
O2iii—Ca2—O2vii77.31 (5)Ca2viii—O2—Ca2xii87.68 (6)
O2iii—Ca2—O2viii77.31 (5)P1xi—O2—Ca198.65 (9)
O2vii—Ca2—O2viii77.31 (5)Ca2viii—O2—Ca196.33 (6)
O2iii—Ca2—O4ix126.33 (6)Ca2xii—O2—Ca196.33 (6)
O2vii—Ca2—O4ix89.80 (4)P1xiii—O3—Ca1139.20 (8)
O2viii—Ca2—O4ix150.21 (6)P1xiii—O3—Ca1xiii96.67 (7)
O2iii—Ca2—O489.80 (4)Ca1—O3—Ca1xiii118.88 (6)
O2vii—Ca2—O4150.21 (6)P1xiii—O3—Ca2viii91.20 (7)
O2viii—Ca2—O4126.33 (6)Ca1—O3—Ca2viii102.95 (6)
O4ix—Ca2—O476.28 (5)Ca1xiii—O3—Ca2viii96.64 (5)
O2iii—Ca2—O4vi150.21 (6)P1vi—O4—Ca1122.69 (10)
O2vii—Ca2—O4vi126.33 (6)P1vi—O4—Ca2i105.28 (7)
O2viii—Ca2—O4vi89.80 (4)Ca1—O4—Ca2i114.54 (6)
O4ix—Ca2—O4vi76.28 (5)P1vi—O4—Ca2105.28 (7)
O4—Ca2—O4vi76.28 (5)Ca1—O4—Ca2114.54 (6)
O2iii—Ca2—O3iii70.94 (5)Ca2i—O4—Ca289.02 (6)
O2vii—Ca2—O3iii82.01 (5)Cl1iv—Cl1—Ca1x117.77 (4)
O2viii—Ca2—O3iii145.16 (5)Cl1iv—Cl1—Ca1117.77 (4)
O4ix—Ca2—O3iii55.65 (5)Ca1x—Cl1—Ca1100.05 (5)
O4—Ca2—O3iii68.36 (5)Cl1iv—Cl1—Ca1xi117.77 (4)
O4vi—Ca2—O3iii125.01 (5)Ca1x—Cl1—Ca1xi100.05 (5)
O2iii—Ca2—O3viii82.01 (5)Ca1—Cl1—Ca1xi100.05 (5)
O2vii—Ca2—O3viii145.16 (5)Cl1iv—Cl1—Ca1iv50.22 (3)
O2viii—Ca2—O3viii70.94 (5)Ca1x—Cl1—Ca1iv87.599 (12)
O4ix—Ca2—O3viii125.01 (5)Ca1—Cl1—Ca1iv167.98 (6)
O4—Ca2—O3viii55.65 (5)Ca1xi—Cl1—Ca1iv87.599 (12)
O4vi—Ca2—O3viii68.36 (5)Cl1iv—Cl1—Ca1xiv50.22 (3)
O3iii—Ca2—O3viii117.142 (18)Ca1x—Cl1—Ca1xiv87.599 (12)
O2iii—Ca2—O3vii145.16 (5)Ca1—Cl1—Ca1xiv87.599 (12)
O2vii—Ca2—O3vii70.94 (5)Ca1xi—Cl1—Ca1xiv167.98 (6)
O2viii—Ca2—O3vii82.01 (5)Ca1iv—Cl1—Ca1xiv83.45 (4)
O4ix—Ca2—O3vii68.36 (5)Cl1iv—Cl1—Ca1xv50.22 (3)
O4—Ca2—O3vii125.01 (5)Ca1x—Cl1—Ca1xv167.98 (6)
O4vi—Ca2—O3vii55.65 (5)Ca1—Cl1—Ca1xv87.599 (12)
O3iii—Ca2—O3vii117.142 (18)Ca1xi—Cl1—Ca1xv87.599 (12)
O3viii—Ca2—O3vii117.142 (18)Ca1iv—Cl1—Ca1xv83.45 (4)
O2iii—Ca2—P199.34 (4)Ca1xiv—Cl1—Ca1xv83.45 (4)
O4—Ca1—P1—O3iii94.89 (7)Cl1—Ca1—O2—Ca2viii164.01 (5)
O3—Ca1—P1—O3iii15.71 (6)Cl1i—Ca1—O2—Ca2viii107.63 (5)
O3i—Ca1—P1—O3iii174.06 (10)Cl1iv—Ca1—O2—Ca2viii176.11 (4)
O3ii—Ca1—P1—O3iii170.23 (14)Cl1v—Ca1—O2—Ca2viii95.53 (5)
Cl1—Ca1—P1—O3iii113.01 (8)O4—Ca1—O2—Ca2xii44.18 (3)
Cl1i—Ca1—P1—O3iii57.22 (8)O3—Ca1—O2—Ca2xii125.20 (6)
Cl1iv—Ca1—P1—O3iii125.05 (8)O3i—Ca1—O2—Ca2xii36.85 (4)
Cl1v—Ca1—P1—O3iii45.18 (8)O3ii—Ca1—O2—Ca2xii41.88 (12)
P1vi—Ca1—P1—O3iii94.89 (7)O3iii—Ca1—O2—Ca2xii130.24 (8)
O4—Ca1—P1—O3ii94.89 (7)Cl1—Ca1—O2—Ca2xii107.63 (5)
O3—Ca1—P1—O3ii174.06 (10)Cl1i—Ca1—O2—Ca2xii164.01 (5)
O3i—Ca1—P1—O3ii15.71 (6)Cl1iv—Ca1—O2—Ca2xii95.53 (5)
O3iii—Ca1—P1—O3ii170.23 (14)Cl1v—Ca1—O2—Ca2xii176.11 (4)
Cl1—Ca1—P1—O3ii57.22 (8)P1vi—Ca1—O2—Ca2xii44.18 (3)
Cl1i—Ca1—P1—O3ii113.01 (8)O4—Ca1—O3—P1xiii32.10 (15)
Cl1iv—Ca1—P1—O3ii45.18 (8)O3i—Ca1—O3—P1xiii115.67 (13)
Cl1v—Ca1—P1—O3ii125.05 (8)O3ii—Ca1—O3—P1xiii31.2 (2)
P1vi—Ca1—P1—O3ii94.89 (7)O3iii—Ca1—O3—P1xiii43.30 (17)
O4—Ca1—P1—O2x180Cl1—Ca1—O3—P1xiii135.30 (12)
O3—Ca1—P1—O2x100.82 (4)Cl1i—Ca1—O3—P1xiii114.50 (15)
O3i—Ca1—P1—O2x100.82 (4)O2—Ca1—O3—P1xiii139.18 (16)
O3ii—Ca1—P1—O2x85.11 (7)P1—Ca1—O3—P1xiii35.64 (15)
O3iii—Ca1—P1—O2x85.11 (7)Cl1iv—Ca1—O3—P1xiii142.87 (11)
Cl1—Ca1—P1—O2x27.89 (4)Cl1v—Ca1—O3—P1xiii110.02 (15)
Cl1i—Ca1—P1—O2x27.89 (4)P1vi—Ca1—O3—P1xiii53.18 (14)
Cl1iv—Ca1—P1—O2x39.93 (3)O4—Ca1—O3—Ca1xiii179.46 (8)
Cl1v—Ca1—P1—O2x39.93 (3)O3i—Ca1—O3—Ca1xiii96.97 (11)
P1vi—Ca1—P1—O2x180O3ii—Ca1—O3—Ca1xiii116.18 (5)
O4—Ca1—P1—O4ix0O3iii—Ca1—O3—Ca1xiii104.07 (4)
O3—Ca1—P1—O4ix79.18 (4)Cl1—Ca1—O3—Ca1xiii12.06 (10)
O3i—Ca1—P1—O4ix79.18 (4)Cl1i—Ca1—O3—Ca1xiii32.86 (6)
O3ii—Ca1—P1—O4ix94.89 (7)O2—Ca1—O3—Ca1xiii73.46 (7)
O3iii—Ca1—P1—O4ix94.89 (7)P1—Ca1—O3—Ca1xiii111.73 (6)
Cl1—Ca1—P1—O4ix152.11 (4)Cl1iv—Ca1—O3—Ca1xiii4.49 (11)
Cl1i—Ca1—P1—O4ix152.11 (4)Cl1v—Ca1—O3—Ca1xiii37.34 (5)
Cl1iv—Ca1—P1—O4ix140.07 (3)P1vi—Ca1—O3—Ca1xiii159.46 (7)
Cl1v—Ca1—P1—O4ix140.07 (3)O4—Ca1—O3—Ca2viii75.32 (5)
P1vi—Ca1—P1—O4ix0O3i—Ca1—O3—Ca2viii8.24 (12)
O4—Ca1—P1—Ca232.984 (11)O3ii—Ca1—O3—Ca2viii138.61 (9)
O3—Ca1—P1—Ca246.19 (4)O3iii—Ca1—O3—Ca2viii150.72 (5)
O3i—Ca1—P1—Ca2112.16 (4)Cl1—Ca1—O3—Ca2viii117.28 (5)
O3ii—Ca1—P1—Ca2127.87 (7)Cl1i—Ca1—O3—Ca2viii138.07 (4)
O3iii—Ca1—P1—Ca261.90 (7)O2—Ca1—O3—Ca2viii31.75 (5)
Cl1—Ca1—P1—Ca2174.91 (4)P1—Ca1—O3—Ca2viii143.06 (3)
Cl1i—Ca1—P1—Ca2119.12 (4)Cl1iv—Ca1—O3—Ca2viii109.71 (6)
Cl1iv—Ca1—P1—Ca2173.05 (3)Cl1v—Ca1—O3—Ca2viii142.55 (5)
Cl1v—Ca1—P1—Ca2107.08 (3)P1vi—Ca1—O3—Ca2viii54.25 (3)
P1vi—Ca1—P1—Ca232.984 (11)O3—Ca1—O4—P1vi67.13 (4)
O4—Ca1—P1—Ca2i32.984 (11)O3i—Ca1—O4—P1vi67.13 (4)
O3—Ca1—P1—Ca2i112.16 (4)O3ii—Ca1—O4—P1vi149.81 (3)
O3i—Ca1—P1—Ca2i46.19 (4)O3iii—Ca1—O4—P1vi149.81 (3)
O3ii—Ca1—P1—Ca2i61.90 (7)Cl1—Ca1—O4—P1vi129.43 (7)
O3iii—Ca1—P1—Ca2i127.87 (7)Cl1i—Ca1—O4—P1vi129.43 (7)
Cl1—Ca1—P1—Ca2i119.12 (4)O2—Ca1—O4—P1vi0
Cl1i—Ca1—P1—Ca2i174.91 (4)P1—Ca1—O4—P1vi180
Cl1iv—Ca1—P1—Ca2i107.08 (3)Cl1iv—Ca1—O4—P1vi117.48 (5)
Cl1v—Ca1—P1—Ca2i173.05 (3)Cl1v—Ca1—O4—P1vi117.47 (5)
P1vi—Ca1—P1—Ca2i32.984 (11)O3—Ca1—O4—Ca2i163.28 (7)
O4—Ca1—P1—Ca1ix0O3i—Ca1—O4—Ca2i62.46 (6)
O3—Ca1—P1—Ca1ix79.18 (4)O3ii—Ca1—O4—Ca2i20.22 (6)
O3i—Ca1—P1—Ca1ix79.18 (4)O3iii—Ca1—O4—Ca2i80.60 (7)
O3ii—Ca1—P1—Ca1ix94.89 (7)Cl1—Ca1—O4—Ca2i0.15 (11)
O3iii—Ca1—P1—Ca1ix94.89 (7)Cl1i—Ca1—O4—Ca2i100.98 (5)
Cl1—Ca1—P1—Ca1ix152.11 (4)O2—Ca1—O4—Ca2i129.59 (5)
Cl1i—Ca1—P1—Ca1ix152.11 (4)P1—Ca1—O4—Ca2i50.41 (5)
Cl1iv—Ca1—P1—Ca1ix140.07 (3)Cl1iv—Ca1—O4—Ca2i12.11 (10)
Cl1v—Ca1—P1—Ca1ix140.07 (3)Cl1v—Ca1—O4—Ca2i112.94 (3)
P1vi—Ca1—P1—Ca1ix0P1vi—Ca1—O4—Ca2i129.59 (5)
O4—Ca1—P1—Ca1x180O3—Ca1—O4—Ca262.46 (6)
O3—Ca1—P1—Ca1x100.82 (4)O3i—Ca1—O4—Ca2163.28 (7)
O3i—Ca1—P1—Ca1x100.82 (4)O3ii—Ca1—O4—Ca280.60 (7)
O3ii—Ca1—P1—Ca1x85.11 (7)O3iii—Ca1—O4—Ca220.22 (6)
O3iii—Ca1—P1—Ca1x85.11 (7)Cl1—Ca1—O4—Ca2100.98 (5)
Cl1—Ca1—P1—Ca1x27.89 (4)Cl1i—Ca1—O4—Ca20.15 (11)
Cl1i—Ca1—P1—Ca1x27.89 (4)O2—Ca1—O4—Ca2129.59 (5)
Cl1iv—Ca1—P1—Ca1x39.93 (3)P1—Ca1—O4—Ca250.41 (5)
Cl1v—Ca1—P1—Ca1x39.93 (3)Cl1iv—Ca1—O4—Ca2112.94 (3)
O2iii—Ca2—P1—O3iii1.15 (7)Cl1v—Ca1—O4—Ca212.11 (10)
O2vii—Ca2—P1—O3iii75.74 (8)P1vi—Ca1—O4—Ca2129.59 (5)
O2viii—Ca2—P1—O3iii73.85 (19)O2iii—Ca2—O4—P1vi87.30 (8)
O4ix—Ca2—P1—O3iii168.04 (9)O2vii—Ca2—O4—P1vi150.66 (9)
O4—Ca2—P1—O3iii86.90 (7)O2viii—Ca2—O4—P1vi13.28 (10)
O4vi—Ca2—P1—O3iii157.66 (8)O4ix—Ca2—O4—P1vi145.06 (8)
O3viii—Ca2—P1—O3iii87.58 (3)O4vi—Ca2—O4—P1vi66.11 (10)
O3vii—Ca2—P1—O3iii146.52 (7)O3iii—Ca2—O4—P1vi156.82 (8)
P1vi—Ca2—P1—O3iii90.40 (7)O3viii—Ca2—O4—P1vi6.86 (5)
P1ix—Ca2—P1—O3iii175.00 (6)O3vii—Ca2—O4—P1vi94.44 (7)
O2iii—Ca2—P1—O3ii97.58 (8)P1—Ca2—O4—P1vi172.45 (7)
O2vii—Ca2—P1—O3ii174.48 (8)P1ix—Ca2—O4—P1vi81.69 (6)
O2viii—Ca2—P1—O3ii172.58 (19)O2iii—Ca2—O4—Ca150.45 (7)
O4ix—Ca2—P1—O3ii93.23 (9)O2vii—Ca2—O4—Ca112.92 (13)
O4—Ca2—P1—O3ii11.83 (8)O2viii—Ca2—O4—Ca1124.47 (7)
O4vi—Ca2—P1—O3ii58.93 (8)O4ix—Ca2—O4—Ca177.20 (10)
O3iii—Ca2—P1—O3ii98.73 (12)O4vi—Ca2—O4—Ca1156.14 (8)
O3viii—Ca2—P1—O3ii11.15 (10)O3iii—Ca2—O4—Ca119.07 (5)
O3vii—Ca2—P1—O3ii114.74 (7)O3viii—Ca2—O4—Ca1130.89 (7)
P1vi—Ca2—P1—O3ii8.33 (7)O3vii—Ca2—O4—Ca1127.81 (5)
P1ix—Ca2—P1—O3ii86.27 (7)P1—Ca2—O4—Ca149.80 (5)
O2iii—Ca2—P1—O2x93.39 (11)P1vi—Ca2—O4—Ca1137.75 (10)
O2vii—Ca2—P1—O2x16.50 (13)P1ix—Ca2—O4—Ca1140.57 (5)
O2viii—Ca2—P1—O2x18.39 (15)O2iii—Ca2—O4—Ca2i167.12 (6)
O4ix—Ca2—P1—O2x75.80 (11)O2vii—Ca2—O4—Ca2i103.75 (9)
O4—Ca2—P1—O2x179.14 (10)O2viii—Ca2—O4—Ca2i118.86 (6)
O4vi—Ca2—P1—O2x110.10 (10)O4ix—Ca2—O4—Ca2i39.473 (16)
O3iii—Ca2—P1—O2x92.24 (11)O4vi—Ca2—O4—Ca2i39.473 (16)
O3viii—Ca2—P1—O2x179.82 (9)O3iii—Ca2—O4—Ca2i97.60 (6)
O3vii—Ca2—P1—O2x54.28 (10)O3viii—Ca2—O4—Ca2i112.44 (7)
P1vi—Ca2—P1—O2x177.36 (9)O3vii—Ca2—O4—Ca2i11.14 (8)
P1ix—Ca2—P1—O2x82.76 (9)P1—Ca2—O4—Ca2i66.87 (4)
O2iii—Ca2—P1—O4ix169.19 (8)P1vi—Ca2—O4—Ca2i105.58 (8)
O2vii—Ca2—P1—O4ix92.30 (8)P1ix—Ca2—O4—Ca2i23.90 (5)
O2viii—Ca2—P1—O4ix94.19 (19)O4—Ca1—Cl1—Cl1iv45.88 (8)
O4—Ca2—P1—O4ix105.05 (10)O3—Ca1—Cl1—Cl1iv155.30 (5)
O4vi—Ca2—P1—O4ix34.30 (8)O3i—Ca1—Cl1—Cl1iv19.84 (4)
O3iii—Ca2—P1—O4ix168.04 (9)O3ii—Ca1—Cl1—Cl1iv66.87 (4)
O3viii—Ca2—P1—O4ix104.38 (8)O3iii—Ca1—Cl1—Cl1iv119.62 (3)
O3vii—Ca2—P1—O4ix21.52 (7)Cl1i—Ca1—Cl1—Cl1iv180.000 (2)
P1vi—Ca2—P1—O4ix101.56 (7)O2—Ca1—Cl1—Cl1iv84.91 (2)
P1ix—Ca2—P1—O4ix6.96 (7)P1—Ca1—Cl1—Cl1iv92.756 (9)
O2iii—Ca2—P1—Ca154.15 (4)Cl1v—Ca1—Cl1—Cl1iv180.000 (2)
O2vii—Ca2—P1—Ca1131.05 (4)P1vi—Ca1—Cl1—Cl1iv6.71 (5)
O2viii—Ca2—P1—Ca1129.15 (18)O4—Ca1—Cl1—Ca1x83.02 (10)
O4ix—Ca2—P1—Ca1136.65 (7)O3—Ca1—Cl1—Ca1x75.80 (5)
O4—Ca2—P1—Ca131.60 (4)O3i—Ca1—Cl1—Ca1x148.74 (5)
O4vi—Ca2—P1—Ca1102.35 (4)O3ii—Ca1—Cl1—Ca1x62.03 (4)
O3iii—Ca2—P1—Ca155.30 (6)O3iii—Ca1—Cl1—Ca1x9.28 (5)
O3viii—Ca2—P1—Ca132.28 (4)Cl1i—Ca1—Cl1—Ca1x51.10 (3)
O3vii—Ca2—P1—Ca1158.17 (3)O2—Ca1—Cl1—Ca1x146.19 (3)
P1vi—Ca2—P1—Ca135.095 (13)P1—Ca1—Cl1—Ca1x36.14 (3)
P1ix—Ca2—P1—Ca1129.696 (12)Cl1iv—Ca1—Cl1—Ca1x128.90 (4)
O2iii—Ca2—P1—Ca2i136.55 (4)Cl1v—Ca1—Cl1—Ca1x51.10 (3)
O2vii—Ca2—P1—Ca2i146.56 (4)P1vi—Ca1—Cl1—Ca1x122.19 (7)
O2viii—Ca2—P1—Ca2i148.45 (18)O4—Ca1—Cl1—Ca1xi174.78 (7)
O4ix—Ca2—P1—Ca2i54.26 (7)O3—Ca1—Cl1—Ca1xi26.40 (7)
O4—Ca2—P1—Ca2i50.80 (4)O3i—Ca1—Cl1—Ca1xi109.06 (5)
O4vi—Ca2—P1—Ca2i19.96 (4)O3ii—Ca1—Cl1—Ca1xi164.23 (6)
O3iii—Ca2—P1—Ca2i137.70 (6)O3iii—Ca1—Cl1—Ca1xi111.48 (4)
O3viii—Ca2—P1—Ca2i50.12 (4)Cl1i—Ca1—Cl1—Ca1xi51.10 (3)
O3vii—Ca2—P1—Ca2i75.78 (3)O2—Ca1—Cl1—Ca1xi43.99 (4)
P1vi—Ca2—P1—Ca2i47.300 (9)P1—Ca1—Cl1—Ca1xi138.34 (4)
P1ix—Ca2—P1—Ca2i47.300 (9)Cl1iv—Ca1—Cl1—Ca1xi128.90 (4)
O2iii—Ca2—P1—Ca1ix143.67 (4)Cl1v—Ca1—Cl1—Ca1xi51.10 (3)
O2vii—Ca2—P1—Ca1ix66.78 (4)P1vi—Ca1—Cl1—Ca1xi135.61 (6)
O2viii—Ca2—P1—Ca1ix68.67 (18)O4—Ca1—Cl1—Ca1iv45.88 (8)
O4ix—Ca2—P1—Ca1ix25.52 (7)O3—Ca1—Cl1—Ca1iv155.30 (5)
O4—Ca2—P1—Ca1ix130.58 (4)O3i—Ca1—Cl1—Ca1iv19.84 (4)
O4vi—Ca2—P1—Ca1ix59.82 (4)O3ii—Ca1—Cl1—Ca1iv66.87 (4)
O3iii—Ca2—P1—Ca1ix142.52 (6)O3iii—Ca1—Cl1—Ca1iv119.62 (3)
O3viii—Ca2—P1—Ca1ix129.90 (4)Cl1i—Ca1—Cl1—Ca1iv180.0000 (10)
O3vii—Ca2—P1—Ca1ix4.00 (3)O2—Ca1—Cl1—Ca1iv84.91 (2)
P1vi—Ca2—P1—Ca1ix127.080 (13)P1—Ca1—Cl1—Ca1iv92.756 (9)
P1ix—Ca2—P1—Ca1ix32.480 (13)Cl1iv—Ca1—Cl1—Ca1iv0
O2iii—Ca2—P1—Ca1x4.03 (5)Cl1v—Ca1—Cl1—Ca1iv180.0000 (10)
O2vii—Ca2—P1—Ca1x72.87 (5)P1vi—Ca1—Cl1—Ca1iv6.71 (5)
O2viii—Ca2—P1—Ca1x70.97 (18)O4—Ca1—Cl1—Ca1xiv4.11 (9)
O4ix—Ca2—P1—Ca1x165.16 (8)O3—Ca1—Cl1—Ca1xiv162.93 (5)
O4—Ca2—P1—Ca1x89.78 (5)O3i—Ca1—Cl1—Ca1xiv61.61 (4)
O4vi—Ca2—P1—Ca1x160.54 (5)O3ii—Ca1—Cl1—Ca1xiv25.10 (4)
O3iii—Ca2—P1—Ca1x2.88 (6)O3iii—Ca1—Cl1—Ca1xiv77.85 (4)
O3viii—Ca2—P1—Ca1x90.46 (5)Cl1i—Ca1—Cl1—Ca1xiv138.23 (2)
O3vii—Ca2—P1—Ca1x143.65 (4)O2—Ca1—Cl1—Ca1xiv126.68 (3)
P1vi—Ca2—P1—Ca1x93.28 (4)P1—Ca1—Cl1—Ca1xiv50.989 (18)
P1ix—Ca2—P1—Ca1x172.12 (3)Cl1iv—Ca1—Cl1—Ca1xiv41.77 (2)
O4—Ca1—O2—P1xi180Cl1v—Ca1—Cl1—Ca1xiv138.23 (2)
O3—Ca1—O2—P1xi98.98 (4)P1vi—Ca1—Cl1—Ca1xiv35.06 (6)
O3i—Ca1—O2—P1xi98.98 (4)O4—Ca1—Cl1—Ca1xv87.64 (7)
O3ii—Ca1—O2—P1xi93.94 (10)O3—Ca1—Cl1—Ca1xv113.54 (6)
O3iii—Ca1—O2—P1xi93.94 (10)O3i—Ca1—Cl1—Ca1xv21.93 (4)
Cl1—Ca1—O2—P1xi28.19 (4)O3ii—Ca1—Cl1—Ca1xv108.64 (5)
Cl1i—Ca1—O2—P1xi28.19 (4)O3iii—Ca1—Cl1—Ca1xv161.39 (4)
Cl1iv—Ca1—O2—P1xi40.29 (3)Cl1i—Ca1—Cl1—Ca1xv138.23 (2)
Cl1v—Ca1—O2—P1xi40.29 (3)O2—Ca1—Cl1—Ca1xv43.14 (3)
O4—Ca1—O2—Ca2viii44.18 (3)P1—Ca1—Cl1—Ca1xv134.52 (3)
O3—Ca1—O2—Ca2viii36.85 (4)Cl1iv—Ca1—Cl1—Ca1xv41.77 (2)
O3i—Ca1—O2—Ca2viii125.20 (6)Cl1v—Ca1—Cl1—Ca1xv138.23 (2)
O3ii—Ca1—O2—Ca2viii130.24 (8)P1vi—Ca1—Cl1—Ca1xv48.47 (5)
O3iii—Ca1—O2—Ca2viii41.88 (12)
Symmetry codes: (i) x, y, z+1/2; (ii) xy+1, x+1, z+1/2; (iii) xy+1, x+1, z; (iv) x, y+2, z+1; (v) x, y+2, z1/2; (vi) y+1, xy+1, z; (vii) y, x+y, z; (viii) x, y+1, z; (ix) x+y, x+1, z; (x) y+1, xy+2, z; (xi) x+y1, x+1, z; (xii) x, y+1, z+1/2; (xiii) y1, x+y, z; (xiv) xy+1, x+1, z+1; (xv) y1, x+y, z+1.
(v_room) chlorapatite top
Crystal data top
3(O4P)·Cl·5(C)aDx = 3.177 Mg m3
Mr = 520.76Mo Kα radiation, λ = 0.7107 Å
Trigonal, P63/mCell parameters from 1874 reflections
Hall symbol: -P 6cθ = 3.9–26.3°
a = 9.6414 (2) ŵ = 3.21 mm1
c = 6.7631 (2) ÅT = 293 K
V = 544.45 (2) Å3Prism, colourless
Z = 20.45 × 0.19 × 0.16 mm
F(000) = 516
Data collection top
BRUKER APPEX-II CCD
diffractometer
405 independent reflections
Radiation source: fine-focus sealed tube392 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.016
ω and phi scansθmax = 26.4°, θmin = 2.4°
Absorption correction: multi-scan
BRUKER SADABS
h = 012
Tmin = 0.746, Tmax = 1k = 120
2637 measured reflectionsl = 80
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.017 w = 1/[σ2(Fo2) + (0.0314P)2 + 0.433P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.052(Δ/σ)max < 0.001
S = 1.12Δρmax = 0.37 e Å3
405 reflectionsΔρmin = 0.36 e Å3
41 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.022 (3)
Crystal data top
3(O4P)·Cl·5(C)aZ = 2
Mr = 520.76Mo Kα radiation
Trigonal, P63/mµ = 3.21 mm1
a = 9.6414 (2) ÅT = 293 K
c = 6.7631 (2) Å0.45 × 0.19 × 0.16 mm
V = 544.45 (2) Å3
Data collection top
BRUKER APPEX-II CCD
diffractometer
405 independent reflections
Absorption correction: multi-scan
BRUKER SADABS
392 reflections with I > 2σ(I)
Tmin = 0.746, Tmax = 1Rint = 0.016
2637 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.01741 parameters
wR(F2) = 0.0520 restraints
S = 1.12Δρmax = 0.37 e Å3
405 reflectionsΔρmin = 0.36 e Å3
Special details top

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ca10.00481 (6)0.74520 (6)0.250.0109 (2)
Ca20.33330.66670.00344 (9)0.0111 (2)
P10.37536 (7)0.96744 (7)0.250.0075 (2)
O20.3438 (2)0.5077 (2)0.250.0137 (4)
O30.08657 (15)0.64629 (18)0.0672 (2)0.0184 (4)
O40.1272 (2)0.5929 (2)0.250.0139 (4)
Cl1010.4438 (2)0.0188 (4)0.5
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0123 (3)0.0118 (3)0.0095 (3)0.0068 (2)00
Ca20.0131 (3)0.0131 (3)0.0071 (3)0.00656 (13)00
P10.0071 (3)0.0066 (3)0.0081 (3)0.0030 (3)00
O20.0192 (10)0.0152 (9)0.0136 (9)0.0137 (8)00
O30.0144 (6)0.0281 (7)0.0162 (7)0.0131 (6)0.0035 (5)0.0114 (6)
O40.0118 (9)0.0080 (9)0.0213 (10)0.0045 (7)00
Cl10.0146 (4)0.0146 (4)0.0271 (11)0.0073 (2)00
Geometric parameters (Å, º) top
Ca1—O42.2984 (18)Ca2—P1vi3.2150 (6)
Ca1—O32.3339 (13)Ca2—P1ix3.2150 (6)
Ca1—O3i2.3339 (13)P1—O3iii1.5313 (13)
Ca1—O3ii2.5405 (14)P1—O3ii1.5313 (13)
Ca1—O3iii2.5405 (14)P1—O2x1.5333 (18)
Ca1—Cl12.8052 (9)P1—O4ix1.5444 (18)
Ca1—Cl1i2.8052 (9)P1—Ca2i3.2150 (6)
Ca1—O22.974 (2)P1—Ca1ix3.3936 (8)
Ca1—P13.1144 (8)O2—P1xi1.5333 (17)
Ca1—Cl1iv3.2310 (11)O2—Ca2viii2.4054 (13)
Ca1—Cl1v3.2310 (11)O2—Ca2xii2.4054 (13)
Ca1—P1vi3.3936 (8)O3—P1xiii1.5313 (13)
Ca2—O2iii2.4054 (13)O3—Ca1xiii2.5405 (14)
Ca2—O2vii2.4054 (13)O3—Ca2viii2.7954 (15)
Ca2—O2viii2.4054 (13)O4—P1vi1.5444 (18)
Ca2—O4ix2.4455 (13)O4—Ca2i2.4455 (13)
Ca2—O42.4455 (13)Cl1—Cl1iv0.760 (3)
Ca2—O4vi2.4455 (13)Cl1—Ca1xi2.8052 (9)
Ca2—O3iii2.7954 (15)Cl1—Ca1x2.8052 (9)
Ca2—O3viii2.7954 (15)Cl1—Ca1xiv3.2310 (11)
Ca2—O3vii2.7954 (15)Cl1—Ca1iv3.2310 (11)
Ca2—P13.2150 (6)Cl1—Ca1xv3.2310 (11)
O4—Ca1—O387.04 (4)O2vii—Ca2—P188.58 (4)
O4—Ca1—O3i87.04 (4)O2viii—Ca2—P1165.81 (4)
O3—Ca1—O3i133.60 (8)O4ix—Ca2—P127.63 (4)
O4—Ca1—O3ii75.09 (5)O4—Ca2—P166.82 (4)
O3—Ca1—O3ii139.47 (5)O4vi—Ca2—P199.13 (4)
O3i—Ca1—O3ii82.27 (3)O3iii—Ca2—P128.44 (3)
O4—Ca1—O3iii75.09 (5)O3viii—Ca2—P1122.54 (3)
O3—Ca1—O3iii82.27 (3)O3vii—Ca2—P193.91 (3)
O3i—Ca1—O3iii139.47 (5)O2iii—Ca2—P1vi88.58 (4)
O3ii—Ca1—O3iii58.24 (6)O2vii—Ca2—P1vi165.81 (4)
O4—Ca1—Cl1142.96 (4)O2viii—Ca2—P1vi99.44 (4)
O3—Ca1—Cl1128.25 (5)O4ix—Ca2—P1vi99.13 (4)
O3i—Ca1—Cl176.13 (4)O4—Ca2—P1vi27.63 (4)
O3ii—Ca1—Cl170.16 (3)O4vi—Ca2—P1vi66.82 (4)
O3iii—Ca1—Cl196.63 (4)O3iii—Ca2—P1vi93.91 (3)
O4—Ca1—Cl1i142.96 (4)O3viii—Ca2—P1vi28.44 (3)
O3—Ca1—Cl1i76.13 (4)O3vii—Ca2—P1vi122.54 (3)
O3i—Ca1—Cl1i128.25 (5)P1—Ca2—P1vi94.224 (14)
O3ii—Ca1—Cl1i96.63 (4)O2iii—Ca2—P1ix165.81 (4)
O3iii—Ca1—Cl1i70.16 (3)O2vii—Ca2—P1ix99.44 (4)
Cl1—Ca1—Cl1i55.71 (6)O2viii—Ca2—P1ix88.58 (4)
O4—Ca1—O2104.57 (5)O4ix—Ca2—P1ix66.82 (4)
O3—Ca1—O268.59 (4)O4—Ca2—P1ix99.13 (4)
O3i—Ca1—O268.59 (4)O4vi—Ca2—P1ix27.63 (4)
O3ii—Ca1—O2150.78 (3)O3iii—Ca2—P1ix122.54 (3)
O3iii—Ca1—O2150.78 (3)O3viii—Ca2—P1ix93.91 (3)
Cl1—Ca1—O299.62 (3)O3vii—Ca2—P1ix28.44 (3)
Cl1i—Ca1—O299.62 (3)P1—Ca2—P1ix94.224 (14)
O4—Ca1—P170.17 (5)P1vi—Ca2—P1ix94.224 (14)
O3—Ca1—P1110.48 (4)O3iii—P1—O3ii107.68 (11)
O3i—Ca1—P1110.48 (4)O3iii—P1—O2x112.05 (6)
O3ii—Ca1—P129.23 (3)O3ii—P1—O2x112.05 (6)
O3iii—Ca1—P129.23 (3)O3iii—P1—O4ix106.78 (7)
Cl1—Ca1—P185.012 (15)O3ii—P1—O4ix106.78 (7)
Cl1i—Ca1—P185.012 (15)O2x—P1—O4ix111.21 (10)
O2—Ca1—P1174.74 (4)O3iii—P1—Ca154.12 (5)
O4—Ca1—Cl1iv133.87 (3)O3ii—P1—Ca154.12 (5)
O3—Ca1—Cl1iv138.92 (4)O2x—P1—Ca1136.14 (8)
O3i—Ca1—Cl1iv64.89 (4)O4ix—P1—Ca1112.66 (7)
O3ii—Ca1—Cl1iv65.85 (3)O3iii—P1—Ca260.38 (6)
O3iii—Ca1—Cl1iv102.40 (4)O3ii—P1—Ca2111.50 (6)
Cl1—Ca1—Cl1iv12.00 (5)O2x—P1—Ca2135.75 (5)
Cl1i—Ca1—Cl1iv67.717 (12)O4ix—P1—Ca247.25 (5)
O2—Ca1—Cl1iv98.35 (3)Ca1—P1—Ca278.204 (14)
P1—Ca1—Cl1iv85.671 (14)O3iii—P1—Ca2i111.50 (6)
O4—Ca1—Cl1v133.87 (3)O3ii—P1—Ca2i60.38 (6)
O3—Ca1—Cl1v64.89 (4)O2x—P1—Ca2i135.75 (5)
O3i—Ca1—Cl1v138.92 (4)O4ix—P1—Ca2i47.25 (5)
O3ii—Ca1—Cl1v102.40 (4)Ca1—P1—Ca2i78.204 (14)
O3iii—Ca1—Cl1v65.85 (3)Ca2—P1—Ca2i64.43 (2)
Cl1—Ca1—Cl1v67.717 (12)O3iii—P1—Ca1ix122.02 (6)
Cl1i—Ca1—Cl1v12.00 (5)O3ii—P1—Ca1ix122.02 (6)
O2—Ca1—Cl1v98.35 (3)O2x—P1—Ca1ix76.52 (7)
P1—Ca1—Cl1v85.671 (14)Ca1—P1—Ca1ix147.34 (2)
Cl1iv—Ca1—Cl1v79.72 (5)Ca2—P1—Ca1ix74.284 (14)
O4—Ca1—P1vi22.48 (4)Ca2i—P1—Ca1ix74.284 (14)
O3—Ca1—P1vi78.64 (4)O3iii—P1—Ca1x80.32 (6)
O3i—Ca1—P1vi78.64 (4)O3ii—P1—Ca1x80.32 (6)
O3ii—Ca1—P1vi94.67 (4)O2x—P1—Ca1x56.07 (7)
O3iii—Ca1—P1vi94.67 (4)O4ix—P1—Ca1x167.27 (7)
Cl1—Ca1—P1vi152.00 (3)Ca1—P1—Ca1x80.07 (2)
Cl1i—Ca1—P1vi152.00 (3)Ca2—P1—Ca1x140.662 (14)
O2—Ca1—P1vi82.09 (4)Ca2i—P1—Ca1x140.662 (14)
P1—Ca1—P1vi92.66 (2)Ca1ix—P1—Ca1x132.59 (2)
Cl1iv—Ca1—P1vi140.05 (2)P1xi—O2—Ca2viii133.41 (4)
Cl1v—Ca1—P1vi140.05 (2)P1xi—O2—Ca2xii133.41 (4)
O2iii—Ca2—O2vii77.24 (5)Ca2viii—O2—Ca2xii87.77 (6)
O2iii—Ca2—O2viii77.24 (5)P1xi—O2—Ca198.61 (8)
O2vii—Ca2—O2viii77.24 (5)Ca2viii—O2—Ca196.43 (5)
O2iii—Ca2—O4ix126.48 (6)Ca2xii—O2—Ca196.43 (5)
O2vii—Ca2—O4ix89.80 (4)P1xiii—O3—Ca1139.31 (8)
O2viii—Ca2—O4ix150.08 (6)P1xiii—O3—Ca1xiii96.64 (7)
O2iii—Ca2—O489.80 (4)Ca1—O3—Ca1xiii118.64 (5)
O2vii—Ca2—O4150.08 (6)P1xiii—O3—Ca2viii91.19 (7)
O2viii—Ca2—O4126.48 (6)Ca1—O3—Ca2viii103.16 (5)
O4ix—Ca2—O476.30 (5)Ca1xiii—O3—Ca2viii96.77 (4)
O2iii—Ca2—O4vi150.08 (6)P1vi—O4—Ca1122.83 (10)
O2vii—Ca2—O4vi126.48 (6)P1vi—O4—Ca2i105.13 (7)
O2viii—Ca2—O4vi89.80 (4)Ca1—O4—Ca2i114.60 (5)
O4ix—Ca2—O4vi76.30 (5)P1vi—O4—Ca2105.13 (7)
O4—Ca2—O4vi76.30 (5)Ca1—O4—Ca2114.60 (5)
O2iii—Ca2—O3iii71.01 (5)Ca2i—O4—Ca289.00 (6)
O2vii—Ca2—O3iii81.97 (5)Cl1iv—Cl1—Ca1xi117.86 (3)
O2viii—Ca2—O3iii145.13 (4)Cl1iv—Cl1—Ca1117.86 (3)
O4ix—Ca2—O3iii55.73 (5)Ca1xi—Cl1—Ca199.93 (4)
O4—Ca2—O3iii68.27 (5)Cl1iv—Cl1—Ca1x117.86 (3)
O4vi—Ca2—O3iii125.04 (4)Ca1xi—Cl1—Ca1x99.93 (4)
O2iii—Ca2—O3viii81.97 (5)Ca1—Cl1—Ca1x99.93 (4)
O2vii—Ca2—O3viii145.13 (4)Cl1iv—Cl1—Ca1xiv50.14 (2)
O2viii—Ca2—O3viii71.01 (5)Ca1xi—Cl1—Ca1xiv168.00 (5)
O4ix—Ca2—O3viii125.04 (4)Ca1—Cl1—Ca1xiv87.716 (10)
O4—Ca2—O3viii55.73 (5)Ca1x—Cl1—Ca1xiv87.716 (10)
O4vi—Ca2—O3viii68.27 (5)Cl1iv—Cl1—Ca1iv50.14 (2)
O3iii—Ca2—O3viii117.142 (17)Ca1xi—Cl1—Ca1iv87.716 (10)
O2iii—Ca2—O3vii145.13 (4)Ca1—Cl1—Ca1iv168.00 (5)
O2vii—Ca2—O3vii71.01 (5)Ca1x—Cl1—Ca1iv87.716 (10)
O2viii—Ca2—O3vii81.97 (5)Ca1xiv—Cl1—Ca1iv83.33 (3)
O4ix—Ca2—O3vii68.27 (5)Cl1iv—Cl1—Ca1xv50.14 (2)
O4—Ca2—O3vii125.04 (4)Ca1xi—Cl1—Ca1xv87.716 (10)
O4vi—Ca2—O3vii55.73 (5)Ca1—Cl1—Ca1xv87.716 (10)
O3iii—Ca2—O3vii117.142 (16)Ca1x—Cl1—Ca1xv168.00 (5)
O3viii—Ca2—O3vii117.142 (16)Ca1xiv—Cl1—Ca1xv83.33 (3)
O2iii—Ca2—P199.44 (4)Ca1iv—Cl1—Ca1xv83.33 (3)
O4—Ca1—P1—O3iii94.82 (7)Cl1—Ca1—O2—Ca2viii164.05 (4)
O3—Ca1—P1—O3iii15.97 (6)Cl1i—Ca1—O2—Ca2viii107.47 (4)
O3i—Ca1—P1—O3iii173.68 (10)Cl1iv—Ca1—O2—Ca2viii176.14 (4)
O3ii—Ca1—P1—O3iii170.35 (14)Cl1v—Ca1—O2—Ca2viii95.39 (4)
Cl1—Ca1—P1—O3iii113.15 (8)P1vi—Ca1—O2—Ca2viii44.24 (3)
Cl1i—Ca1—P1—O3iii57.20 (7)O4—Ca1—O2—Ca2xii44.24 (3)
Cl1iv—Ca1—P1—O3iii125.17 (7)O3—Ca1—O2—Ca2xii125.08 (6)
Cl1v—Ca1—P1—O3iii45.18 (7)O3i—Ca1—O2—Ca2xii36.60 (4)
P1vi—Ca1—P1—O3iii94.82 (7)O3ii—Ca1—O2—Ca2xii41.18 (11)
O4—Ca1—P1—O3ii94.82 (7)O3iii—Ca1—O2—Ca2xii129.65 (8)
O3—Ca1—P1—O3ii173.68 (10)Cl1—Ca1—O2—Ca2xii107.47 (4)
O3i—Ca1—P1—O3ii15.97 (6)Cl1i—Ca1—O2—Ca2xii164.05 (4)
O3iii—Ca1—P1—O3ii170.35 (14)Cl1iv—Ca1—O2—Ca2xii95.39 (4)
Cl1—Ca1—P1—O3ii57.20 (7)Cl1v—Ca1—O2—Ca2xii176.14 (4)
Cl1i—Ca1—P1—O3ii113.15 (8)P1vi—Ca1—O2—Ca2xii44.24 (3)
Cl1iv—Ca1—P1—O3ii45.18 (7)O4—Ca1—O3—P1xiii32.40 (14)
Cl1v—Ca1—P1—O3ii125.17 (7)O3i—Ca1—O3—P1xiii115.47 (12)
P1vi—Ca1—P1—O3ii94.82 (7)O3ii—Ca1—O3—P1xiii30.4 (2)
O4—Ca1—P1—O2x180O3iii—Ca1—O3—P1xiii42.95 (16)
O3—Ca1—P1—O2x101.14 (4)Cl1—Ca1—O3—P1xiii135.31 (12)
O3i—Ca1—P1—O2x101.14 (4)Cl1i—Ca1—O3—P1xiii114.33 (14)
O3ii—Ca1—P1—O2x85.18 (7)O2—Ca1—O3—P1xiii139.30 (15)
O3iii—Ca1—P1—O2x85.18 (7)P1—Ca1—O3—P1xiii35.16 (15)
Cl1—Ca1—P1—O2x27.97 (3)Cl1iv—Ca1—O3—P1xiii142.96 (11)
Cl1i—Ca1—P1—O2x27.97 (3)Cl1v—Ca1—O3—P1xiii109.85 (14)
Cl1iv—Ca1—P1—O2x40.00 (2)P1vi—Ca1—O3—P1xiii53.43 (13)
Cl1v—Ca1—P1—O2x40.00 (2)O4—Ca1—O3—Ca1xiii179.27 (7)
P1vi—Ca1—P1—O2x180O3i—Ca1—O3—Ca1xiii97.66 (10)
O4—Ca1—P1—O4ix0O3ii—Ca1—O3—Ca1xiii116.46 (5)
O3—Ca1—P1—O4ix78.86 (4)O3iii—Ca1—O3—Ca1xiii103.92 (4)
O3i—Ca1—P1—O4ix78.86 (4)Cl1—Ca1—O3—Ca1xiii11.56 (9)
O3ii—Ca1—P1—O4ix94.82 (7)Cl1i—Ca1—O3—Ca1xiii32.54 (5)
O3iii—Ca1—P1—O4ix94.82 (7)O2—Ca1—O3—Ca1xiii73.83 (6)
Cl1—Ca1—P1—O4ix152.03 (3)P1—Ca1—O3—Ca1xiii111.71 (5)
Cl1i—Ca1—P1—O4ix152.03 (3)Cl1iv—Ca1—O3—Ca1xiii3.91 (11)
Cl1iv—Ca1—P1—O4ix140.00 (2)Cl1v—Ca1—O3—Ca1xiii37.02 (5)
Cl1v—Ca1—P1—O4ix140.00 (2)P1vi—Ca1—O3—Ca1xiii159.70 (7)
P1vi—Ca1—P1—O4ix0O4—Ca1—O3—Ca2viii75.33 (5)
O4—Ca1—P1—Ca233.000 (10)O3i—Ca1—O3—Ca2viii7.74 (11)
O3—Ca1—P1—Ca245.86 (4)O3ii—Ca1—O3—Ca2viii138.14 (8)
O3i—Ca1—P1—Ca2111.86 (4)O3iii—Ca1—O3—Ca2viii150.68 (4)
O3ii—Ca1—P1—Ca2127.82 (7)Cl1—Ca1—O3—Ca2viii116.96 (4)
O3iii—Ca1—P1—Ca261.82 (7)Cl1i—Ca1—O3—Ca2viii137.94 (4)
Cl1—Ca1—P1—Ca2174.97 (3)O2—Ca1—O3—Ca2viii31.58 (4)
Cl1i—Ca1—P1—Ca2119.03 (3)P1—Ca1—O3—Ca2viii142.89 (3)
Cl1iv—Ca1—P1—Ca2173.00 (2)Cl1iv—Ca1—O3—Ca2viii109.31 (6)
Cl1v—Ca1—P1—Ca2107.00 (2)Cl1v—Ca1—O3—Ca2viii142.43 (5)
P1vi—Ca1—P1—Ca233.000 (10)P1vi—Ca1—O3—Ca2viii54.30 (3)
O4—Ca1—P1—Ca2i33.000 (10)O3—Ca1—O4—P1vi66.98 (4)
O3—Ca1—P1—Ca2i111.86 (4)O3i—Ca1—O4—P1vi66.98 (4)
O3i—Ca1—P1—Ca2i45.86 (4)O3ii—Ca1—O4—P1vi149.76 (3)
O3ii—Ca1—P1—Ca2i61.82 (7)O3iii—Ca1—O4—P1vi149.76 (3)
O3iii—Ca1—P1—Ca2i127.82 (7)Cl1—Ca1—O4—P1vi129.13 (6)
Cl1—Ca1—P1—Ca2i119.03 (3)Cl1i—Ca1—O4—P1vi129.13 (6)
Cl1i—Ca1—P1—Ca2i174.97 (3)O2—Ca1—O4—P1vi0
Cl1iv—Ca1—P1—Ca2i107.00 (2)P1—Ca1—O4—P1vi180
Cl1v—Ca1—P1—Ca2i173.00 (2)Cl1iv—Ca1—O4—P1vi117.25 (5)
P1vi—Ca1—P1—Ca2i33.000 (10)Cl1v—Ca1—O4—P1vi117.25 (5)
O4—Ca1—P1—Ca1ix0O3—Ca1—O4—Ca2i163.45 (6)
O3—Ca1—P1—Ca1ix78.86 (4)O3i—Ca1—O4—Ca2i62.59 (6)
O3i—Ca1—P1—Ca1ix78.86 (4)O3ii—Ca1—O4—Ca2i20.19 (5)
O3ii—Ca1—P1—Ca1ix94.82 (7)O3iii—Ca1—O4—Ca2i80.67 (6)
O3iii—Ca1—P1—Ca1ix94.82 (7)Cl1—Ca1—O4—Ca2i0.43 (10)
Cl1—Ca1—P1—Ca1ix152.03 (3)Cl1i—Ca1—O4—Ca2i101.30 (4)
Cl1i—Ca1—P1—Ca1ix152.03 (3)O2—Ca1—O4—Ca2i129.57 (5)
Cl1iv—Ca1—P1—Ca1ix140.00 (2)P1—Ca1—O4—Ca2i50.43 (5)
Cl1v—Ca1—P1—Ca1ix140.00 (2)Cl1iv—Ca1—O4—Ca2i12.32 (9)
P1vi—Ca1—P1—Ca1ix0Cl1v—Ca1—O4—Ca2i113.18 (3)
O4—Ca1—P1—Ca1x180P1vi—Ca1—O4—Ca2i129.57 (5)
O3—Ca1—P1—Ca1x101.14 (4)O3—Ca1—O4—Ca262.59 (6)
O3i—Ca1—P1—Ca1x101.14 (4)O3i—Ca1—O4—Ca2163.45 (6)
O3ii—Ca1—P1—Ca1x85.18 (7)O3ii—Ca1—O4—Ca280.67 (6)
O3iii—Ca1—P1—Ca1x85.18 (7)O3iii—Ca1—O4—Ca220.19 (5)
Cl1—Ca1—P1—Ca1x27.97 (3)Cl1—Ca1—O4—Ca2101.30 (4)
Cl1i—Ca1—P1—Ca1x27.97 (3)Cl1i—Ca1—O4—Ca20.43 (10)
Cl1iv—Ca1—P1—Ca1x40.00 (2)O2—Ca1—O4—Ca2129.57 (5)
Cl1v—Ca1—P1—Ca1x40.00 (2)P1—Ca1—O4—Ca250.43 (5)
P1vi—Ca1—P1—Ca1x180Cl1iv—Ca1—O4—Ca2113.18 (3)
O2iii—Ca2—P1—O3iii1.15 (7)Cl1v—Ca1—O4—Ca212.32 (9)
O2vii—Ca2—P1—O3iii75.67 (7)P1vi—Ca1—O4—Ca2129.57 (5)
O2viii—Ca2—P1—O3iii74.04 (18)O2iii—Ca2—O4—P1vi87.32 (7)
O4ix—Ca2—P1—O3iii167.95 (9)O2vii—Ca2—O4—P1vi150.65 (8)
O4—Ca2—P1—O3iii86.84 (7)O2viii—Ca2—O4—P1vi13.42 (9)
O4vi—Ca2—P1—O3iii157.58 (7)O4ix—Ca2—O4—P1vi144.88 (7)
O3viii—Ca2—P1—O3iii87.60 (3)O4vi—Ca2—O4—P1vi65.93 (9)
O3vii—Ca2—P1—O3iii146.52 (7)O3iii—Ca2—O4—P1vi156.90 (7)
P1vi—Ca2—P1—O3iii90.41 (6)O3viii—Ca2—O4—P1vi6.91 (5)
P1ix—Ca2—P1—O3iii175.03 (6)O3vii—Ca2—O4—P1vi94.42 (7)
O2iii—Ca2—P1—O3ii97.57 (7)P1—Ca2—O4—P1vi172.31 (7)
O2vii—Ca2—P1—O3ii174.38 (8)P1ix—Ca2—O4—P1vi81.60 (6)
O2viii—Ca2—P1—O3ii172.76 (18)O2iii—Ca2—O4—Ca150.53 (7)
O4ix—Ca2—P1—O3ii93.34 (9)O2vii—Ca2—O4—Ca112.79 (12)
O4—Ca2—P1—O3ii11.87 (7)O2viii—Ca2—O4—Ca1124.44 (7)
O4vi—Ca2—P1—O3ii58.87 (8)O4ix—Ca2—O4—Ca177.26 (9)
O3iii—Ca2—P1—O3ii98.71 (11)O4vi—Ca2—O4—Ca1156.22 (8)
O3viii—Ca2—P1—O3ii11.11 (9)O3iii—Ca2—O4—Ca119.05 (5)
O3vii—Ca2—P1—O3ii114.76 (7)O3viii—Ca2—O4—Ca1130.94 (7)
P1vi—Ca2—P1—O3ii8.31 (6)O3vii—Ca2—O4—Ca1127.73 (5)
P1ix—Ca2—P1—O3ii86.25 (6)P1—Ca2—O4—Ca149.84 (5)
O2iii—Ca2—P1—O2x93.16 (11)P1vi—Ca2—O4—Ca1137.86 (10)
O2vii—Ca2—P1—O2x16.34 (12)P1ix—Ca2—O4—Ca1140.54 (5)
O2viii—Ca2—P1—O2x17.97 (14)O2iii—Ca2—O4—Ca2i167.27 (6)
O4ix—Ca2—P1—O2x75.93 (11)O2vii—Ca2—O4—Ca2i103.95 (9)
O4—Ca2—P1—O2x178.85 (9)O2viii—Ca2—O4—Ca2i118.83 (5)
O4vi—Ca2—P1—O2x110.41 (9)O4ix—Ca2—O4—Ca2i39.479 (15)
O3iii—Ca2—P1—O2x92.01 (10)O4vi—Ca2—O4—Ca2i39.479 (15)
O3viii—Ca2—P1—O2x179.61 (9)O3iii—Ca2—O4—Ca2i97.69 (5)
O3vii—Ca2—P1—O2x54.51 (9)O3viii—Ca2—O4—Ca2i112.32 (6)
P1vi—Ca2—P1—O2x177.58 (9)O3vii—Ca2—O4—Ca2i10.99 (8)
P1ix—Ca2—P1—O2x83.02 (9)P1—Ca2—O4—Ca2i66.90 (4)
O2iii—Ca2—P1—O4ix169.09 (7)P1vi—Ca2—O4—Ca2i105.41 (8)
O2vii—Ca2—P1—O4ix92.28 (8)P1ix—Ca2—O4—Ca2i23.81 (5)
O2viii—Ca2—P1—O4ix93.90 (18)O4—Ca1—Cl1—Cl1iv45.55 (7)
O4—Ca2—P1—O4ix105.21 (10)O3—Ca1—Cl1—Cl1iv155.12 (5)
O4vi—Ca2—P1—O4ix34.47 (8)O3i—Ca1—Cl1—Cl1iv19.90 (4)
O3iii—Ca2—P1—O4ix167.95 (9)O3ii—Ca1—Cl1—Cl1iv66.77 (3)
O3viii—Ca2—P1—O4ix104.45 (7)O3iii—Ca1—Cl1—Cl1iv119.52 (3)
O3vii—Ca2—P1—O4ix21.42 (7)Cl1i—Ca1—Cl1—Cl1iv180.0000 (10)
P1vi—Ca2—P1—O4ix101.65 (7)O2—Ca1—Cl1—Cl1iv84.859 (18)
P1ix—Ca2—P1—O4ix7.09 (6)P1—Ca1—Cl1—Cl1iv92.644 (9)
O2iii—Ca2—P1—Ca154.10 (4)Cl1v—Ca1—Cl1—Cl1iv180
O2vii—Ca2—P1—Ca1130.92 (4)P1vi—Ca1—Cl1—Cl1iv6.37 (5)
O2viii—Ca2—P1—Ca1129.29 (17)O4—Ca1—Cl1—Ca1xi174.53 (6)
O4ix—Ca2—P1—Ca1136.80 (7)O3—Ca1—Cl1—Ca1xi26.13 (6)
O4—Ca2—P1—Ca131.59 (3)O3i—Ca1—Cl1—Ca1xi109.09 (4)
O4vi—Ca2—P1—Ca1102.33 (4)O3ii—Ca1—Cl1—Ca1xi164.25 (5)
O3iii—Ca2—P1—Ca155.25 (6)O3iii—Ca1—Cl1—Ca1xi111.49 (4)
O3viii—Ca2—P1—Ca132.35 (3)Cl1i—Ca1—Cl1—Ca1xi51.02 (3)
O3vii—Ca2—P1—Ca1158.23 (3)O2—Ca1—Cl1—Ca1xi44.13 (4)
P1vi—Ca2—P1—Ca135.158 (13)P1—Ca1—Cl1—Ca1xi138.37 (3)
P1ix—Ca2—P1—Ca1129.718 (11)Cl1iv—Ca1—Cl1—Ca1xi128.98 (3)
O2iii—Ca2—P1—Ca2i136.54 (4)Cl1v—Ca1—Cl1—Ca1xi51.02 (3)
O2vii—Ca2—P1—Ca2i146.65 (4)P1vi—Ca1—Cl1—Ca1xi135.36 (5)
O2viii—Ca2—P1—Ca2i148.27 (17)O4—Ca1—Cl1—Ca1x83.43 (8)
O4ix—Ca2—P1—Ca2i54.37 (6)O3—Ca1—Cl1—Ca1x75.90 (5)
O4—Ca2—P1—Ca2i50.85 (3)O3i—Ca1—Cl1—Ca1x148.88 (5)
O4vi—Ca2—P1—Ca2i19.89 (4)O3ii—Ca1—Cl1—Ca1x62.22 (4)
O3iii—Ca2—P1—Ca2i137.69 (6)O3iii—Ca1—Cl1—Ca1x9.46 (4)
O3viii—Ca2—P1—Ca2i50.08 (4)Cl1i—Ca1—Cl1—Ca1x51.02 (3)
O3vii—Ca2—P1—Ca2i75.79 (3)O2—Ca1—Cl1—Ca1x146.16 (3)
P1vi—Ca2—P1—Ca2i47.280 (8)P1—Ca1—Cl1—Ca1x36.34 (3)
P1ix—Ca2—P1—Ca2i47.280 (8)Cl1iv—Ca1—Cl1—Ca1x128.98 (3)
O2iii—Ca2—P1—Ca1ix143.67 (4)Cl1v—Ca1—Cl1—Ca1x51.02 (3)
O2vii—Ca2—P1—Ca1ix66.86 (4)P1vi—Ca1—Cl1—Ca1x122.61 (6)
O2viii—Ca2—P1—Ca1ix68.49 (17)O4—Ca1—Cl1—Ca1xiv3.84 (8)
O4ix—Ca2—P1—Ca1ix25.42 (6)O3—Ca1—Cl1—Ca1xiv163.18 (5)
O4—Ca2—P1—Ca1ix130.63 (4)O3i—Ca1—Cl1—Ca1xiv61.60 (4)
O4vi—Ca2—P1—Ca1ix59.89 (4)O3ii—Ca1—Cl1—Ca1xiv25.06 (3)
O3iii—Ca2—P1—Ca1ix142.53 (6)O3iii—Ca1—Cl1—Ca1xiv77.82 (3)
O3viii—Ca2—P1—Ca1ix129.87 (4)Cl1i—Ca1—Cl1—Ca1xiv138.294 (17)
O3vii—Ca2—P1—Ca1ix4.00 (3)O2—Ca1—Cl1—Ca1xiv126.56 (2)
P1vi—Ca2—P1—Ca1ix127.066 (12)P1—Ca1—Cl1—Ca1xiv50.938 (15)
P1ix—Ca2—P1—Ca1ix32.506 (12)Cl1iv—Ca1—Cl1—Ca1xiv41.706 (18)
O2iii—Ca2—P1—Ca1x3.71 (5)Cl1v—Ca1—Cl1—Ca1xiv138.294 (17)
O2vii—Ca2—P1—Ca1x73.10 (5)P1vi—Ca1—Cl1—Ca1xiv35.33 (5)
O2viii—Ca2—P1—Ca1x71.48 (17)O4—Ca1—Cl1—Ca1iv45.55 (7)
O4ix—Ca2—P1—Ca1x165.38 (7)O3—Ca1—Cl1—Ca1iv155.12 (5)
O4—Ca2—P1—Ca1x89.40 (5)O3i—Ca1—Cl1—Ca1iv19.90 (4)
O4vi—Ca2—P1—Ca1x160.14 (5)O3ii—Ca1—Cl1—Ca1iv66.77 (3)
O3iii—Ca2—P1—Ca1x2.56 (6)O3iii—Ca1—Cl1—Ca1iv119.52 (3)
O3viii—Ca2—P1—Ca1x90.17 (4)Cl1i—Ca1—Cl1—Ca1iv180.0000 (10)
O3vii—Ca2—P1—Ca1x143.96 (4)O2—Ca1—Cl1—Ca1iv84.859 (18)
P1vi—Ca2—P1—Ca1x92.97 (4)P1—Ca1—Cl1—Ca1iv92.644 (8)
P1ix—Ca2—P1—Ca1x172.47 (3)Cl1iv—Ca1—Cl1—Ca1iv0
O4—Ca1—O2—P1xi180Cl1v—Ca1—Cl1—Ca1iv180.0000 (10)
O3—Ca1—O2—P1xi99.16 (4)P1vi—Ca1—Cl1—Ca1iv6.37 (5)
O3i—Ca1—O2—P1xi99.16 (4)O4—Ca1—Cl1—Ca1xv87.26 (7)
O3ii—Ca1—O2—P1xi94.58 (9)O3—Ca1—Cl1—Ca1xv113.41 (5)
O3iii—Ca1—O2—P1xi94.58 (9)O3i—Ca1—Cl1—Ca1xv21.81 (4)
Cl1—Ca1—O2—P1xi28.29 (3)O3ii—Ca1—Cl1—Ca1xv108.47 (4)
Cl1i—Ca1—O2—P1xi28.29 (3)O3iii—Ca1—Cl1—Ca1xv161.23 (3)
Cl1iv—Ca1—O2—P1xi40.37 (2)Cl1i—Ca1—Cl1—Ca1xv138.294 (17)
Cl1v—Ca1—O2—P1xi40.37 (2)O2—Ca1—Cl1—Ca1xv43.15 (3)
O4—Ca1—O2—Ca2viii44.24 (3)P1—Ca1—Cl1—Ca1xv134.35 (2)
O3—Ca1—O2—Ca2viii36.60 (4)Cl1iv—Ca1—Cl1—Ca1xv41.706 (18)
O3i—Ca1—O2—Ca2viii125.08 (6)Cl1v—Ca1—Cl1—Ca1xv138.294 (17)
O3ii—Ca1—O2—Ca2viii129.65 (8)P1vi—Ca1—Cl1—Ca1xv48.08 (5)
O3iii—Ca1—O2—Ca2viii41.18 (11)
Symmetry codes: (i) x, y, z+1/2; (ii) xy+1, x+1, z+1/2; (iii) xy+1, x+1, z; (iv) x, y+2, z+1; (v) x, y+2, z1/2; (vi) y+1, xy+1, z; (vii) y, x+y, z; (viii) x, y+1, z; (ix) x+y, x+1, z; (x) y+1, xy+2, z; (xi) x+y1, x+1, z; (xii) x, y+1, z+1/2; (xiii) y1, x+y, z; (xiv) xy+1, x+1, z+1; (xv) y1, x+y, z+1.
(1_low_needle) chlorapatite top
Crystal data top
3(O4P)·Cl·5(Ca)Dx = 3.187 Mg m3
Mr = 520.76Mo Kα radiation, λ = 0.7107 Å
Trigonal, P63/mCell parameters from 2751 reflections
Hall symbol: -P 6cθ = 3.9–26.3°
a = 9.6368 (2) ŵ = 3.23 mm1
c = 6.7482 (2) ÅT = 100 K
V = 542.73 (2) Å3Prism, colourless
Z = 20.34 × 0.02 × 0.02 mm
F(000) = 516
Data collection top
BRUKER APPEX-II CCD
diffractometer
400 independent reflections
Radiation source: fine-focus sealed tube354 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.037
ω and phi scansθmax = 26.3°, θmin = 2.4°
Absorption correction: multi-scan
BRUKER SADABS
h = 1210
Tmin = 0.829, Tmax = 1k = 1112
7462 measured reflectionsl = 88
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.016 w = 1/[σ2(Fo2) + (0.0132P)2 + 0.7087P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.038(Δ/σ)max < 0.001
S = 1.10Δρmax = 0.37 e Å3
400 reflectionsΔρmin = 0.36 e Å3
41 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0040 (8)
Crystal data top
3(O4P)·Cl·5(Ca)Z = 2
Mr = 520.76Mo Kα radiation
Trigonal, P63/mµ = 3.23 mm1
a = 9.6368 (2) ÅT = 100 K
c = 6.7482 (2) Å0.34 × 0.02 × 0.02 mm
V = 542.73 (2) Å3
Data collection top
BRUKER APPEX-II CCD
diffractometer
400 independent reflections
Absorption correction: multi-scan
BRUKER SADABS
354 reflections with I > 2σ(I)
Tmin = 0.829, Tmax = 1Rint = 0.037
7462 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.01641 parameters
wR(F2) = 0.0380 restraints
S = 1.10Δρmax = 0.37 e Å3
400 reflectionsΔρmin = 0.36 e Å3
Special details top

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ca10.00586 (6)0.74549 (6)0.250.00556 (17)
Ca20.33330.66670.00350 (10)0.00608 (19)
P10.37497 (8)0.96726 (8)0.250.00425 (18)
O20.3439 (2)0.5076 (2)0.250.0077 (4)
O30.08685 (16)0.64681 (18)0.0666 (2)0.0123 (3)
O40.1279 (2)0.5929 (2)0.250.0084 (4)
Cl1010.4414 (3)0.0148 (5)0.5
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0067 (3)0.0064 (3)0.0045 (3)0.0040 (2)00
Ca20.0073 (2)0.0073 (2)0.0037 (3)0.00364 (12)00
P10.0039 (3)0.0038 (3)0.0046 (3)0.0016 (3)00
O20.0091 (9)0.0076 (10)0.0085 (10)0.0058 (8)00
O30.0089 (7)0.0203 (8)0.0098 (7)0.0090 (6)0.0031 (6)0.0090 (6)
O40.0054 (9)0.0057 (10)0.0137 (10)0.0024 (8)00
Cl10.0087 (4)0.0087 (4)0.0270 (13)0.0044 (2)00
Geometric parameters (Å, º) top
Ca1—O42.2971 (19)Ca2—P1vi3.2119 (6)
Ca1—O32.3277 (14)Ca2—P1ix3.2119 (6)
Ca1—O3i2.3277 (14)P1—O3iii1.5340 (14)
Ca1—O3ii2.5273 (15)P1—O3ii1.5340 (14)
Ca1—O3iii2.5273 (15)P1—O2x1.534 (2)
Ca1—Cl12.7973 (9)P1—O4ix1.5456 (19)
Ca1—Cl1i2.7973 (9)P1—Ca2i3.2119 (6)
Ca1—O22.981 (2)P1—Ca1ix3.3920 (9)
Ca1—P13.1013 (9)O2—P1xi1.5341 (19)
Ca1—Cl1iv3.2397 (12)O2—Ca2viii2.4021 (14)
Ca1—Cl1v3.2397 (12)O2—Ca2xii2.4021 (14)
Ca1—P1vi3.3920 (9)O3—P1xiii1.5340 (14)
Ca2—O2iii2.4021 (14)O3—Ca1xiii2.5273 (15)
Ca2—O2vii2.4021 (14)O3—Ca2viii2.7958 (15)
Ca2—O2viii2.4021 (14)O4—P1vi1.5456 (19)
Ca2—O4ix2.4377 (14)O4—Ca2i2.4377 (14)
Ca2—O42.4377 (14)Cl1—Cl1iv0.791 (3)
Ca2—O4vi2.4377 (14)Cl1—Ca1xi2.7973 (9)
Ca2—O3iii2.7958 (15)Cl1—Ca1x2.7973 (9)
Ca2—O3viii2.7958 (15)Cl1—Ca1xiv3.2397 (12)
Ca2—O3vii2.7958 (15)Cl1—Ca1iv3.2397 (12)
Ca2—P13.2119 (6)Cl1—Ca1xv3.2397 (12)
O4—Ca1—O387.32 (4)O2vii—Ca2—P188.52 (4)
O4—Ca1—O3i87.32 (4)O2viii—Ca2—P1165.85 (4)
O3—Ca1—O3i133.25 (8)O4ix—Ca2—P127.66 (4)
O4—Ca1—O3ii75.31 (5)O4—Ca2—P166.82 (4)
O3—Ca1—O3ii140.02 (6)O4vi—Ca2—P199.09 (4)
O3i—Ca1—O3ii82.38 (3)O3iii—Ca2—P128.52 (3)
O4—Ca1—O3iii75.31 (5)O3viii—Ca2—P1122.67 (3)
O3—Ca1—O3iii82.38 (3)O3vii—Ca2—P193.91 (3)
O3i—Ca1—O3iii140.02 (6)O2iii—Ca2—P1vi88.52 (4)
O3ii—Ca1—O3iii58.63 (6)O2vii—Ca2—P1vi165.85 (4)
O4—Ca1—Cl1143.38 (4)O2viii—Ca2—P1vi99.36 (4)
O3—Ca1—Cl1127.59 (5)O4ix—Ca2—P1vi99.09 (4)
O3i—Ca1—Cl176.26 (5)O4—Ca2—P1vi27.66 (4)
O3ii—Ca1—Cl170.27 (4)O4vi—Ca2—P1vi66.82 (4)
O3iii—Ca1—Cl196.57 (4)O3iii—Ca2—P1vi93.91 (3)
O4—Ca1—Cl1i143.38 (4)O3viii—Ca2—P1vi28.52 (3)
O3—Ca1—Cl1i76.26 (5)O3vii—Ca2—P1vi122.67 (3)
O3i—Ca1—Cl1i127.59 (5)P1—Ca2—P1vi94.272 (16)
O3ii—Ca1—Cl1i96.57 (4)O2iii—Ca2—P1ix165.85 (4)
O3iii—Ca1—Cl1i70.27 (4)O2vii—Ca2—P1ix99.36 (4)
Cl1—Ca1—Cl1i54.98 (6)O2viii—Ca2—P1ix88.52 (4)
O4—Ca1—O2104.59 (6)O4ix—Ca2—P1ix66.82 (4)
O3—Ca1—O268.31 (4)O4—Ca2—P1ix99.09 (4)
O3i—Ca1—O268.31 (4)O4vi—Ca2—P1ix27.66 (4)
O3ii—Ca1—O2150.60 (3)O3iii—Ca2—P1ix122.67 (3)
O3iii—Ca1—O2150.60 (3)O3viii—Ca2—P1ix93.91 (3)
Cl1—Ca1—O299.40 (4)O3vii—Ca2—P1ix28.52 (3)
Cl1i—Ca1—O299.40 (4)P1—Ca2—P1ix94.272 (16)
O4—Ca1—P170.31 (5)P1vi—Ca2—P1ix94.272 (16)
O3—Ca1—P1110.81 (4)O3iii—P1—O3ii107.54 (12)
O3i—Ca1—P1110.81 (4)O3iii—P1—O2x112.11 (7)
O3ii—Ca1—P129.44 (3)O3ii—P1—O2x112.11 (7)
O3iii—Ca1—P129.44 (3)O3iii—P1—O4ix106.75 (7)
Cl1—Ca1—P185.112 (17)O3ii—P1—O4ix106.75 (7)
Cl1i—Ca1—P185.112 (17)O2x—P1—O4ix111.25 (11)
O2—Ca1—P1174.90 (4)O3iii—P1—Ca154.06 (6)
O4—Ca1—Cl1iv133.87 (3)O3ii—P1—Ca154.06 (6)
O3—Ca1—Cl1iv138.68 (4)O2x—P1—Ca1136.33 (8)
O3i—Ca1—Cl1iv64.58 (4)O4ix—P1—Ca1112.43 (8)
O3ii—Ca1—Cl1iv65.73 (3)O3iii—P1—Ca260.50 (6)
O3iii—Ca1—Cl1iv102.62 (4)O3ii—P1—Ca2111.52 (6)
Cl1—Ca1—Cl1iv12.52 (5)O2x—P1—Ca2135.65 (5)
Cl1i—Ca1—Cl1iv67.501 (14)O4ix—P1—Ca247.07 (5)
O2—Ca1—Cl1iv98.11 (3)Ca1—P1—Ca278.197 (16)
P1—Ca1—Cl1iv85.781 (15)O3iii—P1—Ca2i111.52 (6)
O4—Ca1—Cl1v133.87 (3)O3ii—P1—Ca2i60.50 (6)
O3—Ca1—Cl1v64.58 (4)O2x—P1—Ca2i135.65 (5)
O3i—Ca1—Cl1v138.68 (4)O4ix—P1—Ca2i47.07 (5)
O3ii—Ca1—Cl1v102.62 (4)Ca1—P1—Ca2i78.197 (16)
O3iii—Ca1—Cl1v65.73 (3)Ca2—P1—Ca2i64.36 (2)
Cl1—Ca1—Cl1v67.501 (14)O3iii—P1—Ca1ix122.06 (6)
Cl1i—Ca1—Cl1v12.52 (5)O3ii—P1—Ca1ix122.06 (6)
O2—Ca1—Cl1v98.11 (3)O2x—P1—Ca1ix76.52 (8)
P1—Ca1—Cl1v85.781 (15)Ca1—P1—Ca1ix147.15 (3)
Cl1iv—Ca1—Cl1v80.02 (5)Ca2—P1—Ca1ix74.119 (15)
O4—Ca1—P1vi22.54 (5)Ca2i—P1—Ca1ix74.119 (15)
O3—Ca1—P1vi78.80 (4)O3iii—P1—Ca1x80.29 (6)
O3i—Ca1—P1vi78.80 (4)O3ii—P1—Ca1x80.29 (6)
O3ii—Ca1—P1vi94.91 (4)O2x—P1—Ca1x56.13 (7)
O3iii—Ca1—P1vi94.91 (4)O4ix—P1—Ca1x167.38 (8)
Cl1—Ca1—P1vi152.39 (3)Ca1—P1—Ca1x80.19 (2)
Cl1i—Ca1—P1vi152.39 (3)Ca2—P1—Ca1x140.753 (16)
O2—Ca1—P1vi82.05 (4)Ca2i—P1—Ca1x140.753 (16)
P1—Ca1—P1vi92.85 (3)Ca1ix—P1—Ca1x132.66 (3)
Cl1iv—Ca1—P1vi139.92 (2)P1xi—O2—Ca2viii133.51 (5)
Cl1v—Ca1—P1vi139.92 (2)P1xi—O2—Ca2xii133.51 (5)
O2iii—Ca2—O2vii77.33 (5)Ca2viii—O2—Ca2xii87.65 (7)
O2iii—Ca2—O2viii77.33 (5)P1xi—O2—Ca198.57 (9)
O2vii—Ca2—O2viii77.33 (5)Ca2viii—O2—Ca196.36 (5)
O2iii—Ca2—O4ix126.45 (6)Ca2xii—O2—Ca196.36 (5)
O2vii—Ca2—O4ix89.81 (4)P1xiii—O3—Ca1138.91 (8)
O2viii—Ca2—O4ix150.11 (6)P1xiii—O3—Ca1xiii96.50 (7)
O2iii—Ca2—O489.81 (4)Ca1—O3—Ca1xiii119.18 (6)
O2vii—Ca2—O4150.11 (6)P1xiii—O3—Ca2viii90.98 (7)
O2viii—Ca2—O4126.45 (6)Ca1—O3—Ca2viii103.37 (6)
O4ix—Ca2—O476.19 (5)Ca1xiii—O3—Ca2viii96.73 (5)
O2iii—Ca2—O4vi150.11 (6)P1vi—O4—Ca1122.74 (11)
O2vii—Ca2—O4vi126.45 (6)P1vi—O4—Ca2i105.27 (7)
O2viii—Ca2—O4vi89.81 (4)Ca1—O4—Ca2i114.48 (6)
O4ix—Ca2—O4vi76.19 (5)P1vi—O4—Ca2105.27 (7)
O4—Ca2—O4vi76.19 (5)Ca1—O4—Ca2114.48 (6)
O2iii—Ca2—O3iii70.84 (5)Ca2i—O4—Ca289.14 (7)
O2vii—Ca2—O3iii81.95 (5)Cl1iv—Cl1—Ca1xi117.49 (3)
O2viii—Ca2—O3iii145.07 (5)Cl1iv—Cl1—Ca1117.49 (3)
O4ix—Ca2—O3iii55.86 (5)Ca1xi—Cl1—Ca1100.39 (4)
O4—Ca2—O3iii68.30 (5)Cl1iv—Cl1—Ca1x117.49 (3)
O4vi—Ca2—O3iii125.07 (5)Ca1xi—Cl1—Ca1x100.39 (4)
O2iii—Ca2—O3viii81.95 (5)Ca1—Cl1—Ca1x100.39 (4)
O2vii—Ca2—O3viii145.07 (5)Cl1iv—Cl1—Ca1xiv49.99 (2)
O2viii—Ca2—O3viii70.84 (5)Ca1xi—Cl1—Ca1xiv167.48 (5)
O4ix—Ca2—O3viii125.07 (5)Ca1—Cl1—Ca1xiv87.539 (11)
O4—Ca2—O3viii55.86 (5)Ca1x—Cl1—Ca1xiv87.539 (11)
O4vi—Ca2—O3viii68.30 (5)Cl1iv—Cl1—Ca1iv49.99 (2)
O3iii—Ca2—O3viii117.195 (18)Ca1xi—Cl1—Ca1iv87.539 (11)
O2iii—Ca2—O3vii145.07 (5)Ca1—Cl1—Ca1iv167.48 (5)
O2vii—Ca2—O3vii70.84 (5)Ca1x—Cl1—Ca1iv87.539 (11)
O2viii—Ca2—O3vii81.95 (5)Ca1xiv—Cl1—Ca1iv83.11 (4)
O4ix—Ca2—O3vii68.30 (5)Cl1iv—Cl1—Ca1xv49.99 (3)
O4—Ca2—O3vii125.07 (5)Ca1xi—Cl1—Ca1xv87.539 (11)
O4vi—Ca2—O3vii55.86 (5)Ca1—Cl1—Ca1xv87.539 (11)
O3iii—Ca2—O3vii117.195 (18)Ca1x—Cl1—Ca1xv167.48 (5)
O3viii—Ca2—O3vii117.195 (18)Ca1xiv—Cl1—Ca1xv83.11 (4)
O2iii—Ca2—P199.36 (4)Ca1iv—Cl1—Ca1xv83.11 (4)
O4—Ca1—P1—O3iii94.93 (7)O3iii—Ca1—O2—Ca2viii41.70 (12)
O3—Ca1—P1—O3iii15.83 (6)Cl1—Ca1—O2—Ca2viii163.73 (5)
O3i—Ca1—P1—O3iii174.04 (10)Cl1i—Ca1—O2—Ca2viii107.93 (5)
O3ii—Ca1—P1—O3iii170.13 (14)Cl1iv—Ca1—O2—Ca2viii176.33 (4)
Cl1—Ca1—P1—O3iii112.67 (8)Cl1v—Ca1—O2—Ca2viii95.34 (5)
Cl1i—Ca1—P1—O3iii57.46 (8)O4—Ca1—O2—Ca2xii44.17 (4)
Cl1iv—Ca1—P1—O3iii125.21 (7)O3—Ca1—O2—Ca2xii125.23 (7)
Cl1v—Ca1—P1—O3iii44.93 (7)O3i—Ca1—O2—Ca2xii36.89 (4)
P1vi—Ca1—P1—O3iii94.93 (7)O3ii—Ca1—O2—Ca2xii41.70 (12)
O4—Ca1—P1—O3ii94.93 (7)O3iii—Ca1—O2—Ca2xii130.04 (8)
O3—Ca1—P1—O3ii174.04 (10)Cl1—Ca1—O2—Ca2xii107.93 (5)
O3i—Ca1—P1—O3ii15.83 (6)Cl1i—Ca1—O2—Ca2xii163.73 (5)
O3iii—Ca1—P1—O3ii170.13 (14)Cl1iv—Ca1—O2—Ca2xii95.34 (5)
Cl1—Ca1—P1—O3ii57.46 (8)Cl1v—Ca1—O2—Ca2xii176.33 (4)
Cl1i—Ca1—P1—O3ii112.67 (8)P1vi—Ca1—O2—Ca2xii44.17 (4)
Cl1iv—Ca1—P1—O3ii44.93 (7)O4—Ca1—O3—P1xiii32.35 (14)
Cl1v—Ca1—P1—O3ii125.21 (7)O3i—Ca1—O3—P1xiii116.14 (12)
P1vi—Ca1—P1—O3ii94.93 (7)O3ii—Ca1—O3—P1xiii30.8 (2)
O4—Ca1—P1—O2x180O3iii—Ca1—O3—P1xiii43.18 (16)
O3—Ca1—P1—O2x100.90 (4)Cl1—Ca1—O3—P1xiii135.63 (12)
O3i—Ca1—P1—O2x100.90 (4)Cl1i—Ca1—O3—P1xiii114.64 (14)
O3ii—Ca1—P1—O2x85.07 (7)O2—Ca1—O3—P1xiii139.21 (15)
O3iii—Ca1—P1—O2x85.07 (7)P1—Ca1—O3—P1xiii35.40 (15)
Cl1—Ca1—P1—O2x27.60 (3)Cl1iv—Ca1—O3—P1xiii143.64 (11)
Cl1i—Ca1—P1—O2x27.60 (3)Cl1v—Ca1—O3—P1xiii109.87 (14)
Cl1iv—Ca1—P1—O2x40.14 (2)P1vi—Ca1—O3—P1xiii53.39 (13)
Cl1v—Ca1—P1—O2x40.14 (2)O4—Ca1—O3—Ca1xiii179.24 (8)
P1vi—Ca1—P1—O2x180O3i—Ca1—O3—Ca1xiii96.98 (11)
O4—Ca1—P1—O4ix0O3ii—Ca1—O3—Ca1xiii116.04 (5)
O3—Ca1—P1—O4ix79.10 (4)O3iii—Ca1—O3—Ca1xiii103.71 (4)
O3i—Ca1—P1—O4ix79.10 (4)Cl1—Ca1—O3—Ca1xiii11.26 (9)
O3ii—Ca1—P1—O4ix94.93 (7)Cl1i—Ca1—O3—Ca1xiii32.24 (6)
O3iii—Ca1—P1—O4ix94.93 (7)O2—Ca1—O3—Ca1xiii73.91 (7)
Cl1—Ca1—P1—O4ix152.40 (3)P1—Ca1—O3—Ca1xiii111.48 (5)
Cl1i—Ca1—P1—O4ix152.40 (3)Cl1iv—Ca1—O3—Ca1xiii3.24 (11)
Cl1iv—Ca1—P1—O4ix139.86 (2)Cl1v—Ca1—O3—Ca1xiii37.01 (5)
Cl1v—Ca1—P1—O4ix139.86 (2)P1vi—Ca1—O3—Ca1xiii159.72 (7)
P1vi—Ca1—P1—O4ix0O4—Ca1—O3—Ca2viii75.06 (6)
O4—Ca1—P1—Ca232.964 (11)O3i—Ca1—O3—Ca2viii8.73 (12)
O3—Ca1—P1—Ca246.14 (4)O3ii—Ca1—O3—Ca2viii138.26 (9)
O3i—Ca1—P1—Ca2112.07 (4)O3iii—Ca1—O3—Ca2viii150.59 (5)
O3ii—Ca1—P1—Ca2127.90 (7)Cl1—Ca1—O3—Ca2viii116.96 (5)
O3iii—Ca1—P1—Ca261.97 (7)Cl1i—Ca1—O3—Ca2viii137.95 (4)
Cl1—Ca1—P1—Ca2174.64 (3)O2—Ca1—O3—Ca2viii31.79 (5)
Cl1i—Ca1—P1—Ca2119.43 (3)P1—Ca1—O3—Ca2viii142.81 (3)
Cl1iv—Ca1—P1—Ca2172.83 (3)Cl1iv—Ca1—O3—Ca2viii108.94 (6)
Cl1v—Ca1—P1—Ca2106.90 (3)Cl1v—Ca1—O3—Ca2viii142.72 (5)
P1vi—Ca1—P1—Ca232.964 (11)P1vi—Ca1—O3—Ca2viii54.02 (4)
O4—Ca1—P1—Ca2i32.964 (11)O3—Ca1—O4—P1vi66.77 (4)
O3—Ca1—P1—Ca2i112.07 (4)O3i—Ca1—O4—P1vi66.77 (4)
O3i—Ca1—P1—Ca2i46.14 (4)O3ii—Ca1—O4—P1vi149.59 (3)
O3ii—Ca1—P1—Ca2i61.97 (7)O3iii—Ca1—O4—P1vi149.59 (3)
O3iii—Ca1—P1—Ca2i127.90 (7)Cl1—Ca1—O4—P1vi129.29 (7)
Cl1—Ca1—P1—Ca2i119.43 (3)Cl1i—Ca1—O4—P1vi129.29 (7)
Cl1i—Ca1—P1—Ca2i174.64 (3)O2—Ca1—O4—P1vi0
Cl1iv—Ca1—P1—Ca2i106.90 (3)P1—Ca1—O4—P1vi180
Cl1v—Ca1—P1—Ca2i172.82 (3)Cl1iv—Ca1—O4—P1vi116.90 (5)
P1vi—Ca1—P1—Ca2i32.964 (11)Cl1v—Ca1—O4—P1vi116.90 (5)
O4—Ca1—P1—Ca1ix0O3—Ca1—O4—Ca2i163.68 (7)
O3—Ca1—P1—Ca1ix79.10 (4)O3i—Ca1—O4—Ca2i62.78 (7)
O3i—Ca1—P1—Ca1ix79.10 (4)O3ii—Ca1—O4—Ca2i20.04 (6)
O3ii—Ca1—P1—Ca1ix94.93 (7)O3iii—Ca1—O4—Ca2i80.86 (7)
O3iii—Ca1—P1—Ca1ix94.93 (7)Cl1—Ca1—O4—Ca2i0.26 (11)
Cl1—Ca1—P1—Ca1ix152.40 (3)Cl1i—Ca1—O4—Ca2i101.16 (5)
Cl1i—Ca1—P1—Ca1ix152.40 (3)O2—Ca1—O4—Ca2i129.55 (6)
Cl1iv—Ca1—P1—Ca1ix139.86 (2)P1—Ca1—O4—Ca2i50.45 (6)
Cl1v—Ca1—P1—Ca1ix139.86 (2)Cl1iv—Ca1—O4—Ca2i12.65 (10)
P1vi—Ca1—P1—Ca1ix0Cl1v—Ca1—O4—Ca2i113.55 (3)
O4—Ca1—P1—Ca1x180P1vi—Ca1—O4—Ca2i129.55 (6)
O3—Ca1—P1—Ca1x100.90 (4)O3—Ca1—O4—Ca262.78 (7)
O3i—Ca1—P1—Ca1x100.90 (4)O3i—Ca1—O4—Ca2163.68 (7)
O3ii—Ca1—P1—Ca1x85.07 (7)O3ii—Ca1—O4—Ca280.86 (7)
O3iii—Ca1—P1—Ca1x85.07 (7)O3iii—Ca1—O4—Ca220.04 (6)
Cl1—Ca1—P1—Ca1x27.60 (3)Cl1—Ca1—O4—Ca2101.16 (5)
Cl1i—Ca1—P1—Ca1x27.60 (3)Cl1i—Ca1—O4—Ca20.26 (11)
Cl1iv—Ca1—P1—Ca1x40.14 (2)O2—Ca1—O4—Ca2129.55 (6)
Cl1v—Ca1—P1—Ca1x40.14 (2)P1—Ca1—O4—Ca250.45 (6)
P1vi—Ca1—P1—Ca1x180Cl1iv—Ca1—O4—Ca2113.55 (3)
O2iii—Ca2—P1—O3iii1.14 (8)Cl1v—Ca1—O4—Ca212.65 (10)
O2vii—Ca2—P1—O3iii75.77 (8)P1vi—Ca1—O4—Ca2129.55 (6)
O2viii—Ca2—P1—O3iii74.06 (19)O2iii—Ca2—O4—P1vi87.17 (8)
O4ix—Ca2—P1—O3iii168.19 (10)O2vii—Ca2—O4—P1vi150.70 (9)
O4—Ca2—P1—O3iii86.88 (7)O2viii—Ca2—O4—P1vi13.14 (10)
O4vi—Ca2—P1—O3iii157.52 (8)O4ix—Ca2—O4—P1vi145.05 (8)
O3viii—Ca2—P1—O3iii87.53 (3)O4vi—Ca2—O4—P1vi66.16 (10)
O3vii—Ca2—P1—O3iii146.45 (7)O3iii—Ca2—O4—P1vi156.57 (8)
P1vi—Ca2—P1—O3iii90.34 (7)O3viii—Ca2—O4—P1vi6.78 (6)
P1ix—Ca2—P1—O3iii175.04 (7)O3vii—Ca2—O4—P1vi94.67 (8)
O2iii—Ca2—P1—O3ii97.45 (8)P1—Ca2—O4—P1vi172.56 (8)
O2vii—Ca2—P1—O3ii174.35 (8)P1ix—Ca2—O4—P1vi81.78 (6)
O2viii—Ca2—P1—O3ii172.64 (18)O2iii—Ca2—O4—Ca150.58 (7)
O4ix—Ca2—P1—O3ii93.23 (10)O2vii—Ca2—O4—Ca112.95 (14)
O4—Ca2—P1—O3ii11.70 (8)O2viii—Ca2—O4—Ca1124.61 (7)
O4vi—Ca2—P1—O3ii58.94 (8)O4ix—Ca2—O4—Ca177.20 (10)
O3iii—Ca2—P1—O3ii98.58 (12)O4vi—Ca2—O4—Ca1156.09 (8)
O3viii—Ca2—P1—O3ii11.05 (10)O3iii—Ca2—O4—Ca118.81 (5)
O3vii—Ca2—P1—O3ii114.97 (7)O3viii—Ca2—O4—Ca1130.97 (8)
P1vi—Ca2—P1—O3ii8.24 (7)O3vii—Ca2—O4—Ca1127.57 (5)
P1ix—Ca2—P1—O3ii86.38 (7)P1—Ca2—O4—Ca149.69 (5)
O2iii—Ca2—P1—O2x93.42 (11)P1vi—Ca2—O4—Ca1137.75 (11)
O2vii—Ca2—P1—O2x16.51 (12)P1ix—Ca2—O4—Ca1140.46 (5)
O2viii—Ca2—P1—O2x18.22 (16)O2iii—Ca2—O4—Ca2i167.22 (6)
O4ix—Ca2—P1—O2x75.90 (12)O2vii—Ca2—O4—Ca2i103.70 (10)
O4—Ca2—P1—O2x179.17 (10)O2viii—Ca2—O4—Ca2i118.74 (6)
O4vi—Ca2—P1—O2x110.20 (10)O4ix—Ca2—O4—Ca2i39.445 (16)
O3iii—Ca2—P1—O2x92.28 (10)O4vi—Ca2—O4—Ca2i39.445 (16)
O3viii—Ca2—P1—O2x179.81 (9)O3iii—Ca2—O4—Ca2i97.83 (6)
O3vii—Ca2—P1—O2x54.17 (9)O3viii—Ca2—O4—Ca2i112.39 (7)
P1vi—Ca2—P1—O2x177.38 (9)O3vii—Ca2—O4—Ca2i10.93 (8)
P1ix—Ca2—P1—O2x82.76 (9)P1—Ca2—O4—Ca2i66.95 (4)
O2iii—Ca2—P1—O4ix169.32 (8)P1vi—Ca2—O4—Ca2i105.60 (9)
O2vii—Ca2—P1—O4ix92.42 (8)P1ix—Ca2—O4—Ca2i23.82 (5)
O2viii—Ca2—P1—O4ix94.13 (19)O4—Ca1—Cl1—Cl1iv45.55 (8)
O4—Ca2—P1—O4ix104.93 (11)O3—Ca1—Cl1—Cl1iv154.86 (5)
O4vi—Ca2—P1—O4ix34.29 (8)O3i—Ca1—Cl1—Cl1iv20.27 (4)
O3iii—Ca2—P1—O4ix168.19 (10)O3ii—Ca1—Cl1—Cl1iv66.44 (4)
O3viii—Ca2—P1—O4ix104.28 (8)O3iii—Ca1—Cl1—Cl1iv119.71 (3)
O3vii—Ca2—P1—O4ix21.74 (8)Cl1i—Ca1—Cl1—Cl1iv180.0000 (10)
P1vi—Ca2—P1—O4ix101.47 (7)O2—Ca1—Cl1—Cl1iv85.06 (2)
P1ix—Ca2—P1—O4ix6.86 (7)P1—Ca1—Cl1—Cl1iv92.551 (10)
O2iii—Ca2—P1—Ca154.07 (4)Cl1v—Ca1—Cl1—Cl1iv180.0000 (10)
O2vii—Ca2—P1—Ca1130.97 (4)P1vi—Ca1—Cl1—Cl1iv5.75 (5)
O2viii—Ca2—P1—Ca1129.26 (18)O4—Ca1—Cl1—Ca1xi174.19 (7)
O4ix—Ca2—P1—Ca1136.61 (7)O3—Ca1—Cl1—Ca1xi26.22 (6)
O4—Ca2—P1—Ca131.68 (4)O3i—Ca1—Cl1—Ca1xi108.37 (5)
O4vi—Ca2—P1—Ca1102.32 (4)O3ii—Ca1—Cl1—Ca1xi164.92 (5)
O3iii—Ca2—P1—Ca155.20 (6)O3iii—Ca1—Cl1—Ca1xi111.64 (4)
O3viii—Ca2—P1—Ca132.33 (4)Cl1i—Ca1—Cl1—Ca1xi51.36 (3)
O3vii—Ca2—P1—Ca1158.35 (3)O2—Ca1—Cl1—Ca1xi43.59 (4)
P1vi—Ca2—P1—Ca135.136 (14)P1—Ca1—Cl1—Ca1xi138.80 (3)
P1ix—Ca2—P1—Ca1129.752 (13)Cl1iv—Ca1—Cl1—Ca1xi128.64 (3)
O2iii—Ca2—P1—Ca2i136.51 (4)Cl1v—Ca1—Cl1—Ca1xi51.36 (3)
O2vii—Ca2—P1—Ca2i146.58 (4)P1vi—Ca1—Cl1—Ca1xi134.40 (6)
O2viii—Ca2—P1—Ca2i148.29 (17)O4—Ca1—Cl1—Ca1x83.10 (9)
O4ix—Ca2—P1—Ca2i54.17 (7)O3—Ca1—Cl1—Ca1x76.49 (5)
O4—Ca2—P1—Ca2i50.77 (4)O3i—Ca1—Cl1—Ca1x148.92 (5)
O4vi—Ca2—P1—Ca2i19.87 (4)O3ii—Ca1—Cl1—Ca1x62.21 (4)
O3iii—Ca2—P1—Ca2i137.65 (7)O3iii—Ca1—Cl1—Ca1x8.93 (5)
O3viii—Ca2—P1—Ca2i50.12 (4)Cl1i—Ca1—Cl1—Ca1x51.36 (3)
O3vii—Ca2—P1—Ca2i75.90 (3)O2—Ca1—Cl1—Ca1x146.30 (3)
P1vi—Ca2—P1—Ca2i47.308 (9)P1—Ca1—Cl1—Ca1x36.09 (3)
P1ix—Ca2—P1—Ca2i47.308 (9)Cl1iv—Ca1—Cl1—Ca1x128.64 (3)
O2iii—Ca2—P1—Ca1ix143.80 (4)Cl1v—Ca1—Cl1—Ca1x51.36 (3)
O2vii—Ca2—P1—Ca1ix66.90 (4)P1vi—Ca1—Cl1—Ca1x122.89 (6)
O2viii—Ca2—P1—Ca1ix68.61 (18)O4—Ca1—Cl1—Ca1xiv3.95 (8)
O4ix—Ca2—P1—Ca1ix25.52 (7)O3—Ca1—Cl1—Ca1xiv163.54 (5)
O4—Ca2—P1—Ca1ix130.45 (4)O3i—Ca1—Cl1—Ca1xiv61.88 (4)
O4vi—Ca2—P1—Ca1ix59.81 (4)O3ii—Ca1—Cl1—Ca1xiv24.84 (4)
O3iii—Ca2—P1—Ca1ix142.67 (6)O3iii—Ca1—Cl1—Ca1xiv78.11 (4)
O3viii—Ca2—P1—Ca1ix129.80 (4)Cl1i—Ca1—Cl1—Ca1xiv138.399 (18)
O3vii—Ca2—P1—Ca1ix3.78 (3)O2—Ca1—Cl1—Ca1xiv126.66 (2)
P1vi—Ca2—P1—Ca1ix126.995 (13)P1—Ca1—Cl1—Ca1xiv50.949 (16)
P1ix—Ca2—P1—Ca1ix32.378 (13)Cl1iv—Ca1—Cl1—Ca1xiv41.601 (19)
O2iii—Ca2—P1—Ca1x3.87 (5)Cl1v—Ca1—Cl1—Ca1xiv138.399 (18)
O2vii—Ca2—P1—Ca1x73.04 (5)P1vi—Ca1—Cl1—Ca1xiv35.85 (6)
O2viii—Ca2—P1—Ca1x71.33 (18)O4—Ca1—Cl1—Ca1iv45.55 (8)
O4ix—Ca2—P1—Ca1x165.45 (8)O3—Ca1—Cl1—Ca1iv154.86 (5)
O4—Ca2—P1—Ca1x89.62 (5)O3i—Ca1—Cl1—Ca1iv20.27 (4)
O4vi—Ca2—P1—Ca1x160.26 (5)O3ii—Ca1—Cl1—Ca1iv66.44 (4)
O3iii—Ca2—P1—Ca1x2.73 (6)O3iii—Ca1—Cl1—Ca1iv119.71 (3)
O3viii—Ca2—P1—Ca1x90.26 (5)Cl1i—Ca1—Cl1—Ca1iv180.0000 (10)
O3vii—Ca2—P1—Ca1x143.71 (4)O2—Ca1—Cl1—Ca1iv85.06 (2)
P1vi—Ca2—P1—Ca1x93.07 (4)P1—Ca1—Cl1—Ca1iv92.551 (9)
P1ix—Ca2—P1—Ca1x172.31 (4)Cl1iv—Ca1—Cl1—Ca1iv0
O4—Ca1—O2—P1xi180Cl1v—Ca1—Cl1—Ca1iv180.0000 (10)
O3—Ca1—O2—P1xi98.94 (4)P1vi—Ca1—Cl1—Ca1iv5.75 (5)
O3i—Ca1—O2—P1xi98.94 (4)O4—Ca1—Cl1—Ca1xv87.15 (7)
O3ii—Ca1—O2—P1xi94.13 (10)O3—Ca1—Cl1—Ca1xv113.26 (5)
O3iii—Ca1—O2—P1xi94.13 (10)O3i—Ca1—Cl1—Ca1xv21.33 (4)
Cl1—Ca1—O2—P1xi27.90 (3)O3ii—Ca1—Cl1—Ca1xv108.04 (5)
Cl1i—Ca1—O2—P1xi27.90 (3)O3iii—Ca1—Cl1—Ca1xv161.31 (4)
Cl1iv—Ca1—O2—P1xi40.50 (2)Cl1i—Ca1—Cl1—Ca1xv138.399 (18)
Cl1v—Ca1—O2—P1xi40.50 (2)O2—Ca1—Cl1—Ca1xv43.45 (3)
O4—Ca1—O2—Ca2viii44.17 (4)P1—Ca1—Cl1—Ca1xv134.15 (2)
O3—Ca1—O2—Ca2viii36.89 (4)Cl1iv—Ca1—Cl1—Ca1xv41.601 (19)
O3i—Ca1—O2—Ca2viii125.23 (7)Cl1v—Ca1—Cl1—Ca1xv138.399 (18)
O3ii—Ca1—O2—Ca2viii130.04 (8)P1vi—Ca1—Cl1—Ca1xv47.35 (5)
Symmetry codes: (i) x, y, z+1/2; (ii) xy+1, x+1, z+1/2; (iii) xy+1, x+1, z; (iv) x, y+2, z+1; (v) x, y+2, z1/2; (vi) y+1, xy+1, z; (vii) y, x+y, z; (viii) x, y+1, z; (ix) x+y, x+1, z; (x) y+1, xy+2, z; (xi) x+y1, x+1, z; (xii) x, y+1, z+1/2; (xiii) y1, x+y, z; (xiv) xy+1, x+1, z+1; (xv) y1, x+y, z+1.
(2_low_prism) chlorapatite top
Crystal data top
3(O4P)·Cl·5(Ca)Dx = 3.19 Mg m3
Mr = 520.76Mo Kα radiation, λ = 0.7107 Å
Trigonal, P63/mCell parameters from 1988 reflections
Hall symbol: -P 6cθ = 2.4–27.1°
a = 9.6341 (1) ŵ = 3.23 mm1
c = 6.7445 (2) ÅT = 100 K
V = 542.13 (2) Å3Prism, colourless
Z = 20.17 × 0.07 × 0.05 mm
F(000) = 516
Data collection top
BRUKER APPEX-II CCD
diffractometer
403 independent reflections
Radiation source: fine-focus sealed tube401 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.033
ω and phi scansθmax = 26.3°, θmin = 2.4°
Absorption correction: multi-scan
BRUKER SADABS
h = 012
Tmin = 0.666, Tmax = 1k = 120
6361 measured reflectionsl = 80
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.023 w = 1/[σ2(Fo2) + (0.0305P)2 + 0.5632P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.060(Δ/σ)max < 0.001
S = 1.30Δρmax = 0.40 e Å3
403 reflectionsΔρmin = 0.52 e Å3
41 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.161 (8)
Crystal data top
3(O4P)·Cl·5(Ca)Z = 2
Mr = 520.76Mo Kα radiation
Trigonal, P63/mµ = 3.23 mm1
a = 9.6341 (1) ÅT = 100 K
c = 6.7445 (2) Å0.17 × 0.07 × 0.05 mm
V = 542.13 (2) Å3
Data collection top
BRUKER APPEX-II CCD
diffractometer
403 independent reflections
Absorption correction: multi-scan
BRUKER SADABS
401 reflections with I > 2σ(I)
Tmin = 0.666, Tmax = 1Rint = 0.033
6361 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.02341 parameters
wR(F2) = 0.0600 restraints
S = 1.30Δρmax = 0.40 e Å3
403 reflectionsΔρmin = 0.52 e Å3
Special details top

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ca10.00589 (7)0.74541 (7)0.250.0064 (3)
Ca20.33330.66670.00348 (10)0.0069 (3)
P10.37485 (9)0.96724 (8)0.250.0049 (3)
O20.3439 (3)0.5077 (2)0.250.0085 (5)
O30.08684 (18)0.6471 (2)0.0665 (2)0.0133 (4)
O40.1278 (2)0.5930 (2)0.250.0091 (5)
Cl1010.4417 (3)0.0170 (5)0.5
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0071 (4)0.0068 (4)0.0061 (4)0.0041 (3)00
Ca20.0080 (3)0.0080 (3)0.0049 (4)0.00398 (16)00
P10.0044 (4)0.0041 (4)0.0061 (4)0.0020 (3)00
O20.0108 (11)0.0083 (10)0.0096 (11)0.0072 (8)00
O30.0087 (7)0.0199 (8)0.0137 (9)0.0089 (7)0.0031 (6)0.0093 (7)
O40.0067 (10)0.0047 (10)0.0158 (11)0.0028 (8)00
Cl10.0089 (5)0.0089 (5)0.0331 (14)0.0045 (2)00
Geometric parameters (Å, º) top
Ca1—O42.294 (2)Ca2—P1vi3.2109 (7)
Ca1—O32.3250 (15)Ca2—P1ix3.2109 (7)
Ca1—O3i2.3250 (15)P1—O2x1.533 (2)
Ca1—O3ii2.5251 (16)P1—O3iii1.5348 (15)
Ca1—O3iii2.5251 (16)P1—O3ii1.5348 (15)
Ca1—Cl12.7983 (11)P1—O4ix1.547 (2)
Ca1—Cl1i2.7983 (11)P1—Ca2i3.2109 (7)
Ca1—O22.980 (2)P1—Ca1ix3.3912 (9)
Ca1—P13.0994 (9)O2—P1xi1.533 (2)
Ca1—Cl1iv3.2374 (14)O2—Ca2viii2.4017 (15)
Ca1—Cl1v3.2374 (14)O2—Ca2xii2.4017 (15)
Ca1—P1vi3.3912 (9)O3—P1xiii1.5348 (15)
Ca2—O2iii2.4017 (15)O3—Ca1xiii2.5251 (16)
Ca2—O2vii2.4017 (15)O3—Ca2viii2.7965 (17)
Ca2—O2viii2.4017 (15)O4—P1vi1.547 (2)
Ca2—O4ix2.4377 (15)O4—Ca2i2.4377 (15)
Ca2—O42.4377 (15)Cl1—Cl1iv0.786 (4)
Ca2—O4vi2.4377 (15)Cl1—Ca1xi2.7983 (11)
Ca2—O3iii2.7965 (17)Cl1—Ca1x2.7983 (11)
Ca2—O3viii2.7965 (17)Cl1—Ca1xiv3.2374 (13)
Ca2—O3vii2.7965 (17)Cl1—Ca1iv3.2374 (13)
Ca2—P13.2109 (7)Cl1—Ca1xv3.2374 (13)
O4—Ca1—O387.39 (4)O2vii—Ca2—P188.51 (4)
O4—Ca1—O3i87.39 (4)O2viii—Ca2—P1165.86 (5)
O3—Ca1—O3i133.30 (9)O4ix—Ca2—P127.70 (5)
O4—Ca1—O3ii75.38 (6)O4—Ca2—P166.80 (5)
O3—Ca1—O3ii140.09 (6)O4vi—Ca2—P199.16 (4)
O3i—Ca1—O3ii82.36 (3)O3iii—Ca2—P128.55 (3)
O4—Ca1—O3iii75.38 (6)O3viii—Ca2—P1122.72 (4)
O3—Ca1—O3iii82.36 (3)O3vii—Ca2—P193.92 (3)
O3i—Ca1—O3iii140.09 (6)O2iii—Ca2—P1vi88.51 (4)
O3ii—Ca1—O3iii58.70 (7)O2vii—Ca2—P1vi165.86 (5)
O4—Ca1—Cl1143.37 (5)O2viii—Ca2—P1vi99.32 (5)
O3—Ca1—Cl1127.54 (5)O4ix—Ca2—P1vi99.16 (4)
O3i—Ca1—Cl176.16 (5)O4—Ca2—P1vi27.70 (5)
O3ii—Ca1—Cl170.20 (4)O4vi—Ca2—P1vi66.80 (5)
O3iii—Ca1—Cl196.56 (5)O3iii—Ca2—P1vi93.92 (3)
O4—Ca1—Cl1i143.37 (5)O3viii—Ca2—P1vi28.55 (3)
O3—Ca1—Cl1i76.16 (5)O3vii—Ca2—P1vi122.72 (4)
O3i—Ca1—Cl1i127.54 (5)P1—Ca2—P1vi94.288 (17)
O3ii—Ca1—Cl1i96.56 (5)O2iii—Ca2—P1ix165.86 (5)
O3iii—Ca1—Cl1i70.20 (4)O2vii—Ca2—P1ix99.32 (5)
Cl1—Ca1—Cl1i55.05 (7)O2viii—Ca2—P1ix88.51 (4)
O4—Ca1—O2104.61 (7)O4ix—Ca2—P1ix66.80 (5)
O3—Ca1—O268.31 (4)O4—Ca2—P1ix99.16 (4)
O3i—Ca1—O268.31 (4)O4vi—Ca2—P1ix27.70 (5)
O3ii—Ca1—O2150.57 (4)O3iii—Ca2—P1ix122.72 (4)
O3iii—Ca1—O2150.57 (4)O3viii—Ca2—P1ix93.92 (3)
Cl1—Ca1—O299.37 (4)O3vii—Ca2—P1ix28.55 (3)
Cl1i—Ca1—O299.37 (4)P1—Ca2—P1ix94.288 (17)
O4—Ca1—P170.35 (6)P1vi—Ca2—P1ix94.288 (17)
O3—Ca1—P1110.82 (4)O2x—P1—O3iii112.11 (7)
O3i—Ca1—P1110.82 (4)O2x—P1—O3ii112.11 (7)
O3ii—Ca1—P129.47 (3)O3iii—P1—O3ii107.50 (13)
O3iii—Ca1—P129.47 (3)O2x—P1—O4ix111.13 (12)
Cl1—Ca1—P185.095 (18)O3iii—P1—O4ix106.85 (8)
Cl1i—Ca1—P185.095 (18)O3ii—P1—O4ix106.85 (8)
O2—Ca1—P1174.95 (5)O2x—P1—Ca1136.38 (9)
O4—Ca1—Cl1iv133.92 (3)O3iii—P1—Ca154.05 (6)
O3—Ca1—Cl1iv138.55 (5)O3ii—P1—Ca154.05 (6)
O3i—Ca1—Cl1iv64.56 (5)O4ix—P1—Ca1112.49 (8)
O3ii—Ca1—Cl1iv65.68 (4)O2x—P1—Ca2135.63 (6)
O3iii—Ca1—Cl1iv102.58 (4)O3iii—P1—Ca260.56 (6)
Cl1—Ca1—Cl1iv12.43 (6)O3ii—P1—Ca2111.54 (6)
Cl1i—Ca1—Cl1iv67.480 (15)O4ix—P1—Ca247.11 (5)
O2—Ca1—Cl1iv98.09 (3)Ca1—P1—Ca278.192 (17)
P1—Ca1—Cl1iv85.762 (16)O2x—P1—Ca2i135.63 (6)
O4—Ca1—Cl1v133.92 (3)O3iii—P1—Ca2i111.54 (6)
O3—Ca1—Cl1v64.56 (5)O3ii—P1—Ca2i60.56 (6)
O3i—Ca1—Cl1v138.55 (5)O4ix—P1—Ca2i47.11 (5)
O3ii—Ca1—Cl1v102.58 (4)Ca1—P1—Ca2i78.192 (17)
O3iii—Ca1—Cl1v65.68 (4)Ca2—P1—Ca2i64.34 (3)
Cl1—Ca1—Cl1v67.480 (15)O2x—P1—Ca1ix76.50 (8)
Cl1i—Ca1—Cl1v12.43 (6)O3iii—P1—Ca1ix122.10 (7)
O2—Ca1—Cl1v98.09 (3)O3ii—P1—Ca1ix122.10 (7)
P1—Ca1—Cl1v85.762 (16)Ca1—P1—Ca1ix147.12 (3)
Cl1iv—Ca1—Cl1v79.91 (6)Ca2—P1—Ca1ix74.097 (17)
O4—Ca1—P1vi22.53 (5)Ca2i—P1—Ca1ix74.097 (17)
O3—Ca1—P1vi78.88 (4)O2x—P1—Ca1x56.13 (8)
O3i—Ca1—P1vi78.88 (4)O3iii—P1—Ca1x80.27 (7)
O3ii—Ca1—P1vi94.96 (4)O3ii—P1—Ca1x80.27 (7)
O3iii—Ca1—P1vi94.96 (4)O4ix—P1—Ca1x167.26 (8)
Cl1—Ca1—P1vi152.36 (4)Ca1—P1—Ca1x80.24 (3)
Cl1i—Ca1—P1vi152.36 (4)Ca2—P1—Ca1x140.788 (17)
O2—Ca1—P1vi82.08 (4)Ca2i—P1—Ca1x140.788 (17)
P1—Ca1—P1vi92.88 (3)Ca1ix—P1—Ca1x132.63 (3)
Cl1iv—Ca1—P1vi139.97 (3)P1xi—O2—Ca2viii133.53 (5)
Cl1v—Ca1—P1vi139.97 (3)P1xi—O2—Ca2xii133.53 (5)
O2iii—Ca2—O2vii77.36 (6)Ca2viii—O2—Ca2xii87.62 (7)
O2iii—Ca2—O2viii77.36 (6)P1xi—O2—Ca198.58 (10)
O2vii—Ca2—O2viii77.36 (6)Ca2viii—O2—Ca196.34 (6)
O2iii—Ca2—O4ix126.45 (7)Ca2xii—O2—Ca196.34 (6)
O2vii—Ca2—O4ix89.76 (5)P1xiii—O3—Ca1138.85 (9)
O2viii—Ca2—O4ix150.08 (7)P1xiii—O3—Ca1xiii96.48 (8)
O2iii—Ca2—O489.76 (5)Ca1—O3—Ca1xiii119.31 (6)
O2vii—Ca2—O4150.08 (7)P1xiii—O3—Ca2viii90.89 (7)
O2viii—Ca2—O4126.45 (7)Ca1—O3—Ca2viii103.36 (6)
O4ix—Ca2—O476.24 (5)Ca1xiii—O3—Ca2viii96.69 (5)
O2iii—Ca2—O4vi150.08 (7)P1vi—O4—Ca1122.84 (11)
O2vii—Ca2—O4vi126.45 (7)P1vi—O4—Ca2i105.19 (8)
O2viii—Ca2—O4vi89.76 (5)Ca1—O4—Ca2i114.51 (6)
O4ix—Ca2—O4vi76.24 (5)P1vi—O4—Ca2105.19 (8)
O4—Ca2—O4vi76.24 (5)Ca1—O4—Ca2114.51 (6)
O2iii—Ca2—O3iii70.78 (5)Ca2i—O4—Ca289.07 (7)
O2vii—Ca2—O3iii81.95 (6)Cl1iv—Cl1—Ca1xi117.52 (4)
O2viii—Ca2—O3iii145.05 (5)Cl1iv—Cl1—Ca1117.52 (4)
O4ix—Ca2—O3iii55.92 (6)Ca1xi—Cl1—Ca1100.35 (5)
O4—Ca2—O3iii68.26 (6)Cl1iv—Cl1—Ca1x117.52 (4)
O4vi—Ca2—O3iii125.15 (5)Ca1xi—Cl1—Ca1x100.35 (5)
O2iii—Ca2—O3viii81.95 (6)Ca1—Cl1—Ca1x100.35 (5)
O2vii—Ca2—O3viii145.05 (5)Cl1iv—Cl1—Ca1xiv50.04 (3)
O2viii—Ca2—O3viii70.78 (5)Ca1xi—Cl1—Ca1xiv167.57 (6)
O4ix—Ca2—O3viii125.15 (5)Ca1—Cl1—Ca1xiv87.529 (13)
O4—Ca2—O3viii55.92 (6)Ca1x—Cl1—Ca1xiv87.529 (13)
O4vi—Ca2—O3viii68.26 (6)Cl1iv—Cl1—Ca1iv50.04 (3)
O3iii—Ca2—O3viii117.212 (19)Ca1xi—Cl1—Ca1iv87.529 (13)
O2iii—Ca2—O3vii145.05 (5)Ca1—Cl1—Ca1iv167.57 (6)
O2vii—Ca2—O3vii70.78 (5)Ca1x—Cl1—Ca1iv87.529 (13)
O2viii—Ca2—O3vii81.95 (6)Ca1xiv—Cl1—Ca1iv83.19 (4)
O4ix—Ca2—O3vii68.26 (6)Cl1iv—Cl1—Ca1xv50.04 (3)
O4—Ca2—O3vii125.15 (5)Ca1xi—Cl1—Ca1xv87.529 (13)
O4vi—Ca2—O3vii55.92 (6)Ca1—Cl1—Ca1xv87.529 (13)
O3iii—Ca2—O3vii117.212 (19)Ca1x—Cl1—Ca1xv167.57 (6)
O3viii—Ca2—O3vii117.212 (19)Ca1xiv—Cl1—Ca1xv83.19 (4)
O2iii—Ca2—P199.32 (5)Ca1iv—Cl1—Ca1xv83.19 (4)
O4—Ca1—P1—O2x180O3iii—Ca1—O2—Ca2viii41.90 (13)
O3—Ca1—P1—O2x100.81 (5)Cl1—Ca1—O2—Ca2viii163.78 (5)
O3i—Ca1—P1—O2x100.81 (5)Cl1i—Ca1—O2—Ca2viii107.92 (5)
O3ii—Ca1—P1—O2x85.00 (8)Cl1iv—Ca1—O2—Ca2viii176.29 (4)
O3iii—Ca1—P1—O2x85.00 (8)Cl1v—Ca1—O2—Ca2viii95.41 (5)
Cl1—Ca1—P1—O2x27.63 (4)O4—Ca1—O2—Ca2xii44.15 (4)
Cl1i—Ca1—P1—O2x27.63 (4)O3—Ca1—O2—Ca2xii125.28 (7)
Cl1iv—Ca1—P1—O2x40.09 (3)O3i—Ca1—O2—Ca2xii36.98 (5)
Cl1v—Ca1—P1—O2x40.09 (3)O3ii—Ca1—O2—Ca2xii41.90 (13)
P1vi—Ca1—P1—O2x180O3iii—Ca1—O2—Ca2xii130.20 (9)
O4—Ca1—P1—O3iii95.00 (8)Cl1—Ca1—O2—Ca2xii107.92 (5)
O3—Ca1—P1—O3iii15.81 (7)Cl1i—Ca1—O2—Ca2xii163.78 (5)
O3i—Ca1—P1—O3iii174.19 (11)Cl1iv—Ca1—O2—Ca2xii95.41 (5)
O3ii—Ca1—P1—O3iii170.00 (16)Cl1v—Ca1—O2—Ca2xii176.29 (4)
Cl1—Ca1—P1—O3iii112.63 (9)P1vi—Ca1—O2—Ca2xii44.15 (4)
Cl1i—Ca1—P1—O3iii57.37 (8)O4—Ca1—O3—P1xiii32.23 (16)
Cl1iv—Ca1—P1—O3iii125.09 (8)O3i—Ca1—O3—P1xiii116.18 (14)
Cl1v—Ca1—P1—O3iii44.91 (8)O3ii—Ca1—O3—P1xiii31.1 (2)
P1vi—Ca1—P1—O3iii95.00 (8)O3iii—Ca1—O3—P1xiii43.36 (18)
O4—Ca1—P1—O3ii95.00 (8)Cl1—Ca1—O3—P1xiii135.78 (13)
O3—Ca1—P1—O3ii174.19 (11)Cl1i—Ca1—O3—P1xiii114.76 (15)
O3i—Ca1—P1—O3ii15.81 (7)O2—Ca1—O3—P1xiii139.08 (17)
O3iii—Ca1—P1—O3ii170.00 (16)P1—Ca1—O3—P1xiii35.59 (16)
Cl1—Ca1—P1—O3ii57.37 (8)Cl1iv—Ca1—O3—P1xiii143.72 (12)
Cl1i—Ca1—P1—O3ii112.63 (9)Cl1v—Ca1—O3—P1xiii110.01 (16)
Cl1iv—Ca1—P1—O3ii44.91 (8)P1vi—Ca1—O3—P1xiii53.27 (15)
Cl1v—Ca1—P1—O3ii125.09 (8)O4—Ca1—O3—Ca1xiii179.30 (8)
P1vi—Ca1—P1—O3ii95.00 (8)O3i—Ca1—O3—Ca1xiii96.75 (11)
O4—Ca1—P1—O4ix0O3ii—Ca1—O3—Ca1xiii115.92 (5)
O3—Ca1—P1—O4ix79.19 (5)O3iii—Ca1—O3—Ca1xiii103.70 (4)
O3i—Ca1—P1—O4ix79.19 (5)Cl1—Ca1—O3—Ca1xiii11.28 (11)
O3ii—Ca1—P1—O4ix95.00 (8)Cl1i—Ca1—O3—Ca1xiii32.31 (6)
O3iii—Ca1—P1—O4ix95.00 (8)O2—Ca1—O3—Ca1xiii73.86 (8)
Cl1—Ca1—P1—O4ix152.37 (4)P1—Ca1—O3—Ca1xiii111.48 (6)
Cl1i—Ca1—P1—O4ix152.37 (4)Cl1iv—Ca1—O3—Ca1xiii3.34 (12)
Cl1iv—Ca1—P1—O4ix139.91 (3)Cl1v—Ca1—O3—Ca1xiii37.05 (6)
Cl1v—Ca1—P1—O4ix139.91 (3)P1vi—Ca1—O3—Ca1xiii159.67 (8)
P1vi—Ca1—P1—O4ix0O4—Ca1—O3—Ca2viii74.99 (6)
O4—Ca1—P1—Ca232.953 (12)O3i—Ca1—O3—Ca2viii8.96 (13)
O3—Ca1—P1—Ca246.24 (5)O3ii—Ca1—O3—Ca2viii138.36 (10)
O3i—Ca1—P1—Ca2112.15 (5)O3iii—Ca1—O3—Ca2viii150.58 (5)
O3ii—Ca1—P1—Ca2127.95 (8)Cl1—Ca1—O3—Ca2viii117.00 (5)
O3iii—Ca1—P1—Ca262.05 (8)Cl1i—Ca1—O3—Ca2viii138.02 (5)
Cl1—Ca1—P1—Ca2174.68 (4)O2—Ca1—O3—Ca2viii31.85 (5)
Cl1i—Ca1—P1—Ca2119.41 (4)P1—Ca1—O3—Ca2viii142.81 (3)
Cl1iv—Ca1—P1—Ca2172.86 (3)Cl1iv—Ca1—O3—Ca2viii109.05 (6)
Cl1v—Ca1—P1—Ca2106.96 (3)Cl1v—Ca1—O3—Ca2viii142.76 (5)
P1vi—Ca1—P1—Ca232.953 (12)P1vi—Ca1—O3—Ca2viii53.96 (4)
O4—Ca1—P1—Ca2i32.953 (12)O3—Ca1—O4—P1vi66.79 (4)
O3—Ca1—P1—Ca2i112.15 (5)O3i—Ca1—O4—P1vi66.79 (4)
O3i—Ca1—P1—Ca2i46.24 (5)O3ii—Ca1—O4—P1vi149.57 (4)
O3ii—Ca1—P1—Ca2i62.05 (8)O3iii—Ca1—O4—P1vi149.57 (4)
O3iii—Ca1—P1—Ca2i127.95 (8)Cl1—Ca1—O4—P1vi129.24 (7)
Cl1—Ca1—P1—Ca2i119.41 (4)Cl1i—Ca1—O4—P1vi129.24 (7)
Cl1i—Ca1—P1—Ca2i174.68 (4)O2—Ca1—O4—P1vi0
Cl1iv—Ca1—P1—Ca2i106.96 (3)P1—Ca1—O4—P1vi180
Cl1v—Ca1—P1—Ca2i172.86 (3)Cl1iv—Ca1—O4—P1vi116.93 (6)
P1vi—Ca1—P1—Ca2i32.953 (12)Cl1v—Ca1—O4—P1vi116.93 (6)
O4—Ca1—P1—Ca1ix0O3—Ca1—O4—Ca2i163.64 (8)
O3—Ca1—P1—Ca1ix79.19 (5)O3i—Ca1—O4—Ca2i62.79 (7)
O3i—Ca1—P1—Ca1ix79.19 (5)O3ii—Ca1—O4—Ca2i19.99 (6)
O3ii—Ca1—P1—Ca1ix95.00 (8)O3iii—Ca1—O4—Ca2i80.86 (8)
O3iii—Ca1—P1—Ca1ix95.00 (8)Cl1—Ca1—O4—Ca2i0.34 (12)
Cl1—Ca1—P1—Ca1ix152.37 (4)Cl1i—Ca1—O4—Ca2i101.19 (5)
Cl1i—Ca1—P1—Ca1ix152.37 (4)O2—Ca1—O4—Ca2i129.57 (6)
Cl1iv—Ca1—P1—Ca1ix139.91 (3)P1—Ca1—O4—Ca2i50.43 (6)
Cl1v—Ca1—P1—Ca1ix139.91 (3)Cl1iv—Ca1—O4—Ca2i12.65 (11)
P1vi—Ca1—P1—Ca1ix0Cl1v—Ca1—O4—Ca2i113.50 (4)
O4—Ca1—P1—Ca1x180P1vi—Ca1—O4—Ca2i129.57 (6)
O3—Ca1—P1—Ca1x100.81 (5)O3—Ca1—O4—Ca262.79 (7)
O3i—Ca1—P1—Ca1x100.81 (5)O3i—Ca1—O4—Ca2163.64 (8)
O3ii—Ca1—P1—Ca1x85.00 (8)O3ii—Ca1—O4—Ca280.86 (8)
O3iii—Ca1—P1—Ca1x85.00 (8)O3iii—Ca1—O4—Ca219.99 (6)
Cl1—Ca1—P1—Ca1x27.63 (4)Cl1—Ca1—O4—Ca2101.19 (5)
Cl1i—Ca1—P1—Ca1x27.63 (4)Cl1i—Ca1—O4—Ca20.34 (12)
Cl1iv—Ca1—P1—Ca1x40.09 (3)O2—Ca1—O4—Ca2129.57 (6)
Cl1v—Ca1—P1—Ca1x40.09 (3)P1—Ca1—O4—Ca250.43 (6)
P1vi—Ca1—P1—Ca1x180Cl1iv—Ca1—O4—Ca2113.50 (4)
O2iii—Ca2—P1—O2x93.48 (12)Cl1v—Ca1—O4—Ca212.65 (11)
O2vii—Ca2—P1—O2x16.54 (14)P1vi—Ca1—O4—Ca2129.57 (6)
O2viii—Ca2—P1—O2x18.33 (17)O2iii—Ca2—O4—P1vi87.26 (8)
O4ix—Ca2—P1—O2x75.77 (12)O2vii—Ca2—O4—P1vi150.77 (10)
O4—Ca2—P1—O2x179.17 (10)O2viii—Ca2—O4—P1vi13.24 (10)
O4vi—Ca2—P1—O2x110.16 (10)O4ix—Ca2—O4—P1vi144.96 (9)
O3iii—Ca2—P1—O2x92.35 (11)O4vi—Ca2—O4—P1vi66.03 (11)
O3viii—Ca2—P1—O2x179.86 (10)O3iii—Ca2—O4—P1vi156.61 (8)
O3vii—Ca2—P1—O2x54.07 (10)O3viii—Ca2—O4—P1vi6.83 (6)
P1vi—Ca2—P1—O2x177.33 (10)O3vii—Ca2—O4—P1vi94.65 (8)
P1ix—Ca2—P1—O2x82.69 (10)P1—Ca2—O4—P1vi172.48 (8)
O2iii—Ca2—P1—O3iii1.13 (8)P1ix—Ca2—O4—P1vi81.72 (7)
O2vii—Ca2—P1—O3iii75.80 (8)O2iii—Ca2—O4—Ca150.59 (8)
O2viii—Ca2—P1—O3iii74.0 (2)O2vii—Ca2—O4—Ca112.92 (14)
O4ix—Ca2—P1—O3iii168.11 (10)O2viii—Ca2—O4—Ca1124.61 (8)
O4—Ca2—P1—O3iii86.82 (8)O4ix—Ca2—O4—Ca177.19 (11)
O4vi—Ca2—P1—O3iii157.49 (9)O4vi—Ca2—O4—Ca1156.12 (9)
O3viii—Ca2—P1—O3iii87.51 (4)O3iii—Ca2—O4—Ca118.76 (6)
O3vii—Ca2—P1—O3iii146.42 (8)O3viii—Ca2—O4—Ca1131.03 (8)
P1vi—Ca2—P1—O3iii90.32 (7)O3vii—Ca2—O4—Ca1127.50 (6)
P1ix—Ca2—P1—O3iii175.04 (7)P1—Ca2—O4—Ca149.67 (6)
O2iii—Ca2—P1—O3ii97.40 (8)P1vi—Ca2—O4—Ca1137.85 (11)
O2vii—Ca2—P1—O3ii174.33 (9)P1ix—Ca2—O4—Ca1140.43 (6)
O2viii—Ca2—P1—O3ii172.5 (2)O2iii—Ca2—O4—Ca2i167.24 (7)
O4ix—Ca2—P1—O3ii93.36 (10)O2vii—Ca2—O4—Ca2i103.74 (10)
O4—Ca2—P1—O3ii11.70 (8)O2viii—Ca2—O4—Ca2i118.73 (6)
O4vi—Ca2—P1—O3ii58.96 (9)O4ix—Ca2—O4—Ca2i39.462 (17)
O3iii—Ca2—P1—O3ii98.53 (13)O4vi—Ca2—O4—Ca2i39.462 (17)
O3viii—Ca2—P1—O3ii11.02 (10)O3iii—Ca2—O4—Ca2i97.90 (6)
O3vii—Ca2—P1—O3ii115.05 (8)O3viii—Ca2—O4—Ca2i112.32 (8)
P1vi—Ca2—P1—O3ii8.21 (7)O3vii—Ca2—O4—Ca2i10.85 (9)
P1ix—Ca2—P1—O3ii86.43 (7)P1—Ca2—O4—Ca2i66.99 (4)
O2iii—Ca2—P1—O4ix169.24 (9)P1vi—Ca2—O4—Ca2i105.49 (9)
O2vii—Ca2—P1—O4ix92.31 (9)P1ix—Ca2—O4—Ca2i23.78 (6)
O2viii—Ca2—P1—O4ix94.1 (2)O4—Ca1—Cl1—Cl1iv45.50 (8)
O4—Ca2—P1—O4ix105.06 (11)O3—Ca1—Cl1—Cl1iv154.85 (5)
O4vi—Ca2—P1—O4ix34.40 (9)O3i—Ca1—Cl1—Cl1iv20.31 (4)
O3iii—Ca2—P1—O4ix168.11 (10)O3ii—Ca1—Cl1—Cl1iv66.43 (4)
O3viii—Ca2—P1—O4ix104.38 (9)O3iii—Ca1—Cl1—Cl1iv119.76 (3)
O3vii—Ca2—P1—O4ix21.69 (8)Cl1i—Ca1—Cl1—Cl1iv180.0000 (10)
P1vi—Ca2—P1—O4ix101.56 (8)O2—Ca1—Cl1—Cl1iv85.07 (2)
P1ix—Ca2—P1—O4ix6.93 (7)P1—Ca1—Cl1—Cl1iv92.563 (9)
O2iii—Ca2—P1—Ca154.07 (4)Cl1v—Ca1—Cl1—Cl1iv180.0000 (10)
O2vii—Ca2—P1—Ca1131.00 (5)P1vi—Ca1—Cl1—Cl1iv5.73 (6)
O2viii—Ca2—P1—Ca1129.2 (2)O4—Ca1—Cl1—Ca1xi174.17 (7)
O4ix—Ca2—P1—Ca1136.69 (8)O3—Ca1—Cl1—Ca1xi26.18 (7)
O4—Ca2—P1—Ca131.63 (4)O3i—Ca1—Cl1—Ca1xi108.37 (5)
O4vi—Ca2—P1—Ca1102.29 (5)O3ii—Ca1—Cl1—Ca1xi164.89 (6)
O3iii—Ca2—P1—Ca155.20 (7)O3iii—Ca1—Cl1—Ca1xi111.56 (5)
O3viii—Ca2—P1—Ca132.31 (4)Cl1i—Ca1—Cl1—Ca1xi51.33 (3)
O3vii—Ca2—P1—Ca1158.38 (3)O2—Ca1—Cl1—Ca1xi43.61 (5)
P1vi—Ca2—P1—Ca135.126 (15)P1—Ca1—Cl1—Ca1xi138.76 (4)
P1ix—Ca2—P1—Ca1129.762 (13)Cl1iv—Ca1—Cl1—Ca1xi128.67 (4)
O2iii—Ca2—P1—Ca2i136.51 (4)Cl1v—Ca1—Cl1—Ca1xi51.33 (3)
O2vii—Ca2—P1—Ca2i146.56 (5)P1vi—Ca1—Cl1—Ca1xi134.41 (7)
O2viii—Ca2—P1—Ca2i148.34 (19)O4—Ca1—Cl1—Ca1x83.17 (10)
O4ix—Ca2—P1—Ca2i54.25 (7)O3—Ca1—Cl1—Ca1x76.47 (6)
O4—Ca2—P1—Ca2i50.82 (4)O3i—Ca1—Cl1—Ca1x148.98 (6)
O4vi—Ca2—P1—Ca2i19.85 (5)O3ii—Ca1—Cl1—Ca1x62.24 (5)
O3iii—Ca2—P1—Ca2i137.64 (7)O3iii—Ca1—Cl1—Ca1x8.91 (5)
O3viii—Ca2—P1—Ca2i50.13 (4)Cl1i—Ca1—Cl1—Ca1x51.33 (3)
O3vii—Ca2—P1—Ca2i75.94 (3)O2—Ca1—Cl1—Ca1x146.26 (4)
P1vi—Ca2—P1—Ca2i47.318 (10)P1—Ca1—Cl1—Ca1x36.11 (3)
P1ix—Ca2—P1—Ca2i47.318 (10)Cl1iv—Ca1—Cl1—Ca1x128.67 (4)
O2iii—Ca2—P1—Ca1ix143.81 (4)Cl1v—Ca1—Cl1—Ca1x51.33 (3)
O2vii—Ca2—P1—Ca1ix66.88 (5)P1vi—Ca1—Cl1—Ca1x122.94 (7)
O2viii—Ca2—P1—Ca1ix68.66 (19)O4—Ca1—Cl1—Ca1xiv3.86 (9)
O4ix—Ca2—P1—Ca1ix25.43 (7)O3—Ca1—Cl1—Ca1xiv163.51 (5)
O4—Ca2—P1—Ca1ix130.49 (4)O3i—Ca1—Cl1—Ca1xiv61.95 (5)
O4vi—Ca2—P1—Ca1ix59.83 (5)O3ii—Ca1—Cl1—Ca1xiv24.79 (4)
O3iii—Ca2—P1—Ca1ix142.68 (7)O3iii—Ca1—Cl1—Ca1xiv78.12 (4)
O3viii—Ca2—P1—Ca1ix129.81 (4)Cl1i—Ca1—Cl1—Ca1xiv138.36 (2)
O3vii—Ca2—P1—Ca1ix3.74 (3)O2—Ca1—Cl1—Ca1xiv126.71 (3)
P1vi—Ca2—P1—Ca1ix126.994 (14)P1—Ca1—Cl1—Ca1xiv50.922 (19)
P1ix—Ca2—P1—Ca1ix32.359 (14)Cl1iv—Ca1—Cl1—Ca1xiv41.64 (2)
O2iii—Ca2—P1—Ca1x3.92 (6)Cl1v—Ca1—Cl1—Ca1xiv138.36 (2)
O2vii—Ca2—P1—Ca1x73.01 (5)P1vi—Ca1—Cl1—Ca1xiv35.91 (6)
O2viii—Ca2—P1—Ca1x71.2 (2)O4—Ca1—Cl1—Ca1iv45.50 (8)
O4ix—Ca2—P1—Ca1x165.32 (9)O3—Ca1—Cl1—Ca1iv154.85 (6)
O4—Ca2—P1—Ca1x89.62 (5)O3i—Ca1—Cl1—Ca1iv20.31 (4)
O4vi—Ca2—P1—Ca1x160.28 (6)O3ii—Ca1—Cl1—Ca1iv66.43 (4)
O3iii—Ca2—P1—Ca1x2.80 (7)O3iii—Ca1—Cl1—Ca1iv119.76 (3)
O3viii—Ca2—P1—Ca1x90.30 (5)Cl1i—Ca1—Cl1—Ca1iv180.0000 (10)
O3vii—Ca2—P1—Ca1x143.62 (4)O2—Ca1—Cl1—Ca1iv85.07 (2)
P1vi—Ca2—P1—Ca1x93.12 (4)P1—Ca1—Cl1—Ca1iv92.563 (10)
P1ix—Ca2—P1—Ca1x172.25 (4)Cl1iv—Ca1—Cl1—Ca1iv0
O4—Ca1—O2—P1xi180Cl1v—Ca1—Cl1—Ca1iv180.0000 (10)
O3—Ca1—O2—P1xi98.87 (5)P1vi—Ca1—Cl1—Ca1iv5.73 (6)
O3i—Ca1—O2—P1xi98.87 (5)O4—Ca1—Cl1—Ca1xv87.14 (8)
O3ii—Ca1—O2—P1xi93.95 (11)O3—Ca1—Cl1—Ca1xv113.21 (6)
O3iii—Ca1—O2—P1xi93.95 (11)O3i—Ca1—Cl1—Ca1xv21.33 (5)
Cl1—Ca1—O2—P1xi27.93 (4)O3ii—Ca1—Cl1—Ca1xv108.07 (5)
Cl1i—Ca1—O2—P1xi27.93 (4)O3iii—Ca1—Cl1—Ca1xv161.40 (4)
Cl1iv—Ca1—O2—P1xi40.44 (3)Cl1i—Ca1—Cl1—Ca1xv138.36 (2)
Cl1v—Ca1—O2—P1xi40.44 (3)O2—Ca1—Cl1—Ca1xv43.43 (3)
O4—Ca1—O2—Ca2viii44.15 (4)P1—Ca1—Cl1—Ca1xv134.20 (3)
O3—Ca1—O2—Ca2viii36.98 (5)Cl1iv—Ca1—Cl1—Ca1xv41.64 (2)
O3i—Ca1—O2—Ca2viii125.28 (7)Cl1v—Ca1—Cl1—Ca1xv138.36 (2)
O3ii—Ca1—O2—Ca2viii130.20 (9)P1vi—Ca1—Cl1—Ca1xv47.37 (6)
Symmetry codes: (i) x, y, z+1/2; (ii) xy+1, x+1, z+1/2; (iii) xy+1, x+1, z; (iv) x, y+2, z+1; (v) x, y+2, z1/2; (vi) y+1, xy+1, z; (vii) y, x+y, z; (viii) x, y+1, z; (ix) x+y, x+1, z; (x) y+1, xy+2, z; (xi) x+y1, x+1, z; (xii) x, y+1, z+1/2; (xiii) y1, x+y, z; (xiv) xy+1, x+1, z+1; (xv) y1, x+y, z+1.
(3_low_prism) chlorapatite top
Crystal data top
3(O4P)·Cl·5(Ca)Dx = 3.19 Mg m3
Mr = 520.76Mo Kα radiation, λ = 0.7107 Å
Trigonal, P63/mCell parameters from 1987 reflections
Hall symbol: -P 6cθ = 2.5–27.0°
a = 9.6340 (2) ŵ = 3.23 mm1
c = 6.7440 (3) ÅT = 100 K
V = 542.08 (3) Å3Prism, colourless
Z = 20.25 × 0.12 × 0.05 mm
F(000) = 516
Data collection top
BRUKER APPEX-II CCD
diffractometer
403 independent reflections
Radiation source: fine-focus sealed tube400 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.037
ω and phi scansθmax = 26.3°, θmin = 2.4°
Absorption correction: multi-scan
BRUKER SADABS
h = 012
Tmin = 0.666, Tmax = 1k = 120
5403 measured reflectionsl = 80
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.029Secondary atom site location: difference Fourier map
wR(F2) = 0.081 w = 1/[σ2(Fo2) + (0.0405P)2 + 1.0078P]
where P = (Fo2 + 2Fc2)/3
S = 1.37(Δ/σ)max = 0.001
403 reflectionsΔρmax = 0.45 e Å3
40 parametersΔρmin = 1.23 e Å3
Crystal data top
3(O4P)·Cl·5(Ca)Z = 2
Mr = 520.76Mo Kα radiation
Trigonal, P63/mµ = 3.23 mm1
a = 9.6340 (2) ÅT = 100 K
c = 6.7440 (3) Å0.25 × 0.12 × 0.05 mm
V = 542.08 (3) Å3
Data collection top
BRUKER APPEX-II CCD
diffractometer
403 independent reflections
Absorption correction: multi-scan
BRUKER SADABS
400 reflections with I > 2σ(I)
Tmin = 0.666, Tmax = 1Rint = 0.037
5403 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.02940 parameters
wR(F2) = 0.0810 restraints
S = 1.37Δρmax = 0.45 e Å3
403 reflectionsΔρmin = 1.23 e Å3
Special details top

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ca10.00606 (9)0.74551 (9)0.250.0038 (3)
Ca20.33330.66670.00344 (14)0.0046 (3)
P10.37482 (11)0.96721 (11)0.250.0024 (3)
O20.3438 (3)0.5074 (3)0.250.0060 (6)
O30.0868 (2)0.6471 (3)0.0666 (3)0.0104 (5)
O40.1279 (3)0.5929 (3)0.250.0065 (6)
Cl1010.4413 (4)0.0146 (7)0.5
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0042 (4)0.0040 (4)0.0038 (4)0.0026 (3)00
Ca20.0056 (4)0.0056 (4)0.0026 (5)0.00278 (19)00
P10.0016 (5)0.0011 (5)0.0038 (5)0.0003 (4)00
O20.0079 (14)0.0057 (13)0.0077 (14)0.0059 (11)00
O30.0059 (9)0.0170 (10)0.0099 (11)0.0070 (8)0.0034 (8)0.0091 (9)
O40.0046 (13)0.0029 (13)0.0125 (14)0.0024 (10)00
Cl10.0067 (6)0.0067 (6)0.0303 (18)0.0034 (3)00
Geometric parameters (Å, º) top
Ca1—O42.295 (3)Ca2—P1vi3.2105 (9)
Ca1—O32.326 (2)Ca2—P1ix3.2105 (9)
Ca1—O3i2.326 (2)P1—O3iii1.534 (2)
Ca1—O3ii2.523 (2)P1—O3ii1.534 (2)
Ca1—O3iii2.523 (2)P1—O2x1.537 (3)
Ca1—Cl12.7968 (14)P1—O4ix1.546 (3)
Ca1—Cl1i2.7968 (14)P1—Ca2i3.2105 (9)
Ca1—O22.981 (3)P1—Ca1ix3.3914 (12)
Ca1—P13.0977 (12)O2—P1xi1.537 (3)
Ca1—Cl1iv3.2391 (18)O2—Ca2viii2.399 (2)
Ca1—Cl1v3.2391 (18)O2—Ca2xii2.399 (2)
Ca1—P1vi3.3914 (12)O3—P1xiii1.534 (2)
Ca2—O2iii2.399 (2)O3—Ca1xiii2.523 (2)
Ca2—O2vii2.399 (2)O3—Ca2viii2.797 (2)
Ca2—O2viii2.399 (2)O4—P1vi1.546 (3)
Ca2—O4ix2.436 (2)O4—Ca2i2.436 (2)
Ca2—O42.436 (2)Cl1—Cl1iv0.792 (5)
Ca2—O4vi2.436 (2)Cl1—Ca1x2.7968 (14)
Ca2—O3iii2.797 (2)Cl1—Ca1xi2.7968 (14)
Ca2—O3viii2.797 (2)Cl1—Ca1xiv3.2391 (18)
Ca2—O3vii2.797 (2)Cl1—Ca1iv3.2391 (18)
Ca2—P13.2105 (9)Cl1—Ca1xv3.2391 (18)
O4—Ca1—O387.40 (6)O2vii—Ca2—P188.57 (5)
O4—Ca1—O3i87.40 (6)O2viii—Ca2—P1165.83 (6)
O3—Ca1—O3i133.28 (11)O4ix—Ca2—P127.68 (6)
O4—Ca1—O3ii75.41 (8)O4—Ca2—P166.82 (6)
O3—Ca1—O3ii140.10 (8)O4vi—Ca2—P199.13 (6)
O3i—Ca1—O3ii82.38 (4)O3iii—Ca2—P128.53 (4)
O4—Ca1—O3iii75.41 (8)O3viii—Ca2—P1122.70 (5)
O3—Ca1—O3iii82.38 (4)O3vii—Ca2—P193.92 (4)
O3i—Ca1—O3iii140.10 (8)O2iii—Ca2—P1vi88.57 (6)
O3ii—Ca1—O3iii58.69 (9)O2vii—Ca2—P1vi165.83 (6)
O4—Ca1—Cl1143.44 (6)O2viii—Ca2—P1vi99.34 (6)
O3—Ca1—Cl1127.47 (7)O4ix—Ca2—P1vi99.13 (6)
O3i—Ca1—Cl176.20 (7)O4—Ca2—P1vi27.68 (6)
O3ii—Ca1—Cl170.24 (5)O4vi—Ca2—P1vi66.82 (6)
O3iii—Ca1—Cl196.54 (6)O3iii—Ca2—P1vi93.92 (4)
O4—Ca1—Cl1i143.44 (6)O3viii—Ca2—P1vi28.53 (4)
O3—Ca1—Cl1i76.20 (7)O3vii—Ca2—P1vi122.70 (5)
O3i—Ca1—Cl1i127.47 (7)P1—Ca2—P1vi94.29 (2)
O3ii—Ca1—Cl1i96.54 (6)O2iii—Ca2—P1ix165.83 (6)
O3iii—Ca1—Cl1i70.24 (5)O2vii—Ca2—P1ix99.34 (6)
Cl1—Ca1—Cl1i54.94 (10)O2viii—Ca2—P1ix88.57 (5)
O4—Ca1—O2104.52 (9)O4ix—Ca2—P1ix66.82 (6)
O3—Ca1—O268.29 (5)O4—Ca2—P1ix99.13 (6)
O3i—Ca1—O268.29 (5)O4vi—Ca2—P1ix27.68 (6)
O3ii—Ca1—O2150.58 (5)O3iii—Ca2—P1ix122.70 (5)
O3iii—Ca1—O2150.58 (5)O3viii—Ca2—P1ix93.92 (4)
Cl1—Ca1—O299.40 (5)O3vii—Ca2—P1ix28.53 (4)
Cl1i—Ca1—O299.40 (5)P1—Ca2—P1ix94.29 (2)
O4—Ca1—P170.37 (7)P1vi—Ca2—P1ix94.29 (2)
O3—Ca1—P1110.84 (5)O3iii—P1—O3ii107.46 (16)
O3i—Ca1—P1110.84 (5)O3iii—P1—O2x112.11 (10)
O3ii—Ca1—P129.47 (4)O3ii—P1—O2x112.11 (10)
O3iii—Ca1—P129.47 (4)O3iii—P1—O4ix106.84 (10)
Cl1—Ca1—P185.12 (2)O3ii—P1—O4ix106.84 (10)
Cl1i—Ca1—P185.12 (2)O2x—P1—O4ix111.17 (15)
O2—Ca1—P1174.89 (6)O3iii—P1—Ca154.03 (8)
O4—Ca1—Cl1iv133.91 (4)O3ii—P1—Ca154.03 (8)
O3—Ca1—Cl1iv138.56 (6)O2x—P1—Ca1136.39 (12)
O3i—Ca1—Cl1iv64.51 (6)O4ix—P1—Ca1112.44 (11)
O3ii—Ca1—Cl1iv65.69 (5)O3iii—P1—Ca260.58 (8)
O3iii—Ca1—Cl1iv102.60 (6)O3ii—P1—Ca2111.55 (8)
Cl1—Ca1—Cl1iv12.53 (8)O2x—P1—Ca2135.62 (7)
Cl1i—Ca1—Cl1iv67.466 (19)O4ix—P1—Ca247.07 (7)
O2—Ca1—Cl1iv98.11 (4)Ca1—P1—Ca278.20 (2)
P1—Ca1—Cl1iv85.79 (2)O3iii—P1—Ca2i111.55 (8)
O4—Ca1—Cl1v133.91 (4)O3ii—P1—Ca2i60.58 (8)
O3—Ca1—Cl1v64.51 (6)O2x—P1—Ca2i135.62 (7)
O3i—Ca1—Cl1v138.56 (6)O4ix—P1—Ca2i47.07 (7)
O3ii—Ca1—Cl1v102.60 (6)Ca1—P1—Ca2i78.20 (2)
O3iii—Ca1—Cl1v65.69 (5)Ca2—P1—Ca2i64.33 (3)
Cl1—Ca1—Cl1v67.465 (19)O3iii—P1—Ca1ix122.12 (9)
Cl1i—Ca1—Cl1v12.53 (8)O3ii—P1—Ca1ix122.12 (9)
O2—Ca1—Cl1v98.11 (4)O2x—P1—Ca1ix76.50 (11)
P1—Ca1—Cl1v85.79 (2)Ca1—P1—Ca1ix147.10 (4)
Cl1iv—Ca1—Cl1v79.99 (8)Ca2—P1—Ca1ix74.08 (2)
O4—Ca1—P1vi22.53 (7)Ca2i—P1—Ca1ix74.08 (2)
O3—Ca1—P1vi78.88 (5)O3iii—P1—Ca1x80.25 (9)
O3i—Ca1—P1vi78.88 (5)O3ii—P1—Ca1x80.25 (9)
O3ii—Ca1—P1vi94.99 (5)O2x—P1—Ca1x56.15 (11)
O3iii—Ca1—P1vi94.99 (5)O4ix—P1—Ca1x167.32 (11)
Cl1—Ca1—P1vi152.42 (5)Ca1—P1—Ca1x80.24 (3)
Cl1i—Ca1—P1vi152.42 (5)Ca2—P1—Ca1x140.79 (2)
O2—Ca1—P1vi81.99 (6)Ca2i—P1—Ca1x140.79 (2)
P1—Ca1—P1vi92.90 (4)Ca1ix—P1—Ca1x132.65 (4)
Cl1iv—Ca1—P1vi139.93 (4)P1xi—O2—Ca2viii133.47 (7)
Cl1v—Ca1—P1vi139.93 (4)P1xi—O2—Ca2xii133.47 (7)
O2iii—Ca2—O2vii77.26 (7)Ca2viii—O2—Ca2xii87.74 (9)
O2iii—Ca2—O2viii77.26 (7)P1xi—O2—Ca198.50 (13)
O2vii—Ca2—O2viii77.26 (7)Ca2viii—O2—Ca196.40 (8)
O2iii—Ca2—O4ix126.45 (9)Ca2xii—O2—Ca196.40 (8)
O2vii—Ca2—O4ix89.84 (6)P1xiii—O3—Ca1138.83 (11)
O2viii—Ca2—O4ix150.14 (9)P1xiii—O3—Ca1xiii96.50 (10)
O2iii—Ca2—O489.84 (6)Ca1—O3—Ca1xiii119.33 (8)
O2vii—Ca2—O4150.14 (9)P1xiii—O3—Ca2viii90.88 (10)
O2viii—Ca2—O4126.45 (9)Ca1—O3—Ca2viii103.36 (8)
O4ix—Ca2—O476.22 (7)Ca1xiii—O3—Ca2viii96.69 (7)
O2iii—Ca2—O4vi150.14 (9)P1vi—O4—Ca1122.81 (15)
O2vii—Ca2—O4vi126.45 (9)P1vi—O4—Ca2i105.25 (10)
O2viii—Ca2—O4vi89.84 (6)Ca1—O4—Ca2i114.47 (8)
O4ix—Ca2—O4vi76.22 (7)P1vi—O4—Ca2105.25 (10)
O4—Ca2—O4vi76.22 (7)Ca1—O4—Ca2114.47 (8)
O2iii—Ca2—O3iii70.81 (7)Ca2i—O4—Ca289.10 (9)
O2vii—Ca2—O3iii82.00 (8)Cl1iv—Cl1—Ca1x117.47 (5)
O2viii—Ca2—O3iii145.00 (7)Cl1iv—Cl1—Ca1117.47 (5)
O4ix—Ca2—O3iii55.89 (7)Ca1x—Cl1—Ca1100.42 (6)
O4—Ca2—O3iii68.28 (8)Cl1iv—Cl1—Ca1xi117.47 (5)
O4vi—Ca2—O3iii125.11 (7)Ca1x—Cl1—Ca1xi100.42 (6)
O2iii—Ca2—O3viii82.00 (8)Ca1—Cl1—Ca1xi100.42 (6)
O2vii—Ca2—O3viii145.00 (7)Cl1iv—Cl1—Ca1xiv50.00 (4)
O2viii—Ca2—O3viii70.81 (7)Ca1x—Cl1—Ca1xiv87.514 (17)
O4ix—Ca2—O3viii125.11 (7)Ca1—Cl1—Ca1xiv87.514 (17)
O4—Ca2—O3viii55.89 (7)Ca1xi—Cl1—Ca1xiv167.47 (8)
O4vi—Ca2—O3viii68.28 (8)Cl1iv—Cl1—Ca1iv50.00 (4)
O3iii—Ca2—O3viii117.20 (3)Ca1x—Cl1—Ca1iv87.514 (17)
O2iii—Ca2—O3vii145.00 (7)Ca1—Cl1—Ca1iv167.47 (8)
O2vii—Ca2—O3vii70.81 (7)Ca1xi—Cl1—Ca1iv87.514 (17)
O2viii—Ca2—O3vii82.00 (8)Ca1xiv—Cl1—Ca1iv83.13 (6)
O4ix—Ca2—O3vii68.28 (8)Cl1iv—Cl1—Ca1xv50.00 (4)
O4—Ca2—O3vii125.11 (7)Ca1x—Cl1—Ca1xv167.47 (8)
O4vi—Ca2—O3vii55.89 (7)Ca1—Cl1—Ca1xv87.514 (17)
O3iii—Ca2—O3vii117.20 (3)Ca1xi—Cl1—Ca1xv87.514 (17)
O3viii—Ca2—O3vii117.20 (2)Ca1xiv—Cl1—Ca1xv83.13 (6)
O2iii—Ca2—P199.34 (6)Ca1iv—Cl1—Ca1xv83.13 (6)
O4—Ca1—P1—O3iii95.02 (10)O3ii—Ca1—O2—Ca2viii130.17 (12)
O3—Ca1—P1—O3iii15.82 (9)O3iii—Ca1—O2—Ca2viii41.73 (17)
O3i—Ca1—P1—O3iii174.23 (14)Cl1—Ca1—O2—Ca2viii163.66 (7)
O3ii—Ca1—P1—O3iii170.0 (2)Cl1i—Ca1—O2—Ca2viii107.91 (7)
Cl1—Ca1—P1—O3iii112.55 (11)Cl1iv—Ca1—O2—Ca2viii176.27 (6)
Cl1i—Ca1—P1—O3iii57.40 (11)Cl1v—Ca1—O2—Ca2viii95.30 (7)
Cl1iv—Ca1—P1—O3iii125.10 (11)P1vi—Ca1—O2—Ca2viii44.22 (5)
Cl1v—Ca1—P1—O3iii44.85 (11)O3—Ca1—O2—Ca2xii125.38 (9)
P1vi—Ca1—P1—O3iii95.02 (10)O3i—Ca1—O2—Ca2xii36.95 (6)
O4—Ca1—P1—O3ii95.02 (10)O3ii—Ca1—O2—Ca2xii41.73 (17)
O3—Ca1—P1—O3ii174.23 (14)O3iii—Ca1—O2—Ca2xii130.17 (12)
O3i—Ca1—P1—O3ii15.82 (9)Cl1—Ca1—O2—Ca2xii107.91 (7)
O3iii—Ca1—P1—O3ii170.0 (2)Cl1i—Ca1—O2—Ca2xii163.66 (7)
Cl1—Ca1—P1—O3ii57.40 (11)Cl1iv—Ca1—O2—Ca2xii95.30 (7)
Cl1i—Ca1—P1—O3ii112.55 (11)Cl1v—Ca1—O2—Ca2xii176.27 (6)
Cl1iv—Ca1—P1—O3ii44.85 (11)O4—Ca1—O3—P1xiii32.2 (2)
Cl1v—Ca1—P1—O3ii125.10 (11)O3i—Ca1—O3—P1xiii116.19 (18)
P1vi—Ca1—P1—O3ii95.02 (10)O3ii—Ca1—O3—P1xiii31.2 (3)
O4—Ca1—P1—O2x180O3iii—Ca1—O3—P1xiii43.4 (2)
O3—Ca1—P1—O2x100.80 (6)Cl1—Ca1—O3—P1xiii135.82 (17)
O3i—Ca1—P1—O2x100.80 (6)Cl1i—Ca1—O3—P1xiii114.8 (2)
O3ii—Ca1—P1—O2x84.98 (10)O2—Ca1—O3—P1xiii139.0 (2)
O3iii—Ca1—P1—O2x84.98 (10)P1—Ca1—O3—P1xiii35.6 (2)
Cl1—Ca1—P1—O2x27.58 (5)Cl1iv—Ca1—O3—P1xiii143.83 (15)
Cl1i—Ca1—P1—O2x27.58 (5)Cl1v—Ca1—O3—P1xiii110.0 (2)
Cl1iv—Ca1—P1—O2x40.13 (4)P1vi—Ca1—O3—P1xiii53.25 (19)
Cl1v—Ca1—P1—O2x40.13 (4)O4—Ca1—O3—Ca1xiii179.32 (11)
P1vi—Ca1—P1—O2x180O3i—Ca1—O3—Ca1xiii96.71 (15)
O4—Ca1—P1—O4ix0O3ii—Ca1—O3—Ca1xiii115.91 (7)
O3—Ca1—P1—O4ix79.20 (6)O3iii—Ca1—O3—Ca1xiii103.70 (6)
O3i—Ca1—P1—O4ix79.20 (6)Cl1—Ca1—O3—Ca1xiii11.28 (14)
O3ii—Ca1—P1—O4ix95.02 (10)Cl1i—Ca1—O3—Ca1xiii32.27 (8)
O3iii—Ca1—P1—O4ix95.02 (10)O2—Ca1—O3—Ca1xiii73.93 (10)
Cl1—Ca1—P1—O4ix152.42 (5)P1—Ca1—O3—Ca1xiii111.48 (8)
Cl1i—Ca1—P1—O4ix152.42 (5)Cl1iv—Ca1—O3—Ca1xiii3.27 (16)
Cl1iv—Ca1—P1—O4ix139.87 (4)Cl1v—Ca1—O3—Ca1xiii37.06 (7)
Cl1v—Ca1—P1—O4ix139.87 (4)P1vi—Ca1—O3—Ca1xiii159.65 (10)
P1vi—Ca1—P1—O4ix0O4—Ca1—O3—Ca2viii74.97 (8)
O4—Ca1—P1—Ca232.948 (16)O3i—Ca1—O3—Ca2viii8.99 (17)
O3—Ca1—P1—Ca246.25 (6)O3ii—Ca1—O3—Ca2viii138.39 (12)
O3i—Ca1—P1—Ca2112.15 (6)O3iii—Ca1—O3—Ca2viii150.59 (7)
O3ii—Ca1—P1—Ca2127.97 (10)Cl1—Ca1—O3—Ca2viii116.98 (7)
O3iii—Ca1—P1—Ca262.08 (10)Cl1i—Ca1—O3—Ca2viii137.98 (6)
Cl1—Ca1—P1—Ca2174.63 (5)O2—Ca1—O3—Ca2viii31.78 (7)
Cl1i—Ca1—P1—Ca2119.47 (5)P1—Ca1—O3—Ca2viii142.81 (5)
Cl1iv—Ca1—P1—Ca2172.82 (4)Cl1iv—Ca1—O3—Ca2viii108.97 (8)
Cl1v—Ca1—P1—Ca2106.93 (4)Cl1v—Ca1—O3—Ca2viii142.76 (7)
P1vi—Ca1—P1—Ca232.948 (16)P1vi—Ca1—O3—Ca2viii53.94 (5)
O4—Ca1—P1—Ca2i32.948 (16)O3—Ca1—O4—P1vi66.78 (6)
O3—Ca1—P1—Ca2i112.15 (6)O3i—Ca1—O4—P1vi66.78 (6)
O3i—Ca1—P1—Ca2i46.25 (6)O3ii—Ca1—O4—P1vi149.58 (5)
O3ii—Ca1—P1—Ca2i62.08 (10)O3iii—Ca1—O4—P1vi149.58 (5)
O3iii—Ca1—P1—Ca2i127.97 (10)Cl1—Ca1—O4—P1vi129.25 (10)
Cl1—Ca1—P1—Ca2i119.47 (5)Cl1i—Ca1—O4—P1vi129.25 (10)
Cl1i—Ca1—P1—Ca2i174.63 (5)O2—Ca1—O4—P1vi0
Cl1iv—Ca1—P1—Ca2i106.93 (4)P1—Ca1—O4—P1vi180
Cl1v—Ca1—P1—Ca2i172.82 (4)Cl1iv—Ca1—O4—P1vi116.85 (7)
P1vi—Ca1—P1—Ca2i32.948 (16)Cl1v—Ca1—O4—P1vi116.85 (7)
O4—Ca1—P1—Ca1ix0O3—Ca1—O4—Ca2i163.65 (10)
O3—Ca1—P1—Ca1ix79.20 (6)O3i—Ca1—O4—Ca2i62.80 (9)
O3i—Ca1—P1—Ca1ix79.20 (6)O3ii—Ca1—O4—Ca2i20.00 (8)
O3ii—Ca1—P1—Ca1ix95.02 (10)O3iii—Ca1—O4—Ca2i80.84 (10)
O3iii—Ca1—P1—Ca1ix95.02 (10)Cl1—Ca1—O4—Ca2i0.33 (16)
Cl1—Ca1—P1—Ca1ix152.42 (5)Cl1i—Ca1—O4—Ca2i101.18 (7)
Cl1i—Ca1—P1—Ca1ix152.42 (5)O2—Ca1—O4—Ca2i129.58 (8)
Cl1iv—Ca1—P1—Ca1ix139.87 (4)P1—Ca1—O4—Ca2i50.42 (8)
Cl1v—Ca1—P1—Ca1ix139.87 (4)Cl1iv—Ca1—O4—Ca2i12.73 (15)
P1vi—Ca1—P1—Ca1ix0Cl1v—Ca1—O4—Ca2i113.57 (5)
O4—Ca1—P1—Ca1x180P1vi—Ca1—O4—Ca2i129.58 (8)
O3—Ca1—P1—Ca1x100.80 (6)O3—Ca1—O4—Ca262.80 (9)
O3i—Ca1—P1—Ca1x100.80 (6)O3i—Ca1—O4—Ca2163.65 (10)
O3ii—Ca1—P1—Ca1x84.98 (10)O3ii—Ca1—O4—Ca280.84 (10)
O3iii—Ca1—P1—Ca1x84.98 (10)O3iii—Ca1—O4—Ca220.00 (8)
Cl1—Ca1—P1—Ca1x27.58 (5)Cl1—Ca1—O4—Ca2101.18 (7)
Cl1i—Ca1—P1—Ca1x27.58 (5)Cl1i—Ca1—O4—Ca20.33 (16)
Cl1iv—Ca1—P1—Ca1x40.13 (4)O2—Ca1—O4—Ca2129.58 (8)
Cl1v—Ca1—P1—Ca1x40.13 (4)P1—Ca1—O4—Ca250.42 (8)
P1vi—Ca1—P1—Ca1x180Cl1iv—Ca1—O4—Ca2113.57 (5)
O2iii—Ca2—P1—O3iii1.06 (11)Cl1v—Ca1—O4—Ca212.73 (15)
O2vii—Ca2—P1—O3iii75.79 (11)P1vi—Ca1—O4—Ca2129.58 (8)
O2viii—Ca2—P1—O3iii73.8 (3)O2iii—Ca2—O4—P1vi87.22 (11)
O4ix—Ca2—P1—O3iii168.18 (13)O2vii—Ca2—O4—P1vi150.63 (13)
O4—Ca2—P1—O3iii86.84 (11)O2viii—Ca2—O4—P1vi13.25 (14)
O4vi—Ca2—P1—O3iii157.49 (11)O4ix—Ca2—O4—P1vi145.02 (11)
O3viii—Ca2—P1—O3iii87.50 (5)O4vi—Ca2—O4—P1vi66.11 (14)
O3vii—Ca2—P1—O3iii146.45 (10)O3iii—Ca2—O4—P1vi156.57 (11)
P1vi—Ca2—P1—O3iii90.31 (9)O3viii—Ca2—O4—P1vi6.79 (8)
P1ix—Ca2—P1—O3iii175.05 (9)O3vii—Ca2—O4—P1vi94.68 (10)
O2iii—Ca2—P1—O3ii97.44 (11)P1—Ca2—O4—P1vi172.54 (11)
O2vii—Ca2—P1—O3ii174.29 (11)P1ix—Ca2—O4—P1vi81.76 (9)
O2viii—Ca2—P1—O3ii172.3 (3)O2iii—Ca2—O4—Ca150.60 (10)
O4ix—Ca2—P1—O3ii93.33 (14)O2vii—Ca2—O4—Ca112.81 (19)
O4—Ca2—P1—O3ii11.65 (10)O2viii—Ca2—O4—Ca1124.57 (10)
O4vi—Ca2—P1—O3ii59.00 (11)O4ix—Ca2—O4—Ca177.16 (14)
O3iii—Ca2—P1—O3ii98.50 (17)O4vi—Ca2—O4—Ca1156.07 (12)
O3viii—Ca2—P1—O3ii10.99 (14)O3iii—Ca2—O4—Ca118.75 (8)
O3vii—Ca2—P1—O3ii115.06 (10)O3viii—Ca2—O4—Ca1131.03 (11)
P1vi—Ca2—P1—O3ii8.19 (9)O3vii—Ca2—O4—Ca1127.50 (8)
P1ix—Ca2—P1—O3ii86.46 (9)P1—Ca2—O4—Ca149.64 (8)
O2iii—Ca2—P1—O2x93.44 (16)P1vi—Ca2—O4—Ca1137.82 (15)
O2vii—Ca2—P1—O2x16.60 (18)P1ix—Ca2—O4—Ca1140.42 (8)
O2viii—Ca2—P1—O2x18.6 (2)O2iii—Ca2—O4—Ca2i167.21 (9)
O4ix—Ca2—P1—O2x75.79 (16)O2vii—Ca2—O4—Ca2i103.80 (14)
O4—Ca2—P1—O2x179.23 (14)O2viii—Ca2—O4—Ca2i118.81 (8)
O4vi—Ca2—P1—O2x110.12 (14)O3iii—Ca2—O4—Ca2i97.86 (8)
O3iii—Ca2—P1—O2x92.39 (15)O3viii—Ca2—O4—Ca2i112.35 (10)
O3viii—Ca2—P1—O2x179.89 (13)O3vii—Ca2—O4—Ca2i10.89 (12)
O3vii—Ca2—P1—O2x54.06 (13)P1—Ca2—O4—Ca2i66.98 (6)
P1vi—Ca2—P1—O2x177.30 (13)P1vi—Ca2—O4—Ca2i105.57 (12)
P1ix—Ca2—P1—O2x82.66 (13)P1ix—Ca2—O4—Ca2i23.80 (7)
O2iii—Ca2—P1—O4ix169.23 (11)O4—Ca1—Cl1—Cl1iv45.48 (11)
O2vii—Ca2—P1—O4ix92.39 (12)O3—Ca1—Cl1—Cl1iv154.84 (7)
O2viii—Ca2—P1—O4ix94.4 (3)O3i—Ca1—Cl1—Cl1iv20.33 (6)
O4—Ca2—P1—O4ix104.98 (15)O3ii—Ca1—Cl1—Cl1iv66.42 (5)
O4vi—Ca2—P1—O4ix34.33 (12)O3iii—Ca1—Cl1—Cl1iv119.75 (4)
O3iii—Ca2—P1—O4ix168.18 (13)Cl1i—Ca1—Cl1—Cl1iv180.000 (2)
O3viii—Ca2—P1—O4ix104.32 (11)O2—Ca1—Cl1—Cl1iv85.06 (3)
O3vii—Ca2—P1—O4ix21.73 (11)P1—Ca1—Cl1—Cl1iv92.543 (12)
P1vi—Ca2—P1—O4ix101.51 (10)Cl1v—Ca1—Cl1—Cl1iv180.000 (2)
P1ix—Ca2—P1—O4ix6.87 (10)P1vi—Ca1—Cl1—Cl1iv5.63 (8)
O2iii—Ca2—P1—Ca154.13 (6)O4—Ca1—Cl1—Ca1x83.14 (13)
O2vii—Ca2—P1—Ca1130.97 (6)O3—Ca1—Cl1—Ca1x76.53 (8)
O2viii—Ca2—P1—Ca1129.0 (3)O3i—Ca1—Cl1—Ca1x148.95 (7)
O4ix—Ca2—P1—Ca1136.64 (10)O3ii—Ca1—Cl1—Ca1x62.21 (6)
O4—Ca2—P1—Ca131.66 (5)O3iii—Ca1—Cl1—Ca1x8.87 (7)
O4vi—Ca2—P1—Ca1102.31 (6)Cl1i—Ca1—Cl1—Ca1x51.38 (5)
O3iii—Ca2—P1—Ca155.18 (9)O2—Ca1—Cl1—Ca1x146.32 (5)
O3viii—Ca2—P1—Ca132.32 (5)P1—Ca1—Cl1—Ca1x36.08 (4)
O3vii—Ca2—P1—Ca1158.37 (4)Cl1iv—Ca1—Cl1—Ca1x128.62 (5)
P1vi—Ca2—P1—Ca135.13 (2)Cl1v—Ca1—Cl1—Ca1x51.38 (5)
P1ix—Ca2—P1—Ca1129.769 (18)P1vi—Ca1—Cl1—Ca1x122.99 (9)
O2iii—Ca2—P1—Ca2i136.57 (6)O4—Ca1—Cl1—Ca1xi174.11 (10)
O2vii—Ca2—P1—Ca2i146.58 (6)O3—Ca1—Cl1—Ca1xi26.22 (9)
O2viii—Ca2—P1—Ca2i148.6 (3)O3i—Ca1—Cl1—Ca1xi108.29 (7)
O4ix—Ca2—P1—Ca2i54.19 (10)O3ii—Ca1—Cl1—Ca1xi164.96 (8)
O4—Ca2—P1—Ca2i50.79 (5)O3iii—Ca1—Cl1—Ca1xi111.62 (6)
O4vi—Ca2—P1—Ca2i19.86 (6)Cl1i—Ca1—Cl1—Ca1xi51.38 (5)
O3iii—Ca2—P1—Ca2i137.63 (9)O2—Ca1—Cl1—Ca1xi43.56 (6)
O3viii—Ca2—P1—Ca2i50.13 (5)P1—Ca1—Cl1—Ca1xi138.83 (5)
O3vii—Ca2—P1—Ca2i75.92 (4)Cl1iv—Ca1—Cl1—Ca1xi128.62 (5)
P1vi—Ca2—P1—Ca2i47.321 (13)Cl1v—Ca1—Cl1—Ca1xi51.38 (5)
P1ix—Ca2—P1—Ca2i47.321 (13)P1vi—Ca1—Cl1—Ca1xi134.25 (9)
O2iii—Ca2—P1—Ca1ix143.76 (6)O4—Ca1—Cl1—Ca1xiv3.87 (12)
O2vii—Ca2—P1—Ca1ix66.92 (6)O3—Ca1—Cl1—Ca1xiv163.54 (7)
O2viii—Ca2—P1—Ca1ix68.9 (3)O3i—Ca1—Cl1—Ca1xiv61.94 (6)
O4ix—Ca2—P1—Ca1ix25.47 (10)O3ii—Ca1—Cl1—Ca1xiv24.81 (5)
O4—Ca2—P1—Ca1ix130.45 (5)O3iii—Ca1—Cl1—Ca1xiv78.14 (5)
O4vi—Ca2—P1—Ca1ix59.80 (6)Cl1i—Ca1—Cl1—Ca1xiv138.39 (3)
O3iii—Ca2—P1—Ca1ix142.71 (9)O2—Ca1—Cl1—Ca1xiv126.67 (4)
O3viii—Ca2—P1—Ca1ix129.79 (5)P1—Ca1—Cl1—Ca1xiv50.93 (2)
O3vii—Ca2—P1—Ca1ix3.74 (4)Cl1iv—Ca1—Cl1—Ca1xiv41.61 (3)
P1vi—Ca2—P1—Ca1ix126.984 (19)Cl1v—Ca1—Cl1—Ca1xiv138.39 (3)
P1ix—Ca2—P1—Ca1ix32.342 (19)P1vi—Ca1—Cl1—Ca1xiv35.98 (8)
O2iii—Ca2—P1—Ca1x3.86 (7)O4—Ca1—Cl1—Ca1iv45.48 (11)
O2vii—Ca2—P1—Ca1x72.98 (7)O3—Ca1—Cl1—Ca1iv154.84 (7)
O2viii—Ca2—P1—Ca1x71.0 (3)O3i—Ca1—Cl1—Ca1iv20.33 (5)
O4ix—Ca2—P1—Ca1x165.37 (11)O3ii—Ca1—Cl1—Ca1iv66.42 (5)
O4—Ca2—P1—Ca1x89.65 (7)O3iii—Ca1—Cl1—Ca1iv119.75 (4)
O4vi—Ca2—P1—Ca1x160.30 (7)Cl1i—Ca1—Cl1—Ca1iv180.000 (2)
O3iii—Ca2—P1—Ca1x2.81 (9)O2—Ca1—Cl1—Ca1iv85.06 (3)
O3viii—Ca2—P1—Ca1x90.31 (7)P1—Ca1—Cl1—Ca1iv92.543 (13)
O3vii—Ca2—P1—Ca1x143.64 (6)Cl1iv—Ca1—Cl1—Ca1iv0
P1vi—Ca2—P1—Ca1x93.12 (6)Cl1v—Ca1—Cl1—Ca1iv180.000 (2)
P1ix—Ca2—P1—Ca1x172.24 (5)P1vi—Ca1—Cl1—Ca1iv5.63 (8)
O4—Ca1—O2—P1xi180O4—Ca1—Cl1—Ca1xv87.09 (10)
O3—Ca1—O2—P1xi98.83 (6)O3—Ca1—Cl1—Ca1xv113.23 (8)
O3i—Ca1—O2—P1xi98.83 (6)O3i—Ca1—Cl1—Ca1xv21.28 (6)
O3ii—Ca1—O2—P1xi94.05 (14)O3ii—Ca1—Cl1—Ca1xv108.03 (7)
O3iii—Ca1—O2—P1xi94.05 (14)O3iii—Ca1—Cl1—Ca1xv161.37 (5)
Cl1—Ca1—O2—P1xi27.88 (5)Cl1i—Ca1—Cl1—Ca1xv138.39 (3)
Cl1i—Ca1—O2—P1xi27.88 (5)O2—Ca1—Cl1—Ca1xv43.45 (4)
Cl1iv—Ca1—O2—P1xi40.48 (4)P1—Ca1—Cl1—Ca1xv134.15 (4)
Cl1v—Ca1—O2—P1xi40.48 (4)Cl1iv—Ca1—Cl1—Ca1xv41.61 (3)
O3—Ca1—O2—Ca2viii36.95 (6)Cl1v—Ca1—Cl1—Ca1xv138.39 (3)
O3i—Ca1—O2—Ca2viii125.38 (9)P1vi—Ca1—Cl1—Ca1xv47.24 (8)
Symmetry codes: (i) x, y, z+1/2; (ii) xy+1, x+1, z+1/2; (iii) xy+1, x+1, z; (iv) x, y+2, z+1; (v) x, y+2, z1/2; (vi) y+1, xy+1, z; (vii) y, x+y, z; (viii) x, y+1, z; (ix) x+y, x+1, z; (x) y+1, xy+2, z; (xi) x+y1, x+1, z; (xii) x, y+1, z+1/2; (xiii) y1, x+y, z; (xiv) xy+1, x+1, z+1; (xv) y1, x+y, z+1.
(4_low_needle) chlorapatite top
Crystal data top
3(O4P)·Cl·5(Ca)Dx = 3.191 Mg m3
Mr = 520.76Mo Kα radiation, λ = 0.7107 Å
Trigonal, P63/mCell parameters from 1998 reflections
Hall symbol: -P 6cθ = 3.9–37.3°
a = 9.6343 (1) ŵ = 3.23 mm1
c = 6.7430 (1) ÅT = 100 K
V = 542.03 (1) Å3Prism, colourless
Z = 20.17 × 0.07 × 0.05 mm
F(000) = 516
Data collection top
BRUKER APPEX-II CCD
diffractometer
435 independent reflections
Radiation source: fine-focus sealed tube414 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.044
ω and phi scansθmax = 27.1°, θmin = 2.4°
Absorption correction: multi-scan
BRUKER SADABS
h = 120
Tmin = 0.685, Tmax = 1k = 012
15064 measured reflectionsl = 08
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.015 w = 1/[σ2(Fo2) + (0.016P)2 + 0.5862P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.037(Δ/σ)max < 0.001
S = 1.05Δρmax = 0.32 e Å3
435 reflectionsΔρmin = 0.29 e Å3
41 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0213 (12)
Crystal data top
3(O4P)·Cl·5(Ca)Z = 2
Mr = 520.76Mo Kα radiation
Trigonal, P63/mµ = 3.23 mm1
a = 9.6343 (1) ÅT = 100 K
c = 6.7430 (1) Å0.17 × 0.07 × 0.05 mm
V = 542.03 (1) Å3
Data collection top
BRUKER APPEX-II CCD
diffractometer
435 independent reflections
Absorption correction: multi-scan
BRUKER SADABS
414 reflections with I > 2σ(I)
Tmin = 0.685, Tmax = 1Rint = 0.044
15064 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.01541 parameters
wR(F2) = 0.0370 restraints
S = 1.05Δρmax = 0.32 e Å3
435 reflectionsΔρmin = 0.29 e Å3
Special details top

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ca10.00612 (5)0.74564 (5)0.250.00567 (14)
Ca20.33330.66670.00351 (7)0.00628 (15)
P10.37500 (6)0.96722 (6)0.250.00424 (15)
O20.34398 (19)0.50758 (18)0.250.0082 (3)
O30.08685 (13)0.64682 (14)0.06647 (17)0.0119 (3)
O40.12817 (18)0.59312 (18)0.250.0089 (3)
Cl1010.4417 (2)0.0142 (3)0.5
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0065 (2)0.0064 (2)0.0048 (2)0.00381 (17)00
Ca20.00763 (19)0.00763 (19)0.0036 (3)0.00382 (9)00
P10.0042 (3)0.0037 (3)0.0046 (3)0.0018 (2)00
O20.0099 (7)0.0080 (7)0.0089 (7)0.0062 (6)00
O30.0082 (5)0.0194 (6)0.0102 (6)0.0084 (5)0.0032 (4)0.0091 (5)
O40.0060 (7)0.0056 (7)0.0140 (8)0.0020 (6)00
Cl10.0084 (3)0.0084 (3)0.0257 (8)0.00421 (16)00
Geometric parameters (Å, º) top
Ca1—O42.2956 (16)Ca2—P1vi3.2102 (5)
Ca1—O32.3259 (11)Ca2—P1ix3.2102 (5)
Ca1—O3i2.3259 (11)P1—O3iii1.5342 (11)
Ca1—O3ii2.5249 (12)P1—O3ii1.5342 (11)
Ca1—O3iii2.5249 (12)P1—O2x1.5340 (16)
Ca1—Cl12.7973 (8)P1—O4ix1.5465 (16)
Ca1—Cl1i2.7973 (8)P1—Ca2i3.2102 (5)
Ca1—O22.9835 (16)P1—Ca1ix3.3908 (7)
Ca1—P13.0985 (7)O2—P1xi1.5340 (16)
Ca1—Cl1iv3.2363 (9)O2—Ca2viii2.4007 (11)
Ca1—Cl1v3.2363 (9)O2—Ca2xii2.4007 (11)
Ca1—P1vi3.3908 (7)O3—P1xiii1.5342 (11)
Ca2—O2iii2.4007 (11)O3—Ca1xiii2.5249 (12)
Ca2—O2vii2.4007 (11)O3—Ca2viii2.7949 (12)
Ca2—O2viii2.4007 (11)O4—P1vi1.5465 (16)
Ca2—O4ix2.4353 (11)O4—Ca2i2.4353 (11)
Ca2—O42.4353 (11)Cl1—Cl1iv0.786 (3)
Ca2—O4vi2.4353 (11)Cl1—Ca1x2.7973 (8)
Ca2—O3iii2.7949 (12)Cl1—Ca1xi2.7973 (8)
Ca2—O3viii2.7949 (12)Cl1—Ca1xiv3.2363 (9)
Ca2—O3vii2.7949 (12)Cl1—Ca1iv3.2363 (9)
Ca2—P13.2102 (5)Cl1—Ca1xv3.2363 (9)
O4—Ca1—O387.34 (3)O2vii—Ca2—P188.49 (3)
O4—Ca1—O3i87.34 (3)O2viii—Ca2—P1165.84 (3)
O3—Ca1—O3i133.12 (6)O4ix—Ca2—P127.70 (4)
O4—Ca1—O3ii75.31 (4)O4—Ca2—P166.79 (4)
O3—Ca1—O3ii140.12 (5)O4vi—Ca2—P199.10 (3)
O3i—Ca1—O3ii82.42 (2)O3iii—Ca2—P128.54 (2)
O4—Ca1—O3iii75.31 (4)O3viii—Ca2—P1122.70 (3)
O3—Ca1—O3iii82.42 (2)O3vii—Ca2—P193.92 (3)
O3i—Ca1—O3iii140.12 (5)O2iii—Ca2—P1vi88.49 (3)
O3ii—Ca1—O3iii58.70 (5)O2vii—Ca2—P1vi165.84 (3)
O4—Ca1—Cl1143.39 (3)O2viii—Ca2—P1vi99.36 (3)
O3—Ca1—Cl1127.60 (4)O4ix—Ca2—P1vi99.10 (3)
O3i—Ca1—Cl176.24 (4)O4—Ca2—P1vi27.70 (4)
O3ii—Ca1—Cl170.28 (3)O4vi—Ca2—P1vi66.79 (4)
O3iii—Ca1—Cl196.65 (3)O3iii—Ca2—P1vi93.92 (3)
O4—Ca1—Cl1i143.39 (3)O3viii—Ca2—P1vi28.54 (2)
O3—Ca1—Cl1i76.24 (4)O3vii—Ca2—P1vi122.70 (3)
O3i—Ca1—Cl1i127.60 (4)P1—Ca2—P1vi94.282 (12)
O3ii—Ca1—Cl1i96.65 (3)O2iii—Ca2—P1ix165.84 (3)
O3iii—Ca1—Cl1i70.28 (3)O2vii—Ca2—P1ix99.36 (3)
Cl1—Ca1—Cl1i55.06 (5)O2viii—Ca2—P1ix88.49 (3)
O4—Ca1—O2104.59 (5)O4ix—Ca2—P1ix66.79 (4)
O3—Ca1—O268.24 (3)O4—Ca2—P1ix99.10 (3)
O3i—Ca1—O268.24 (3)O4vi—Ca2—P1ix27.70 (4)
O3ii—Ca1—O2150.57 (3)O3iii—Ca2—P1ix122.70 (3)
O3iii—Ca1—O2150.57 (3)O3viii—Ca2—P1ix93.92 (3)
Cl1—Ca1—O299.35 (3)O3vii—Ca2—P1ix28.54 (2)
Cl1i—Ca1—O299.35 (3)P1—Ca2—P1ix94.282 (12)
O4—Ca1—P170.30 (4)P1vi—Ca2—P1ix94.282 (12)
O3—Ca1—P1110.87 (3)O3iii—P1—O3ii107.54 (9)
O3i—Ca1—P1110.87 (3)O3iii—P1—O2x112.10 (5)
O3ii—Ca1—P129.47 (3)O3ii—P1—O2x112.10 (5)
O3iii—Ca1—P129.47 (3)O3iii—P1—O4ix106.75 (6)
Cl1—Ca1—P185.169 (13)O3ii—P1—O4ix106.75 (6)
Cl1i—Ca1—P185.169 (13)O2x—P1—O4ix111.28 (9)
O2—Ca1—P1174.89 (3)O3iii—P1—Ca154.07 (5)
O4—Ca1—Cl1iv133.93 (2)O3ii—P1—Ca154.07 (5)
O3—Ca1—Cl1iv138.60 (4)O2x—P1—Ca1136.32 (7)
O3i—Ca1—Cl1iv64.63 (4)O4ix—P1—Ca1112.40 (6)
O3ii—Ca1—Cl1iv65.76 (3)O3iii—P1—Ca260.52 (5)
O3iii—Ca1—Cl1iv102.65 (3)O3ii—P1—Ca2111.53 (5)
Cl1—Ca1—Cl1iv12.43 (4)O2x—P1—Ca2135.65 (4)
Cl1i—Ca1—Cl1iv67.490 (11)O4ix—P1—Ca247.04 (4)
O2—Ca1—Cl1iv98.08 (2)Ca1—P1—Ca278.200 (13)
P1—Ca1—Cl1iv85.825 (12)O3iii—P1—Ca2i111.53 (5)
O4—Ca1—Cl1v133.93 (2)O3ii—P1—Ca2i60.52 (5)
O3—Ca1—Cl1v64.63 (4)O2x—P1—Ca2i135.65 (4)
O3i—Ca1—Cl1v138.60 (4)O4ix—P1—Ca2i47.04 (4)
O3ii—Ca1—Cl1v102.65 (3)Ca1—P1—Ca2i78.200 (13)
O3iii—Ca1—Cl1v65.76 (3)Ca2—P1—Ca2i64.349 (18)
Cl1—Ca1—Cl1v67.490 (11)O3iii—P1—Ca1ix122.06 (5)
Cl1i—Ca1—Cl1v12.43 (4)O3ii—P1—Ca1ix122.06 (5)
O2—Ca1—Cl1v98.08 (2)O2x—P1—Ca1ix76.55 (6)
P1—Ca1—Cl1v85.825 (12)Ca1—P1—Ca1ix147.13 (2)
Cl1iv—Ca1—Cl1v79.92 (4)Ca2—P1—Ca1ix74.098 (12)
O4—Ca1—P1vi22.57 (4)Ca2i—P1—Ca1ix74.098 (12)
O3—Ca1—P1vi78.79 (3)O3iii—P1—Ca1x80.26 (5)
O3i—Ca1—P1vi78.79 (3)O3ii—P1—Ca1x80.26 (5)
O3ii—Ca1—P1vi94.93 (3)O2x—P1—Ca1x56.15 (6)
O3iii—Ca1—P1vi94.93 (3)O4ix—P1—Ca1x167.43 (6)
Cl1—Ca1—P1vi152.36 (3)Ca1—P1—Ca1x80.168 (19)
Cl1i—Ca1—P1vi152.36 (3)Ca2—P1—Ca1x140.748 (13)
O2—Ca1—P1vi82.02 (3)Ca2i—P1—Ca1x140.748 (13)
P1—Ca1—P1vi92.87 (2)Ca1ix—P1—Ca1x132.70 (2)
Cl1iv—Ca1—P1vi139.97 (2)P1xi—O2—Ca2viii133.53 (4)
Cl1v—Ca1—P1vi139.97 (2)P1xi—O2—Ca2xii133.53 (4)
O2iii—Ca2—O2vii77.35 (4)Ca2viii—O2—Ca2xii87.63 (5)
O2iii—Ca2—O2viii77.35 (4)P1xi—O2—Ca198.57 (7)
O2vii—Ca2—O2viii77.35 (4)Ca2viii—O2—Ca196.34 (4)
O2iii—Ca2—O4ix126.49 (5)Ca2xii—O2—Ca196.34 (4)
O2vii—Ca2—O4ix89.80 (4)P1xiii—O3—Ca1138.87 (6)
O2viii—Ca2—O4ix150.06 (5)P1xiii—O3—Ca1xiii96.46 (6)
O2iii—Ca2—O489.80 (4)Ca1—O3—Ca1xiii119.23 (5)
O2vii—Ca2—O4150.06 (5)P1xiii—O3—Ca2viii90.94 (5)
O2viii—Ca2—O4126.49 (5)Ca1—O3—Ca2viii103.46 (5)
O4ix—Ca2—O476.17 (4)Ca1xiii—O3—Ca2viii96.72 (4)
O2iii—Ca2—O4vi150.06 (5)P1vi—O4—Ca1122.70 (8)
O2vii—Ca2—O4vi126.49 (5)P1vi—O4—Ca2i105.26 (6)
O2viii—Ca2—O4vi89.80 (4)Ca1—O4—Ca2i114.50 (5)
O4ix—Ca2—O4vi76.17 (4)P1vi—O4—Ca2105.26 (6)
O4—Ca2—O4vi76.17 (4)Ca1—O4—Ca2114.50 (5)
O2iii—Ca2—O3iii70.82 (4)Ca2i—O4—Ca289.17 (5)
O2vii—Ca2—O3iii81.91 (4)Cl1iv—Cl1—Ca1117.53 (3)
O2viii—Ca2—O3iii145.06 (4)Cl1iv—Cl1—Ca1x117.53 (3)
O4ix—Ca2—O3iii55.92 (4)Ca1—Cl1—Ca1x100.34 (3)
O4—Ca2—O3iii68.29 (4)Cl1iv—Cl1—Ca1xi117.53 (3)
O4vi—Ca2—O3iii125.09 (4)Ca1—Cl1—Ca1xi100.34 (3)
O2iii—Ca2—O3viii81.91 (4)Ca1x—Cl1—Ca1xi100.34 (3)
O2vii—Ca2—O3viii145.06 (4)Cl1iv—Cl1—Ca1xiv50.038 (19)
O2viii—Ca2—O3viii70.82 (4)Ca1—Cl1—Ca1xiv87.536 (9)
O4ix—Ca2—O3viii125.09 (4)Ca1x—Cl1—Ca1xiv87.536 (9)
O4—Ca2—O3viii55.92 (4)Ca1xi—Cl1—Ca1xiv167.57 (4)
O4vi—Ca2—O3viii68.29 (4)Cl1iv—Cl1—Ca1iv50.04 (2)
O3iii—Ca2—O3viii117.209 (14)Ca1—Cl1—Ca1iv167.57 (4)
O2iii—Ca2—O3vii145.06 (4)Ca1x—Cl1—Ca1iv87.536 (9)
O2vii—Ca2—O3vii70.82 (4)Ca1xi—Cl1—Ca1iv87.536 (9)
O2viii—Ca2—O3vii81.91 (4)Ca1xiv—Cl1—Ca1iv83.18 (3)
O4ix—Ca2—O3vii68.29 (4)Cl1iv—Cl1—Ca1xv50.04 (2)
O4—Ca2—O3vii125.09 (4)Ca1—Cl1—Ca1xv87.536 (9)
O4vi—Ca2—O3vii55.92 (4)Ca1x—Cl1—Ca1xv167.57 (4)
O3iii—Ca2—O3vii117.209 (14)Ca1xi—Cl1—Ca1xv87.536 (9)
O3viii—Ca2—O3vii117.209 (14)Ca1xiv—Cl1—Ca1xv83.18 (3)
O2iii—Ca2—P199.36 (3)Ca1iv—Cl1—Ca1xv83.18 (3)
O4—Ca1—P1—O3iii94.95 (6)O3i—Ca1—O2—Ca2viii125.21 (5)
O3—Ca1—P1—O3iii15.86 (5)O3ii—Ca1—O2—Ca2viii130.04 (7)
O3i—Ca1—P1—O3iii174.04 (8)O3iii—Ca1—O2—Ca2viii41.73 (10)
O3ii—Ca1—P1—O3iii170.09 (11)Cl1—Ca1—O2—Ca2viii163.78 (4)
Cl1—Ca1—P1—O3iii112.68 (6)Cl1i—Ca1—O2—Ca2viii107.91 (4)
Cl1i—Ca1—P1—O3iii57.41 (6)Cl1iv—Ca1—O2—Ca2viii176.29 (3)
Cl1iv—Ca1—P1—O3iii125.14 (6)Cl1v—Ca1—O2—Ca2viii95.40 (4)
Cl1v—Ca1—P1—O3iii44.96 (6)O4—Ca1—O2—Ca2xii44.15 (3)
P1vi—Ca1—P1—O3iii94.95 (6)O3—Ca1—O2—Ca2xii125.21 (5)
O4—Ca1—P1—O3ii94.95 (6)O3i—Ca1—O2—Ca2xii36.90 (4)
O3—Ca1—P1—O3ii174.04 (8)O3ii—Ca1—O2—Ca2xii41.73 (10)
O3i—Ca1—P1—O3ii15.86 (5)O3iii—Ca1—O2—Ca2xii130.04 (7)
O3iii—Ca1—P1—O3ii170.09 (11)Cl1—Ca1—O2—Ca2xii107.91 (4)
Cl1—Ca1—P1—O3ii57.41 (6)Cl1i—Ca1—O2—Ca2xii163.78 (4)
Cl1i—Ca1—P1—O3ii112.68 (6)Cl1iv—Ca1—O2—Ca2xii95.40 (4)
Cl1iv—Ca1—P1—O3ii44.96 (6)Cl1v—Ca1—O2—Ca2xii176.29 (3)
Cl1v—Ca1—P1—O3ii125.14 (6)O4—Ca1—O3—P1xiii32.37 (11)
P1vi—Ca1—P1—O3ii94.95 (6)O3i—Ca1—O3—P1xiii116.23 (10)
O4—Ca1—P1—O2x180O3ii—Ca1—O3—P1xiii30.79 (18)
O3—Ca1—P1—O2x100.91 (3)O3iii—Ca1—O3—P1xiii43.16 (13)
O3i—Ca1—P1—O2x100.91 (3)Cl1—Ca1—O3—P1xiii135.73 (9)
O3ii—Ca1—P1—O2x85.05 (6)Cl1i—Ca1—O3—P1xiii114.63 (11)
O3iii—Ca1—P1—O2x85.05 (6)O2—Ca1—O3—P1xiii139.24 (12)
Cl1—Ca1—P1—O2x27.64 (3)P1—Ca1—O3—P1xiii35.36 (12)
Cl1i—Ca1—P1—O2x27.63 (3)Cl1iv—Ca1—O3—P1xiii143.71 (9)
Cl1iv—Ca1—P1—O2x40.09 (2)Cl1v—Ca1—O3—P1xiii109.87 (11)
Cl1v—Ca1—P1—O2x40.09 (2)P1vi—Ca1—O3—P1xiii53.44 (11)
P1vi—Ca1—P1—O2x180O4—Ca1—O3—Ca1xiii179.18 (6)
O4—Ca1—P1—O4ix0O3i—Ca1—O3—Ca1xiii96.97 (8)
O3—Ca1—P1—O4ix79.09 (3)O3ii—Ca1—O3—Ca1xiii116.01 (4)
O3i—Ca1—P1—O4ix79.09 (3)O3iii—Ca1—O3—Ca1xiii103.65 (3)
O3ii—Ca1—P1—O4ix94.95 (6)Cl1—Ca1—O3—Ca1xiii11.08 (8)
O3iii—Ca1—P1—O4ix94.95 (6)Cl1i—Ca1—O3—Ca1xiii32.18 (5)
Cl1—Ca1—P1—O4ix152.37 (3)O2—Ca1—O3—Ca1xiii73.96 (6)
Cl1i—Ca1—P1—O4ix152.36 (3)P1—Ca1—O3—Ca1xiii111.44 (4)
Cl1iv—Ca1—P1—O4ix139.91 (2)Cl1iv—Ca1—O3—Ca1xiii3.10 (9)
Cl1v—Ca1—P1—O4ix139.91 (2)Cl1v—Ca1—O3—Ca1xiii36.93 (4)
P1vi—Ca1—P1—O4ix0P1vi—Ca1—O3—Ca1xiii159.76 (5)
O4—Ca1—P1—Ca232.956 (9)O4—Ca1—O3—Ca2viii75.05 (5)
O3—Ca1—P1—Ca246.13 (4)O3i—Ca1—O3—Ca2viii8.80 (9)
O3i—Ca1—P1—Ca2112.05 (3)O3ii—Ca1—O3—Ca2viii138.22 (7)
O3ii—Ca1—P1—Ca2127.91 (6)O3iii—Ca1—O3—Ca2viii150.59 (4)
O3iii—Ca1—P1—Ca262.00 (6)Cl1—Ca1—O3—Ca2viii116.85 (4)
Cl1—Ca1—P1—Ca2174.68 (3)Cl1i—Ca1—O3—Ca2viii137.94 (4)
Cl1i—Ca1—P1—Ca2119.41 (3)O2—Ca1—O3—Ca2viii31.81 (4)
Cl1iv—Ca1—P1—Ca2172.87 (2)P1—Ca1—O3—Ca2viii142.79 (3)
Cl1v—Ca1—P1—Ca2106.95 (2)Cl1iv—Ca1—O3—Ca2viii108.86 (5)
P1vi—Ca1—P1—Ca232.956 (9)Cl1v—Ca1—O3—Ca2viii142.70 (4)
O4—Ca1—P1—Ca2i32.956 (9)P1vi—Ca1—O3—Ca2viii53.99 (3)
O3—Ca1—P1—Ca2i112.05 (3)O3—Ca1—O4—P1vi66.70 (3)
O3i—Ca1—P1—Ca2i46.13 (4)O3i—Ca1—O4—P1vi66.70 (3)
O3ii—Ca1—P1—Ca2i62.00 (6)O3ii—Ca1—O4—P1vi149.56 (3)
O3iii—Ca1—P1—Ca2i127.91 (6)O3iii—Ca1—O4—P1vi149.56 (3)
Cl1—Ca1—P1—Ca2i119.41 (3)Cl1—Ca1—O4—P1vi129.20 (5)
Cl1i—Ca1—P1—Ca2i174.68 (3)Cl1i—Ca1—O4—P1vi129.20 (5)
Cl1iv—Ca1—P1—Ca2i106.95 (2)O2—Ca1—O4—P1vi0
Cl1v—Ca1—P1—Ca2i172.87 (2)P1—Ca1—O4—P1vi180
P1vi—Ca1—P1—Ca2i32.956 (9)Cl1iv—Ca1—O4—P1vi116.89 (4)
O4—Ca1—P1—Ca1ix0Cl1v—Ca1—O4—P1vi116.89 (4)
O3—Ca1—P1—Ca1ix79.09 (3)O3—Ca1—O4—Ca2i163.78 (5)
O3i—Ca1—P1—Ca1ix79.09 (3)O3i—Ca1—O4—Ca2i62.82 (5)
O3ii—Ca1—P1—Ca1ix94.95 (6)O3ii—Ca1—O4—Ca2i20.04 (5)
O3iii—Ca1—P1—Ca1ix94.95 (6)O3iii—Ca1—O4—Ca2i80.92 (6)
Cl1—Ca1—P1—Ca1ix152.37 (3)Cl1—Ca1—O4—Ca2i0.32 (9)
Cl1i—Ca1—P1—Ca1ix152.36 (3)Cl1i—Ca1—O4—Ca2i101.28 (4)
Cl1iv—Ca1—P1—Ca1ix139.91 (2)O2—Ca1—O4—Ca2i129.52 (4)
Cl1v—Ca1—P1—Ca1ix139.91 (2)P1—Ca1—O4—Ca2i50.48 (4)
P1vi—Ca1—P1—Ca1ix0Cl1iv—Ca1—O4—Ca2i12.63 (8)
O4—Ca1—P1—Ca1x180Cl1v—Ca1—O4—Ca2i113.59 (3)
O3—Ca1—P1—Ca1x100.91 (3)P1vi—Ca1—O4—Ca2i129.52 (4)
O3i—Ca1—P1—Ca1x100.91 (3)O3—Ca1—O4—Ca262.82 (5)
O3ii—Ca1—P1—Ca1x85.05 (6)O3i—Ca1—O4—Ca2163.78 (5)
O3iii—Ca1—P1—Ca1x85.05 (6)O3ii—Ca1—O4—Ca280.92 (6)
Cl1—Ca1—P1—Ca1x27.64 (3)O3iii—Ca1—O4—Ca220.04 (5)
Cl1i—Ca1—P1—Ca1x27.64 (3)Cl1—Ca1—O4—Ca2101.28 (4)
Cl1iv—Ca1—P1—Ca1x40.09 (2)Cl1i—Ca1—O4—Ca20.32 (9)
Cl1v—Ca1—P1—Ca1x40.09 (2)O2—Ca1—O4—Ca2129.52 (4)
P1vi—Ca1—P1—Ca1x180P1—Ca1—O4—Ca250.48 (4)
O2iii—Ca2—P1—O3iii1.17 (6)Cl1iv—Ca1—O4—Ca2113.59 (3)
O2vii—Ca2—P1—O3iii75.75 (6)Cl1v—Ca1—O4—Ca212.63 (8)
O2viii—Ca2—P1—O3iii74.14 (15)P1vi—Ca1—O4—Ca2129.52 (4)
O4ix—Ca2—P1—O3iii168.20 (8)O2iii—Ca2—O4—P1vi87.13 (6)
O4—Ca2—P1—O3iii86.90 (6)O2vii—Ca2—O4—P1vi150.72 (7)
O4vi—Ca2—P1—O3iii157.50 (6)O2viii—Ca2—O4—P1vi13.09 (8)
O3viii—Ca2—P1—O3iii87.52 (3)O4ix—Ca2—O4—P1vi145.04 (6)
O3vii—Ca2—P1—O3iii146.41 (6)O4vi—Ca2—O4—P1vi66.16 (8)
P1vi—Ca2—P1—O3iii90.34 (5)O3iii—Ca2—O4—P1vi156.51 (6)
P1ix—Ca2—P1—O3iii175.03 (5)O3viii—Ca2—O4—P1vi6.77 (4)
O2iii—Ca2—P1—O3ii97.42 (6)O3vii—Ca2—O4—P1vi94.72 (6)
O2vii—Ca2—P1—O3ii174.33 (6)P1—Ca2—O4—P1vi172.59 (6)
O2viii—Ca2—P1—O3ii172.72 (15)P1ix—Ca2—O4—P1vi81.81 (5)
O4ix—Ca2—P1—O3ii93.22 (8)O2iii—Ca2—O4—Ca150.58 (6)
O4—Ca2—P1—O3ii11.69 (6)O2vii—Ca2—O4—Ca113.01 (11)
O4vi—Ca2—P1—O3ii58.92 (6)O2viii—Ca2—O4—Ca1124.62 (6)
O3iii—Ca2—P1—O3ii98.58 (10)O4ix—Ca2—O4—Ca177.25 (8)
O3viii—Ca2—P1—O3ii11.06 (8)O4vi—Ca2—O4—Ca1156.13 (7)
O3vii—Ca2—P1—O3ii115.01 (6)O3iii—Ca2—O4—Ca118.80 (4)
P1vi—Ca2—P1—O3ii8.24 (5)O3viii—Ca2—O4—Ca1130.93 (6)
P1ix—Ca2—P1—O3ii86.39 (5)O3vii—Ca2—O4—Ca1127.57 (4)
O2iii—Ca2—P1—O2x93.45 (9)P1—Ca2—O4—Ca149.70 (4)
O2vii—Ca2—P1—O2x16.53 (10)P1vi—Ca2—O4—Ca1137.71 (8)
O2viii—Ca2—P1—O2x18.14 (13)P1ix—Ca2—O4—Ca1140.48 (4)
O4ix—Ca2—P1—O2x75.92 (9)O2iii—Ca2—O4—Ca2i167.27 (5)
O4—Ca2—P1—O2x179.18 (8)O2vii—Ca2—O4—Ca2i103.68 (8)
O4vi—Ca2—P1—O2x110.22 (8)O2viii—Ca2—O4—Ca2i118.69 (5)
O3iii—Ca2—P1—O2x92.28 (8)O3iii—Ca2—O4—Ca2i97.89 (5)
O3viii—Ca2—P1—O2x179.80 (7)O3viii—Ca2—O4—Ca2i112.37 (6)
O3vii—Ca2—P1—O2x54.13 (8)O3vii—Ca2—O4—Ca2i10.88 (7)
P1vi—Ca2—P1—O2x177.38 (7)P1—Ca2—O4—Ca2i66.99 (3)
P1ix—Ca2—P1—O2x82.75 (7)P1vi—Ca2—O4—Ca2i105.60 (7)
O2iii—Ca2—P1—O4ix169.37 (7)P1ix—Ca2—O4—Ca2i23.79 (4)
O2vii—Ca2—P1—O4ix92.45 (7)O4—Ca1—Cl1—Cl1iv45.45 (6)
O2viii—Ca2—P1—O4ix94.07 (15)O3—Ca1—Cl1—Cl1iv154.75 (4)
O4—Ca2—P1—O4ix104.90 (9)O3i—Ca1—Cl1—Cl1iv20.36 (3)
O4vi—Ca2—P1—O4ix34.30 (7)O3ii—Ca1—Cl1—Cl1iv66.40 (3)
O3iii—Ca2—P1—O4ix168.20 (8)O3iii—Ca1—Cl1—Cl1iv119.72 (3)
O3viii—Ca2—P1—O4ix104.28 (7)Cl1i—Ca1—Cl1—Cl1iv180
O3vii—Ca2—P1—O4ix21.79 (6)O2—Ca1—Cl1—Cl1iv85.075 (16)
P1vi—Ca2—P1—O4ix101.46 (6)P1—Ca1—Cl1—Cl1iv92.525 (7)
P1ix—Ca2—P1—O4ix6.83 (6)Cl1v—Ca1—Cl1—Cl1iv180
O2iii—Ca2—P1—Ca154.04 (3)P1vi—Ca1—Cl1—Cl1iv5.57 (4)
O2vii—Ca2—P1—Ca1130.96 (3)O4—Ca1—Cl1—Ca1x83.23 (7)
O2viii—Ca2—P1—Ca1129.34 (14)O3—Ca1—Cl1—Ca1x76.57 (4)
O4ix—Ca2—P1—Ca1136.59 (6)O3i—Ca1—Cl1—Ca1x149.04 (4)
O4—Ca2—P1—Ca131.69 (3)O3ii—Ca1—Cl1—Ca1x62.28 (3)
O4vi—Ca2—P1—Ca1102.29 (3)O3iii—Ca1—Cl1—Ca1x8.96 (4)
O3iii—Ca2—P1—Ca155.21 (5)Cl1i—Ca1—Cl1—Ca1x51.32 (2)
O3viii—Ca2—P1—Ca132.31 (3)O2—Ca1—Cl1—Ca1x146.25 (2)
O3vii—Ca2—P1—Ca1158.38 (3)P1—Ca1—Cl1—Ca1x36.15 (2)
P1vi—Ca2—P1—Ca135.133 (11)Cl1iv—Ca1—Cl1—Ca1x128.68 (3)
P1ix—Ca2—P1—Ca1129.762 (10)Cl1v—Ca1—Cl1—Ca1x51.32 (2)
O2iii—Ca2—P1—Ca2i136.49 (3)P1vi—Ca1—Cl1—Ca1x123.11 (5)
O2vii—Ca2—P1—Ca2i146.59 (3)O4—Ca1—Cl1—Ca1xi174.13 (5)
O2viii—Ca2—P1—Ca2i148.21 (14)O3—Ca1—Cl1—Ca1xi26.07 (5)
O4ix—Ca2—P1—Ca2i54.14 (6)O3i—Ca1—Cl1—Ca1xi108.32 (4)
O4—Ca2—P1—Ca2i50.76 (3)O3ii—Ca1—Cl1—Ca1xi164.92 (4)
O4vi—Ca2—P1—Ca2i19.84 (3)O3iii—Ca1—Cl1—Ca1xi111.60 (3)
O3iii—Ca2—P1—Ca2i137.66 (5)Cl1i—Ca1—Cl1—Ca1xi51.32 (2)
O3viii—Ca2—P1—Ca2i50.13 (3)O2—Ca1—Cl1—Ca1xi43.60 (3)
O3vii—Ca2—P1—Ca2i75.93 (2)P1—Ca1—Cl1—Ca1xi138.80 (3)
P1vi—Ca2—P1—Ca2i47.314 (7)Cl1iv—Ca1—Cl1—Ca1xi128.68 (3)
P1ix—Ca2—P1—Ca2i47.314 (7)Cl1v—Ca1—Cl1—Ca1xi51.32 (2)
O2iii—Ca2—P1—Ca1ix143.83 (3)P1vi—Ca1—Cl1—Ca1xi134.25 (5)
O2vii—Ca2—P1—Ca1ix66.92 (3)O4—Ca1—Cl1—Ca1xiv3.82 (7)
O2viii—Ca2—P1—Ca1ix68.53 (14)O3—Ca1—Cl1—Ca1xiv163.61 (4)
O4ix—Ca2—P1—Ca1ix25.53 (6)O3i—Ca1—Cl1—Ca1xiv62.00 (3)
O4—Ca2—P1—Ca1ix130.44 (3)O3ii—Ca1—Cl1—Ca1xiv24.76 (3)
O4vi—Ca2—P1—Ca1ix59.83 (3)O3iii—Ca1—Cl1—Ca1xiv78.08 (3)
O3iii—Ca2—P1—Ca1ix142.67 (5)Cl1i—Ca1—Cl1—Ca1xiv138.364 (15)
O3viii—Ca2—P1—Ca1ix129.81 (3)O2—Ca1—Cl1—Ca1xiv126.71 (2)
O3vii—Ca2—P1—Ca1ix3.74 (2)P1—Ca1—Cl1—Ca1xiv50.889 (13)
P1vi—Ca2—P1—Ca1ix126.989 (10)Cl1iv—Ca1—Cl1—Ca1xiv41.636 (16)
P1ix—Ca2—P1—Ca1ix32.361 (11)Cl1v—Ca1—Cl1—Ca1xiv138.364 (15)
O2iii—Ca2—P1—Ca1x3.86 (4)P1vi—Ca1—Cl1—Ca1xiv36.07 (5)
O2vii—Ca2—P1—Ca1x73.06 (4)O4—Ca1—Cl1—Ca1iv45.45 (6)
O2viii—Ca2—P1—Ca1x71.44 (15)O3—Ca1—Cl1—Ca1iv154.75 (4)
O4ix—Ca2—P1—Ca1x165.51 (7)O3i—Ca1—Cl1—Ca1iv20.36 (3)
O4—Ca2—P1—Ca1x89.59 (4)O3ii—Ca1—Cl1—Ca1iv66.40 (3)
O4vi—Ca2—P1—Ca1x160.19 (4)O3iii—Ca1—Cl1—Ca1iv119.72 (3)
O3iii—Ca2—P1—Ca1x2.69 (5)Cl1i—Ca1—Cl1—Ca1iv180
O3viii—Ca2—P1—Ca1x90.21 (4)O2—Ca1—Cl1—Ca1iv85.075 (16)
O3vii—Ca2—P1—Ca1x143.72 (3)P1—Ca1—Cl1—Ca1iv92.525 (7)
P1vi—Ca2—P1—Ca1x93.03 (3)Cl1iv—Ca1—Cl1—Ca1iv0
P1ix—Ca2—P1—Ca1x172.34 (3)Cl1v—Ca1—Cl1—Ca1iv180
O4—Ca1—O2—P1xi180P1vi—Ca1—Cl1—Ca1iv5.57 (4)
O3—Ca1—O2—P1xi98.94 (3)O4—Ca1—Cl1—Ca1xv87.09 (6)
O3i—Ca1—O2—P1xi98.94 (3)O3—Ca1—Cl1—Ca1xv113.12 (4)
O3ii—Ca1—O2—P1xi94.11 (8)O3i—Ca1—Cl1—Ca1xv21.28 (3)
O3iii—Ca1—O2—P1xi94.11 (8)O3ii—Ca1—Cl1—Ca1xv108.04 (4)
Cl1—Ca1—O2—P1xi27.93 (3)O3iii—Ca1—Cl1—Ca1xv161.36 (3)
Cl1i—Ca1—O2—P1xi27.93 (3)Cl1i—Ca1—Cl1—Ca1xv138.364 (15)
Cl1iv—Ca1—O2—P1xi40.44 (2)O2—Ca1—Cl1—Ca1xv43.44 (2)
Cl1v—Ca1—O2—P1xi40.44 (2)P1—Ca1—Cl1—Ca1xv134.161 (19)
P1vi—Ca1—O2—P1xi180Cl1iv—Ca1—Cl1—Ca1xv41.636 (16)
O4—Ca1—O2—Ca2viii44.15 (3)Cl1v—Ca1—Cl1—Ca1xv138.364 (15)
O3—Ca1—O2—Ca2viii36.90 (4)P1vi—Ca1—Cl1—Ca1xv47.21 (4)
Symmetry codes: (i) x, y, z+1/2; (ii) xy+1, x+1, z+1/2; (iii) xy+1, x+1, z; (iv) x, y+2, z+1; (v) x, y+2, z1/2; (vi) y+1, xy+1, z; (vii) y, x+y, z; (viii) x, y+1, z; (ix) x+y, x+1, z; (x) y+1, xy+2, z; (xi) x+y1, x+1, z; (xii) x, y+1, z+1/2; (xiii) y1, x+y, z; (xiv) xy+1, x+1, z+1; (xv) y1, x+y, z+1.
(C_mono) top
Crystal data top
Ca5ClO12P3F(000) = 1032
Mr = 520.76Dx = 3.176 Mg m3
MOnoclinic, P21/cMo Kα radiation, λ = 0.7107 Å
Hall symbol: -P 2ybcCell parameters from 1997 reflections
a = 9.6410 (2) Åθ = 3.9–27.4°
b = 6.7620 (3) ŵ = 3.21 mm1
c = 19.2850 (6) ÅT = 293 K
β = 119.984 (1)°Prism, colourless
V = 1088.97 (6) Å30.25 × 0.12 × 0.05 mm
Z = 4
Data collection top
BRUKER APPEX-II CCD
diffractometer
2218 independent reflections
Radiation source: fine-focus sealed tube1276 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.024
ω and phi scansθmax = 26.4°, θmin = 2.4°
Absorption correction: multi-scan
BRUKER SADABS
h = 1210
Tmin = 0.836, Tmax = 1k = 08
2218 measured reflectionsl = 024
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.023 w = 1/[σ2(Fo2) + (0.0326P)2 + 1.2162P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.073(Δ/σ)max < 0.001
S = 1.10Δρmax = 0.45 e Å3
2218 reflectionsΔρmin = 0.43 e Å3
201 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0128 (5)
Crystal data top
Ca5ClO12P3V = 1088.97 (6) Å3
Mr = 520.76Z = 4
MOnoclinic, P21/cMo Kα radiation
a = 9.6410 (2) ŵ = 3.21 mm1
b = 6.7620 (3) ÅT = 293 K
c = 19.2850 (6) Å0.25 × 0.12 × 0.05 mm
β = 119.984 (1)°
Data collection top
BRUKER APPEX-II CCD
diffractometer
2218 independent reflections
Absorption correction: multi-scan
BRUKER SADABS
1276 reflections with I > 2σ(I)
Tmin = 0.836, Tmax = 1Rint = 0.024
2218 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.023201 parameters
wR(F2) = 0.0730 restraints
S = 1.10Δρmax = 0.45 e Å3
2218 reflectionsΔρmin = 0.43 e Å3
Special details top

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ca10.74427 (6)1.24994 (11)0.00218 (3)0.01032 (15)
Ca20.66623 (8)0.99678 (9)0.16680 (4)0.01149 (18)
Ca30.66711 (8)0.50351 (9)0.16656 (4)0.00955 (18)
Ca40.26017 (6)0.25004 (12)0.12789 (3)0.01037 (15)
Ca50.00431 (6)0.75013 (12)0.13005 (3)0.01043 (15)
O10.9139 (2)1.0673 (3)0.13375 (13)0.0136 (5)
O20.8727 (2)1.2492 (4)0.23252 (10)0.0137 (4)
O30.5922 (2)1.2513 (4)0.06349 (11)0.0141 (4)
O40.3531 (3)1.0675 (4)0.04315 (13)0.0188 (5)
O50.5351 (2)1.2508 (4)0.20397 (10)0.0135 (4)
O60.7335 (3)1.0672 (4)0.32352 (14)0.0181 (5)
O70.6562 (2)0.7502 (4)0.07418 (11)0.0136 (4)
O80.8516 (2)0.7490 (4)0.25390 (11)0.0136 (4)
O90.4919 (2)0.7509 (4)0.17192 (11)0.0138 (4)
O100.9127 (3)0.4332 (4)0.13292 (15)0.0235 (6)
O110.7328 (3)0.4335 (4)0.32309 (15)0.0186 (5)
O120.3539 (3)0.4326 (4)0.04367 (13)0.0179 (5)
P10.96738 (7)1.25012 (14)0.18741 (4)0.00696 (16)
P20.40743 (7)1.25011 (14)0.01632 (4)0.00685 (16)
P30.62516 (7)1.25027 (14)0.29630 (4)0.00677 (16)
Cl1A0.0038 (3)0.5571 (3)0.00083 (16)0.0288 (9)0.503 (3)
Cl1B0.0035 (3)0.9453 (3)0.00075 (16)0.0234 (8)0.497 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0125 (3)0.0080 (3)0.0125 (3)0.0003 (3)0.0077 (2)0.0002 (3)
Ca20.0138 (3)0.0063 (4)0.0140 (4)0.0001 (2)0.0067 (3)0.0001 (2)
Ca30.0125 (3)0.0058 (4)0.0118 (3)0.0000 (2)0.0072 (3)0.0001 (2)
Ca40.0104 (3)0.0079 (3)0.0125 (3)0.0010 (3)0.0055 (2)0.0013 (3)
Ca50.0127 (3)0.0079 (3)0.0103 (3)0.0002 (3)0.0055 (2)0.0004 (3)
O10.0123 (11)0.0085 (12)0.0104 (11)0.0013 (10)0.0015 (9)0.0080 (10)
O20.0121 (8)0.0216 (10)0.0096 (8)0.0003 (12)0.0069 (7)0.0024 (12)
O30.0085 (8)0.0223 (11)0.0121 (9)0.0020 (11)0.0057 (7)0.0030 (12)
O40.0323 (14)0.0158 (14)0.0143 (12)0.0139 (12)0.0161 (11)0.0055 (11)
O50.0102 (8)0.0208 (10)0.0078 (9)0.0019 (11)0.0033 (7)0.0006 (12)
O60.0203 (12)0.0137 (14)0.0276 (13)0.0103 (11)0.0175 (11)0.0143 (11)
O70.0202 (9)0.0120 (9)0.0088 (9)0.0034 (11)0.0073 (7)0.0039 (11)
O80.0081 (8)0.0122 (9)0.0150 (9)0.0028 (11)0.0018 (7)0.0008 (12)
O90.0164 (9)0.0118 (9)0.0207 (10)0.0014 (11)0.0149 (8)0.0031 (12)
O100.0171 (12)0.0243 (15)0.0217 (13)0.0079 (12)0.0041 (11)0.0086 (12)
O110.0129 (11)0.0165 (14)0.0302 (14)0.0059 (10)0.0137 (11)0.0104 (12)
O120.0253 (13)0.0151 (14)0.0161 (12)0.0104 (11)0.0124 (11)0.0034 (11)
P10.0069 (3)0.0072 (3)0.0067 (3)0.0009 (4)0.0033 (2)0.0002 (4)
P20.0075 (3)0.0070 (3)0.0067 (3)0.0010 (4)0.0040 (2)0.0005 (4)
P30.0068 (3)0.0071 (3)0.0073 (3)0.0003 (4)0.0042 (2)0.0001 (4)
Cl1A0.0166 (8)0.055 (2)0.0156 (8)0.0025 (15)0.0089 (7)0.0029 (16)
Cl1B0.0143 (8)0.043 (2)0.0148 (8)0.0021 (14)0.0085 (7)0.0007 (15)
Geometric parameters (Å, º) top
Ca1—O32.2983 (18)Ca5—Cl1Avii3.215 (3)
Ca1—O4i2.331 (2)Ca5—Cl1Bx3.253 (2)
Ca1—O12i2.335 (2)Ca5—P1vi3.3922 (8)
Ca1—O10ii2.537 (3)O1—P11.527 (2)
Ca1—O12.548 (2)O1—Ca5iii2.330 (2)
Ca1—Cl1Ai2.768 (2)O2—P11.5443 (18)
Ca1—Cl1Bi2.852 (3)O2—Ca5ix2.2999 (18)
Ca1—O9i2.969 (2)O2—Ca3ii2.446 (2)
Ca1—P13.1157 (8)O3—P21.5428 (18)
Ca1—Cl1Biii3.197 (3)O3—Ca3ii2.438 (2)
Ca1—Cl1Aiv3.275 (2)O4—P21.529 (2)
Ca1—P23.3920 (8)O4—Ca1i2.331 (2)
Ca2—O92.401 (2)O4—Ca4ii2.541 (2)
Ca2—O72.410 (2)O5—P31.5424 (18)
Ca2—O82.413 (2)O5—Ca4ii2.3001 (18)
Ca2—O22.441 (2)O5—Ca3ii2.445 (2)
Ca2—O52.443 (2)O6—P31.533 (2)
Ca2—O32.453 (2)O6—Ca4ix2.329 (2)
Ca2—O62.797 (2)O6—Ca5ix2.541 (2)
Ca2—O42.799 (3)O7—P2i1.5335 (18)
Ca2—O12.803 (2)O7—Ca5iii2.9679 (19)
Ca2—P33.2125 (10)O8—P1xi1.5339 (18)
Ca2—P23.2163 (10)O8—Ca4ix2.969 (2)
Ca2—P13.2201 (10)O9—P3vi1.5300 (18)
Ca3—O82.400 (2)O9—Ca1i2.969 (2)
Ca3—O72.404 (2)O10—P1v1.537 (3)
Ca3—O92.416 (2)O10—Ca5iii2.329 (3)
Ca3—O3v2.438 (2)O10—Ca1v2.537 (3)
Ca3—O5v2.445 (2)O11—P3v1.530 (2)
Ca3—O2v2.446 (2)O11—Ca4ix2.327 (3)
Ca3—O102.790 (2)O11—Ca5vi2.547 (2)
Ca3—O122.795 (2)O12—P2v1.529 (2)
Ca3—O112.798 (3)O12—Ca1i2.335 (2)
Ca3—P1v3.2117 (10)P1—O8xii1.5339 (18)
Ca3—P2v3.2169 (10)P1—O10ii1.537 (3)
Ca3—P3v3.2199 (10)P1—Ca3ii3.2117 (10)
Ca4—O5v2.3001 (18)P1—Ca5ix3.3922 (8)
Ca4—O11vi2.327 (3)P2—O12ii1.529 (2)
Ca4—O6vi2.329 (2)P2—O7i1.5335 (18)
Ca4—O122.538 (2)P2—Ca4ii3.1143 (8)
Ca4—O4v2.541 (2)P2—Ca3ii3.2169 (10)
Ca4—Cl1Bvii2.808 (3)P3—O9ix1.5300 (18)
Ca4—Cl1Avii2.819 (3)P3—O11ii1.530 (2)
Ca4—O8vi2.969 (2)P3—Ca5ix3.1156 (8)
Ca4—P2v3.1143 (8)P3—Ca3ii3.2199 (10)
Ca4—Cl1A3.233 (3)P3—Ca4ii3.3923 (8)
Ca4—Cl1Bv3.239 (2)Cl1A—Cl1Avii0.779 (4)
Ca4—P3v3.3923 (8)Cl1A—Ca1i2.768 (2)
Ca5—O2vi2.2999 (18)Cl1A—Ca4vii2.819 (3)
Ca5—O10viii2.329 (3)Cl1A—Ca5vii3.215 (3)
Ca5—O1viii2.330 (2)Cl1A—Ca1xiii3.275 (2)
Ca5—O6vi2.541 (2)Cl1B—Cl1Bx0.744 (4)
Ca5—O11ix2.547 (2)Cl1B—Ca4vii2.808 (3)
Ca5—Cl1B2.789 (2)Cl1B—Ca1i2.852 (3)
Ca5—Cl1A2.839 (3)Cl1B—Ca1viii3.197 (3)
Ca5—O7viii2.9679 (19)Cl1B—Ca4ii3.239 (2)
Ca5—P3vi3.1156 (8)Cl1B—Ca5x3.253 (2)
O3—Ca1—O4i87.47 (8)O2vi—Ca5—Cl1B143.09 (8)
O3—Ca1—O12i87.08 (9)O10viii—Ca5—Cl1B128.00 (8)
O4i—Ca1—O12i133.94 (7)O1viii—Ca5—Cl1B75.42 (8)
O3—Ca1—O10ii75.09 (7)O6vi—Ca5—Cl1B97.07 (8)
O4i—Ca1—O10ii139.49 (9)O11ix—Ca5—Cl1B70.39 (7)
O12i—Ca1—O10ii82.19 (9)O2vi—Ca5—Cl1A142.56 (9)
O3—Ca1—O175.32 (7)O10viii—Ca5—Cl1A76.48 (8)
O4i—Ca1—O182.23 (8)O1viii—Ca5—Cl1A128.02 (8)
O12i—Ca1—O1139.46 (8)O6vi—Ca5—Cl1A69.45 (8)
O10ii—Ca1—O158.23 (6)O11ix—Ca5—Cl1A95.64 (7)
O3—Ca1—Cl1Ai142.31 (9)Cl1B—Ca5—Cl1A55.63 (5)
O4i—Ca1—Cl1Ai128.39 (8)O2vi—Ca5—O7viii104.88 (6)
O12i—Ca1—Cl1Ai75.79 (8)O10viii—Ca5—O7viii68.61 (8)
O10ii—Ca1—Cl1Ai69.55 (8)O1viii—Ca5—O7viii68.81 (8)
O1—Ca1—Cl1Ai96.21 (8)O6vi—Ca5—O7viii150.82 (8)
O3—Ca1—Cl1Bi143.40 (8)O11ix—Ca5—O7viii150.79 (8)
O4i—Ca1—Cl1Bi76.04 (7)Cl1B—Ca5—O7viii98.91 (7)
O12i—Ca1—Cl1Bi127.70 (7)Cl1A—Ca5—O7viii100.26 (7)
O10ii—Ca1—Cl1Bi96.54 (8)O2vi—Ca5—P3vi70.19 (5)
O1—Ca1—Cl1Bi70.28 (7)O10viii—Ca5—P3vi110.58 (7)
Cl1Ai—Ca1—Cl1Bi55.69 (5)O1viii—Ca5—P3vi110.30 (6)
O3—Ca1—O9i104.82 (6)O6vi—Ca5—P3vi29.26 (5)
O4i—Ca1—O9i68.70 (8)O11ix—Ca5—P3vi29.22 (6)
O12i—Ca1—O9i68.71 (8)Cl1B—Ca5—P3vi85.42 (6)
O10ii—Ca1—O9i150.80 (9)Cl1A—Ca5—P3vi84.12 (6)
O1—Ca1—O9i150.83 (8)O7viii—Ca5—P3vi175.07 (4)
Cl1Ai—Ca1—O9i99.84 (7)O2vi—Ca5—Cl1Avii133.64 (8)
Cl1Bi—Ca1—O9i99.27 (7)O10viii—Ca5—Cl1Avii63.98 (7)
O3—Ca1—P170.28 (5)O1viii—Ca5—Cl1Avii138.95 (7)
O4i—Ca1—P1110.38 (6)O6vi—Ca5—Cl1Avii66.00 (7)
O12i—Ca1—P1110.53 (6)O11ix—Ca5—Cl1Avii102.94 (7)
O10ii—Ca1—P129.33 (6)Cl1B—Ca5—Cl1Avii68.51 (7)
O1—Ca1—P129.13 (5)Cl1A—Ca5—Cl1Avii12.96 (8)
Cl1Ai—Ca1—P184.51 (6)O7viii—Ca5—Cl1Avii97.67 (6)
Cl1Bi—Ca1—P185.02 (6)P3vi—Ca5—Cl1Avii86.09 (5)
O9i—Ca1—P1175.10 (4)O2vi—Ca5—Cl1Bx134.05 (8)
O3—Ca1—Cl1Biii133.68 (8)O10viii—Ca5—Cl1Bx138.33 (8)
O4i—Ca1—Cl1Biii64.45 (7)O1viii—Ca5—Cl1Bx65.49 (7)
O12i—Ca1—Cl1Biii139.04 (7)O6vi—Ca5—Cl1Bx101.40 (7)
O10ii—Ca1—Cl1Biii102.21 (8)O11ix—Ca5—Cl1Bx65.37 (7)
O1—Ca1—Cl1Biii65.41 (7)Cl1B—Ca5—Cl1Bx11.08 (9)
Cl1Ai—Ca1—Cl1Biii68.22 (8)Cl1A—Ca5—Cl1Bx66.63 (7)
Cl1Bi—Ca1—Cl1Biii12.54 (7)O7viii—Ca5—Cl1Bx98.88 (6)
O9i—Ca1—Cl1Biii98.38 (7)P3vi—Ca5—Cl1Bx84.90 (5)
P1—Ca1—Cl1Biii85.29 (5)Cl1Avii—Ca5—Cl1Bx79.54 (5)
O3—Ca1—Cl1Aiv134.13 (8)O2vi—Ca5—P1vi22.54 (5)
O4i—Ca1—Cl1Aiv138.20 (7)O10viii—Ca5—P1vi79.05 (7)
O12i—Ca1—Cl1Aiv65.08 (8)O1viii—Ca5—P1vi78.78 (6)
O10ii—Ca1—Cl1Aiv65.97 (7)O6vi—Ca5—P1vi94.84 (5)
O1—Ca1—Cl1Aiv102.08 (7)O11ix—Ca5—P1vi94.71 (6)
Cl1Ai—Ca1—Cl1Aiv11.27 (10)Cl1B—Ca5—P1vi151.65 (6)
Cl1Bi—Ca1—Cl1Aiv66.95 (7)Cl1A—Ca5—P1vi152.38 (5)
O9i—Ca1—Cl1Aiv98.17 (7)O7viii—Ca5—P1vi82.34 (4)
P1—Ca1—Cl1Aiv85.65 (5)P3vi—Ca5—P1vi92.73 (2)
Cl1Biii—Ca1—Cl1Aiv79.48 (5)Cl1Avii—Ca5—P1vi139.68 (5)
O3—Ca1—P222.47 (4)Cl1Bx—Ca5—P1vi140.57 (5)
O4i—Ca1—P278.95 (6)P1—O1—Ca5iii139.59 (13)
O12i—Ca1—P278.88 (6)P1—O1—Ca196.54 (11)
O10ii—Ca1—P294.75 (6)Ca5iii—O1—Ca1118.65 (9)
O1—Ca1—P294.82 (5)P1—O1—Ca291.21 (9)
Cl1Ai—Ca1—P2151.67 (6)Ca5iii—O1—Ca2102.98 (8)
Cl1Bi—Ca1—P2152.30 (5)Ca1—O1—Ca296.49 (7)
O9i—Ca1—P282.35 (4)P1—O2—Ca5ix122.65 (10)
P1—Ca1—P292.75 (2)P1—O2—Ca2105.58 (11)
Cl1Biii—Ca1—P2139.79 (4)Ca5ix—O2—Ca2114.67 (10)
Cl1Aiv—Ca1—P2140.53 (5)P1—O2—Ca3ii104.93 (11)
O9—Ca2—O777.40 (8)Ca5ix—O2—Ca3ii114.49 (9)
O9—Ca2—O877.33 (7)Ca2—O2—Ca3ii89.03 (6)
O7—Ca2—O877.11 (7)P2—O3—Ca1122.82 (10)
O9—Ca2—O2150.30 (7)P2—O3—Ca3ii105.59 (11)
O7—Ca2—O2126.07 (7)Ca1—O3—Ca3ii114.63 (9)
O8—Ca2—O289.77 (8)P2—O3—Ca2104.89 (11)
O9—Ca2—O589.96 (8)Ca1—O3—Ca2114.41 (9)
O7—Ca2—O5150.35 (7)Ca3ii—O3—Ca288.93 (6)
O8—Ca2—O5126.57 (7)P2—O4—Ca1i139.33 (12)
O2—Ca2—O576.31 (7)P2—O4—Ca4ii96.67 (12)
O9—Ca2—O3126.41 (7)Ca1i—O4—Ca4ii118.90 (8)
O7—Ca2—O389.77 (8)P2—O4—Ca291.15 (10)
O8—Ca2—O3150.02 (7)Ca1i—O4—Ca2102.87 (9)
O2—Ca2—O376.24 (7)Ca4ii—O4—Ca296.43 (7)
O5—Ca2—O376.22 (7)P3—O5—Ca4ii122.75 (10)
O9—Ca2—O682.10 (7)P3—O5—Ca2105.16 (11)
O7—Ca2—O6145.14 (8)Ca4ii—O5—Ca2114.30 (9)
O8—Ca2—O671.03 (7)P3—O5—Ca3ii105.45 (11)
O2—Ca2—O668.36 (7)Ca4ii—O5—Ca3ii114.66 (9)
O5—Ca2—O655.78 (6)Ca2—O5—Ca3ii89.00 (6)
O3—Ca2—O6125.04 (8)P3—O6—Ca4ix139.26 (12)
O9—Ca2—O470.98 (7)P3—O6—Ca5ix96.62 (12)
O7—Ca2—O481.97 (7)Ca4ix—O6—Ca5ix119.00 (9)
O8—Ca2—O4145.09 (8)P3—O6—Ca290.98 (10)
O2—Ca2—O4125.12 (8)Ca4ix—O6—Ca2102.89 (9)
O5—Ca2—O468.51 (6)Ca5ix—O6—Ca296.68 (7)
O3—Ca2—O455.67 (6)P2i—O7—Ca3133.37 (15)
O6—Ca2—O4117.40 (6)P2i—O7—Ca2133.58 (15)
O9—Ca2—O1145.14 (8)Ca3—O7—Ca287.71 (6)
O7—Ca2—O170.87 (7)P2i—O7—Ca5iii98.62 (9)
O8—Ca2—O181.82 (7)Ca3—O7—Ca5iii96.21 (7)
O2—Ca2—O155.45 (6)Ca2—O7—Ca5iii96.42 (7)
O5—Ca2—O1124.87 (8)P1xi—O8—Ca3133.79 (15)
O3—Ca2—O168.37 (6)P1xi—O8—Ca2133.16 (15)
O6—Ca2—O1116.93 (6)Ca3—O8—Ca287.73 (6)
O4—Ca2—O1117.13 (7)P1xi—O8—Ca4ix98.58 (9)
O9—Ca2—P388.67 (6)Ca3—O8—Ca4ix96.57 (7)
O7—Ca2—P3166.05 (6)Ca2—O8—Ca4ix96.10 (7)
O8—Ca2—P399.52 (6)P3vi—O9—Ca2133.63 (15)
O2—Ca2—P366.96 (5)P3vi—O9—Ca3133.38 (15)
O5—Ca2—P327.61 (4)Ca2—O9—Ca387.65 (6)
O3—Ca2—P399.09 (6)P3vi—O9—Ca1i98.66 (9)
O6—Ca2—P328.50 (5)Ca2—O9—Ca1i96.42 (7)
O4—Ca2—P394.10 (5)Ca3—O9—Ca1i96.19 (7)
O1—Ca2—P3122.41 (5)P1v—O10—Ca5iii138.84 (14)
O9—Ca2—P299.36 (5)P1v—O10—Ca1v96.69 (13)
O7—Ca2—P288.52 (6)Ca5iii—O10—Ca1v119.19 (10)
O8—Ca2—P2165.62 (6)P1v—O10—Ca391.12 (10)
O2—Ca2—P299.19 (6)Ca5iii—O10—Ca3102.99 (10)
O5—Ca2—P266.95 (5)Ca1v—O10—Ca396.80 (8)
O3—Ca2—P227.62 (4)P3v—O11—Ca4ix139.38 (12)
O6—Ca2—P2122.73 (5)P3v—O11—Ca5vi96.44 (12)
O4—Ca2—P228.38 (5)Ca4ix—O11—Ca5vi118.79 (9)
O1—Ca2—P293.96 (5)P3v—O11—Ca391.32 (11)
P3—Ca2—P294.35 (3)Ca4ix—O11—Ca3103.15 (9)
O9—Ca2—P1165.89 (6)Ca5vi—O11—Ca396.52 (7)
O7—Ca2—P199.16 (5)P2v—O12—Ca1i138.93 (13)
O8—Ca2—P188.57 (6)P2v—O12—Ca496.78 (12)
O2—Ca2—P127.51 (4)Ca1i—O12—Ca4118.88 (8)
O5—Ca2—P199.02 (6)P2v—O12—Ca391.31 (10)
O3—Ca2—P166.77 (5)Ca1i—O12—Ca3103.00 (9)
O6—Ca2—P193.91 (5)Ca4—O12—Ca396.90 (7)
O4—Ca2—P1122.44 (5)O1—P1—O8xii111.74 (13)
O1—Ca2—P128.30 (5)O1—P1—O10ii107.73 (11)
P3—Ca2—P194.24 (3)O8xii—P1—O10ii112.57 (14)
P2—Ca2—P194.19 (3)O1—P1—O2106.50 (13)
O8—Ca3—O777.46 (7)O8xii—P1—O2111.06 (10)
O8—Ca3—O977.28 (7)O10ii—P1—O2106.91 (14)
O7—Ca3—O977.22 (7)O1—P1—Ca154.33 (9)
O8—Ca3—O3v150.40 (7)O8xii—P1—Ca1136.47 (8)
O7—Ca3—O3v89.76 (8)O10ii—P1—Ca153.98 (10)
O9—Ca3—O3v126.19 (7)O2—P1—Ca1112.46 (7)
O8—Ca3—O5v126.06 (7)O1—P1—Ca3ii111.66 (8)
O7—Ca3—O5v150.13 (7)O8xii—P1—Ca3ii135.81 (10)
O9—Ca3—O5v89.60 (8)O10ii—P1—Ca3ii60.30 (9)
O3v—Ca3—O5v76.46 (7)O2—P1—Ca3ii47.38 (9)
O8—Ca3—O2v89.87 (8)Ca1—P1—Ca3ii78.11 (2)
O7—Ca3—O2v126.66 (7)O1—P1—Ca260.49 (8)
O9—Ca3—O2v150.06 (7)O8xii—P1—Ca2135.38 (10)
O3v—Ca3—O2v76.42 (7)O10ii—P1—Ca2111.34 (9)
O5v—Ca3—O2v76.18 (7)O2—P1—Ca246.91 (9)
O8—Ca3—O1082.17 (7)Ca1—P1—Ca278.17 (2)
O7—Ca3—O1070.97 (7)Ca3ii—P1—Ca264.383 (17)
O9—Ca3—O10145.13 (8)O1—P1—Ca5ix121.88 (10)
O3v—Ca3—O1068.38 (7)O8xii—P1—Ca5ix76.26 (7)
O5v—Ca3—O10125.23 (8)O10ii—P1—Ca5ix122.12 (11)
O2v—Ca3—O1055.95 (7)Ca1—P1—Ca5ix147.27 (2)
O8—Ca3—O12145.22 (8)Ca3ii—P1—Ca5ix74.33 (2)
O7—Ca3—O1282.09 (7)Ca2—P1—Ca5ix74.22 (2)
O9—Ca3—O1270.91 (7)O1—P1—Ca4iv80.44 (8)
O3v—Ca3—O1255.55 (6)O8xii—P1—Ca4iv56.05 (7)
O5v—Ca3—O1268.22 (6)O10ii—P1—Ca4iv80.52 (9)
O2v—Ca3—O12124.85 (8)O2—P1—Ca4iv167.11 (7)
O10—Ca3—O12117.15 (7)Ca1—P1—Ca4iv80.427 (19)
O8—Ca3—O1170.80 (7)Ca3ii—P1—Ca4iv140.77 (3)
O7—Ca3—O11145.04 (8)Ca2—P1—Ca4iv140.90 (3)
O9—Ca3—O1181.78 (7)Ca5ix—P1—Ca4iv132.30 (2)
O3v—Ca3—O11125.18 (8)O4—P2—O12ii107.62 (11)
O5v—Ca3—O1155.51 (6)O4—P2—O7i111.97 (13)
O2v—Ca3—O1168.42 (6)O12ii—P2—O7i112.43 (13)
O10—Ca3—O11117.47 (7)O4—P2—O3107.13 (14)
O12—Ca3—O11116.85 (6)O12ii—P2—O3106.36 (14)
O8—Ca3—P1v88.61 (5)O7i—P2—O3111.01 (10)
O7—Ca3—P1v99.54 (6)O4—P2—Ca4ii54.15 (9)
O9—Ca3—P1v165.88 (6)O12ii—P2—Ca4ii54.04 (9)
O3v—Ca3—P1v67.06 (5)O7i—P2—Ca4ii136.46 (8)
O5v—Ca3—P1v99.20 (6)O3—P2—Ca4ii112.53 (7)
O2v—Ca3—P1v27.68 (4)O4—P2—Ca260.47 (10)
O10—Ca3—P1v28.58 (5)O12ii—P2—Ca2111.21 (9)
O12—Ca3—P1v122.61 (5)O7i—P2—Ca2135.63 (10)
O11—Ca3—P1v94.06 (5)O3—P2—Ca247.49 (9)
O8—Ca3—P2v166.07 (6)Ca4ii—P2—Ca278.02 (2)
O7—Ca3—P2v88.63 (6)O4—P2—Ca3ii111.68 (9)
O9—Ca3—P2v99.28 (6)O12ii—P2—Ca3ii60.31 (9)
O3v—Ca3—P2v27.51 (4)O7i—P2—Ca3ii135.59 (10)
O5v—Ca3—P2v66.92 (5)O3—P2—Ca3ii46.89 (9)
O2v—Ca3—P2v99.06 (6)Ca4ii—P2—Ca3ii78.24 (2)
O10—Ca3—P2v93.94 (6)Ca2—P2—Ca3ii64.367 (17)
O12—Ca3—P2v28.38 (5)O4—P2—Ca1122.06 (10)
O11—Ca3—P2v122.43 (5)O12ii—P2—Ca1121.99 (10)
P1v—Ca3—P2v94.34 (3)O7i—P2—Ca176.30 (7)
O8—Ca3—P3v99.17 (6)Ca4ii—P2—Ca1147.23 (2)
O7—Ca3—P3v165.67 (6)Ca2—P2—Ca174.35 (2)
O9—Ca3—P3v88.45 (6)Ca3ii—P2—Ca174.17 (2)
O3v—Ca3—P3v99.22 (6)O4—P2—Ca5x80.33 (10)
O5v—Ca3—P3v27.50 (4)O12ii—P2—Ca5x80.68 (9)
O2v—Ca3—P3v66.78 (5)O7i—P2—Ca5x56.01 (7)
O10—Ca3—P3v122.73 (6)O3—P2—Ca5x167.02 (7)
O12—Ca3—P3v93.75 (5)Ca4ii—P2—Ca5x80.452 (18)
O11—Ca3—P3v28.37 (5)Ca2—P2—Ca5x140.76 (3)
P1v—Ca3—P3v94.26 (3)Ca3ii—P2—Ca5x140.93 (3)
P2v—Ca3—P3v94.20 (2)Ca1—P2—Ca5x132.31 (2)
O5v—Ca4—O11vi87.28 (9)O9ix—P3—O11ii111.95 (13)
O5v—Ca4—O6vi87.19 (9)O9ix—P3—O6112.19 (13)
O11vi—Ca4—O6vi133.95 (8)O11ii—P3—O6107.88 (11)
O5v—Ca4—O1275.05 (7)O9ix—P3—O5111.09 (10)
O11vi—Ca4—O12139.42 (8)O11ii—P3—O5106.47 (14)
O6vi—Ca4—O1282.15 (8)O6—P3—O5106.95 (14)
O5v—Ca4—O4v75.36 (8)O9ix—P3—Ca5ix136.44 (8)
O11vi—Ca4—O4v82.32 (8)O11ii—P3—Ca5ix54.34 (9)
O6vi—Ca4—O4v139.38 (8)O6—P3—Ca5ix54.12 (9)
O12—Ca4—O4v58.14 (6)O5—P3—Ca5ix112.47 (7)
O5v—Ca4—Cl1Bvii142.20 (9)O9ix—P3—Ca2135.65 (10)
O11vi—Ca4—Cl1Bvii76.12 (8)O11ii—P3—Ca2111.61 (8)
O6vi—Ca4—Cl1Bvii128.54 (8)O6—P3—Ca260.52 (9)
O12—Ca4—Cl1Bvii95.83 (7)O5—P3—Ca247.23 (9)
O4v—Ca4—Cl1Bvii68.99 (7)Ca5ix—P3—Ca278.20 (2)
O5v—Ca4—Cl1Avii143.64 (8)O9ix—P3—Ca3ii135.57 (10)
O11vi—Ca4—Cl1Avii127.51 (7)O11ii—P3—Ca3ii60.31 (9)
O6vi—Ca4—Cl1Avii75.80 (8)O6—P3—Ca3ii111.52 (8)
O12—Ca4—Cl1Avii71.00 (7)O5—P3—Ca3ii47.05 (9)
O4v—Ca4—Cl1Avii96.94 (8)Ca5ix—P3—Ca3ii78.10 (2)
Cl1Bvii—Ca4—Cl1Avii55.64 (5)Ca2—P3—Ca3ii64.375 (17)
O5v—Ca4—O8vi104.77 (6)O9ix—P3—Ca4ii76.33 (7)
O11vi—Ca4—O8vi68.54 (8)O11ii—P3—Ca4ii121.83 (10)
O6vi—Ca4—O8vi68.89 (7)O6—P3—Ca4ii122.05 (11)
O12—Ca4—O8vi150.96 (8)Ca5ix—P3—Ca4ii147.24 (2)
O4v—Ca4—O8vi150.74 (8)Ca2—P3—Ca4ii74.18 (2)
Cl1Bvii—Ca4—O8vi100.35 (6)Ca3ii—P3—Ca4ii74.30 (2)
Cl1Avii—Ca4—O8vi98.75 (7)O9ix—P3—Ca1xiv56.04 (7)
O5v—Ca4—P2v70.30 (5)O11ii—P3—Ca1xiv80.58 (9)
O11vi—Ca4—P2v110.48 (6)O6—P3—Ca1xiv80.33 (9)
O6vi—Ca4—P2v110.39 (6)O5—P3—Ca1xiv167.13 (7)
O12—Ca4—P2v29.19 (5)Ca5ix—P3—Ca1xiv80.403 (18)
O4v—Ca4—P2v29.19 (5)Ca2—P3—Ca1xiv140.80 (3)
Cl1Bvii—Ca4—P2v83.93 (5)Ca3ii—P3—Ca1xiv140.86 (3)
Cl1Avii—Ca4—P2v85.68 (5)Ca4ii—P3—Ca1xiv132.36 (2)
O8vi—Ca4—P2v175.06 (4)Cl1Avii—Cl1A—Ca1i124.7 (4)
O5v—Ca4—Cl1A133.11 (8)Cl1Avii—Cl1A—Ca4vii115.6 (4)
O11vi—Ca4—Cl1A139.35 (7)Ca1i—Cl1A—Ca4vii100.90 (7)
O6vi—Ca4—Cl1A64.77 (8)Cl1Avii—Cl1A—Ca5112.2 (4)
O12—Ca4—Cl1A64.93 (7)Ca1i—Cl1A—Ca5100.37 (8)
O4v—Ca4—Cl1A101.42 (8)Ca4vii—Cl1A—Ca599.19 (8)
Cl1Bvii—Ca4—Cl1A68.03 (8)Cl1Avii—Cl1A—Ca5vii54.8 (4)
Cl1Avii—Ca4—Cl1A12.55 (9)Ca1i—Cl1A—Ca5vii88.79 (7)
O8vi—Ca4—Cl1A99.18 (6)Ca4vii—Cl1A—Ca5vii87.91 (8)
P2v—Ca4—Cl1A84.66 (5)Ca5—Cl1A—Ca5vii167.04 (8)
O5v—Ca4—Cl1Bv134.64 (8)Cl1Avii—Cl1A—Ca451.9 (4)
O11vi—Ca4—Cl1Bv64.85 (8)Ca1i—Cl1A—Ca488.41 (7)
O6vi—Ca4—Cl1Bv138.01 (7)Ca4vii—Cl1A—Ca4167.45 (9)
O12—Ca4—Cl1Bv102.74 (7)Ca5—Cl1A—Ca487.23 (7)
O4v—Ca4—Cl1Bv66.41 (7)Ca5vii—Cl1A—Ca483.87 (7)
Cl1Bvii—Ca4—Cl1Bv11.55 (9)Ca1i—Cl1A—Ca1xiii168.73 (10)
Cl1Avii—Ca4—Cl1Bv67.05 (8)Ca4vii—Cl1A—Ca1xiii86.72 (7)
O8vi—Ca4—Cl1Bv97.53 (6)Ca5—Cl1A—Ca1xiii86.42 (6)
P2v—Ca4—Cl1Bv86.18 (5)Ca5vii—Cl1A—Ca1xiii83.16 (6)
Cl1A—Ca4—Cl1Bv79.50 (5)Ca4—Cl1A—Ca1xiii82.91 (5)
O5v—Ca4—P3v22.48 (5)Cl1Bx—Cl1B—Ca5122.9 (4)
O11vi—Ca4—P3v78.80 (6)Cl1Bx—Cl1B—Ca4vii119.4 (4)
O6vi—Ca4—P3v78.95 (6)Ca5—Cl1B—Ca4vii100.69 (6)
O12—Ca4—P3v94.69 (6)Cl1Bx—Cl1B—Ca1i111.2 (4)
O4v—Ca4—P3v94.91 (6)Ca5—Cl1B—Ca1i99.56 (8)
Cl1Bvii—Ca4—P3v151.69 (6)Ca4vii—Cl1B—Ca1i99.13 (8)
Cl1Avii—Ca4—P3v152.36 (6)Cl1Bx—Cl1B—Ca1viii56.3 (4)
O8vi—Ca4—P3v82.28 (4)Ca5—Cl1B—Ca1viii88.75 (7)
P2v—Ca4—P3v92.78 (2)Ca4vii—Cl1B—Ca1viii88.43 (7)
Cl1A—Ca4—P3v139.82 (5)Ca1i—Cl1B—Ca1viii167.46 (7)
Cl1Bv—Ca4—P3v140.47 (5)Cl1Bx—Cl1B—Ca4ii49.1 (4)
O2vi—Ca5—O10viii87.32 (9)Ca5—Cl1B—Ca4ii87.93 (7)
O2vi—Ca5—O1viii87.28 (9)Ca4vii—Cl1B—Ca4ii168.45 (9)
O10viii—Ca5—O1viii133.96 (7)Ca1i—Cl1B—Ca4ii86.87 (6)
O2vi—Ca5—O6vi75.12 (7)Ca1viii—Cl1B—Ca4ii84.05 (6)
O10viii—Ca5—O6vi82.32 (8)Cl1Bx—Cl1B—Ca5x46.1 (4)
O1viii—Ca5—O6vi139.35 (8)Ca5—Cl1B—Ca5x168.92 (9)
O2vi—Ca5—O11ix75.16 (8)Ca4vii—Cl1B—Ca5x87.32 (7)
O10viii—Ca5—O11ix139.59 (9)Ca1i—Cl1B—Ca5x86.57 (6)
O1viii—Ca5—O11ix82.08 (8)Ca1viii—Cl1B—Ca5x83.79 (6)
O6vi—Ca5—O11ix58.24 (6)Ca4ii—Cl1B—Ca5x83.17 (5)
Symmetry codes: (i) x+1, y+2, z; (ii) x, y+1, z; (iii) x+1, y, z; (iv) x+1, y+1, z; (v) x, y1, z; (vi) x+1, y1/2, z+1/2; (vii) x, y+1, z; (viii) x1, y, z; (ix) x+1, y+1/2, z+1/2; (x) x, y+2, z; (xi) x+2, y1/2, z+1/2; (xii) x+2, y+1/2, z+1/2; (xiii) x1, y1, z; (xiv) x, y+5/2, z+1/2.
(E_mono) top
Crystal data top
Ca5ClO12P3F(000) = 1032
Mr = 520.76Dx = 3.175 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.7107 Å
Hall symbol: -P 2ybcCell parameters from 1997 reflections
a = 9.6430 (3) Åθ = 3.9–27.4°
b = 6.7641 (2) ŵ = 3.21 mm1
c = 19.2882 (6) ÅT = 293 K
β = 120.003 (1)°Prism, colourless
V = 1089.51 (6) Å30.29 × 0.12 × 0.10 mm
Z = 4
Data collection top
BRUKER APPEX-II CCD
diffractometer
2208 independent reflections
Radiation source: fine-focus sealed tube1255 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.027
ω and phi scansθmax = 26.4°, θmin = 2.4°
Absorption correction: multi-scan
BRUKER SADABS
h = 1210
Tmin = 0.682, Tmax = 1k = 08
11773 measured reflectionsl = 024
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.023 w = 1/[σ2(Fo2) + (0.0344P)2 + 1.3169P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.076(Δ/σ)max < 0.001
S = 1.06Δρmax = 0.44 e Å3
2208 reflectionsΔρmin = 0.52 e Å3
201 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0407 (11)
Crystal data top
Ca5ClO12P3V = 1089.51 (6) Å3
Mr = 520.76Z = 4
Monoclinic, P21/cMo Kα radiation
a = 9.6430 (3) ŵ = 3.21 mm1
b = 6.7641 (2) ÅT = 293 K
c = 19.2882 (6) Å0.29 × 0.12 × 0.10 mm
β = 120.003 (1)°
Data collection top
BRUKER APPEX-II CCD
diffractometer
2208 independent reflections
Absorption correction: multi-scan
BRUKER SADABS
1255 reflections with I > 2σ(I)
Tmin = 0.682, Tmax = 1Rint = 0.027
11773 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.023201 parameters
wR(F2) = 0.0760 restraints
S = 1.06Δρmax = 0.44 e Å3
2208 reflectionsΔρmin = 0.52 e Å3
Special details top

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ca10.74421 (6)1.25000 (13)0.00219 (3)0.01100 (16)
Ca20.66670 (12)0.99695 (10)0.16667 (5)0.0118 (2)
Ca30.66656 (11)0.50371 (9)0.16662 (5)0.0101 (2)
Ca40.26013 (6)0.24994 (13)0.12786 (3)0.01097 (16)
Ca50.00431 (6)0.74991 (12)0.13005 (3)0.01085 (16)
O10.9133 (3)1.0672 (4)0.13323 (15)0.0158 (6)
O20.8728 (2)1.2499 (4)0.23264 (11)0.0146 (4)
O30.5924 (2)1.2495 (5)0.06367 (11)0.0139 (4)
O40.3531 (3)1.0670 (4)0.04315 (15)0.0194 (6)
O50.5349 (2)1.2493 (5)0.20390 (11)0.0137 (4)
O60.7330 (3)1.0672 (4)0.32328 (16)0.0154 (6)
O70.6565 (2)0.7494 (4)0.07413 (11)0.0135 (4)
O80.8520 (2)0.7499 (4)0.25415 (11)0.0135 (4)
O90.4920 (2)0.7508 (4)0.17181 (12)0.0136 (4)
O100.9134 (3)0.4326 (4)0.13347 (16)0.0217 (6)
O110.7333 (3)0.4326 (4)0.32332 (18)0.0230 (7)
O120.3535 (3)0.4328 (4)0.04349 (16)0.0187 (6)
P10.96750 (8)1.25012 (16)0.18748 (4)0.00720 (18)
P20.40738 (8)1.24998 (16)0.01626 (4)0.00720 (18)
P30.62525 (8)1.25028 (15)0.29632 (4)0.00716 (18)
Cl1A0.0011 (4)0.5562 (4)0.00127 (18)0.0264 (10)0.501 (4)
Cl1B0.0010 (4)0.9443 (4)0.00127 (18)0.0260 (10)0.499 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0123 (3)0.0093 (3)0.0122 (3)0.0002 (4)0.0067 (2)0.0001 (4)
Ca20.0129 (5)0.0074 (4)0.0138 (5)0.0009 (3)0.0058 (4)0.0007 (3)
Ca30.0119 (5)0.0070 (4)0.0115 (4)0.0008 (3)0.0059 (4)0.0008 (3)
Ca40.0103 (3)0.0086 (3)0.0125 (3)0.0001 (4)0.0047 (2)0.0007 (4)
Ca50.0119 (3)0.0090 (3)0.0101 (3)0.0001 (4)0.0044 (2)0.0002 (4)
O10.0106 (15)0.0144 (14)0.0130 (14)0.0054 (13)0.0011 (13)0.0050 (12)
O20.0131 (9)0.0216 (11)0.0109 (9)0.0017 (15)0.0075 (8)0.0002 (14)
O30.0071 (9)0.0217 (11)0.0111 (9)0.0017 (14)0.0032 (8)0.0032 (13)
O40.0327 (19)0.0160 (15)0.0121 (14)0.0143 (15)0.0132 (14)0.0051 (12)
O50.0100 (9)0.0217 (11)0.0070 (9)0.0020 (14)0.0025 (8)0.0016 (13)
O60.0161 (15)0.0103 (13)0.0215 (15)0.0069 (13)0.0107 (13)0.0096 (12)
O70.0185 (10)0.0133 (10)0.0078 (9)0.0007 (15)0.0059 (8)0.0025 (13)
O80.0067 (9)0.0125 (10)0.0139 (10)0.0010 (14)0.0003 (8)0.0001 (13)
O90.0142 (10)0.0133 (10)0.0191 (10)0.0034 (15)0.0126 (9)0.0028 (14)
O100.0162 (17)0.0192 (15)0.0181 (16)0.0041 (15)0.0001 (14)0.0105 (13)
O110.0151 (16)0.0260 (16)0.0352 (18)0.0090 (15)0.0181 (15)0.0144 (15)
O120.0254 (17)0.0172 (15)0.0158 (15)0.0115 (15)0.0121 (14)0.0037 (13)
P10.0058 (3)0.0082 (3)0.0062 (3)0.0016 (5)0.0020 (3)0.0015 (4)
P20.0071 (3)0.0078 (3)0.0062 (3)0.0002 (5)0.0029 (3)0.0009 (4)
P30.0061 (3)0.0083 (3)0.0067 (3)0.0015 (5)0.0029 (3)0.0009 (4)
Cl1A0.0151 (13)0.048 (2)0.0148 (11)0.0035 (17)0.0068 (10)0.0060 (17)
Cl1B0.0162 (13)0.047 (2)0.0154 (11)0.0053 (18)0.0086 (10)0.0070 (17)
Geometric parameters (Å, º) top
Ca1—O32.2992 (18)Ca5—Cl1Avii3.214 (3)
Ca1—O4i2.328 (3)Ca5—Cl1Bx3.258 (2)
Ca1—O12i2.332 (3)Ca5—P1vi3.3918 (8)
Ca1—O12.540 (3)O1—P11.533 (3)
Ca1—O10ii2.543 (3)O1—Ca5iii2.331 (3)
Ca1—Cl1Ai2.792 (3)O2—P11.5455 (18)
Ca1—Cl1Bi2.834 (3)O2—Ca5ix2.2978 (19)
Ca1—O9i2.967 (2)O2—Ca3ii2.448 (3)
Ca1—P13.1166 (8)O3—P21.5451 (19)
Ca1—Cl1Biii3.218 (3)O3—Ca3ii2.448 (3)
Ca1—Cl1Aiv3.255 (3)O4—P21.532 (3)
Ca1—P23.3920 (8)O4—Ca1i2.328 (3)
Ca2—O92.406 (2)O4—Ca4ii2.544 (2)
Ca2—O82.412 (3)O5—P31.5439 (19)
Ca2—O72.413 (3)O5—Ca4ii2.299 (2)
Ca2—O32.440 (3)O5—Ca3ii2.450 (3)
Ca2—O52.441 (3)O6—P31.531 (3)
Ca2—O22.443 (3)O6—Ca4ix2.331 (3)
Ca2—O62.798 (3)O6—Ca5ix2.544 (3)
Ca2—O12.799 (2)O7—P2i1.5314 (18)
Ca2—O42.800 (3)O7—Ca5iii2.965 (2)
Ca2—P13.2160 (12)O8—P1xi1.5290 (19)
Ca2—P23.2161 (12)O8—Ca4ix2.9679 (19)
Ca2—P33.2171 (10)O9—P3vi1.5333 (17)
Ca3—O72.404 (2)O9—Ca1i2.967 (2)
Ca3—O92.409 (2)O10—P1v1.529 (3)
Ca3—O82.408 (3)O10—Ca5iii2.332 (3)
Ca3—O2v2.448 (3)O10—Ca1v2.543 (3)
Ca3—O3v2.448 (3)O11—P3v1.528 (3)
Ca3—O5v2.450 (3)O11—Ca4ix2.332 (3)
Ca3—O122.795 (3)O11—Ca5vi2.542 (3)
Ca3—O102.798 (3)O12—P2v1.532 (3)
Ca3—O112.799 (3)O12—Ca1i2.332 (3)
Ca3—P3v3.2174 (10)P1—O8xii1.5290 (19)
Ca3—P2v3.2178 (12)P1—O10ii1.529 (3)
Ca3—P1v3.2184 (11)P1—Ca3ii3.2184 (11)
Ca4—O5v2.299 (2)P1—Ca5ix3.3918 (8)
Ca4—O6vi2.331 (3)P2—O7i1.5314 (18)
Ca4—O11vi2.332 (3)P2—O12ii1.532 (3)
Ca4—O122.541 (2)P2—Ca4ii3.1154 (8)
Ca4—O4v2.544 (2)P2—Ca3ii3.2178 (12)
Ca4—Cl1Bvii2.819 (3)P3—O11ii1.528 (3)
Ca4—Cl1Avii2.806 (3)P3—O9ix1.5333 (17)
Ca4—O8vi2.9679 (19)P3—Ca5ix3.1151 (8)
Ca4—P2v3.1154 (8)P3—Ca3ii3.2174 (10)
Ca4—Cl1A3.242 (3)P3—Ca4ii3.3931 (8)
Ca4—Cl1Bv3.229 (3)Cl1A—Cl1Avii0.763 (5)
Ca4—P3v3.3931 (8)Cl1A—Ca1i2.792 (3)
Ca5—O2vi2.2978 (19)Cl1A—Ca4vii2.806 (3)
Ca5—O10viii2.332 (3)Cl1A—Ca5vii3.214 (3)
Ca5—O1viii2.331 (3)Cl1A—Ca1xiii3.255 (3)
Ca5—O11ix2.542 (3)Cl1B—Cl1Bx0.756 (5)
Ca5—O6vi2.544 (3)Cl1B—Ca4vii2.819 (3)
Ca5—Cl1B2.788 (2)Cl1B—Ca1i2.834 (3)
Ca5—Cl1A2.838 (3)Cl1B—Ca1viii3.218 (3)
Ca5—O7viii2.965 (2)Cl1B—Ca4ii3.229 (3)
Ca5—P3vi3.1151 (8)Cl1B—Ca5x3.258 (2)
O3—Ca1—O4i87.21 (9)O10viii—Ca5—Cl1B128.29 (9)
O3—Ca1—O12i87.41 (9)O1viii—Ca5—Cl1B75.51 (8)
O4i—Ca1—O12i133.99 (8)O11ix—Ca5—Cl1B69.98 (9)
O3—Ca1—O175.14 (8)O6vi—Ca5—Cl1B96.65 (8)
O4i—Ca1—O182.14 (9)O2vi—Ca5—Cl1A142.92 (9)
O12i—Ca1—O1139.53 (9)O10viii—Ca5—Cl1A76.35 (8)
O3—Ca1—O10ii75.17 (8)O1viii—Ca5—Cl1A127.75 (8)
O4i—Ca1—O10ii139.34 (9)O11ix—Ca5—Cl1A96.02 (8)
O12i—Ca1—O10ii82.30 (10)O6vi—Ca5—Cl1A69.89 (8)
O1—Ca1—O10ii58.18 (6)Cl1B—Ca5—Cl1A55.63 (5)
O3—Ca1—Cl1Ai142.47 (9)O2vi—Ca5—O7viii104.89 (6)
O4i—Ca1—Cl1Ai128.36 (8)O10viii—Ca5—O7viii68.68 (9)
O12i—Ca1—Cl1Ai75.89 (8)O1viii—Ca5—O7viii68.81 (8)
O1—Ca1—Cl1Ai96.07 (8)O11ix—Ca5—O7viii150.91 (9)
O10ii—Ca1—Cl1Ai69.51 (8)O6vi—Ca5—O7viii150.80 (9)
O3—Ca1—Cl1Bi143.21 (9)Cl1B—Ca5—O7viii99.37 (8)
O4i—Ca1—Cl1Bi75.93 (9)Cl1A—Ca5—O7viii99.75 (8)
O12i—Ca1—Cl1Bi127.65 (7)O2vi—Ca5—P3vi70.22 (5)
O1—Ca1—Cl1Bi70.37 (7)O10viii—Ca5—P3vi110.46 (8)
O10ii—Ca1—Cl1Bi96.65 (9)O1viii—Ca5—P3vi110.37 (7)
Cl1Ai—Ca1—Cl1Bi55.65 (5)O11ix—Ca5—P3vi29.16 (7)
O3—Ca1—O9i104.88 (6)O6vi—Ca5—P3vi29.22 (6)
O4i—Ca1—O9i68.68 (9)Cl1B—Ca5—P3vi84.94 (7)
O12i—Ca1—O9i68.76 (9)Cl1A—Ca5—P3vi84.58 (7)
O1—Ca1—O9i150.71 (9)O7viii—Ca5—P3vi175.11 (4)
O10ii—Ca1—O9i150.96 (9)O2vi—Ca5—Cl1Avii133.66 (9)
Cl1Ai—Ca1—O9i100.01 (7)O10viii—Ca5—Cl1Avii64.40 (8)
Cl1Bi—Ca1—O9i99.10 (8)O1viii—Ca5—Cl1Avii138.82 (8)
O3—Ca1—P170.21 (5)O11ix—Ca5—Cl1Avii102.43 (8)
O4i—Ca1—P1110.40 (7)O6vi—Ca5—Cl1Avii65.74 (8)
O12i—Ca1—P1110.48 (7)Cl1B—Ca5—Cl1Avii68.25 (8)
O1—Ca1—P129.25 (6)Cl1A—Ca5—Cl1Avii12.63 (8)
O10ii—Ca1—P129.16 (6)O7viii—Ca5—Cl1Avii98.03 (7)
Cl1Ai—Ca1—P184.35 (6)P3vi—Ca5—Cl1Avii85.68 (6)
Cl1Bi—Ca1—P185.20 (7)O2vi—Ca5—Cl1Bx134.03 (10)
O9i—Ca1—P1175.09 (4)O10viii—Ca5—Cl1Bx138.48 (9)
O3—Ca1—Cl1Biii133.37 (9)O1viii—Ca5—Cl1Bx65.06 (8)
O4i—Ca1—Cl1Biii64.64 (9)O11ix—Ca5—Cl1Bx65.64 (9)
O12i—Ca1—Cl1Biii138.99 (7)O6vi—Ca5—Cl1Bx101.79 (8)
O1—Ca1—Cl1Biii65.21 (7)Cl1B—Ca5—Cl1Bx11.28 (11)
O10ii—Ca1—Cl1Biii101.90 (9)Cl1A—Ca5—Cl1Bx66.90 (8)
Cl1Ai—Ca1—Cl1Biii67.99 (9)O7viii—Ca5—Cl1Bx98.53 (7)
Cl1Bi—Ca1—Cl1Biii12.38 (9)P3vi—Ca5—Cl1Bx85.25 (6)
O9i—Ca1—Cl1Biii98.57 (7)Cl1Avii—Ca5—Cl1Bx79.52 (5)
P1—Ca1—Cl1Biii85.12 (6)O2vi—Ca5—P1vi22.55 (5)
O3—Ca1—Cl1Aiv134.34 (9)O10viii—Ca5—P1vi78.88 (7)
O4i—Ca1—Cl1Aiv138.26 (8)O1viii—Ca5—P1vi78.95 (6)
O12i—Ca1—Cl1Aiv64.84 (8)O11ix—Ca5—P1vi94.79 (6)
O1—Ca1—Cl1Aiv102.33 (8)O6vi—Ca5—P1vi94.82 (6)
O10ii—Ca1—Cl1Aiv66.14 (7)Cl1B—Ca5—P1vi151.70 (7)
Cl1Ai—Ca1—Cl1Aiv11.54 (10)Cl1A—Ca5—P1vi152.34 (6)
Cl1Bi—Ca1—Cl1Aiv67.15 (8)O7viii—Ca5—P1vi82.34 (4)
O9i—Ca1—Cl1Aiv98.02 (7)P3vi—Ca5—P1vi92.77 (2)
P1—Ca1—Cl1Aiv85.81 (6)Cl1Avii—Ca5—P1vi139.83 (5)
Cl1Biii—Ca1—Cl1Aiv79.50 (5)Cl1Bx—Ca5—P1vi140.44 (6)
O3—Ca1—P222.56 (5)P1—O1—Ca5iii139.15 (16)
O4i—Ca1—P278.92 (6)P1—O1—Ca196.69 (13)
O12i—Ca1—P278.93 (6)Ca5iii—O1—Ca1118.99 (10)
O1—Ca1—P294.84 (6)P1—O1—Ca291.06 (10)
O10ii—Ca1—P294.79 (6)Ca5iii—O1—Ca2102.95 (9)
Cl1Ai—Ca1—P2151.78 (6)Ca1—O1—Ca296.62 (8)
Cl1Bi—Ca1—P2152.25 (6)P1—O2—Ca5ix122.68 (11)
O9i—Ca1—P282.32 (4)P1—O2—Ca2105.26 (12)
P1—Ca1—P292.77 (2)Ca5ix—O2—Ca2114.64 (10)
Cl1Biii—Ca1—P2139.88 (6)P1—O2—Ca3ii105.16 (12)
Cl1Aiv—Ca1—P2140.41 (6)Ca5ix—O2—Ca3ii114.60 (10)
O9—Ca2—O877.32 (8)Ca2—O2—Ca3ii89.01 (7)
O9—Ca2—O777.28 (8)P2—O3—Ca1122.64 (10)
O8—Ca2—O777.21 (8)P2—O3—Ca2105.39 (13)
O9—Ca2—O3126.26 (8)Ca1—O3—Ca2114.67 (10)
O8—Ca2—O3150.21 (7)P2—O3—Ca3ii105.14 (12)
O7—Ca2—O389.82 (9)Ca1—O3—Ca3ii114.48 (10)
O9—Ca2—O589.63 (9)Ca2—O3—Ca3ii89.06 (6)
O8—Ca2—O5126.25 (8)P2—O4—Ca1i139.35 (13)
O7—Ca2—O5150.26 (8)P2—O4—Ca4ii96.55 (13)
O3—Ca2—O576.46 (8)Ca1i—O4—Ca4ii118.94 (9)
O9—Ca2—O2150.16 (7)P2—O4—Ca291.05 (12)
O8—Ca2—O289.76 (9)Ca1i—O4—Ca2102.99 (11)
O7—Ca2—O2126.36 (8)Ca4ii—O4—Ca296.51 (8)
O3—Ca2—O276.41 (8)P3—O5—Ca4ii122.79 (10)
O5—Ca2—O276.38 (8)P3—O5—Ca2105.46 (13)
O9—Ca2—O681.94 (7)Ca4ii—O5—Ca2114.66 (11)
O8—Ca2—O670.91 (7)P3—O5—Ca3ii105.06 (13)
O7—Ca2—O6145.01 (8)Ca4ii—O5—Ca3ii114.36 (10)
O3—Ca2—O6125.14 (8)Ca2—O5—Ca3ii88.99 (6)
O5—Ca2—O655.60 (7)P3—O6—Ca4ix139.39 (13)
O2—Ca2—O668.37 (7)P3—O6—Ca5ix96.54 (12)
O9—Ca2—O1145.12 (8)Ca4ix—O6—Ca5ix118.82 (11)
O8—Ca2—O182.03 (8)P3—O6—Ca291.19 (11)
O7—Ca2—O170.88 (7)Ca4ix—O6—Ca2103.00 (9)
O3—Ca2—O168.34 (7)Ca5ix—O6—Ca296.55 (7)
O5—Ca2—O1125.21 (8)P2i—O7—Ca3133.68 (17)
O2—Ca2—O155.76 (7)P2i—O7—Ca2133.21 (16)
O6—Ca2—O1117.27 (8)Ca3—O7—Ca287.66 (6)
O9—Ca2—O470.83 (8)P2i—O7—Ca5iii98.75 (8)
O8—Ca2—O4145.04 (9)Ca3—O7—Ca5iii96.45 (8)
O7—Ca2—O482.00 (8)Ca2—O7—Ca5iii96.31 (8)
O3—Ca2—O455.69 (7)P1xi—O8—Ca2133.36 (16)
O5—Ca2—O468.43 (7)P1xi—O8—Ca3133.61 (16)
O2—Ca2—O4125.16 (8)Ca2—O8—Ca387.60 (6)
O6—Ca2—O4117.16 (7)P1xi—O8—Ca4ix98.77 (9)
O1—Ca2—O4117.12 (7)Ca2—O8—Ca4ix96.31 (7)
O9—Ca2—P1165.90 (7)Ca3—O8—Ca4ix96.33 (7)
O8—Ca2—P188.59 (6)P3vi—O9—Ca2133.62 (16)
O7—Ca2—P199.34 (6)P3vi—O9—Ca3133.30 (16)
O3—Ca2—P166.93 (5)Ca2—O9—Ca387.72 (6)
O5—Ca2—P199.25 (6)P3vi—O9—Ca1i98.66 (9)
O2—Ca2—P127.62 (4)Ca2—O9—Ca1i96.42 (7)
O6—Ca2—P194.01 (6)Ca3—O9—Ca1i96.26 (7)
O1—Ca2—P128.47 (5)P1v—O10—Ca5iii139.23 (17)
O4—Ca2—P1122.62 (6)P1v—O10—Ca1v96.70 (14)
O9—Ca2—P299.26 (6)Ca5iii—O10—Ca1v118.81 (10)
O8—Ca2—P2165.84 (6)P1v—O10—Ca391.29 (10)
O7—Ca2—P288.64 (6)Ca5iii—O10—Ca3102.90 (10)
O3—Ca2—P227.59 (5)Ca1v—O10—Ca396.64 (9)
O5—Ca2—P266.97 (5)P3v—O11—Ca4ix139.16 (13)
O2—Ca2—P299.22 (6)P3v—O11—Ca5vi96.71 (14)
O6—Ca2—P2122.57 (6)Ca4ix—O11—Ca5vi118.91 (12)
O1—Ca2—P293.94 (6)P3v—O11—Ca391.22 (13)
O4—Ca2—P228.44 (5)Ca4ix—O11—Ca3102.88 (11)
P1—Ca2—P294.31 (3)Ca5vi—O11—Ca396.68 (7)
O9—Ca2—P388.56 (6)P2v—O12—Ca1i139.06 (14)
O8—Ca2—P399.31 (6)P2v—O12—Ca496.67 (13)
O7—Ca2—P3165.83 (6)Ca1i—O12—Ca4118.95 (9)
O3—Ca2—P399.20 (6)P2v—O12—Ca391.31 (12)
O5—Ca2—P327.55 (5)Ca1i—O12—Ca3102.93 (10)
O2—Ca2—P366.85 (5)Ca4—O12—Ca396.74 (9)
O6—Ca2—P328.41 (5)O8xii—P1—O10ii112.19 (15)
O1—Ca2—P3122.61 (6)O8xii—P1—O1112.05 (15)
O4—Ca2—P394.03 (5)O10ii—P1—O1107.62 (11)
P1—Ca2—P394.26 (3)O8xii—P1—O2111.17 (11)
P2—Ca2—P394.30 (3)O10ii—P1—O2106.75 (15)
O7—Ca3—O977.39 (8)O1—P1—O2106.74 (15)
O7—Ca3—O877.45 (8)O8xii—P1—Ca1136.36 (8)
O9—Ca3—O877.33 (8)O10ii—P1—Ca154.14 (11)
O7—Ca3—O2v126.27 (8)O1—P1—Ca154.05 (10)
O9—Ca3—O2v150.19 (7)O2—P1—Ca1112.47 (8)
O8—Ca3—O2v89.71 (9)O8xii—P1—Ca2135.64 (11)
O7—Ca3—O3v89.80 (9)O10ii—P1—Ca2111.45 (11)
O9—Ca3—O3v126.45 (8)O1—P1—Ca260.46 (9)
O8—Ca3—O3v150.19 (7)O2—P1—Ca247.12 (10)
O2v—Ca3—O3v76.18 (8)Ca1—P1—Ca278.11 (3)
O7—Ca3—O5v150.30 (8)O8xii—P1—Ca3ii135.73 (11)
O9—Ca3—O5v89.98 (9)O10ii—P1—Ca3ii60.35 (10)
O8—Ca3—O5v126.29 (8)O1—P1—Ca3ii111.50 (10)
O2v—Ca3—O5v76.12 (8)O2—P1—Ca3ii47.23 (10)
O3v—Ca3—O5v76.15 (8)Ca1—P1—Ca3ii78.12 (3)
O7—Ca3—O1282.10 (8)Ca2—P1—Ca3ii64.380 (18)
O9—Ca3—O1270.99 (8)O8xii—P1—Ca5ix76.41 (7)
O8—Ca3—O12145.30 (9)O10ii—P1—Ca5ix122.02 (11)
O2v—Ca3—O12124.95 (8)O1—P1—Ca5ix122.07 (10)
O3v—Ca3—O1255.72 (7)Ca1—P1—Ca5ix147.23 (2)
O5v—Ca3—O1268.34 (7)Ca2—P1—Ca5ix74.25 (2)
O7—Ca3—O1070.88 (8)Ca3ii—P1—Ca5ix74.30 (2)
O9—Ca3—O10145.15 (8)O8xii—P1—Ca4iv55.96 (7)
O8—Ca3—O1082.00 (8)O10ii—P1—Ca4iv80.50 (10)
O2v—Ca3—O1055.64 (7)O1—P1—Ca4iv80.38 (9)
O3v—Ca3—O1068.33 (8)O2—P1—Ca4iv167.13 (8)
O5v—Ca3—O10124.84 (8)Ca1—P1—Ca4iv80.404 (19)
O12—Ca3—O10117.19 (8)Ca2—P1—Ca4iv140.80 (3)
O7—Ca3—O11145.30 (9)Ca3ii—P1—Ca4iv140.81 (3)
O9—Ca3—O1182.10 (8)Ca5ix—P1—Ca4iv132.36 (2)
O8—Ca3—O1170.89 (8)O4—P2—O7i112.12 (15)
O2v—Ca3—O1168.25 (7)O4—P2—O12ii107.72 (11)
O3v—Ca3—O11124.85 (9)O7i—P2—O12ii112.07 (15)
O5v—Ca3—O1155.64 (7)O4—P2—O3106.67 (16)
O12—Ca3—O11117.10 (7)O7i—P2—O3111.22 (11)
O10—Ca3—O11117.04 (8)O12ii—P2—O3106.72 (16)
O7—Ca3—P3v166.04 (6)O4—P2—Ca4ii54.21 (9)
O9—Ca3—P3v88.66 (6)O7i—P2—Ca4ii136.36 (8)
O8—Ca3—P3v99.23 (6)O12ii—P2—Ca4ii54.09 (9)
O2v—Ca3—P3v66.80 (5)O3—P2—Ca4ii112.42 (7)
O3v—Ca3—P3v99.03 (6)O4—P2—Ca260.51 (12)
O5v—Ca3—P3v27.60 (5)O7i—P2—Ca2135.82 (11)
O12—Ca3—P3v93.91 (5)O12ii—P2—Ca2111.36 (11)
O10—Ca3—P3v122.44 (6)O3—P2—Ca247.02 (10)
O11—Ca3—P3v28.35 (6)Ca4ii—P2—Ca278.12 (2)
O7—Ca3—P2v88.56 (6)O4—P2—Ca3ii111.64 (10)
O9—Ca3—P2v99.41 (6)O7i—P2—Ca3ii135.53 (11)
O8—Ca3—P2v166.00 (6)O12ii—P2—Ca3ii60.27 (11)
O2v—Ca3—P2v99.06 (6)O3—P2—Ca3ii47.24 (10)
O3v—Ca3—P2v27.61 (5)Ca4ii—P2—Ca3ii78.13 (2)
O5v—Ca3—P2v66.86 (5)Ca2—P2—Ca3ii64.386 (18)
O12—Ca3—P2v28.42 (5)O4—P2—Ca1122.01 (12)
O10—Ca3—P2v93.93 (6)O7i—P2—Ca176.41 (8)
O11—Ca3—P2v122.49 (6)O12ii—P2—Ca1121.98 (11)
P3v—Ca3—P2v94.26 (3)Ca4ii—P2—Ca1147.23 (3)
O7—Ca3—P1v99.23 (6)Ca2—P2—Ca174.25 (2)
O9—Ca3—P1v165.82 (7)Ca3ii—P2—Ca174.27 (2)
O8—Ca3—P1v88.50 (6)O4—P2—Ca5x80.40 (12)
O2v—Ca3—P1v27.61 (4)O7i—P2—Ca5x55.93 (7)
O3v—Ca3—P1v66.82 (5)O12ii—P2—Ca5x80.55 (11)
O5v—Ca3—P1v98.98 (6)O3—P2—Ca5x167.14 (7)
O12—Ca3—P1v122.53 (6)Ca4ii—P2—Ca5x80.436 (19)
O10—Ca3—P1v28.36 (5)Ca2—P2—Ca5x140.87 (3)
O11—Ca3—P1v93.86 (6)Ca3ii—P2—Ca5x140.78 (3)
P3v—Ca3—P1v94.20 (3)Ca1—P2—Ca5x132.34 (2)
P2v—Ca3—P1v94.23 (3)O11ii—P3—O6107.80 (12)
O5v—Ca4—O6vi87.32 (10)O11ii—P3—O9ix112.06 (14)
O5v—Ca4—O11vi87.18 (11)O6—P3—O9ix112.14 (14)
O6vi—Ca4—O11vi133.99 (8)O11ii—P3—O5106.98 (16)
O5v—Ca4—O1275.22 (9)O6—P3—O5106.50 (15)
O6vi—Ca4—O1282.15 (8)O9ix—P3—O5111.07 (11)
O11vi—Ca4—O12139.46 (8)O11ii—P3—Ca5ix54.14 (11)
O5v—Ca4—O4v75.22 (9)O6—P3—Ca5ix54.24 (10)
O6vi—Ca4—O4v139.43 (8)O9ix—P3—Ca5ix136.43 (8)
O11vi—Ca4—O4v82.21 (8)O5—P3—Ca5ix112.51 (7)
O12—Ca4—O4v58.24 (6)O11ii—P3—Ca3ii60.44 (11)
O5v—Ca4—Cl1Bvii142.40 (9)O6—P3—Ca3ii111.61 (8)
O6vi—Ca4—Cl1Bvii128.28 (9)O9ix—P3—Ca3ii135.51 (11)
O11vi—Ca4—Cl1Bvii76.16 (9)O5—P3—Ca3ii47.34 (10)
O12—Ca4—Cl1Bvii95.88 (8)Ca5ix—P3—Ca3ii78.19 (3)
O4v—Ca4—Cl1Bvii69.34 (9)O11ii—P3—Ca2111.48 (9)
O5v—Ca4—Cl1Avii143.40 (9)O6—P3—Ca260.40 (10)
O6vi—Ca4—Cl1Avii75.72 (9)O9ix—P3—Ca2135.71 (11)
O11vi—Ca4—Cl1Avii127.78 (9)O5—P3—Ca246.99 (10)
O12—Ca4—Cl1Avii70.54 (8)Ca5ix—P3—Ca278.12 (3)
O4v—Ca4—Cl1Avii96.88 (9)Ca3ii—P3—Ca264.379 (17)
Cl1Bvii—Ca4—Cl1Avii55.64 (5)O11ii—P3—Ca4ii122.09 (13)
O5v—Ca4—O8vi104.85 (6)O6—P3—Ca4ii121.86 (12)
O6vi—Ca4—O8vi68.77 (8)O9ix—P3—Ca4ii76.34 (8)
O11vi—Ca4—O8vi68.71 (8)Ca5ix—P3—Ca4ii147.23 (2)
O12—Ca4—O8vi150.81 (9)Ca3ii—P3—Ca4ii74.24 (2)
O4v—Ca4—O8vi150.81 (9)Ca2—P3—Ca4ii74.22 (3)
Cl1Bvii—Ca4—O8vi100.11 (7)O11ii—P3—Ca1xiv80.49 (11)
Cl1Avii—Ca4—O8vi98.89 (7)O6—P3—Ca1xiv80.46 (10)
O5v—Ca4—P2v70.29 (5)O9ix—P3—Ca1xiv55.98 (8)
O6vi—Ca4—P2v110.40 (6)O5—P3—Ca1xiv167.04 (8)
O11vi—Ca4—P2v110.45 (7)Ca5ix—P3—Ca1xiv80.449 (19)
O12—Ca4—P2v29.23 (6)Ca3ii—P3—Ca1xiv140.88 (4)
O4v—Ca4—P2v29.24 (6)Ca2—P3—Ca1xiv140.83 (3)
Cl1Bvii—Ca4—P2v84.17 (5)Ca4ii—P3—Ca1xiv132.32 (2)
Cl1Avii—Ca4—P2v85.40 (5)Cl1Avii—Cl1A—Ca1i121.4 (5)
O8vi—Ca4—P2v175.14 (4)Cl1Avii—Cl1A—Ca4vii118.7 (5)
O5v—Ca4—Cl1A133.68 (9)Ca1i—Cl1A—Ca4vii100.66 (7)
O6vi—Ca4—Cl1A65.01 (9)Cl1Avii—Cl1A—Ca5113.0 (4)
O11vi—Ca4—Cl1A138.87 (9)Ca1i—Cl1A—Ca599.90 (10)
O12—Ca4—Cl1A65.20 (8)Ca4vii—Cl1A—Ca599.51 (9)
O4v—Ca4—Cl1A101.59 (8)Cl1Avii—Cl1A—Ca5vii54.4 (4)
Cl1Bvii—Ca4—Cl1A67.49 (9)Ca1i—Cl1A—Ca5vii88.40 (7)
Cl1Avii—Ca4—Cl1A11.92 (11)Ca4vii—Cl1A—Ca5vii88.17 (8)
O8vi—Ca4—Cl1A98.81 (7)Ca5—Cl1A—Ca5vii167.37 (8)
P2v—Ca4—Cl1A84.91 (5)Cl1Avii—Cl1A—Ca449.4 (4)
O5v—Ca4—Cl1Bv134.06 (10)Ca1i—Cl1A—Ca487.86 (8)
O6vi—Ca4—Cl1Bv138.48 (9)Ca4vii—Cl1A—Ca4168.08 (11)
O11vi—Ca4—Cl1Bv64.50 (9)Ca5—Cl1A—Ca487.07 (8)
O12—Ca4—Cl1Bv102.68 (8)Ca5vii—Cl1A—Ca483.72 (6)
O4v—Ca4—Cl1Bv66.10 (8)Cl1Avii—Cl1A—Ca1xiii47.0 (4)
Cl1Bvii—Ca4—Cl1Bv12.09 (9)Ca1i—Cl1A—Ca1xiii168.46 (10)
Cl1Avii—Ca4—Cl1Bv67.66 (9)Ca4vii—Cl1A—Ca1xiii87.35 (8)
O8vi—Ca4—Cl1Bv97.72 (7)Ca5—Cl1A—Ca1xiii86.80 (6)
P2v—Ca4—Cl1Bv85.99 (5)Ca5vii—Cl1A—Ca1xiii83.54 (7)
Cl1A—Ca4—Cl1Bv79.53 (5)Ca4—Cl1A—Ca1xiii83.08 (5)
O5v—Ca4—P3v22.49 (4)Cl1Bx—Cl1B—Ca5122.6 (4)
O6vi—Ca4—P3v78.82 (7)Cl1Bx—Cl1B—Ca4vii116.6 (5)
O11vi—Ca4—P3v78.95 (8)Ca5—Cl1B—Ca4vii100.40 (8)
O12—Ca4—P3v94.74 (7)Cl1Bx—Cl1B—Ca1i114.2 (4)
O4v—Ca4—P3v94.89 (7)Ca5—Cl1B—Ca1i100.10 (8)
Cl1Bvii—Ca4—P3v152.02 (6)Ca4vii—Cl1B—Ca1i99.32 (9)
Cl1Avii—Ca4—P3v152.01 (7)Cl1Bx—Cl1B—Ca1viii53.4 (4)
O8vi—Ca4—P3v82.36 (4)Ca5—Cl1B—Ca1viii88.40 (7)
P2v—Ca4—P3v92.78 (2)Ca4vii—Cl1B—Ca1viii87.85 (8)
Cl1A—Ca4—P3v140.09 (6)Ca1i—Cl1B—Ca1viii167.62 (9)
Cl1Bv—Ca4—P3v140.17 (6)Cl1Bx—Cl1B—Ca4ii51.3 (5)
O2vi—Ca5—O10viii87.24 (10)Ca5—Cl1B—Ca4ii88.19 (8)
O2vi—Ca5—O1viii87.35 (10)Ca4vii—Cl1B—Ca4ii167.91 (9)
O10viii—Ca5—O1viii134.02 (8)Ca1i—Cl1B—Ca4ii87.39 (9)
O2vi—Ca5—O11ix75.15 (8)Ca1viii—Cl1B—Ca4ii83.88 (7)
O10viii—Ca5—O11ix139.40 (10)Cl1Bx—Cl1B—Ca5x46.2 (4)
O1viii—Ca5—O11ix82.20 (9)Ca5—Cl1B—Ca5x168.72 (11)
O2vi—Ca5—O6vi75.15 (8)Ca4vii—Cl1B—Ca5x87.09 (8)
O10viii—Ca5—O6vi82.23 (9)Ca1i—Cl1B—Ca5x86.85 (6)
O1viii—Ca5—O6vi139.39 (9)Ca1viii—Cl1B—Ca5x83.43 (6)
O11ix—Ca5—O6vi58.14 (6)Ca4ii—Cl1B—Ca5x83.23 (6)
O2vi—Ca5—Cl1B142.74 (10)
Symmetry codes: (i) x+1, y+2, z; (ii) x, y+1, z; (iii) x+1, y, z; (iv) x+1, y+1, z; (v) x, y1, z; (vi) x+1, y1/2, z+1/2; (vii) x, y+1, z; (viii) x1, y, z; (ix) x+1, y+1/2, z+1/2; (x) x, y+2, z; (xi) x+2, y1/2, z+1/2; (xii) x+2, y+1/2, z+1/2; (xiii) x1, y1, z; (xiv) x, y+5/2, z+1/2.
(H_mono) top
Crystal data top
Ca5ClO12P3F(000) = 1032
Mr = 520.76Dx = 3.174 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.7107 Å
Hall symbol: -P 2ybcCell parameters from 1997 reflections
a = 9.6434 (3) Åθ = 5.7–27.0°
b = 6.7635 (2) ŵ = 3.21 mm1
c = 19.2846 (6) ÅT = 293 K
β = 119.965 (2)°Needle, colourless
V = 1089.67 (6) Å30.34 × 0.02 × 0.02 mm
Z = 4
Data collection top
BRUKER APPEX-II CCD
diffractometer
2208 independent reflections
Radiation source: fine-focus sealed tube981 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.054
ω and phi scansθmax = 26.4°, θmin = 2.4°
Absorption correction: multi-scan
BRUKER SADABS
h = 1210
Tmin = 0.815, Tmax = 1k = 08
12810 measured reflectionsl = 024
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.039Secondary atom site location: difference Fourier map
wR(F2) = 0.109 w = 1/[σ2(Fo2) + (0.0478P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.02(Δ/σ)max = 0.005
2208 reflectionsΔρmax = 1.12 e Å3
129 parametersΔρmin = 0.76 e Å3
Crystal data top
Ca5ClO12P3V = 1089.67 (6) Å3
Mr = 520.76Z = 4
Monoclinic, P21/cMo Kα radiation
a = 9.6434 (3) ŵ = 3.21 mm1
b = 6.7635 (2) ÅT = 293 K
c = 19.2846 (6) Å0.34 × 0.02 × 0.02 mm
β = 119.965 (2)°
Data collection top
BRUKER APPEX-II CCD
diffractometer
2208 independent reflections
Absorption correction: multi-scan
BRUKER SADABS
981 reflections with I > 2σ(I)
Tmin = 0.815, Tmax = 1Rint = 0.054
12810 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.039129 parameters
wR(F2) = 0.1090 restraints
S = 1.02Δρmax = 1.12 e Å3
2208 reflectionsΔρmin = 0.76 e Å3
Special details top

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ca10.74415 (12)1.2492 (3)0.00231 (6)0.0098 (3)
Ca20.6665 (2)0.9970 (3)0.16674 (11)0.0098 (4)
Ca30.6666 (2)0.5041 (3)0.16651 (11)0.0101 (5)
Ca40.26033 (12)0.2512 (3)0.12800 (6)0.0099 (3)
Ca50.00446 (12)0.7504 (3)0.13023 (6)0.0104 (3)
O10.9148 (6)1.0745 (7)0.1304 (3)0.0135 (3)
O20.8728 (4)1.2545 (11)0.2326 (2)0.0135 (3)
O30.5929 (4)1.2518 (11)0.0638 (2)0.0135 (3)
O40.3638 (6)1.0590 (7)0.0463 (3)0.0135 (3)
O50.5347 (4)1.2471 (10)0.2037 (2)0.0135 (3)
O60.7315 (6)1.0623 (8)0.3220 (3)0.0135 (3)
O70.6570 (4)0.7546 (10)0.0746 (2)0.0135 (3)
O80.8513 (4)0.7532 (10)0.2542 (2)0.0135 (3)
O90.4927 (4)0.7486 (10)0.1719 (2)0.0135 (3)
O100.9126 (6)0.4398 (8)0.1369 (3)0.0135 (3)
O110.7345 (6)0.4280 (8)0.3246 (3)0.0135 (3)
O120.3427 (5)0.4247 (7)0.0405 (3)0.0135 (3)
P10.96764 (14)1.2494 (4)0.18748 (8)0.0064 (3)
P20.40738 (14)1.2488 (4)0.01621 (8)0.0067 (3)
P30.62523 (14)1.2513 (4)0.29621 (8)0.0069 (3)
Cl1A0.0009 (13)0.5532 (8)0.0012 (8)0.0301 (8)0.493 (4)
Cl1B0.0006 (10)0.9400 (7)0.0013 (6)0.0301 (8)0.507 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0120 (5)0.0079 (5)0.0105 (6)0.0006 (10)0.0063 (5)0.0034 (12)
Ca20.0111 (9)0.0044 (9)0.0109 (12)0.0005 (8)0.0032 (9)0.0006 (9)
Ca30.0149 (10)0.0053 (10)0.0124 (12)0.0000 (8)0.0084 (10)0.0004 (9)
Ca40.0100 (5)0.0082 (5)0.0103 (6)0.0023 (11)0.0041 (5)0.0021 (12)
Ca50.0120 (5)0.0092 (5)0.0094 (6)0.0013 (11)0.0048 (5)0.0000 (12)
O10.0143 (6)0.0128 (6)0.0131 (7)0.0003 (10)0.0067 (5)0.0005 (11)
O20.0143 (6)0.0128 (6)0.0131 (7)0.0003 (10)0.0067 (5)0.0005 (11)
O30.0143 (6)0.0128 (6)0.0131 (7)0.0003 (10)0.0067 (5)0.0005 (11)
O40.0143 (6)0.0128 (6)0.0131 (7)0.0003 (10)0.0067 (5)0.0005 (11)
O50.0143 (6)0.0128 (6)0.0131 (7)0.0003 (10)0.0067 (5)0.0005 (11)
O60.0143 (6)0.0128 (6)0.0131 (7)0.0003 (10)0.0067 (5)0.0005 (11)
O70.0143 (6)0.0128 (6)0.0131 (7)0.0003 (10)0.0067 (5)0.0005 (11)
O80.0143 (6)0.0128 (6)0.0131 (7)0.0003 (10)0.0067 (5)0.0005 (11)
O90.0143 (6)0.0128 (6)0.0131 (7)0.0003 (10)0.0067 (5)0.0005 (11)
O100.0143 (6)0.0128 (6)0.0131 (7)0.0003 (10)0.0067 (5)0.0005 (11)
O110.0143 (6)0.0128 (6)0.0131 (7)0.0003 (10)0.0067 (5)0.0005 (11)
O120.0143 (6)0.0128 (6)0.0131 (7)0.0003 (10)0.0067 (5)0.0005 (11)
P10.0065 (6)0.0064 (6)0.0056 (7)0.0032 (13)0.0025 (5)0.0022 (15)
P20.0073 (6)0.0071 (6)0.0056 (7)0.0036 (13)0.0031 (5)0.0025 (15)
P30.0072 (6)0.0070 (7)0.0068 (7)0.0045 (13)0.0038 (6)0.0020 (15)
Cl1A0.0173 (8)0.057 (2)0.0176 (11)0.000 (5)0.0100 (8)0.003 (6)
Cl1B0.0173 (8)0.057 (2)0.0176 (11)0.000 (5)0.0100 (8)0.003 (6)
Geometric parameters (Å, º) top
Ca1—O32.293 (3)Ca5—Cl1Bx3.237 (9)
Ca1—O4i2.309 (6)Ca5—Cl1Avii3.242 (9)
Ca1—O12i2.357 (5)Ca5—P1vi3.3890 (16)
Ca1—O12.478 (5)O1—P11.520 (5)
Ca1—O10ii2.612 (5)O1—Ca5iv2.357 (6)
Ca1—Cl1Bi2.793 (7)O2—P11.545 (3)
Ca1—Cl1Ai2.829 (10)O2—Ca5ix2.296 (4)
Ca1—O9i2.973 (4)O2—Ca3ii2.428 (6)
Ca1—P13.1159 (17)O3—P21.550 (3)
Ca1—Cl1Aiii3.227 (9)O3—Ca3ii2.436 (6)
Ca1—Cl1Biv3.257 (7)O4—P21.550 (5)
Ca1—P23.3895 (14)O4—Ca1i2.309 (6)
Ca2—O72.387 (6)O4—Ca4ii2.596 (5)
Ca2—O82.395 (6)O5—P31.545 (4)
Ca2—O92.410 (6)O5—Ca4ii2.297 (3)
Ca2—O52.427 (6)O5—Ca3ii2.462 (6)
Ca2—O32.451 (6)O6—P31.557 (6)
Ca2—O22.466 (6)O6—Ca4ix2.299 (6)
Ca2—O42.705 (5)O6—Ca5ix2.570 (5)
Ca2—O62.771 (6)O7—P2i1.538 (4)
Ca2—O12.860 (5)O7—Ca5iv2.964 (3)
Ca2—P23.213 (3)O8—P1xi1.534 (4)
Ca2—P33.216 (3)O8—Ca4ix2.960 (3)
Ca2—P13.217 (3)O9—P3vi1.540 (3)
Ca3—O92.394 (6)O9—Ca1i2.973 (4)
Ca3—O72.421 (6)O10—P1v1.541 (5)
Ca3—O82.421 (6)O10—Ca5iv2.308 (6)
Ca3—O2v2.428 (6)O10—Ca1v2.612 (5)
Ca3—O3v2.436 (6)O11—P3v1.504 (6)
Ca3—O5v2.462 (6)O11—Ca4ix2.360 (6)
Ca3—O102.738 (5)O11—Ca5vi2.520 (5)
Ca3—O112.828 (6)O12—P2v1.521 (5)
Ca3—O122.893 (5)O12—Ca1i2.357 (5)
Ca3—P3v3.215 (3)P1—O8xii1.534 (4)
Ca3—P1v3.223 (2)P1—O10ii1.541 (5)
Ca3—P2v3.224 (3)P1—Ca3ii3.223 (2)
Ca4—O5v2.297 (4)P1—Ca5ix3.3890 (16)
Ca4—O6vi2.299 (6)P2—O12ii1.521 (5)
Ca4—O11vi2.360 (6)P2—O7i1.538 (4)
Ca4—O122.489 (5)P2—Ca4ii3.1164 (14)
Ca4—O4v2.596 (5)P2—Ca3ii3.224 (3)
Ca4—Cl1Bvii2.794 (9)P3—O11ii1.504 (6)
Ca4—Cl1Avii2.835 (12)P3—O9ix1.540 (3)
Ca4—O8vi2.960 (3)P3—Ca5ix3.1152 (15)
Ca4—P2v3.1164 (14)P3—Ca3ii3.215 (3)
Ca4—Cl1A3.209 (11)P3—Ca4ii3.3915 (16)
Ca4—Cl1Bv3.273 (8)Cl1A—Cl1Avii0.721 (10)
Ca4—P3v3.3915 (16)Cl1A—Ca1i2.829 (9)
Ca5—O2vi2.296 (4)Cl1A—Ca4vii2.835 (12)
Ca5—O10viii2.308 (6)Cl1A—Ca1xiii3.227 (9)
Ca5—O1viii2.357 (6)Cl1A—Ca5vii3.242 (9)
Ca5—O11ix2.520 (5)Cl1B—Cl1Bx0.813 (10)
Ca5—O6vi2.570 (5)Cl1B—Ca1i2.793 (7)
Ca5—Cl1A2.808 (10)Cl1B—Ca4vii2.794 (9)
Ca5—Cl1B2.821 (9)Cl1B—Ca5x3.237 (9)
Ca5—O7viii2.964 (3)Cl1B—Ca1viii3.257 (7)
Ca5—P3vi3.1152 (15)Cl1B—Ca4ii3.273 (8)
O3—Ca1—O4i86.7 (2)O10viii—Ca5—Cl1A77.4 (2)
O3—Ca1—O12i88.1 (2)O1viii—Ca5—Cl1A126.9 (2)
O4i—Ca1—O12i133.89 (14)O11ix—Ca5—Cl1A95.8 (2)
O3—Ca1—O176.45 (16)O6vi—Ca5—Cl1A69.7 (3)
O4i—Ca1—O185.09 (19)O2vi—Ca5—Cl1B142.9 (2)
O12i—Ca1—O1137.53 (19)O10viii—Ca5—Cl1B129.0 (2)
O3—Ca1—O10ii73.93 (16)O1viii—Ca5—Cl1B74.72 (17)
O4i—Ca1—O10ii141.19 (19)O11ix—Ca5—Cl1B70.1 (2)
O12i—Ca1—O10ii79.74 (18)O6vi—Ca5—Cl1B96.7 (2)
O1—Ca1—O10ii58.08 (11)Cl1A—Ca5—Cl1B55.40 (11)
O3—Ca1—Cl1Bi143.2 (3)O2vi—Ca5—O7viii104.84 (11)
O4i—Ca1—Cl1Bi78.74 (17)O10viii—Ca5—O7viii68.48 (19)
O12i—Ca1—Cl1Bi125.97 (18)O1viii—Ca5—O7viii69.06 (18)
O1—Ca1—Cl1Bi68.8 (2)O11ix—Ca5—O7viii150.94 (19)
O10ii—Ca1—Cl1Bi96.9 (2)O6vi—Ca5—O7viii150.78 (19)
O3—Ca1—Cl1Ai142.5 (3)Cl1A—Ca5—O7viii99.9 (2)
O4i—Ca1—Cl1Ai129.6 (2)Cl1B—Ca5—O7viii99.3 (2)
O12i—Ca1—Cl1Ai73.18 (19)O2vi—Ca5—P3vi70.21 (8)
O1—Ca1—Cl1Ai95.6 (3)O10viii—Ca5—P3vi111.16 (15)
O10ii—Ca1—Cl1Ai71.0 (3)O1viii—Ca5—P3vi109.59 (15)
Cl1Bi—Ca1—Cl1Ai55.47 (10)O11ix—Ca5—P3vi28.53 (13)
O3—Ca1—O9i104.83 (11)O6vi—Ca5—P3vi29.86 (12)
O4i—Ca1—O9i67.03 (19)Cl1A—Ca5—P3vi84.7 (2)
O12i—Ca1—O9i70.23 (19)Cl1B—Ca5—P3vi84.81 (18)
O1—Ca1—O9i151.81 (19)O7viii—Ca5—P3vi175.01 (8)
O10ii—Ca1—O9i149.97 (19)O2vi—Ca5—Cl1Bx132.8 (2)
Cl1Bi—Ca1—O9i100.2 (2)O10viii—Ca5—Cl1Bx140.7 (2)
Cl1Ai—Ca1—O9i99.0 (3)O1viii—Ca5—Cl1Bx62.33 (16)
O3—Ca1—P170.24 (10)O11ix—Ca5—Cl1Bx65.4 (2)
O4i—Ca1—P1112.27 (16)O6vi—Ca5—Cl1Bx102.98 (18)
O12i—Ca1—P1108.79 (15)Cl1A—Ca5—Cl1Bx68.7 (3)
O1—Ca1—P128.75 (12)Cl1B—Ca5—Cl1Bx13.3 (2)
O10ii—Ca1—P129.58 (12)O7viii—Ca5—Cl1Bx97.94 (18)
Cl1Bi—Ca1—P184.3 (2)P3vi—Ca5—Cl1Bx85.37 (16)
Cl1Ai—Ca1—P185.2 (3)O2vi—Ca5—Cl1Avii134.9 (3)
O9i—Ca1—P1175.06 (7)O10viii—Ca5—Cl1Avii67.1 (2)
O3—Ca1—Cl1Aiii133.4 (2)O1viii—Ca5—Cl1Avii136.6 (2)
O4i—Ca1—Cl1Aiii139.9 (2)O11ix—Ca5—Cl1Avii101.3 (2)
O12i—Ca1—Cl1Aiii62.70 (19)O6vi—Ca5—Cl1Avii66.0 (2)
O1—Ca1—Cl1Aiii100.4 (2)Cl1A—Ca5—Cl1Avii10.9 (3)
O10ii—Ca1—Cl1Aiii66.0 (2)Cl1B—Ca5—Cl1Avii66.3 (3)
Cl1Bi—Ca1—Cl1Aiii66.9 (2)O7viii—Ca5—Cl1Avii98.6 (2)
Cl1Ai—Ca1—Cl1Aiii11.4 (3)P3vi—Ca5—Cl1Avii85.7 (2)
O9i—Ca1—Cl1Aiii98.5 (2)Cl1Bx—Ca5—Cl1Avii79.60 (10)
P1—Ca1—Cl1Aiii85.0 (2)O2vi—Ca5—P1vi22.59 (8)
O3—Ca1—Cl1Biv134.3 (2)O10viii—Ca5—P1vi76.98 (14)
O4i—Ca1—Cl1Biv66.68 (18)O1viii—Ca5—P1vi80.78 (13)
O12i—Ca1—Cl1Biv137.19 (18)O11ix—Ca5—P1vi95.42 (13)
O1—Ca1—Cl1Biv65.3 (2)O6vi—Ca5—P1vi94.38 (13)
O10ii—Ca1—Cl1Biv103.7 (2)Cl1A—Ca5—P1vi151.36 (19)
Cl1Bi—Ca1—Cl1Biv12.7 (2)Cl1B—Ca5—P1vi152.91 (15)
Cl1Ai—Ca1—Cl1Biv68.1 (2)O7viii—Ca5—P1vi82.27 (7)
O9i—Ca1—Cl1Biv98.1 (2)P3vi—Ca5—P1vi92.79 (4)
P1—Ca1—Cl1Biv85.82 (18)Cl1Bx—Ca5—P1vi139.70 (14)
Cl1Aiii—Ca1—Cl1Biv79.53 (8)Cl1Avii—Ca5—P1vi140.51 (18)
O3—Ca1—P222.68 (9)P1—O1—Ca5iv137.2 (3)
O4i—Ca1—P277.04 (12)P1—O1—Ca199.6 (2)
O12i—Ca1—P280.88 (12)Ca5iv—O1—Ca1120.2 (2)
O1—Ca1—P296.10 (11)P1—O1—Ca289.1 (2)
O10ii—Ca1—P293.84 (11)Ca5iv—O1—Ca2100.50 (17)
Cl1Bi—Ca1—P2152.47 (16)Ca1—O1—Ca296.39 (17)
Cl1Ai—Ca1—P2151.75 (16)P1—O2—Ca5ix122.60 (19)
O9i—Ca1—P282.16 (7)P1—O2—Ca3ii106.3 (3)
P1—Ca1—P292.92 (4)Ca5ix—O2—Ca3ii115.4 (2)
Cl1Aiii—Ca1—P2140.34 (16)P1—O2—Ca2104.3 (3)
Cl1Biv—Ca1—P2139.93 (15)Ca5ix—O2—Ca2113.8 (2)
O7—Ca2—O877.86 (17)Ca3ii—O2—Ca288.97 (12)
O7—Ca2—O977.46 (16)P2—O3—Ca1122.5 (2)
O8—Ca2—O977.24 (17)P2—O3—Ca3ii105.8 (3)
O7—Ca2—O5150.11 (15)Ca1—O3—Ca3ii115.0 (2)
O8—Ca2—O5125.98 (15)P2—O3—Ca2104.6 (3)
O9—Ca2—O589.83 (19)Ca1—O3—Ca2114.3 (2)
O7—Ca2—O389.53 (19)Ca3ii—O3—Ca289.13 (12)
O8—Ca2—O3150.11 (13)P2—O4—Ca1i138.3 (3)
O9—Ca2—O3126.70 (16)P2—O4—Ca4ii94.1 (2)
O5—Ca2—O376.46 (16)Ca1i—O4—Ca4ii117.80 (19)
O7—Ca2—O2126.13 (15)P2—O4—Ca294.1 (2)
O8—Ca2—O289.91 (19)Ca1i—O4—Ca2106.43 (18)
O9—Ca2—O2150.47 (14)Ca4ii—O4—Ca297.67 (18)
O5—Ca2—O276.27 (16)P3—O5—Ca4ii122.73 (17)
O3—Ca2—O275.72 (17)P3—O5—Ca2106.0 (3)
O7—Ca2—O481.00 (15)Ca4ii—O5—Ca2115.3 (2)
O8—Ca2—O4144.64 (18)P3—O5—Ca3ii104.3 (3)
O9—Ca2—O470.68 (16)Ca4ii—O5—Ca3ii113.9 (2)
O5—Ca2—O469.24 (14)Ca2—O5—Ca3ii89.08 (11)
O3—Ca2—O456.21 (14)P3—O6—Ca4ix139.9 (3)
O2—Ca2—O4125.44 (18)P3—O6—Ca5ix94.8 (2)
O7—Ca2—O6144.90 (18)Ca4ix—O6—Ca5ix118.8 (2)
O8—Ca2—O670.22 (16)P3—O6—Ca291.6 (3)
O9—Ca2—O681.56 (14)Ca4ix—O6—Ca2104.42 (19)
O5—Ca2—O655.98 (15)Ca5ix—O6—Ca296.60 (17)
O3—Ca2—O6125.53 (18)P2i—O7—Ca2134.5 (4)
O2—Ca2—O669.03 (14)P2i—O7—Ca3132.0 (4)
O4—Ca2—O6117.90 (16)Ca2—O7—Ca387.82 (12)
O7—Ca2—O170.64 (15)P2i—O7—Ca5iv98.81 (14)
O8—Ca2—O183.07 (14)Ca2—O7—Ca5iv96.95 (15)
O9—Ca2—O1145.34 (18)Ca3—O7—Ca5iv96.05 (15)
O5—Ca2—O1124.73 (17)P1xi—O8—Ca2134.6 (4)
O3—Ca2—O167.14 (14)P1xi—O8—Ca3132.1 (4)
O2—Ca2—O155.78 (14)Ca2—O8—Ca387.62 (12)
O4—Ca2—O1115.95 (17)P1xi—O8—Ca4ix98.87 (16)
O6—Ca2—O1118.07 (17)Ca2—O8—Ca4ix96.65 (15)
O7—Ca2—P288.17 (13)Ca3—O8—Ca4ix96.33 (15)
O8—Ca2—P2166.01 (14)P3vi—O9—Ca3134.3 (4)
O9—Ca2—P299.42 (13)P3vi—O9—Ca2132.5 (4)
O5—Ca2—P267.11 (11)Ca3—O9—Ca287.91 (11)
O3—Ca2—P227.84 (9)P3vi—O9—Ca1i98.47 (16)
O2—Ca2—P298.88 (14)Ca3—O9—Ca1i96.55 (15)
O4—Ca2—P228.77 (11)Ca2—O9—Ca1i96.19 (16)
O6—Ca2—P2123.09 (13)P1v—O10—Ca5iv140.8 (3)
O1—Ca2—P292.86 (12)P1v—O10—Ca1v93.6 (2)
O7—Ca2—P3166.47 (13)Ca5iv—O10—Ca1v117.4 (2)
O8—Ca2—P399.12 (12)P1v—O10—Ca393.5 (2)
O9—Ca2—P389.01 (13)Ca5iv—O10—Ca3105.27 (18)
O5—Ca2—P327.52 (10)Ca1v—O10—Ca396.43 (17)
O3—Ca2—P398.92 (14)P3v—O11—Ca4ix138.8 (3)
O2—Ca2—P366.64 (10)P3v—O11—Ca5vi98.3 (2)
O4—Ca2—P394.87 (12)Ca4ix—O11—Ca5vi118.9 (2)
O6—Ca2—P328.94 (11)P3v—O11—Ca390.5 (3)
O1—Ca2—P3122.40 (12)Ca4ix—O11—Ca3101.40 (19)
P2—Ca2—P394.36 (7)Ca5vi—O11—Ca396.46 (17)
O7—Ca2—P198.83 (11)P2v—O12—Ca1i138.8 (3)
O8—Ca2—P188.27 (13)P2v—O12—Ca499.1 (2)
O9—Ca2—P1165.48 (15)Ca1i—O12—Ca4120.0 (2)
O5—Ca2—P199.57 (14)P2v—O12—Ca388.1 (2)
O3—Ca2—P166.78 (10)Ca1i—O12—Ca399.57 (16)
O2—Ca2—P127.75 (9)Ca4—O12—Ca395.39 (17)
O4—Ca2—P1122.99 (13)O1—P1—O8xii113.0 (3)
O6—Ca2—P194.48 (12)O1—P1—O10ii107.8 (2)
O1—Ca2—P128.20 (11)O8xii—P1—O10ii110.9 (3)
P2—Ca2—P194.45 (7)O1—P1—O2110.3 (3)
P3—Ca2—P194.24 (7)O8xii—P1—O2111.3 (2)
O9—Ca3—O777.11 (16)O10ii—P1—O2103.0 (3)
O9—Ca3—O877.03 (17)O1—P1—Ca151.7 (2)
O7—Ca3—O876.70 (16)O8xii—P1—Ca1136.29 (14)
O9—Ca3—O2v149.91 (14)O10ii—P1—Ca156.8 (2)
O7—Ca3—O2v126.33 (15)O2—P1—Ca1112.33 (14)
O8—Ca3—O2v89.63 (19)O1—P1—Ca262.74 (18)
O9—Ca3—O3v126.37 (16)O8xii—P1—Ca2136.6 (2)
O7—Ca3—O3v90.33 (18)O10ii—P1—Ca2111.1 (2)
O8—Ca3—O3v150.40 (13)O2—P1—Ca248.0 (2)
O2v—Ca3—O3v76.67 (17)Ca1—P1—Ca278.03 (5)
O9—Ca3—O5v90.01 (19)O1—P1—Ca3ii111.7 (2)
O7—Ca3—O5v150.59 (15)O8xii—P1—Ca3ii135.0 (3)
O8—Ca3—O5v126.47 (15)O10ii—P1—Ca3ii58.02 (18)
O2v—Ca3—O5v76.31 (16)O2—P1—Ca3ii46.3 (2)
O3v—Ca3—O5v76.07 (16)Ca1—P1—Ca3ii78.01 (5)
O9—Ca3—O10144.81 (19)Ca2—P1—Ca3ii64.36 (3)
O7—Ca3—O1071.23 (16)O1—P1—Ca5ix125.3 (2)
O8—Ca3—O1081.07 (15)O8xii—P1—Ca5ix76.57 (13)
O2v—Ca3—O1055.34 (14)O10ii—P1—Ca5ix118.6 (2)
O3v—Ca3—O1069.52 (14)Ca1—P1—Ca5ix147.13 (4)
O5v—Ca3—O10125.18 (17)Ca2—P1—Ca5ix74.28 (5)
O9—Ca3—O1182.47 (14)Ca3ii—P1—Ca5ix74.27 (5)
O7—Ca3—O11145.16 (18)O1—P1—Ca4iii78.51 (18)
O8—Ca3—O1171.36 (16)O8xii—P1—Ca4iii55.76 (13)
O2v—Ca3—O1167.66 (14)O10ii—P1—Ca4iii82.52 (18)
O3v—Ca3—O11124.45 (18)O2—P1—Ca4iii167.04 (15)
O5v—Ca3—O1155.42 (15)Ca1—P1—Ca4iii80.54 (4)
O10—Ca3—O11115.99 (17)Ca2—P1—Ca4iii141.12 (9)
O9—Ca3—O1271.28 (15)Ca3ii—P1—Ca4iii140.53 (9)
O7—Ca3—O1283.36 (14)Ca5ix—P1—Ca4iii132.33 (5)
O8—Ca3—O12145.57 (17)O12ii—P2—O7i111.5 (3)
O2v—Ca3—O12124.71 (18)O12ii—P2—O4107.64 (19)
O3v—Ca3—O1255.44 (14)O7i—P2—O4112.5 (3)
O5v—Ca3—O1267.41 (14)O12ii—P2—O3109.7 (3)
O10—Ca3—O12118.65 (17)O7i—P2—O3111.38 (18)
O11—Ca3—O12116.33 (16)O4—P2—O3103.8 (3)
O9—Ca3—P3v88.39 (13)O12ii—P2—Ca4ii52.06 (19)
O7—Ca3—P3v165.46 (13)O7i—P2—Ca4ii136.29 (13)
O8—Ca3—P3v99.24 (12)O4—P2—Ca4ii56.19 (18)
O2v—Ca3—P3v67.01 (10)O3—P2—Ca4ii112.33 (14)
O3v—Ca3—P3v99.27 (14)O12ii—P2—Ca2113.0 (2)
O5v—Ca3—P3v27.76 (10)O7i—P2—Ca2135.3 (2)
O10—Ca3—P3v122.35 (13)O4—P2—Ca257.12 (19)
O11—Ca3—P3v27.89 (11)O3—P2—Ca247.6 (2)
O12—Ca3—P3v93.07 (11)Ca4ii—P2—Ca278.18 (5)
O9—Ca3—P1v166.01 (15)O12ii—P2—Ca3ii63.74 (19)
O7—Ca3—P1v99.69 (11)O7i—P2—Ca3ii136.2 (2)
O8—Ca3—P1v88.98 (13)O4—P2—Ca3ii109.9 (2)
O2v—Ca3—P1v27.41 (9)O3—P2—Ca3ii46.6 (2)
O3v—Ca3—P1v66.81 (10)Ca4ii—P2—Ca3ii77.98 (5)
O5v—Ca3—P1v98.64 (14)Ca2—P2—Ca3ii64.38 (4)
O10—Ca3—P1v28.51 (11)O12ii—P2—Ca1125.4 (2)
O11—Ca3—P1v93.36 (12)O7i—P2—Ca176.60 (13)
O12—Ca3—P1v122.22 (12)O4—P2—Ca1118.7 (2)
P3v—Ca3—P1v94.14 (7)Ca4ii—P2—Ca1147.11 (5)
O9—Ca3—P2v99.42 (13)Ca2—P2—Ca174.24 (5)
O7—Ca3—P2v89.29 (13)Ca3ii—P2—Ca174.18 (5)
O8—Ca3—P2v165.98 (14)O12ii—P2—Ca5x77.01 (19)
O2v—Ca3—P2v99.41 (14)O7i—P2—Ca5x55.78 (12)
O3v—Ca3—P2v27.57 (9)O4—P2—Ca5x83.92 (19)
O5v—Ca3—P2v66.59 (11)O3—P2—Ca5x167.12 (14)
O10—Ca3—P2v95.21 (12)Ca4ii—P2—Ca5x80.51 (4)
O11—Ca3—P2v121.99 (13)Ca2—P2—Ca5x141.04 (8)
O12—Ca3—P2v28.14 (10)Ca3ii—P2—Ca5x140.63 (8)
P3v—Ca3—P2v94.18 (7)Ca1—P2—Ca5x132.38 (5)
P1v—Ca3—P2v94.13 (7)O11ii—P3—O9ix112.7 (4)
O5v—Ca4—O6vi87.6 (2)O11ii—P3—O5108.9 (3)
O5v—Ca4—O11vi87.0 (2)O9ix—P3—O5110.91 (19)
O6vi—Ca4—O11vi134.08 (13)O11ii—P3—O6107.8 (2)
O5v—Ca4—O1277.31 (16)O9ix—P3—O6111.2 (4)
O6vi—Ca4—O1284.10 (18)O5—P3—O6104.9 (3)
O11vi—Ca4—O12138.31 (18)O11ii—P3—Ca5ix53.2 (2)
O5v—Ca4—O4v73.13 (16)O9ix—P3—Ca5ix136.51 (15)
O6vi—Ca4—O4v140.32 (18)O5—P3—Ca5ix112.55 (13)
O11vi—Ca4—O4v80.27 (18)O6—P3—Ca5ix55.3 (2)
O12—Ca4—O4v58.32 (11)O11ii—P3—Ca3ii61.6 (2)
O5v—Ca4—Cl1Bvii142.7 (2)O9ix—P3—Ca3ii136.1 (3)
O6vi—Ca4—Cl1Bvii128.18 (19)O5—P3—Ca3ii47.9 (2)
O11vi—Ca4—Cl1Bvii75.3 (2)O6—P3—Ca3ii111.6 (2)
O12—Ca4—Cl1Bvii94.3 (2)Ca5ix—P3—Ca3ii78.22 (5)
O4v—Ca4—Cl1Bvii71.69 (19)O11ii—P3—Ca2111.8 (2)
O5v—Ca4—Cl1Avii143.2 (3)O9ix—P3—Ca2134.9 (3)
O6vi—Ca4—Cl1Avii76.7 (2)O5—P3—Ca246.5 (2)
O11vi—Ca4—Cl1Avii127.6 (2)O6—P3—Ca259.5 (2)
O12—Ca4—Cl1Avii68.2 (2)Ca5ix—P3—Ca278.13 (5)
O4v—Ca4—Cl1Avii98.2 (2)Ca3ii—P3—Ca264.45 (3)
Cl1Bvii—Ca4—Cl1Avii55.40 (10)O11ii—P3—Ca4ii123.5 (2)
O5v—Ca4—O8vi104.90 (11)O9ix—P3—Ca4ii76.21 (14)
O6vi—Ca4—O8vi67.88 (19)O6—P3—Ca4ii120.6 (2)
O11vi—Ca4—O8vi69.68 (18)Ca5ix—P3—Ca4ii147.28 (5)
O12—Ca4—O8vi151.6 (2)Ca3ii—P3—Ca4ii74.25 (5)
O4v—Ca4—O8vi149.9 (2)Ca2—P3—Ca4ii74.27 (5)
Cl1Bvii—Ca4—O8vi99.4 (2)O11ii—P3—Ca1xiv79.4 (2)
Cl1Avii—Ca4—O8vi99.7 (2)O9ix—P3—Ca1xiv56.07 (14)
O5v—Ca4—P2v70.24 (9)O5—P3—Ca1xiv166.95 (13)
O6vi—Ca4—P2v111.27 (15)O6—P3—Ca1xiv81.2 (2)
O11vi—Ca4—P2v109.50 (15)Ca5ix—P3—Ca1xiv80.45 (4)
O12—Ca4—P2v28.82 (12)Ca3ii—P3—Ca1xiv140.96 (9)
O4v—Ca4—P2v29.75 (12)Ca2—P3—Ca1xiv140.71 (9)
Cl1Bvii—Ca4—P2v84.92 (18)Ca4ii—P3—Ca1xiv132.27 (4)
Cl1Avii—Ca4—P2v84.6 (2)Cl1Avii—Cl1A—Ca5121 (2)
O8vi—Ca4—P2v175.14 (8)Cl1Avii—Cl1A—Ca1i117.6 (17)
O5v—Ca4—Cl1A134.8 (2)Ca5—Cl1A—Ca1i99.8 (3)
O6vi—Ca4—Cl1A65.6 (2)Cl1Avii—Cl1A—Ca4vii115 (2)
O11vi—Ca4—Cl1A137.9 (2)Ca5—Cl1A—Ca4vii99.7 (2)
O12—Ca4—Cl1A64.8 (2)Ca1i—Cl1A—Ca4vii99.2 (3)
O4v—Ca4—Cl1A104.2 (2)Cl1Avii—Cl1A—Ca453.1 (18)
Cl1Bvii—Ca4—Cl1A67.1 (3)Ca5—Cl1A—Ca488.1 (3)
Cl1Avii—Ca4—Cl1A11.7 (3)Ca1i—Cl1A—Ca487.9 (3)
O8vi—Ca4—Cl1A97.9 (2)Ca4vii—Cl1A—Ca4168.3 (3)
P2v—Ca4—Cl1A85.8 (2)Cl1Avii—Cl1A—Ca1xiii51.0 (15)
O5v—Ca4—Cl1Bv132.8 (2)Ca5—Cl1A—Ca1xiii88.1 (3)
O6vi—Ca4—Cl1Bv139.48 (19)Ca1i—Cl1A—Ca1xiii168.6 (3)
O11vi—Ca4—Cl1Bv63.8 (2)Ca4vii—Cl1A—Ca1xiii87.4 (3)
O12—Ca4—Cl1Bv99.8 (2)Ca4—Cl1A—Ca1xiii84.2 (2)
O4v—Ca4—Cl1Bv66.29 (18)Cl1Avii—Cl1A—Ca5vii47.7 (17)
Cl1Bvii—Ca4—Cl1Bv12.5 (3)Ca5—Cl1A—Ca5vii169.1 (3)
Cl1Avii—Ca4—Cl1Bv67.9 (3)Ca1i—Cl1A—Ca5vii87.4 (3)
O8vi—Ca4—Cl1Bv98.73 (19)Ca4vii—Cl1A—Ca5vii87.0 (3)
P2v—Ca4—Cl1Bv84.95 (16)Ca4—Cl1A—Ca5vii83.95 (17)
Cl1A—Ca4—Cl1Bv79.56 (9)Ca1xiii—Cl1A—Ca5vii83.62 (18)
O5v—Ca4—P3v22.54 (8)Cl1Bx—Cl1B—Ca1i118.2 (12)
O6vi—Ca4—P3v78.29 (16)Cl1Bx—Cl1B—Ca4vii119.6 (15)
O11vi—Ca4—P3v79.55 (15)Ca1i—Cl1B—Ca4vii101.1 (2)
O12—Ca4—P3v96.80 (12)Cl1Bx—Cl1B—Ca5114.0 (14)
O4v—Ca4—P3v92.92 (12)Ca1i—Cl1B—Ca5100.4 (3)
Cl1Bvii—Ca4—P3v152.30 (16)Ca4vii—Cl1B—Ca5100.4 (2)
Cl1Avii—Ca4—P3v151.97 (17)Cl1Bx—Cl1B—Ca5x52.8 (13)
O8vi—Ca4—P3v82.37 (7)Ca1i—Cl1B—Ca5x87.8 (2)
P2v—Ca4—P3v92.77 (4)Ca4vii—Cl1B—Ca5x88.1 (3)
Cl1A—Ca4—P3v140.37 (17)Ca5—Cl1B—Ca5x166.7 (2)
Cl1Bv—Ca4—P3v139.85 (16)Cl1Bx—Cl1B—Ca1viii49.1 (10)
O2vi—Ca5—O10viii86.5 (2)Ca1i—Cl1B—Ca1viii167.3 (2)
O2vi—Ca5—O1viii88.0 (2)Ca4vii—Cl1B—Ca1viii87.6 (2)
O10viii—Ca5—O1viii134.06 (12)Ca5—Cl1B—Ca1viii86.9 (2)
O2vi—Ca5—O11ix75.23 (17)Ca5x—Cl1B—Ca1viii83.22 (17)
O10viii—Ca5—O11ix139.43 (19)Cl1Bx—Cl1B—Ca4ii47.9 (13)
O1viii—Ca5—O11ix81.95 (18)Ca1i—Cl1B—Ca4ii87.3 (2)
O2vi—Ca5—O6vi75.23 (18)Ca4vii—Cl1B—Ca4ii167.5 (3)
O10viii—Ca5—O6vi82.45 (18)Ca5—Cl1B—Ca4ii86.9 (3)
O1viii—Ca5—O6vi139.30 (19)Ca5x—Cl1B—Ca4ii83.03 (15)
O11ix—Ca5—O6vi58.14 (11)Ca1viii—Cl1B—Ca4ii82.68 (14)
O2vi—Ca5—Cl1A142.9 (3)
Symmetry codes: (i) x+1, y+2, z; (ii) x, y+1, z; (iii) x+1, y+1, z; (iv) x+1, y, z; (v) x, y1, z; (vi) x+1, y1/2, z+1/2; (vii) x, y+1, z; (viii) x1, y, z; (ix) x+1, y+1/2, z+1/2; (x) x, y+2, z; (xi) x+2, y1/2, z+1/2; (xii) x+2, y+1/2, z+1/2; (xiii) x1, y1, z; (xiv) x, y+5/2, z+1/2.
(G_mono) top
Crystal data top
Ca5ClO12P3F(000) = 1032
Mr = 520.76Dx = 3.177 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.7107 Å
Hall symbol: -P 2ybcCell parameters from 1997 reflections
a = 9.6397 (4) Åθ = 5.7–27.0°
b = 6.7657 (3) ŵ = 3.21 mm1
c = 19.2731 (9) ÅT = 293 K
β = 119.984 (3)°Plate, colourless
V = 1088.75 (8) Å30.20 × 0.17 × 0.02 mm
Z = 4
Data collection top
BRUKER APPEX-II CCD
diffractometer
2209 independent reflections
Radiation source: fine-focus sealed tube1142 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.042
ω and phi scansθmax = 26.4°, θmin = 2.4°
Absorption correction: multi-scan
BRUKER SADABS
h = 1210
Tmin = 0.859, Tmax = 1k = 08
15519 measured reflectionsl = 024
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.022 w = 1/[σ2(Fo2) + (0.0467P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.076(Δ/σ)max < 0.001
S = 0.90Δρmax = 0.49 e Å3
2209 reflectionsΔρmin = 0.39 e Å3
201 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0098 (5)
Crystal data top
Ca5ClO12P3V = 1088.75 (8) Å3
Mr = 520.76Z = 4
Monoclinic, P21/cMo Kα radiation
a = 9.6397 (4) ŵ = 3.21 mm1
b = 6.7657 (3) ÅT = 293 K
c = 19.2731 (9) Å0.20 × 0.17 × 0.02 mm
β = 119.984 (3)°
Data collection top
BRUKER APPEX-II CCD
diffractometer
2209 independent reflections
Absorption correction: multi-scan
BRUKER SADABS
1142 reflections with I > 2σ(I)
Tmin = 0.859, Tmax = 1Rint = 0.042
15519 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.022201 parameters
wR(F2) = 0.0760 restraints
S = 0.90Δρmax = 0.49 e Å3
2209 reflectionsΔρmin = 0.39 e Å3
Special details top

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ca10.74352 (6)1.25036 (13)0.00194 (3)0.01126 (15)
Ca20.66674 (8)0.99677 (10)0.16667 (4)0.0115 (2)
Ca30.66651 (8)0.50346 (10)0.16669 (4)0.0108 (2)
Ca40.26048 (6)0.24998 (13)0.12828 (3)0.01114 (15)
Ca50.00387 (6)0.75076 (13)0.13020 (3)0.01128 (16)
O10.9128 (3)1.0667 (4)0.13296 (14)0.0188 (7)
O20.8736 (2)1.2500 (4)0.23254 (11)0.0150 (4)
O30.5915 (2)1.2535 (4)0.06331 (11)0.0146 (4)
O40.3529 (3)1.0665 (4)0.04296 (13)0.0181 (7)
O50.5351 (2)1.2510 (4)0.20417 (11)0.0147 (4)
O60.7330 (3)1.0661 (4)0.32365 (16)0.0237 (7)
O70.6563 (2)0.7517 (4)0.07391 (11)0.0145 (4)
O80.8518 (2)0.7483 (4)0.25434 (11)0.0142 (4)
O90.4919 (2)0.7495 (4)0.17182 (12)0.0144 (4)
O100.9142 (2)0.4312 (4)0.13355 (14)0.0210 (7)
O110.7344 (3)0.4307 (4)0.32300 (14)0.0169 (6)
O120.3538 (3)0.4315 (4)0.04382 (14)0.0209 (7)
P10.96745 (7)1.24982 (17)0.18725 (4)0.00756 (17)
P20.40708 (8)1.24962 (17)0.01629 (4)0.00738 (17)
P30.62539 (7)1.25085 (16)0.29639 (4)0.00757 (17)
Cl1A0.0020 (5)0.5551 (4)0.0005 (2)0.0240 (8)0.4571 (14)
Cl1B0.0023 (6)0.9414 (5)0.0005 (3)0.0461 (13)0.5429 (14)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0127 (3)0.0082 (3)0.0137 (3)0.0001 (4)0.0073 (2)0.0004 (5)
Ca20.0138 (4)0.0055 (4)0.0148 (5)0.0003 (3)0.0067 (4)0.0006 (3)
Ca30.0122 (4)0.0065 (4)0.0133 (5)0.0005 (3)0.0061 (4)0.0004 (3)
Ca40.0101 (3)0.0081 (3)0.0137 (3)0.0009 (4)0.0048 (2)0.0005 (4)
Ca50.0130 (3)0.0081 (3)0.0116 (3)0.0007 (4)0.0053 (2)0.0008 (5)
O10.0172 (15)0.0149 (14)0.0156 (16)0.0038 (12)0.0017 (13)0.0076 (13)
O20.0108 (9)0.0225 (10)0.0124 (10)0.0002 (14)0.0064 (8)0.0020 (16)
O30.0085 (9)0.0208 (10)0.0125 (10)0.0007 (14)0.0037 (8)0.0013 (16)
O40.0279 (15)0.0146 (14)0.0157 (16)0.0117 (13)0.0138 (13)0.0046 (13)
O50.0107 (9)0.0223 (10)0.0097 (10)0.0045 (14)0.0042 (8)0.0014 (15)
O60.0178 (15)0.0159 (15)0.043 (2)0.0124 (13)0.0194 (15)0.0193 (15)
O70.0202 (10)0.0115 (9)0.0099 (10)0.0067 (14)0.0061 (8)0.0019 (15)
O80.0082 (9)0.0120 (9)0.0157 (10)0.0004 (14)0.0010 (8)0.0022 (15)
O90.0147 (10)0.0124 (9)0.0215 (11)0.0000 (14)0.0131 (9)0.0050 (16)
O100.0122 (14)0.0180 (15)0.0197 (17)0.0059 (12)0.0019 (13)0.0113 (14)
O110.0165 (14)0.0170 (15)0.0218 (16)0.0058 (12)0.0131 (13)0.0088 (14)
O120.0323 (16)0.0193 (15)0.0151 (16)0.0157 (13)0.0147 (14)0.0043 (14)
P10.0061 (3)0.0069 (3)0.0078 (3)0.0013 (5)0.0021 (3)0.0009 (6)
P20.0074 (3)0.0070 (3)0.0075 (4)0.0007 (5)0.0035 (3)0.0005 (6)
P30.0069 (3)0.0067 (3)0.0090 (3)0.0003 (5)0.0039 (3)0.0007 (6)
Cl1A0.0165 (12)0.043 (2)0.0146 (12)0.0052 (19)0.0092 (10)0.000 (2)
Cl1B0.0171 (11)0.097 (4)0.0210 (12)0.003 (3)0.0069 (9)0.000 (3)
Geometric parameters (Å, º) top
Ca1—O32.298 (2)Ca5—Cl1Avii3.239 (3)
Ca1—O4i2.325 (3)Ca5—Cl1Bx3.248 (5)
Ca1—O12i2.337 (3)Ca5—P1vi3.3886 (9)
Ca1—O12.543 (2)O1—P11.535 (2)
Ca1—O10ii2.543 (2)O1—Ca5iv2.321 (2)
Ca1—Cl1Ai2.805 (4)O2—P11.540 (2)
Ca1—Cl1Bi2.825 (5)O2—Ca5ix2.296 (2)
Ca1—O9i2.961 (2)O2—Ca3ii2.450 (2)
Ca1—P13.1160 (9)O3—P21.5400 (19)
Ca1—Cl1Aiii3.245 (3)O3—Ca3ii2.432 (2)
Ca1—Cl1Biv3.239 (5)O4—P21.529 (3)
Ca1—P23.3899 (8)O4—Ca1i2.325 (3)
Ca2—O72.403 (2)O4—Ca4ii2.550 (3)
Ca2—O92.411 (2)O5—P31.5395 (19)
Ca2—O82.419 (2)O5—Ca4ii2.2974 (19)
Ca2—O22.448 (2)O5—Ca3ii2.441 (2)
Ca2—O52.451 (3)O6—P31.539 (2)
Ca2—O32.463 (3)O6—Ca4ix2.319 (3)
Ca2—O12.795 (3)O6—Ca5ix2.556 (2)
Ca2—O42.802 (2)O7—P2i1.528 (2)
Ca2—O62.802 (3)O7—Ca5iv2.962 (2)
Ca2—P13.2159 (11)O8—P1xi1.5308 (18)
Ca2—P23.2157 (11)O8—Ca4ix2.956 (2)
Ca2—P33.2188 (11)O9—P3vi1.5321 (19)
Ca3—O82.402 (2)O9—Ca1i2.961 (2)
Ca3—O92.404 (2)O10—P1v1.520 (3)
Ca3—O72.419 (2)O10—Ca5iv2.341 (3)
Ca3—O3v2.432 (2)O10—Ca1v2.543 (2)
Ca3—O5v2.441 (2)O11—P3v1.520 (2)
Ca3—O2v2.450 (2)O11—Ca4ix2.346 (3)
Ca3—O112.788 (3)O11—Ca5vi2.527 (2)
Ca3—O122.792 (2)O12—P2v1.527 (3)
Ca3—O102.806 (3)O12—Ca1i2.337 (3)
Ca3—P3v3.2121 (11)P1—O10ii1.520 (3)
Ca3—P2v3.2186 (11)P1—O8xii1.5308 (18)
Ca3—P1v3.2199 (11)P1—Ca3ii3.2199 (11)
Ca4—O5v2.2974 (19)P1—Ca5ix3.3886 (9)
Ca4—O6vi2.319 (3)P2—O12ii1.527 (3)
Ca4—O11vi2.346 (3)P2—O7i1.528 (2)
Ca4—O122.536 (3)P2—Ca4ii3.1152 (9)
Ca4—O4v2.550 (3)P2—Ca3ii3.2186 (11)
Ca4—Cl1Bvii2.794 (5)P3—O11ii1.520 (2)
Ca4—Cl1Avii2.833 (4)P3—O9ix1.5321 (19)
Ca4—O8vi2.956 (2)P3—Ca5ix3.1177 (8)
Ca4—P2v3.1152 (9)P3—Ca3ii3.2121 (11)
Ca4—Cl1A3.225 (3)P3—Ca4ii3.3882 (8)
Ca4—Cl1Bv3.264 (4)Cl1A—Cl1Avii0.746 (5)
Ca4—P3v3.3882 (8)Cl1A—Ca1i2.805 (4)
Ca5—O2vi2.296 (2)Cl1A—Ca4vii2.833 (4)
Ca5—O1viii2.321 (2)Cl1A—Ca5vii3.239 (3)
Ca5—O10viii2.341 (3)Cl1A—Ca1xiii3.245 (3)
Ca5—O11ix2.527 (2)Cl1B—Cl1Bx0.794 (6)
Ca5—O6vi2.556 (2)Cl1B—Ca4vii2.794 (5)
Ca5—Cl1B2.804 (5)Cl1B—Ca1i2.825 (5)
Ca5—Cl1A2.820 (4)Cl1B—Ca1viii3.239 (5)
Ca5—O7viii2.962 (2)Cl1B—Ca5x3.248 (5)
Ca5—P3vi3.1177 (8)Cl1B—Ca4ii3.264 (4)
O3—Ca1—O4i87.75 (9)O1viii—Ca5—Cl1B76.02 (11)
O3—Ca1—O12i86.95 (9)O10viii—Ca5—Cl1B127.38 (11)
O4i—Ca1—O12i134.28 (8)O11ix—Ca5—Cl1B70.63 (11)
O3—Ca1—O175.60 (8)O6vi—Ca5—Cl1B96.28 (12)
O4i—Ca1—O181.82 (9)O2vi—Ca5—Cl1A142.35 (10)
O12i—Ca1—O1139.66 (9)O1viii—Ca5—Cl1A128.14 (9)
O3—Ca1—O10ii75.13 (8)O10viii—Ca5—Cl1A75.63 (9)
O4i—Ca1—O10ii138.93 (9)O11ix—Ca5—Cl1A96.06 (10)
O12i—Ca1—O10ii82.59 (9)O6vi—Ca5—Cl1A69.18 (10)
O1—Ca1—O10ii58.02 (6)Cl1B—Ca5—Cl1A55.40 (6)
O3—Ca1—Cl1Ai142.43 (10)O2vi—Ca5—O7viii104.99 (6)
O4i—Ca1—Cl1Ai128.08 (9)O1viii—Ca5—O7viii68.58 (8)
O12i—Ca1—Cl1Ai75.58 (9)O10viii—Ca5—O7viii69.30 (8)
O1—Ca1—Cl1Ai96.52 (9)O11ix—Ca5—O7viii151.00 (8)
O10ii—Ca1—Cl1Ai69.87 (10)O6vi—Ca5—O7viii150.81 (8)
O3—Ca1—Cl1Bi143.42 (12)Cl1B—Ca5—O7viii99.07 (11)
O4i—Ca1—Cl1Bi76.33 (10)Cl1A—Ca5—O7viii99.87 (9)
O12i—Ca1—Cl1Bi127.53 (11)O2vi—Ca5—P3vi70.36 (5)
O1—Ca1—Cl1Bi69.73 (13)O1viii—Ca5—P3vi110.50 (7)
O10ii—Ca1—Cl1Bi95.53 (12)O10viii—Ca5—P3vi110.05 (7)
Cl1Ai—Ca1—Cl1Bi55.33 (6)O11ix—Ca5—P3vi28.89 (6)
O3—Ca1—O9i104.87 (6)O6vi—Ca5—P3vi29.41 (6)
O4i—Ca1—O9i68.98 (8)Cl1B—Ca5—P3vi84.99 (11)
O12i—Ca1—O9i68.71 (8)Cl1A—Ca5—P3vi84.29 (8)
O1—Ca1—O9i150.69 (8)O7viii—Ca5—P3vi175.35 (4)
O10ii—Ca1—O9i151.18 (8)O2vi—Ca5—Cl1Avii133.94 (9)
Cl1Ai—Ca1—O9i99.39 (9)O1viii—Ca5—Cl1Avii138.27 (9)
Cl1Bi—Ca1—O9i99.82 (12)O10viii—Ca5—Cl1Avii64.42 (9)
O3—Ca1—P170.41 (5)O11ix—Ca5—Cl1Avii102.22 (9)
O4i—Ca1—P1110.16 (7)O6vi—Ca5—Cl1Avii65.60 (9)
O12i—Ca1—P1110.55 (7)Cl1B—Ca5—Cl1Avii67.09 (13)
O1—Ca1—P129.31 (6)Cl1A—Ca5—Cl1Avii11.72 (12)
O10ii—Ca1—P128.95 (6)O7viii—Ca5—Cl1Avii98.03 (8)
Cl1Ai—Ca1—P184.80 (8)P3vi—Ca5—Cl1Avii85.62 (7)
Cl1Bi—Ca1—P184.34 (11)O2vi—Ca5—Cl1Bx133.63 (11)
O9i—Ca1—P1175.28 (4)O1viii—Ca5—Cl1Bx64.59 (11)
O3—Ca1—Cl1Aiii133.51 (9)O10viii—Ca5—Cl1Bx138.91 (10)
O4i—Ca1—Cl1Aiii138.49 (9)O11ix—Ca5—Cl1Bx65.51 (10)
O12i—Ca1—Cl1Aiii64.97 (8)O6vi—Ca5—Cl1Bx101.73 (11)
O1—Ca1—Cl1Aiii101.79 (9)Cl1B—Ca5—Cl1Bx12.52 (16)
O10ii—Ca1—Cl1Aiii65.53 (9)Cl1A—Ca5—Cl1Bx67.88 (13)
Cl1Ai—Ca1—Cl1Aiii11.47 (11)O7viii—Ca5—Cl1Bx98.49 (10)
Cl1Bi—Ca1—Cl1Aiii66.79 (11)P3vi—Ca5—Cl1Bx84.98 (9)
O9i—Ca1—Cl1Aiii98.52 (8)Cl1Avii—Ca5—Cl1Bx79.59 (6)
P1—Ca1—Cl1Aiii85.14 (8)O2vi—Ca5—P1vi22.42 (5)
O3—Ca1—Cl1Biv134.04 (11)O1viii—Ca5—P1vi79.25 (7)
O4i—Ca1—Cl1Biv64.16 (9)O10viii—Ca5—P1vi79.01 (7)
O12i—Ca1—Cl1Biv138.83 (11)O11ix—Ca5—P1vi94.67 (6)
O1—Ca1—Cl1Biv65.43 (11)O6vi—Ca5—P1vi94.93 (7)
O10ii—Ca1—Cl1Biv102.00 (11)Cl1B—Ca5—P1vi152.58 (9)
Cl1Ai—Ca1—Cl1Biv68.18 (12)Cl1A—Ca5—P1vi151.67 (7)
Cl1Bi—Ca1—Cl1Biv12.86 (14)O7viii—Ca5—P1vi82.57 (4)
O9i—Ca1—Cl1Biv98.14 (11)P3vi—Ca5—P1vi92.78 (2)
P1—Ca1—Cl1Biv85.42 (10)Cl1Avii—Ca5—P1vi140.10 (7)
Cl1Aiii—Ca1—Cl1Biv79.65 (6)Cl1Bx—Ca5—P1vi140.08 (9)
O3—Ca1—P222.44 (5)P1—O1—Ca5iv138.94 (13)
O4i—Ca1—P278.93 (6)P1—O1—Ca196.52 (12)
O12i—Ca1—P279.17 (6)Ca5iv—O1—Ca1119.32 (10)
O1—Ca1—P294.80 (6)P1—O1—Ca291.14 (11)
O10ii—Ca1—P295.04 (6)Ca5iv—O1—Ca2102.95 (9)
Cl1Ai—Ca1—P2151.94 (7)Ca1—O1—Ca296.63 (7)
Cl1Bi—Ca1—P2152.37 (8)P1—O2—Ca5ix122.92 (10)
O9i—Ca1—P282.44 (4)P1—O2—Ca3ii105.33 (12)
P1—Ca1—P292.83 (2)Ca5ix—O2—Ca3ii114.36 (10)
Cl1Aiii—Ca1—P2140.50 (6)P1—O2—Ca2105.21 (12)
Cl1Biv—Ca1—P2139.62 (8)Ca5ix—O2—Ca2114.58 (10)
O7—Ca2—O977.38 (8)Ca3ii—O2—Ca288.84 (6)
O7—Ca2—O877.42 (8)P2—O3—Ca1122.85 (11)
O9—Ca2—O877.04 (7)P2—O3—Ca3ii106.09 (12)
O7—Ca2—O2126.11 (8)Ca1—O3—Ca3ii115.03 (9)
O9—Ca2—O2150.34 (8)P2—O3—Ca2104.52 (12)
O8—Ca2—O289.95 (8)Ca1—O3—Ca2113.83 (9)
O7—Ca2—O5150.24 (7)Ca3ii—O3—Ca288.91 (7)
O9—Ca2—O589.95 (8)P2—O4—Ca1i139.64 (14)
O8—Ca2—O5126.26 (8)P2—O4—Ca4ii96.34 (12)
O2—Ca2—O576.31 (7)Ca1i—O4—Ca4ii119.02 (10)
O7—Ca2—O389.94 (8)P2—O4—Ca291.02 (10)
O9—Ca2—O3126.37 (7)Ca1i—O4—Ca2102.84 (9)
O8—Ca2—O3150.62 (7)Ca4ii—O4—Ca296.31 (7)
O2—Ca2—O376.13 (7)P3—O5—Ca4ii122.80 (11)
O5—Ca2—O375.94 (7)P3—O5—Ca3ii105.34 (12)
O7—Ca2—O170.66 (7)Ca4ii—O5—Ca3ii114.64 (10)
O9—Ca2—O1144.95 (8)P3—O5—Ca2105.24 (12)
O8—Ca2—O182.22 (7)Ca4ii—O5—Ca2114.32 (10)
O2—Ca2—O155.69 (7)Ca3ii—O5—Ca288.97 (6)
O5—Ca2—O1125.06 (8)P3—O6—Ca4ix139.85 (14)
O3—Ca2—O168.52 (7)P3—O6—Ca5ix95.97 (12)
O7—Ca2—O481.78 (7)Ca4ix—O6—Ca5ix119.20 (9)
O9—Ca2—O470.88 (7)P3—O6—Ca290.93 (11)
O8—Ca2—O4144.81 (8)Ca4ix—O6—Ca2102.89 (10)
O2—Ca2—O4125.21 (8)Ca5ix—O6—Ca296.24 (8)
O5—Ca2—O468.58 (7)P2i—O7—Ca2134.01 (16)
O3—Ca2—O455.71 (7)P2i—O7—Ca3133.04 (16)
O1—Ca2—O4117.03 (7)Ca2—O7—Ca387.60 (7)
O7—Ca2—O6145.18 (8)P2i—O7—Ca5iv98.77 (9)
O9—Ca2—O681.87 (7)Ca2—O7—Ca5iv96.30 (7)
O8—Ca2—O670.82 (7)Ca3—O7—Ca5iv96.14 (7)
O2—Ca2—O668.64 (7)P1xi—O8—Ca3134.02 (15)
O5—Ca2—O655.69 (7)P1xi—O8—Ca2132.84 (15)
O3—Ca2—O6124.85 (9)Ca3—O8—Ca287.62 (6)
O1—Ca2—O6117.43 (7)P1xi—O8—Ca4ix98.90 (9)
O4—Ca2—O6117.21 (7)Ca3—O8—Ca4ix96.49 (7)
O7—Ca2—P199.16 (6)Ca2—O8—Ca4ix96.18 (7)
O9—Ca2—P1165.84 (6)P3vi—O9—Ca3133.81 (15)
O8—Ca2—P188.81 (6)P3vi—O9—Ca2133.10 (15)
O2—Ca2—P127.52 (5)Ca3—O9—Ca287.75 (6)
O5—Ca2—P199.07 (6)P3vi—O9—Ca1i98.66 (9)
O3—Ca2—P166.88 (5)Ca3—O9—Ca1i96.33 (7)
O1—Ca2—P128.51 (5)Ca2—O9—Ca1i96.30 (7)
O4—Ca2—P1122.59 (6)P1v—O10—Ca5iv139.54 (13)
O6—Ca2—P194.17 (5)P1v—O10—Ca1v96.94 (13)
O7—Ca2—P288.41 (6)Ca5iv—O10—Ca1v118.72 (10)
O9—Ca2—P299.26 (6)P1v—O10—Ca391.24 (11)
O8—Ca2—P2165.80 (6)Ca5iv—O10—Ca3102.31 (9)
O2—Ca2—P299.23 (6)Ca1v—O10—Ca396.36 (7)
O5—Ca2—P266.92 (5)P3v—O11—Ca4ix138.16 (14)
O3—Ca2—P227.62 (5)P3v—O11—Ca5vi97.66 (12)
O1—Ca2—P293.97 (5)Ca4ix—O11—Ca5vi118.90 (9)
O4—Ca2—P228.39 (5)P3v—O11—Ca391.57 (11)
O6—Ca2—P2122.61 (6)Ca4ix—O11—Ca3102.51 (9)
P1—Ca2—P294.34 (3)Ca5vi—O11—Ca397.13 (8)
O7—Ca2—P3166.13 (6)P2v—O12—Ca1i138.79 (14)
O9—Ca2—P388.75 (6)P2v—O12—Ca496.97 (13)
O8—Ca2—P399.38 (6)Ca1i—O12—Ca4118.94 (10)
O2—Ca2—P366.93 (5)P2v—O12—Ca391.56 (10)
O5—Ca2—P327.48 (5)Ca1i—O12—Ca3102.66 (10)
O3—Ca2—P398.68 (6)Ca4—O12—Ca396.83 (8)
O1—Ca2—P3122.62 (6)O10ii—P1—O1107.66 (11)
O4—Ca2—P394.07 (6)O10ii—P1—O8xii112.28 (14)
O6—Ca2—P328.57 (5)O1—P1—O8xii111.86 (14)
P1—Ca2—P394.23 (3)O10ii—P1—O2106.94 (14)
P2—Ca2—P394.20 (3)O1—P1—O2106.77 (14)
O8—Ca3—O977.48 (7)O8xii—P1—O2111.02 (11)
O8—Ca3—O777.44 (8)O10ii—P1—Ca154.11 (10)
O9—Ca3—O777.22 (8)O1—P1—Ca154.16 (9)
O8—Ca3—O3v150.21 (7)O8xii—P1—Ca1136.46 (8)
O9—Ca3—O3v125.99 (8)O2—P1—Ca1112.52 (8)
O7—Ca3—O3v89.53 (8)O10ii—P1—Ca2111.67 (9)
O8—Ca3—O5v125.99 (8)O1—P1—Ca260.35 (10)
O9—Ca3—O5v89.72 (8)O8xii—P1—Ca2135.37 (10)
O7—Ca3—O5v150.35 (7)O2—P1—Ca247.27 (9)
O3v—Ca3—O5v76.70 (8)Ca1—P1—Ca278.10 (2)
O8—Ca3—O2v89.50 (8)O10ii—P1—Ca3ii60.61 (10)
O9—Ca3—O2v150.35 (7)O1—P1—Ca3ii111.42 (9)
O7—Ca3—O2v126.20 (8)O8xii—P1—Ca3ii135.94 (10)
O3v—Ca3—O2v76.67 (7)O2—P1—Ca3ii47.20 (9)
O5v—Ca3—O2v76.45 (7)Ca1—P1—Ca3ii78.04 (2)
O8—Ca3—O1170.81 (7)Ca2—P1—Ca3ii64.371 (18)
O9—Ca3—O1182.47 (7)O10ii—P1—Ca5ix122.03 (12)
O7—Ca3—O11145.28 (8)O1—P1—Ca5ix122.10 (11)
O3v—Ca3—O11125.14 (9)O8xii—P1—Ca5ix76.36 (8)
O5v—Ca3—O1155.47 (7)Ca1—P1—Ca5ix147.18 (3)
O2v—Ca3—O1168.05 (7)Ca2—P1—Ca5ix74.33 (2)
O8—Ca3—O12145.55 (8)Ca3ii—P1—Ca5ix74.21 (2)
O9—Ca3—O1271.00 (7)O10ii—P1—Ca4iii80.36 (10)
O7—Ca3—O1282.31 (7)O1—P1—Ca4iii80.68 (10)
O3v—Ca3—O1255.31 (7)O8xii—P1—Ca4iii55.75 (8)
O5v—Ca3—O1268.23 (7)O2—P1—Ca4iii166.77 (8)
O2v—Ca3—O12124.90 (8)Ca1—P1—Ca4iii80.71 (2)
O11—Ca3—O12117.17 (7)Ca2—P1—Ca4iii140.97 (4)
O8—Ca3—O1082.07 (7)Ca3ii—P1—Ca4iii140.92 (4)
O9—Ca3—O10145.37 (8)Ca5ix—P1—Ca4iii132.11 (2)
O7—Ca3—O1071.20 (7)O12ii—P2—O4107.79 (11)
O3v—Ca3—O1068.33 (7)O12ii—P2—O7i112.79 (14)
O5v—Ca3—O10124.88 (8)O4—P2—O7i111.60 (14)
O2v—Ca3—O1055.28 (7)O12ii—P2—O3105.76 (14)
O11—Ca3—O10116.63 (7)O4—P2—O3107.66 (14)
O12—Ca3—O10117.22 (7)O7i—P2—O3110.92 (11)
O8—Ca3—P3v99.04 (6)O12ii—P2—Ca4ii53.91 (10)
O9—Ca3—P3v88.59 (6)O4—P2—Ca4ii54.46 (10)
O7—Ca3—P3v165.79 (6)O7i—P2—Ca4ii136.61 (8)
O3v—Ca3—P3v99.54 (6)O3—P2—Ca4ii112.47 (8)
O5v—Ca3—P3v27.53 (5)O12ii—P2—Ca2111.17 (9)
O2v—Ca3—P3v67.04 (5)O4—P2—Ca260.59 (9)
O11—Ca3—P3v28.23 (5)O7i—P2—Ca2135.31 (11)
O12—Ca3—P3v93.81 (6)O3—P2—Ca247.86 (10)
O10—Ca3—P3v122.31 (6)Ca4ii—P2—Ca278.13 (2)
O8—Ca3—P2v166.20 (6)O12ii—P2—Ca3ii60.13 (9)
O9—Ca3—P2v99.31 (6)O4—P2—Ca3ii111.82 (9)
O7—Ca3—P2v88.77 (6)O7i—P2—Ca3ii135.78 (10)
O3v—Ca3—P2v27.37 (5)O3—P2—Ca3ii46.54 (9)
O5v—Ca3—P2v66.96 (5)Ca4ii—P2—Ca3ii78.05 (2)
O2v—Ca3—P2v99.11 (6)Ca2—P2—Ca3ii64.388 (18)
O11—Ca3—P2v122.41 (6)O12ii—P2—Ca1121.92 (11)
O12—Ca3—P2v28.31 (5)O4—P2—Ca1121.98 (11)
O10—Ca3—P2v93.94 (5)O7i—P2—Ca176.22 (8)
P3v—Ca3—P2v94.27 (3)Ca4ii—P2—Ca1147.17 (3)
O8—Ca3—P1v88.48 (6)Ca2—P2—Ca174.26 (2)
O9—Ca3—P1v165.95 (6)Ca3ii—P2—Ca174.23 (2)
O7—Ca3—P1v99.35 (6)O12ii—P2—Ca5x80.84 (9)
O3v—Ca3—P1v67.10 (5)O4—P2—Ca5x80.40 (9)
O5v—Ca3—P1v99.17 (6)O7i—P2—Ca5x55.93 (8)
O2v—Ca3—P1v27.46 (5)O3—P2—Ca5x166.82 (8)
O11—Ca3—P1v93.57 (5)Ca4ii—P2—Ca5x80.67 (2)
O12—Ca3—P1v122.40 (6)Ca2—P2—Ca5x140.95 (4)
O10—Ca3—P1v28.15 (5)Ca3ii—P2—Ca5x140.92 (4)
P3v—Ca3—P1v94.28 (3)Ca1—P2—Ca5x132.15 (2)
P2v—Ca3—P1v94.20 (3)O11ii—P3—O6107.50 (11)
O5v—Ca4—O6vi87.16 (9)O11ii—P3—O9ix113.19 (14)
O5v—Ca4—O11vi87.76 (9)O6—P3—O9ix111.41 (15)
O6vi—Ca4—O11vi134.29 (8)O11ii—P3—O5106.60 (14)
O5v—Ca4—O1275.03 (7)O6—P3—O5106.87 (16)
O6vi—Ca4—O1282.08 (9)O9ix—P3—O5110.94 (11)
O11vi—Ca4—O12139.43 (9)O11ii—P3—Ca5ix53.45 (9)
O5v—Ca4—O4v75.47 (7)O6—P3—Ca5ix54.61 (9)
O6vi—Ca4—O4v139.28 (9)O9ix—P3—Ca5ix136.58 (8)
O11vi—Ca4—O4v82.29 (9)O5—P3—Ca5ix112.48 (8)
O12—Ca4—O4v58.09 (6)O11ii—P3—Ca3ii60.20 (10)
O5v—Ca4—Cl1Bvii142.92 (12)O6—P3—Ca3ii111.93 (10)
O6vi—Ca4—Cl1Bvii127.87 (11)O9ix—P3—Ca3ii135.82 (10)
O11vi—Ca4—Cl1Bvii75.96 (11)O5—P3—Ca3ii47.13 (9)
O12—Ca4—Cl1Bvii95.97 (12)Ca5ix—P3—Ca3ii78.11 (2)
O4v—Ca4—Cl1Bvii69.54 (12)O11ii—P3—Ca2110.89 (9)
O5v—Ca4—Cl1Avii142.84 (10)O6—P3—Ca260.50 (11)
O6vi—Ca4—Cl1Avii75.81 (9)O9ix—P3—Ca2135.26 (10)
O11vi—Ca4—Cl1Avii127.61 (8)O5—P3—Ca247.28 (10)
O12—Ca4—Cl1Avii70.12 (9)Ca5ix—P3—Ca278.09 (2)
O4v—Ca4—Cl1Avii96.22 (9)Ca3ii—P3—Ca264.426 (18)
Cl1Bvii—Ca4—Cl1Avii55.35 (6)O11ii—P3—Ca4ii122.44 (10)
O5v—Ca4—O8vi105.00 (6)O6—P3—Ca4ii121.70 (11)
O6vi—Ca4—O8vi69.21 (8)O9ix—P3—Ca4ii76.19 (8)
O11vi—Ca4—O8vi68.44 (8)Ca5ix—P3—Ca4ii147.22 (3)
O12—Ca4—O8vi151.19 (9)Ca3ii—P3—Ca4ii74.32 (2)
O4v—Ca4—O8vi150.60 (8)Ca2—P3—Ca4ii74.26 (2)
Cl1Bvii—Ca4—O8vi99.63 (12)O11ii—P3—Ca1xiv80.94 (10)
Cl1Avii—Ca4—O8vi99.46 (9)O6—P3—Ca1xiv80.26 (11)
O5v—Ca4—P2v70.35 (5)O9ix—P3—Ca1xiv55.96 (8)
O6vi—Ca4—P2v110.26 (7)O5—P3—Ca1xiv166.90 (8)
O11vi—Ca4—P2v110.52 (7)Ca5ix—P3—Ca1xiv80.63 (2)
O12—Ca4—P2v29.12 (6)Ca3ii—P3—Ca1xiv141.07 (4)
O4v—Ca4—P2v29.20 (6)Ca2—P3—Ca1xiv140.72 (3)
Cl1Bvii—Ca4—P2v84.35 (12)Ca4ii—P3—Ca1xiv132.15 (2)
Cl1Avii—Ca4—P2v84.77 (8)Cl1Avii—Cl1A—Ca1i120.1 (6)
O8vi—Ca4—P2v175.34 (4)Cl1Avii—Cl1A—Ca5118.1 (7)
O5v—Ca4—Cl1A133.55 (9)Ca1i—Cl1A—Ca5100.16 (10)
O6vi—Ca4—Cl1A64.59 (9)Cl1Avii—Cl1A—Ca4vii115.4 (6)
O11vi—Ca4—Cl1A138.47 (8)Ca1i—Cl1A—Ca4vii99.91 (11)
O12—Ca4—Cl1A65.58 (9)Ca5—Cl1A—Ca4vii99.52 (10)
O4v—Ca4—Cl1A101.83 (9)Cl1Avii—Cl1A—Ca452.5 (6)
Cl1Bvii—Ca4—Cl1A67.41 (12)Ca1i—Cl1A—Ca487.99 (10)
Cl1Avii—Ca4—Cl1A12.06 (11)Ca5—Cl1A—Ca487.92 (11)
O8vi—Ca4—Cl1A98.52 (8)Ca4vii—Cl1A—Ca4167.94 (11)
P2v—Ca4—Cl1A85.21 (7)Cl1Avii—Cl1A—Ca5vii50.2 (6)
O5v—Ca4—Cl1Bv134.08 (11)Ca1i—Cl1A—Ca5vii87.82 (10)
O6vi—Ca4—Cl1Bv138.55 (10)Ca5—Cl1A—Ca5vii168.28 (12)
O11vi—Ca4—Cl1Bv64.44 (10)Ca4vii—Cl1A—Ca5vii87.41 (11)
O12—Ca4—Cl1Bv102.19 (11)Ca4—Cl1A—Ca5vii83.77 (7)
O4v—Ca4—Cl1Bv65.60 (11)Cl1Avii—Cl1A—Ca1xiii48.4 (5)
Cl1Bvii—Ca4—Cl1Bv12.17 (16)Ca1i—Cl1A—Ca1xiii168.53 (11)
Cl1Avii—Ca4—Cl1Bv67.51 (12)Ca5—Cl1A—Ca1xiii87.46 (11)
O8vi—Ca4—Cl1Bv97.91 (11)Ca4vii—Cl1A—Ca1xiii87.12 (10)
P2v—Ca4—Cl1Bv85.48 (10)Ca4—Cl1A—Ca1xiii83.71 (7)
Cl1A—Ca4—Cl1Bv79.57 (6)Ca5vii—Cl1A—Ca1xiii83.43 (7)
O5v—Ca4—P3v22.45 (5)Cl1Bx—Cl1B—Ca4vii119.9 (8)
O6vi—Ca4—P3v78.96 (6)Cl1Bx—Cl1B—Ca5117.5 (9)
O11vi—Ca4—P3v79.32 (6)Ca4vii—Cl1B—Ca5100.86 (13)
O12—Ca4—P3v94.65 (6)Cl1Bx—Cl1B—Ca1i114.8 (8)
O4v—Ca4—P3v94.99 (5)Ca4vii—Cl1B—Ca1i100.39 (15)
Cl1Bvii—Ca4—P3v152.28 (9)Ca5—Cl1B—Ca1i100.09 (14)
Cl1Avii—Ca4—P3v152.00 (7)Cl1Bx—Cl1B—Ca1viii52.4 (7)
O8vi—Ca4—P3v82.55 (4)Ca4vii—Cl1B—Ca1viii87.99 (14)
P2v—Ca4—P3v92.80 (2)Ca5—Cl1B—Ca1viii87.74 (15)
Cl1A—Ca4—P3v139.97 (7)Ca1i—Cl1B—Ca1viii167.14 (14)
Cl1Bv—Ca4—P3v140.24 (8)Cl1Bx—Cl1B—Ca5x50.0 (8)
O2vi—Ca5—O1viii87.61 (9)Ca4vii—Cl1B—Ca5x87.67 (15)
O2vi—Ca5—O10viii87.18 (9)Ca5—Cl1B—Ca5x167.48 (16)
O1viii—Ca5—O10viii134.48 (8)Ca1i—Cl1B—Ca5x87.21 (15)
O2vi—Ca5—O11ix75.08 (8)Ca1viii—Cl1B—Ca5x83.39 (10)
O1viii—Ca5—O11ix82.51 (8)Cl1Bx—Cl1B—Ca4ii47.9 (7)
O10viii—Ca5—O11ix138.72 (8)Ca4vii—Cl1B—Ca4ii167.83 (16)
O2vi—Ca5—O6vi75.41 (8)Ca5—Cl1B—Ca4ii87.20 (15)
O1viii—Ca5—O6vi139.74 (8)Ca1i—Cl1B—Ca4ii86.99 (13)
O10viii—Ca5—O6vi81.64 (8)Ca1viii—Cl1B—Ca4ii83.19 (9)
O11ix—Ca5—O6vi58.07 (6)Ca5x—Cl1B—Ca4ii83.01 (9)
O2vi—Ca5—Cl1B143.50 (12)
Symmetry codes: (i) x+1, y+2, z; (ii) x, y+1, z; (iii) x+1, y+1, z; (iv) x+1, y, z; (v) x, y1, z; (vi) x+1, y1/2, z+1/2; (vii) x, y+1, z; (viii) x1, y, z; (ix) x+1, y+1/2, z+1/2; (x) x, y+2, z; (xi) x+2, y1/2, z+1/2; (xii) x+2, y+1/2, z+1/2; (xiii) x1, y1, z; (xiv) x, y+5/2, z+1/2.
(B_mono) top
Crystal data top
Ca5ClO12P3F(000) = 1032
Mr = 520.76Dx = 3.187 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.7107 Å
Hall symbol: -P 2ybcCell parameters from 1895 reflections
a = 9.6370 (3) Åθ = 3.9–26.3°
b = 6.7479 (2) ŵ = 3.22 mm1
c = 19.2702 (7) ÅT = 100 K
β = 120.002 (1)°Needle, colourless
V = 1085.22 (6) Å30.34 × 0.02 × 0.02 mm
Z = 4
Data collection top
BRUKER APPEX-II CCD
diffractometer
2153 independent reflections
Radiation source: fine-focus sealed tube998 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.045
ω and phi scansθmax = 26.4°, θmin = 2.4°
Absorption correction: multi-scan
BRUKER SADABS
h = 1212
Tmin = 0.875, Tmax = 1k = 88
16759 measured reflectionsl = 2324
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.029 w = 1/[σ2(Fo2) + (0.0303P)2 + 6.853P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.085(Δ/σ)max = 0.05
S = 0.94Δρmax = 1.02 e Å3
2153 reflectionsΔρmin = 0.58 e Å3
147 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0011 (2)
Crystal data top
Ca5ClO12P3V = 1085.22 (6) Å3
Mr = 520.76Z = 4
Monoclinic, P21/cMo Kα radiation
a = 9.6370 (3) ŵ = 3.22 mm1
b = 6.7479 (2) ÅT = 100 K
c = 19.2702 (7) Å0.34 × 0.02 × 0.02 mm
β = 120.002 (1)°
Data collection top
BRUKER APPEX-II CCD
diffractometer
2153 independent reflections
Absorption correction: multi-scan
BRUKER SADABS
998 reflections with I > 2σ(I)
Tmin = 0.875, Tmax = 1Rint = 0.045
16759 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.029147 parameters
wR(F2) = 0.0850 restraints
S = 0.94Δρmax = 1.02 e Å3
2153 reflectionsΔρmin = 0.58 e Å3
Special details top

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ca10.74552 (10)1.2500 (4)0.00293 (5)0.0058 (2)
Ca20.6667 (3)0.9951 (3)0.16673 (14)0.0054 (5)
Ca30.6666 (3)0.5021 (3)0.16661 (14)0.0073 (6)
Ca40.26043 (10)0.2504 (4)0.12730 (5)0.0057 (2)
Ca50.00585 (10)0.7499 (4)0.13019 (5)0.0059 (2)
O10.9127 (9)1.0660 (12)0.1333 (4)0.0122 (10)
O20.8725 (3)1.2497 (15)0.23265 (17)0.0087 (4)
O30.5934 (3)1.2483 (15)0.06416 (17)0.0087 (4)
O40.3564 (8)1.0642 (11)0.0435 (4)0.0122 (10)
O50.5346 (3)1.2500 (15)0.20356 (17)0.0087 (4)
O60.7359 (8)1.0697 (11)0.3255 (4)0.0122 (10)
O70.6564 (3)0.7507 (14)0.07439 (17)0.0078 (4)
O80.8519 (3)0.7509 (14)0.25375 (17)0.0078 (4)
O90.4925 (3)0.7498 (14)0.17167 (17)0.0078 (4)
O100.9134 (9)0.4325 (12)0.1330 (4)0.0116 (10)
O110.7318 (8)0.4360 (11)0.3216 (4)0.0116 (10)
O120.3501 (8)0.4303 (11)0.0432 (4)0.0116 (10)
P10.96721 (12)1.2496 (6)0.18747 (6)0.0047 (2)
P20.40759 (12)1.2503 (6)0.01639 (6)0.0045 (2)
P30.62518 (12)1.2504 (6)0.29610 (6)0.0045 (2)
Cl1A0.0003 (8)0.5582 (10)0.0009 (4)0.0148 (4)0.500 (6)
Cl1B0.0004 (8)0.9410 (9)0.0009 (4)0.0148 (4)0.500 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0064 (4)0.0046 (4)0.0072 (4)0.0013 (13)0.0040 (3)0.0003 (13)
Ca20.0073 (13)0.0028 (14)0.0061 (12)0.0005 (8)0.0034 (10)0.0007 (8)
Ca30.0073 (13)0.0045 (14)0.0096 (13)0.0004 (8)0.0040 (11)0.0012 (8)
Ca40.0054 (4)0.0046 (4)0.0067 (4)0.0011 (12)0.0027 (3)0.0001 (12)
Ca50.0072 (4)0.0050 (4)0.0056 (4)0.0005 (12)0.0034 (3)0.0010 (12)
O10.014 (2)0.009 (2)0.014 (2)0.002 (2)0.007 (2)0.001 (2)
O20.0066 (8)0.0142 (9)0.0063 (8)0.004 (3)0.0041 (7)0.002 (3)
O30.0066 (8)0.0142 (9)0.0063 (8)0.004 (3)0.0041 (7)0.002 (3)
O40.014 (2)0.009 (2)0.014 (2)0.002 (2)0.007 (2)0.001 (2)
O50.0066 (8)0.0142 (9)0.0063 (8)0.004 (3)0.0041 (7)0.002 (3)
O60.014 (2)0.009 (2)0.014 (2)0.002 (2)0.007 (2)0.001 (2)
O70.0074 (9)0.0092 (9)0.0064 (8)0.001 (3)0.0031 (7)0.001 (3)
O80.0074 (9)0.0092 (9)0.0064 (8)0.001 (3)0.0031 (7)0.001 (3)
O90.0074 (9)0.0092 (9)0.0064 (8)0.001 (3)0.0031 (7)0.001 (3)
O100.013 (2)0.011 (3)0.012 (2)0.002 (2)0.007 (2)0.000 (2)
O110.013 (2)0.011 (3)0.012 (2)0.002 (2)0.007 (2)0.000 (2)
O120.013 (2)0.011 (3)0.012 (2)0.002 (2)0.007 (2)0.000 (2)
P10.0039 (5)0.0053 (5)0.0044 (5)0.0001 (16)0.0018 (4)0.0005 (16)
P20.0043 (5)0.0051 (5)0.0039 (5)0.0005 (16)0.0021 (4)0.0022 (16)
P30.0045 (5)0.0047 (5)0.0047 (5)0.0000 (16)0.0026 (4)0.0026 (16)
Cl1A0.0083 (7)0.0274 (11)0.0083 (7)0.002 (4)0.0037 (6)0.002 (4)
Cl1B0.0083 (7)0.0274 (11)0.0083 (7)0.002 (4)0.0037 (6)0.002 (4)
Geometric parameters (Å, º) top
Ca1—O32.296 (3)Ca5—Cl1Bx3.227 (7)
Ca1—O12i2.340 (8)Ca5—Cl1Avii3.252 (7)
Ca1—O4i2.320 (8)Ca5—P1vi3.3913 (13)
Ca1—O12.530 (8)O1—P11.533 (9)
Ca1—O10ii2.523 (8)O1—Ca5iv2.327 (8)
Ca1—Cl1Bi2.785 (7)O2—P11.545 (3)
Ca1—Cl1Ai2.809 (7)O2—Ca5ix2.294 (3)
Ca1—O9i2.977 (3)O2—Ca3ii2.436 (8)
Ca1—P13.1004 (13)O3—P21.551 (3)
Ca1—Cl1Aiii3.229 (7)O3—Ca3ii2.437 (8)
Ca1—Cl1Biv3.250 (7)O4—P21.534 (8)
Ca1—P23.3937 (13)O4—Ca1i2.320 (8)
Ca2—O82.391 (7)O4—Ca4ii2.557 (7)
Ca2—O72.391 (7)O5—P31.544 (3)
Ca2—O92.393 (7)O5—Ca4ii2.293 (3)
Ca2—O32.435 (7)O5—Ca3ii2.434 (8)
Ca2—O52.447 (8)O6—P31.530 (8)
Ca2—O22.445 (7)O6—Ca4ix2.332 (8)
Ca2—O62.832 (7)O6—Ca5ix2.506 (7)
Ca2—O42.774 (7)O7—P2i1.537 (3)
Ca2—O12.791 (8)O7—Ca5iv2.980 (3)
Ca2—P33.216 (3)O8—P1xi1.532 (3)
Ca2—P23.219 (3)O8—Ca4ix2.985 (3)
Ca2—P13.215 (3)O9—P3vi1.542 (3)
Ca3—O92.404 (7)O9—Ca1i2.977 (3)
Ca3—O82.414 (7)O10—P1v1.533 (8)
Ca3—O72.410 (7)O10—Ca5iv2.330 (9)
Ca3—O2v2.436 (8)O10—Ca1v2.523 (8)
Ca3—O5v2.434 (8)O11—P3v1.536 (8)
Ca3—O3v2.437 (8)O11—Ca4ix2.324 (8)
Ca3—O102.799 (7)O11—Ca5vi2.546 (7)
Ca3—O112.764 (7)O12—P2v1.528 (8)
Ca3—O122.817 (7)O12—Ca1i2.340 (8)
Ca3—P2v3.205 (3)P1—O10ii1.533 (9)
Ca3—P1v3.208 (3)P1—O8xii1.532 (3)
Ca3—P3v3.204 (3)P1—Ca3ii3.208 (3)
Ca4—O5v2.293 (3)P1—Ca5ix3.3913 (13)
Ca4—O6vi2.332 (8)P2—O12ii1.528 (8)
Ca4—O11vi2.324 (8)P2—O7i1.537 (3)
Ca4—O4v2.557 (7)P2—Ca4ii3.1001 (13)
Ca4—O122.499 (7)P2—Ca3ii3.205 (3)
Ca4—Cl1Avii2.804 (7)P3—O11ii1.536 (8)
Ca4—Cl1Bvii2.792 (7)P3—O9ix1.542 (3)
Ca4—O8vi2.985 (3)P3—Ca5ix3.1001 (13)
Ca4—P2v3.1001 (13)P3—Ca3ii3.204 (3)
Ca4—Cl1Bv3.248 (7)P3—Ca4ii3.3915 (13)
Ca4—Cl1A3.231 (7)Cl1A—Cl1Avii0.787 (13)
Ca4—P3v3.3915 (13)Cl1A—Ca4vii2.804 (7)
Ca5—O2vi2.294 (3)Cl1A—Ca1i2.809 (7)
Ca5—O1viii2.327 (8)Cl1A—Ca1xiii3.229 (7)
Ca5—O10viii2.330 (9)Cl1A—Ca5vii3.252 (7)
Ca5—O11ix2.546 (7)Cl1B—Cl1Bx0.797 (13)
Ca5—O6vi2.506 (7)Cl1B—Ca1i2.785 (7)
Ca5—Cl1A2.781 (7)Cl1B—Ca4vii2.792 (7)
Ca5—Cl1B2.813 (7)Cl1B—Ca5x3.227 (7)
Ca5—O7viii2.980 (3)Cl1B—Ca4ii3.248 (7)
Ca5—P3vi3.1001 (13)Cl1B—Ca1viii3.250 (7)
O3—Ca1—O12i88.2 (3)O1viii—Ca5—Cl1A127.9 (2)
O3—Ca1—O4i86.4 (3)O10viii—Ca5—Cl1A75.9 (2)
O12i—Ca1—O4i133.28 (12)O11ix—Ca5—Cl1A97.4 (2)
O3—Ca1—O175.0 (2)O6vi—Ca5—Cl1A69.6 (2)
O12i—Ca1—O1139.8 (3)O2vi—Ca5—Cl1B143.5 (3)
O4i—Ca1—O182.6 (3)O1viii—Ca5—Cl1B76.6 (2)
O3—Ca1—O10ii75.5 (2)O10viii—Ca5—Cl1B127.4 (2)
O12i—Ca1—O10ii82.1 (3)O11ix—Ca5—Cl1B70.8 (2)
O4i—Ca1—O10ii140.1 (3)O6vi—Ca5—Cl1B95.6 (2)
O1—Ca1—O10ii58.61 (10)Cl1A—Ca5—Cl1B55.01 (7)
O3—Ca1—Cl1Bi142.8 (3)O2vi—Ca5—O7viii104.49 (9)
O12i—Ca1—Cl1Bi127.1 (2)O1viii—Ca5—O7viii68.1 (3)
O4i—Ca1—Cl1Bi77.1 (2)O10viii—Ca5—O7viii68.5 (3)
O1—Ca1—Cl1Bi70.1 (2)O11ix—Ca5—O7viii150.2 (3)
O10ii—Ca1—Cl1Bi96.2 (2)O6vi—Ca5—O7viii151.0 (3)
O3—Ca1—Cl1Ai143.8 (3)Cl1A—Ca5—O7viii99.42 (18)
O12i—Ca1—Cl1Ai75.4 (2)Cl1B—Ca5—O7viii99.48 (17)
O4i—Ca1—Cl1Ai128.2 (2)O2vi—Ca5—P3vi70.35 (8)
O1—Ca1—Cl1Ai97.0 (2)O1viii—Ca5—P3vi110.9 (2)
O10ii—Ca1—Cl1Ai70.5 (2)O10viii—Ca5—P3vi110.8 (2)
Cl1Bi—Ca1—Cl1Ai55.00 (7)O11ix—Ca5—P3vi29.55 (18)
O3—Ca1—O9i104.57 (9)O6vi—Ca5—P3vi29.31 (17)
O12i—Ca1—O9i68.6 (3)Cl1A—Ca5—P3vi85.22 (15)
O4i—Ca1—O9i68.0 (3)Cl1B—Ca5—P3vi85.02 (15)
O1—Ca1—O9i150.5 (3)O7viii—Ca5—P3vi174.83 (6)
O10ii—Ca1—O9i150.7 (3)O2vi—Ca5—Cl1Bx133.7 (3)
Cl1Bi—Ca1—O9i99.81 (18)O1viii—Ca5—Cl1Bx64.5 (2)
Cl1Ai—Ca1—O9i99.18 (18)O10viii—Ca5—Cl1Bx138.8 (2)
O3—Ca1—P170.21 (8)O11ix—Ca5—Cl1Bx66.1 (2)
O12i—Ca1—P1110.6 (2)O6vi—Ca5—Cl1Bx102.0 (2)
O4i—Ca1—P1111.0 (2)Cl1A—Ca5—Cl1Bx68.0 (2)
O1—Ca1—P129.4 (2)Cl1B—Ca5—Cl1Bx13.0 (2)
O10ii—Ca1—P129.4 (2)O7viii—Ca5—Cl1Bx97.98 (18)
Cl1Bi—Ca1—P184.80 (15)P3vi—Ca5—Cl1Bx85.82 (14)
Cl1Ai—Ca1—P185.45 (15)O2vi—Ca5—Cl1Avii134.1 (3)
O9i—Ca1—P1174.78 (6)O1viii—Ca5—Cl1Avii138.6 (2)
O3—Ca1—Cl1Aiii133.8 (3)O10viii—Ca5—Cl1Avii64.7 (2)
O12i—Ca1—Cl1Aiii63.8 (2)O11ix—Ca5—Cl1Avii103.1 (2)
O4i—Ca1—Cl1Aiii139.6 (2)O6vi—Ca5—Cl1Avii65.3 (2)
O1—Ca1—Cl1Aiii102.6 (2)Cl1A—Ca5—Cl1Avii12.0 (3)
O10ii—Ca1—Cl1Aiii65.4 (2)Cl1B—Ca5—Cl1Avii67.0 (2)
Cl1Bi—Ca1—Cl1Aiii67.7 (3)O7viii—Ca5—Cl1Avii98.30 (19)
Cl1Ai—Ca1—Cl1Aiii12.7 (2)P3vi—Ca5—Cl1Avii85.77 (14)
O9i—Ca1—Cl1Aiii98.44 (18)Cl1Bx—Ca5—Cl1Avii80.01 (6)
P1—Ca1—Cl1Aiii85.55 (14)O2vi—Ca5—P1vi22.48 (7)
O3—Ca1—Cl1Biv133.8 (3)O1viii—Ca5—P1vi78.72 (19)
O12i—Ca1—Cl1Biv137.8 (2)O10viii—Ca5—P1vi78.88 (19)
O4i—Ca1—Cl1Biv65.4 (2)O11ix—Ca5—P1vi94.29 (15)
O1—Ca1—Cl1Biv66.1 (2)O6vi—Ca5—P1vi95.65 (16)
O10ii—Ca1—Cl1Biv102.7 (2)Cl1A—Ca5—P1vi152.14 (19)
Cl1Bi—Ca1—Cl1Biv12.3 (3)Cl1B—Ca5—P1vi152.61 (18)
Cl1Ai—Ca1—Cl1Biv67.3 (2)O7viii—Ca5—P1vi82.01 (6)
O9i—Ca1—Cl1Biv97.97 (18)P3vi—Ca5—P1vi92.82 (3)
P1—Ca1—Cl1Biv86.00 (13)Cl1Bx—Ca5—P1vi139.70 (16)
Cl1Aiii—Ca1—Cl1Biv80.01 (6)Cl1Avii—Ca5—P1vi140.14 (16)
O3—Ca1—P222.63 (7)P1—O1—Ca5iv138.9 (4)
O12i—Ca1—P279.50 (17)P1—O1—Ca196.4 (4)
O4i—Ca1—P278.03 (17)Ca5iv—O1—Ca1119.1 (3)
O1—Ca1—P294.78 (17)P1—O1—Ca291.3 (3)
O10ii—Ca1—P294.98 (17)Ca5iv—O1—Ca2103.4 (3)
Cl1Bi—Ca1—P2152.32 (19)Ca1—O1—Ca296.9 (2)
Cl1Ai—Ca1—P2152.44 (18)P1—O2—Ca5ix122.94 (16)
O9i—Ca1—P281.94 (6)P1—O2—Ca3ii105.2 (3)
P1—Ca1—P292.84 (3)Ca5ix—O2—Ca3ii114.5 (3)
Cl1Aiii—Ca1—P2139.75 (16)P1—O2—Ca2105.1 (4)
Cl1Biv—Ca1—P2140.09 (16)Ca5ix—O2—Ca2114.4 (3)
O8—Ca2—O777.6 (2)Ca3ii—O2—Ca289.02 (10)
O8—Ca2—O977.8 (2)P2—O3—Ca1122.63 (16)
O7—Ca2—O977.5 (2)P2—O3—Ca3ii104.8 (4)
O8—Ca2—O3149.84 (16)Ca1—O3—Ca3ii114.3 (3)
O7—Ca2—O389.6 (3)P2—O3—Ca2105.6 (3)
O9—Ca2—O3126.37 (17)Ca1—O3—Ca2114.8 (3)
O8—Ca2—O5126.52 (18)Ca3ii—O3—Ca289.23 (10)
O7—Ca2—O5150.06 (15)P2—O4—Ca1i139.8 (4)
O9—Ca2—O589.9 (3)P2—O4—Ca4ii95.3 (3)
O3—Ca2—O576.1 (2)Ca1i—O4—Ca4ii118.4 (3)
O8—Ca2—O289.6 (3)P2—O4—Ca292.1 (3)
O7—Ca2—O2126.33 (18)Ca1i—O4—Ca2104.1 (3)
O9—Ca2—O2150.25 (15)Ca4ii—O4—Ca296.7 (2)
O3—Ca2—O276.1 (2)P3—O5—Ca4ii123.00 (16)
O5—Ca2—O276.1 (2)P3—O5—Ca3ii105.1 (4)
O8—Ca2—O671.0 (2)Ca4ii—O5—Ca3ii114.5 (3)
O7—Ca2—O6145.7 (2)P3—O5—Ca2105.1 (4)
O9—Ca2—O682.57 (19)Ca4ii—O5—Ca2114.5 (3)
O3—Ca2—O6124.6 (2)Ca3ii—O5—Ca289.02 (10)
O5—Ca2—O655.75 (18)P3—O6—Ca4ix138.8 (4)
O2—Ca2—O667.81 (17)P3—O6—Ca5ix97.4 (4)
O8—Ca2—O4145.4 (3)Ca4ix—O6—Ca5ix119.8 (3)
O7—Ca2—O481.54 (18)P3—O6—Ca289.9 (3)
O9—Ca2—O470.9 (2)Ca4ix—O6—Ca2101.9 (2)
O3—Ca2—O455.68 (18)Ca5ix—O6—Ca296.4 (2)
O5—Ca2—O468.64 (17)P2i—O7—Ca2133.9 (5)
O2—Ca2—O4125.0 (2)P2i—O7—Ca3133.0 (5)
O6—Ca2—O4117.7 (2)Ca2—O7—Ca387.71 (10)
O8—Ca2—O181.8 (2)P2i—O7—Ca5iv98.53 (13)
O7—Ca2—O170.8 (2)Ca2—O7—Ca5iv96.53 (18)
O9—Ca2—O1145.2 (3)Ca3—O7—Ca5iv96.34 (18)
O3—Ca2—O168.15 (18)P1xi—O8—Ca2134.2 (5)
O5—Ca2—O1124.9 (3)P1xi—O8—Ca3133.0 (5)
O2—Ca2—O155.78 (19)Ca2—O8—Ca387.61 (10)
O6—Ca2—O1116.8 (2)P1xi—O8—Ca4ix98.50 (13)
O4—Ca2—O1116.7 (2)Ca2—O8—Ca4ix96.27 (18)
O8—Ca2—P399.44 (14)Ca3—O8—Ca4ix96.15 (19)
O7—Ca2—P3166.24 (19)P3vi—O9—Ca2133.3 (5)
O9—Ca2—P388.74 (17)P3vi—O9—Ca3133.4 (5)
O3—Ca2—P398.94 (19)Ca2—O9—Ca387.81 (10)
O5—Ca2—P327.62 (9)P3vi—O9—Ca1i98.56 (13)
O2—Ca2—P366.66 (11)Ca2—O9—Ca1i96.56 (18)
O6—Ca2—P328.42 (15)Ca3—O9—Ca1i96.52 (18)
O4—Ca2—P394.29 (15)P1v—O10—Ca5iv138.9 (4)
O1—Ca2—P3122.43 (18)P1v—O10—Ca1v96.7 (4)
O8—Ca2—P2166.14 (17)Ca5iv—O10—Ca1v119.2 (3)
O7—Ca2—P288.53 (16)P1v—O10—Ca390.7 (3)
O9—Ca2—P299.32 (14)Ca5iv—O10—Ca3103.3 (3)
O3—Ca2—P227.65 (9)Ca1v—O10—Ca396.6 (2)
O5—Ca2—P266.61 (11)P3v—O11—Ca4ix139.0 (4)
O2—Ca2—P298.87 (18)P3v—O11—Ca5vi95.6 (3)
O6—Ca2—P2122.34 (16)Ca4ix—O11—Ca5vi118.7 (3)
O4—Ca2—P228.43 (16)P3v—O11—Ca391.8 (3)
O1—Ca2—P293.83 (17)Ca4ix—O11—Ca3104.6 (3)
P3—Ca2—P294.01 (8)Ca5vi—O11—Ca397.0 (2)
O8—Ca2—P188.32 (17)P2v—O12—Ca1i138.1 (4)
O7—Ca2—P199.24 (15)P2v—O12—Ca497.8 (4)
O9—Ca2—P1166.07 (18)Ca1i—O12—Ca4119.7 (3)
O3—Ca2—P166.67 (11)P2v—O12—Ca390.0 (3)
O5—Ca2—P198.94 (17)Ca1i—O12—Ca3102.5 (3)
O2—Ca2—P127.63 (9)Ca4—O12—Ca396.7 (2)
O6—Ca2—P193.44 (16)O1—P1—O10ii107.55 (17)
O4—Ca2—P1122.34 (17)O1—P1—O8xii112.6 (5)
O1—Ca2—P128.48 (17)O10ii—P1—O8xii111.8 (5)
P3—Ca2—P194.07 (8)O1—P1—O2106.6 (4)
P2—Ca2—P194.09 (8)O10ii—P1—O2107.0 (4)
O9—Ca3—O877.1 (2)O8xii—P1—O2110.98 (16)
O9—Ca3—O776.9 (2)O1—P1—Ca154.2 (3)
O8—Ca3—O776.8 (2)O10ii—P1—Ca153.9 (3)
O9—Ca3—O2v150.18 (16)O8xii—P1—Ca1136.44 (12)
O8—Ca3—O2v89.8 (3)O2—P1—Ca1112.58 (12)
O7—Ca3—O2v126.47 (17)O1—P1—Ca3ii111.3 (3)
O9—Ca3—O5v89.8 (3)O10ii—P1—Ca3ii60.7 (3)
O8—Ca3—O5v126.55 (19)O8xii—P1—Ca3ii135.4 (3)
O7—Ca3—O5v150.19 (15)O2—P1—Ca3ii47.1 (3)
O2v—Ca3—O5v76.5 (2)Ca1—P1—Ca3ii78.15 (6)
O9—Ca3—O3v126.61 (17)O1—P1—Ca260.2 (3)
O8—Ca3—O3v150.03 (15)O10ii—P1—Ca2111.7 (3)
O7—Ca3—O3v90.2 (3)O8xii—P1—Ca2135.7 (3)
O2v—Ca3—O3v76.2 (2)O2—P1—Ca247.2 (3)
O5v—Ca3—O3v76.3 (2)Ca1—P1—Ca278.27 (6)
O9—Ca3—O10144.8 (3)Ca3ii—P1—Ca264.37 (3)
O8—Ca3—O1081.9 (2)O1—P1—Ca5ix121.9 (3)
O7—Ca3—O1070.9 (2)O10ii—P1—Ca5ix122.2 (3)
O2v—Ca3—O1055.88 (19)O8xii—P1—Ca5ix76.39 (11)
O5v—Ca3—O10125.4 (3)Ca1—P1—Ca5ix147.16 (4)
O3v—Ca3—O1068.29 (18)Ca3ii—P1—Ca5ix74.10 (6)
O9—Ca3—O1181.65 (18)Ca2—P1—Ca5ix74.14 (6)
O8—Ca3—O1170.8 (2)O1—P1—Ca4iii80.6 (3)
O7—Ca3—O11144.4 (2)O10ii—P1—Ca4iii80.1 (3)
O2v—Ca3—O1168.70 (17)O8xii—P1—Ca4iii56.24 (11)
O5v—Ca3—O1155.99 (19)O2—P1—Ca4iii167.22 (12)
O3v—Ca3—O11125.4 (2)Ca1—P1—Ca4iii80.21 (3)
O10—Ca3—O11117.5 (2)Ca3ii—P1—Ca4iii140.76 (12)
O9—Ca3—O1270.8 (2)Ca2—P1—Ca4iii140.78 (11)
O8—Ca3—O12145.0 (2)Ca5ix—P1—Ca4iii132.63 (4)
O7—Ca3—O1282.51 (18)O12ii—P2—O4107.63 (17)
O2v—Ca3—O12125.2 (2)O12ii—P2—O7i112.5 (4)
O5v—Ca3—O1267.86 (17)O4—P2—O7i111.7 (5)
O3v—Ca3—O1256.11 (18)O12ii—P2—O3108.2 (4)
O10—Ca3—O12117.5 (2)O4—P2—O3105.2 (4)
O11—Ca3—O12116.7 (2)O7i—P2—O3111.26 (16)
O9—Ca3—P2v99.27 (15)O12ii—P2—Ca4ii53.0 (3)
O8—Ca3—P2v165.48 (17)O4—P2—Ca4ii55.2 (3)
O7—Ca3—P2v88.67 (16)O7i—P2—Ca4ii136.34 (12)
O2v—Ca3—P2v99.45 (18)O3—P2—Ca4ii112.40 (11)
O5v—Ca3—P2v66.97 (12)O12ii—P2—Ca3ii61.5 (3)
O3v—Ca3—P2v27.89 (9)O4—P2—Ca3ii111.4 (3)
O10—Ca3—P2v94.03 (17)O7i—P2—Ca3ii135.9 (3)
O11—Ca3—P2v122.96 (17)O3—P2—Ca3ii47.3 (3)
O12—Ca3—P2v28.47 (15)Ca4ii—P2—Ca3ii78.19 (6)
O9—Ca3—P1v165.64 (18)O12ii—P2—Ca2111.7 (3)
O8—Ca3—P1v88.55 (16)O4—P2—Ca259.5 (3)
O7—Ca3—P1v99.41 (15)O7i—P2—Ca2135.3 (3)
O2v—Ca3—P1v27.68 (9)O3—P2—Ca246.8 (3)
O5v—Ca3—P1v99.39 (18)Ca4ii—P2—Ca278.23 (7)
O3v—Ca3—P1v66.77 (11)Ca3ii—P2—Ca264.37 (3)
O10—Ca3—P1v28.53 (17)O12ii—P2—Ca1123.4 (3)
O11—Ca3—P1v94.34 (16)O4—P2—Ca1120.6 (3)
O12—Ca3—P1v122.88 (17)O7i—P2—Ca176.53 (11)
P2v—Ca3—P1v94.48 (8)Ca4ii—P2—Ca1147.14 (4)
O9—Ca3—P3v88.62 (17)Ca3ii—P2—Ca174.08 (6)
O8—Ca3—P3v99.43 (14)Ca2—P2—Ca174.11 (6)
O7—Ca3—P3v165.53 (19)O12ii—P2—Ca5x79.5 (3)
O2v—Ca3—P3v66.95 (11)O4—P2—Ca5x81.2 (3)
O5v—Ca3—P3v27.73 (9)O7i—P2—Ca5x56.12 (11)
O3v—Ca3—P3v99.20 (18)O3—P2—Ca5x167.36 (12)
O10—Ca3—P3v122.83 (18)Ca4ii—P2—Ca5x80.22 (3)
O11—Ca3—P3v28.63 (16)Ca3ii—P2—Ca5x140.93 (11)
O12—Ca3—P3v93.56 (15)Ca2—P2—Ca5x140.63 (11)
P2v—Ca3—P3v94.49 (8)Ca1—P2—Ca5x132.64 (4)
P1v—Ca3—P3v94.42 (8)O11ii—P3—O6107.46 (18)
O5v—Ca4—O6vi87.9 (3)O11ii—P3—O9ix112.5 (5)
O5v—Ca4—O11vi86.8 (3)O6—P3—O9ix111.4 (4)
O6vi—Ca4—O11vi133.43 (11)O11ii—P3—O5105.8 (4)
O5v—Ca4—O4v74.9 (2)O6—P3—O5108.2 (5)
O6vi—Ca4—O4v139.5 (3)O9ix—P3—O5111.13 (16)
O11vi—Ca4—O4v82.7 (3)O11ii—P3—Ca5ix54.8 (3)
O5v—Ca4—O1275.8 (2)O6—P3—Ca5ix53.3 (3)
O6vi—Ca4—O1282.0 (3)O9ix—P3—Ca5ix136.21 (12)
O11vi—Ca4—O12140.3 (3)O5—P3—Ca5ix112.67 (12)
O4v—Ca4—O1258.50 (10)O11ii—P3—Ca3ii59.6 (3)
O5v—Ca4—Cl1Avii143.2 (3)O6—P3—Ca3ii112.1 (3)
O6vi—Ca4—Cl1Avii75.6 (2)O9ix—P3—Ca3ii135.9 (3)
O11vi—Ca4—Cl1Avii128.2 (2)O5—P3—Ca3ii47.2 (3)
O4v—Ca4—Cl1Avii96.7 (2)Ca5ix—P3—Ca3ii78.25 (7)
O12—Ca4—Cl1Avii69.6 (2)O11ii—P3—Ca2111.2 (3)
O5v—Ca4—Cl1Bvii143.6 (3)O6—P3—Ca261.7 (3)
O6vi—Ca4—Cl1Bvii126.8 (2)O9ix—P3—Ca2135.5 (3)
O11vi—Ca4—Cl1Bvii76.8 (2)O5—P3—Ca247.3 (3)
O4v—Ca4—Cl1Bvii71.0 (2)Ca5ix—P3—Ca278.21 (7)
O12—Ca4—Cl1Bvii96.4 (2)Ca3ii—P3—Ca264.41 (3)
Cl1Avii—Ca4—Cl1Bvii54.98 (7)O11ii—P3—Ca4ii120.9 (3)
O5v—Ca4—O8vi104.60 (9)O6—P3—Ca4ii123.5 (3)
O6vi—Ca4—O8vi68.9 (2)O9ix—P3—Ca4ii76.58 (12)
O11vi—Ca4—O8vi67.9 (2)Ca5ix—P3—Ca4ii147.22 (4)
O4v—Ca4—O8vi150.5 (3)Ca3ii—P3—Ca4ii74.10 (6)
O12—Ca4—O8vi150.8 (3)Ca2—P3—Ca4ii74.19 (6)
Cl1Avii—Ca4—O8vi99.70 (18)O11ii—P3—Ca1xiv81.4 (2)
Cl1Bvii—Ca4—O8vi99.02 (18)O6—P3—Ca1xiv78.9 (2)
O5v—Ca4—P2v70.37 (7)O9ix—P3—Ca1xiv56.01 (11)
O6vi—Ca4—P2v110.2 (2)O5—P3—Ca1xiv167.14 (12)
O11vi—Ca4—P2v111.3 (2)Ca5ix—P3—Ca1xiv80.20 (3)
O4v—Ca4—P2v29.51 (18)Ca3ii—P3—Ca1xiv140.95 (11)
O12—Ca4—P2v29.23 (18)Ca2—P3—Ca1xiv140.57 (11)
Cl1Avii—Ca4—P2v84.73 (15)Ca4ii—P3—Ca1xiv132.59 (4)
Cl1Bvii—Ca4—P2v85.47 (15)Cl1Avii—Cl1A—Ca5120.5 (11)
O8vi—Ca4—P2v174.97 (7)Cl1Avii—Cl1A—Ca4vii116.3 (11)
O5v—Ca4—Cl1Bv133.7 (3)Ca5—Cl1A—Ca4vii100.6 (2)
O6vi—Ca4—Cl1Bv138.2 (2)Cl1Avii—Cl1A—Ca1i115.6 (11)
O11vi—Ca4—Cl1Bv65.5 (2)Ca5—Cl1A—Ca1i100.5 (2)
O4v—Ca4—Cl1Bv65.7 (2)Ca4vii—Cl1A—Ca1i99.9 (2)
O12—Ca4—Cl1Bv101.8 (2)Cl1Avii—Cl1A—Ca1xiii51.7 (10)
Cl1Avii—Ca4—Cl1Bv67.4 (2)Ca5—Cl1A—Ca1xiii88.0 (2)
Cl1Bvii—Ca4—Cl1Bv12.5 (2)Ca4vii—Cl1A—Ca1xiii87.58 (19)
O8vi—Ca4—Cl1Bv98.43 (19)Ca1i—Cl1A—Ca1xiii167.3 (2)
P2v—Ca4—Cl1Bv85.45 (14)Cl1Avii—Cl1A—Ca451.1 (9)
O5v—Ca4—Cl1A134.1 (3)Ca5—Cl1A—Ca487.92 (19)
O6vi—Ca4—Cl1A63.5 (2)Ca4vii—Cl1A—Ca4167.4 (3)
O11vi—Ca4—Cl1A139.0 (2)Ca1i—Cl1A—Ca487.46 (19)
O4v—Ca4—Cl1A103.3 (2)Ca1xiii—Cl1A—Ca483.43 (16)
O12—Ca4—Cl1A65.8 (2)Cl1Avii—Cl1A—Ca5vii47.4 (10)
Cl1Avii—Ca4—Cl1A12.6 (3)Ca5—Cl1A—Ca5vii168.0 (3)
Cl1Bvii—Ca4—Cl1A67.6 (2)Ca4vii—Cl1A—Ca5vii87.11 (19)
O8vi—Ca4—Cl1A97.70 (19)Ca1i—Cl1A—Ca5vii87.1 (2)
P2v—Ca4—Cl1A86.10 (14)Ca1xiii—Cl1A—Ca5vii83.08 (16)
Cl1Bv—Ca4—Cl1A80.01 (6)Ca4—Cl1A—Ca5vii83.05 (16)
O5v—Ca4—P3v22.45 (7)Cl1Bx—Cl1B—Ca1i119.3 (11)
O6vi—Ca4—P3v79.60 (19)Cl1Bx—Cl1B—Ca4vii118.4 (11)
O11vi—Ca4—P3v78.20 (19)Ca1i—Cl1B—Ca4vii100.8 (2)
O4v—Ca4—P3v94.41 (16)Cl1Bx—Cl1B—Ca5114.6 (11)
O12—Ca4—P3v95.34 (17)Ca1i—Cl1B—Ca5100.3 (2)
Cl1Avii—Ca4—P3v152.41 (18)Ca4vii—Cl1B—Ca5100.1 (2)
Cl1Bvii—Ca4—P3v152.36 (18)Cl1Bx—Cl1B—Ca5x52.4 (9)
O8vi—Ca4—P3v82.15 (6)Ca1i—Cl1B—Ca5x88.0 (2)
P2v—Ca4—P3v92.82 (3)Ca4vii—Cl1B—Ca5x87.95 (19)
Cl1Bv—Ca4—P3v139.91 (16)Ca5—Cl1B—Ca5x167.0 (2)
Cl1A—Ca4—P3v139.93 (16)Cl1Bx—Cl1B—Ca4ii49.1 (9)
O2vi—Ca5—O1viii87.3 (3)Ca1i—Cl1B—Ca4ii87.63 (19)
O2vi—Ca5—O10viii87.3 (3)Ca4vii—Cl1B—Ca4ii167.5 (2)
O1viii—Ca5—O10viii133.23 (11)Ca5—Cl1B—Ca4ii87.19 (19)
O2vi—Ca5—O11ix74.8 (2)Ca5x—Cl1B—Ca4ii83.18 (16)
O1viii—Ca5—O11ix82.2 (3)Cl1Bx—Cl1B—Ca1viii48.4 (9)
O10viii—Ca5—O11ix140.0 (3)Ca1i—Cl1B—Ca1viii167.7 (3)
O2vi—Ca5—O6vi76.1 (2)Ca4vii—Cl1B—Ca1viii87.47 (19)
O1viii—Ca5—O6vi140.0 (3)Ca5—Cl1B—Ca1viii87.07 (19)
O10viii—Ca5—O6vi82.7 (3)Ca5x—Cl1B—Ca1viii83.13 (16)
O11ix—Ca5—O6vi58.60 (10)Ca4ii—Cl1B—Ca1viii82.82 (16)
O2vi—Ca5—Cl1A143.3 (3)
Symmetry codes: (i) x+1, y+2, z; (ii) x, y+1, z; (iii) x+1, y+1, z; (iv) x+1, y, z; (v) x, y1, z; (vi) x+1, y1/2, z+1/2; (vii) x, y+1, z; (viii) x1, y, z; (ix) x+1, y+1/2, z+1/2; (x) x, y+2, z; (xi) x+2, y1/2, z+1/2; (xii) x+2, y+1/2, z+1/2; (xiii) x1, y1, z; (xiv) x, y+5/2, z+1/2.
(D_mono) top
Crystal data top
Ca5ClO12P3F(000) = 1032
Mr = 520.76Dx = 3.193 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.7107 Å
Hall symbol: -P 2ybcCell parameters from 1987 reflections
a = 9.6307 (4) Åθ = 3.3–27.6°
b = 6.7425 (3) ŵ = 3.23 mm1
c = 19.2602 (7) ÅT = 100 K
β = 119.969 (1)°Prism, colourless
V = 1083.44 (8) Å30.25 × 0.12 × 0.05 mm
Z = 4
Data collection top
BRUKER APPEX-II CCD
diffractometer
2216 independent reflections
Radiation source: fine-focus sealed tube1444 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.027
ω and phi scansθmax = 26.4°, θmin = 2.4°
Absorption correction: multi-scan
BRUKER SADABS
h = 1210
Tmin = 0.806, Tmax = 1k = 08
14216 measured reflectionsl = 024
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.039 w = 1/[σ2(Fo2) + (0.0303P)2 + 6.853P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.095(Δ/σ)max < 0.001
S = 1.15Δρmax = 1.03 e Å3
2216 reflectionsΔρmin = 0.66 e Å3
130 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0099 (6)
Crystal data top
Ca5ClO12P3V = 1083.44 (8) Å3
Mr = 520.76Z = 4
Monoclinic, P21/cMo Kα radiation
a = 9.6307 (4) ŵ = 3.23 mm1
b = 6.7425 (3) ÅT = 100 K
c = 19.2602 (7) Å0.25 × 0.12 × 0.05 mm
β = 119.969 (1)°
Data collection top
BRUKER APPEX-II CCD
diffractometer
2216 independent reflections
Absorption correction: multi-scan
BRUKER SADABS
1444 reflections with I > 2σ(I)
Tmin = 0.806, Tmax = 1Rint = 0.027
14216 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.039130 parameters
wR(F2) = 0.0950 restraints
S = 1.15Δρmax = 1.03 e Å3
2216 reflectionsΔρmin = 0.66 e Å3
Special details top

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ca10.74539 (9)1.25015 (14)0.00299 (5)0.0058 (2)
Ca20.66663 (10)0.99471 (11)0.16666 (5)0.0048 (2)
Ca30.66673 (10)0.50152 (11)0.16669 (5)0.0084 (2)
Ca40.26060 (9)0.25007 (14)0.12728 (5)0.0058 (2)
Ca50.00605 (9)0.75023 (14)0.13030 (5)0.0059 (2)
O10.9133 (4)1.0668 (5)0.13303 (18)0.0102 (2)
O20.8721 (3)1.2502 (5)0.23263 (17)0.0102 (2)
O30.5929 (3)1.2500 (5)0.06386 (17)0.0102 (2)
O40.3530 (4)1.0668 (5)0.04338 (18)0.0102 (2)
O50.5349 (3)1.2500 (5)0.20360 (17)0.0102 (2)
O60.7337 (4)1.0663 (5)0.32341 (18)0.0102 (2)
O70.6559 (3)0.7504 (5)0.07428 (17)0.0102 (2)
O80.8514 (3)0.7506 (5)0.25364 (17)0.0102 (2)
O90.4929 (3)0.7499 (5)0.17220 (17)0.0102 (2)
O100.9131 (4)0.4337 (5)0.13308 (18)0.0102 (2)
O110.7338 (4)0.4333 (5)0.32349 (18)0.0102 (2)
O120.3528 (4)0.4337 (5)0.04323 (18)0.0102 (2)
P10.96721 (11)1.25005 (18)0.18741 (6)0.0047 (2)
P20.40765 (12)1.25027 (17)0.01642 (6)0.0047 (2)
P30.62512 (11)1.24988 (18)0.29616 (6)0.0047 (2)
Cl1A0.0019 (3)0.5600 (4)0.00045 (15)0.0160 (4)0.496 (2)
Cl1B0.0017 (3)0.9433 (4)0.00051 (15)0.0160 (4)0.504 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0059 (4)0.0055 (4)0.0067 (4)0.0003 (3)0.0037 (3)0.0001 (4)
Ca20.0049 (4)0.0054 (5)0.0046 (4)0.0015 (3)0.0026 (3)0.0007 (3)
Ca30.0102 (4)0.0033 (5)0.0105 (4)0.0015 (3)0.0043 (4)0.0009 (3)
Ca40.0046 (4)0.0058 (4)0.0058 (4)0.0002 (3)0.0017 (3)0.0002 (4)
Ca50.0064 (4)0.0057 (4)0.0050 (4)0.0001 (4)0.0024 (3)0.0004 (3)
O10.0093 (4)0.0116 (5)0.0092 (4)0.0003 (4)0.0043 (4)0.0002 (4)
O20.0093 (4)0.0116 (5)0.0092 (4)0.0003 (4)0.0043 (4)0.0002 (4)
O30.0093 (4)0.0116 (5)0.0092 (4)0.0003 (4)0.0043 (4)0.0002 (4)
O40.0093 (4)0.0116 (5)0.0092 (4)0.0003 (4)0.0043 (4)0.0002 (4)
O50.0093 (4)0.0116 (5)0.0092 (4)0.0003 (4)0.0043 (4)0.0002 (4)
O60.0093 (4)0.0116 (5)0.0092 (4)0.0003 (4)0.0043 (4)0.0002 (4)
O70.0093 (4)0.0116 (5)0.0092 (4)0.0003 (4)0.0043 (4)0.0002 (4)
O80.0093 (4)0.0116 (5)0.0092 (4)0.0003 (4)0.0043 (4)0.0002 (4)
O90.0093 (4)0.0116 (5)0.0092 (4)0.0003 (4)0.0043 (4)0.0002 (4)
O100.0093 (4)0.0116 (5)0.0092 (4)0.0003 (4)0.0043 (4)0.0002 (4)
O110.0093 (4)0.0116 (5)0.0092 (4)0.0003 (4)0.0043 (4)0.0002 (4)
O120.0093 (4)0.0116 (5)0.0092 (4)0.0003 (4)0.0043 (4)0.0002 (4)
P10.0039 (5)0.0059 (5)0.0040 (5)0.0006 (4)0.0017 (4)0.0001 (4)
P20.0043 (4)0.0058 (5)0.0041 (5)0.0001 (4)0.0021 (4)0.0002 (4)
P30.0037 (4)0.0057 (5)0.0043 (4)0.0003 (4)0.0017 (4)0.0002 (4)
Cl1A0.0080 (6)0.0313 (10)0.0088 (6)0.0006 (10)0.0042 (5)0.0004 (11)
Cl1B0.0080 (6)0.0313 (10)0.0088 (6)0.0006 (10)0.0042 (5)0.0004 (11)
Geometric parameters (Å, º) top
Ca1—O32.291 (3)Ca5—Cl1Bx3.215 (3)
Ca1—O12i2.322 (3)Ca5—Cl1Avii3.258 (3)
Ca1—O4i2.328 (3)Ca5—P1vi3.3896 (12)
Ca1—O12.524 (3)O1—P11.533 (3)
Ca1—O10ii2.525 (3)O1—Ca5iv2.325 (3)
Ca1—Cl1Bi2.784 (3)O2—P11.547 (3)
Ca1—Cl1Ai2.812 (3)O2—Ca5ix2.292 (3)
Ca1—O9i2.986 (3)O2—Ca3ii2.427 (3)
Ca1—P13.0983 (12)O3—P21.546 (3)
Ca1—Cl1Aiii3.226 (3)O3—Ca3ii2.428 (3)
Ca1—Cl1Biv3.248 (3)O4—P21.533 (3)
Ca1—P23.3893 (12)O4—Ca1i2.328 (3)
Ca2—O82.388 (3)O4—Ca4ii2.523 (3)
Ca2—O72.389 (3)O5—P31.545 (3)
Ca2—O92.390 (3)O5—Ca4ii2.294 (3)
Ca2—O52.445 (3)O5—Ca3ii2.428 (3)
Ca2—O32.446 (3)O6—P31.534 (3)
Ca2—O22.447 (3)O6—Ca4ix2.324 (3)
Ca2—O62.796 (3)O6—Ca5ix2.526 (3)
Ca2—O42.799 (3)O7—P2i1.535 (3)
Ca2—O12.799 (3)O7—Ca5iv2.983 (3)
Ca2—P33.2152 (13)O8—P1xi1.536 (3)
Ca2—P13.2168 (13)O8—Ca4ix2.983 (3)
Ca2—P23.2176 (13)O9—P3vi1.535 (3)
Ca3—O92.407 (3)O9—Ca1i2.986 (3)
Ca3—O72.410 (3)O10—P1v1.534 (3)
Ca3—O82.411 (3)O10—Ca5iv2.326 (3)
Ca3—O2v2.427 (3)O10—Ca1v2.525 (3)
Ca3—O5v2.428 (3)O11—P3v1.533 (3)
Ca3—O3v2.428 (3)O11—Ca4ix2.327 (3)
Ca3—O102.791 (3)O11—Ca5vi2.523 (3)
Ca3—O112.793 (3)O12—P2v1.532 (3)
Ca3—O122.796 (3)O12—Ca1i2.322 (3)
Ca3—P1v3.2022 (13)P1—O10ii1.534 (3)
Ca3—P3v3.2026 (13)P1—O8xii1.536 (3)
Ca3—P2v3.2027 (13)P1—Ca3ii3.2022 (13)
Ca4—O5v2.294 (3)P1—Ca5ix3.3896 (12)
Ca4—O6vi2.324 (3)P2—O12ii1.532 (3)
Ca4—O11vi2.327 (3)P2—O7i1.535 (3)
Ca4—O4v2.523 (3)P2—Ca4ii3.0961 (12)
Ca4—O122.526 (3)P2—Ca3ii3.2027 (13)
Ca4—Cl1Avii2.789 (3)P3—O11ii1.533 (3)
Ca4—Cl1Bvii2.807 (3)P3—O9ix1.535 (3)
Ca4—O8vi2.983 (3)P3—Ca5ix3.0980 (12)
Ca4—P2v3.0961 (12)P3—Ca3ii3.2026 (13)
Ca4—Cl1Bv3.228 (3)P3—Ca4ii3.3906 (12)
Ca4—Cl1A3.249 (3)Cl1A—Cl1Avii0.810 (5)
Ca4—P3v3.3906 (12)Cl1A—Ca4vii2.789 (3)
Ca5—O2vi2.292 (3)Cl1A—Ca1i2.812 (3)
Ca5—O1viii2.325 (3)Cl1A—Ca1xiii3.226 (3)
Ca5—O10viii2.326 (3)Cl1A—Ca5vii3.258 (3)
Ca5—O11ix2.523 (3)Cl1B—Cl1Bx0.767 (5)
Ca5—O6vi2.526 (3)Cl1B—Ca1i2.784 (3)
Ca5—Cl1A2.777 (3)Cl1B—Ca4vii2.807 (3)
Ca5—Cl1B2.817 (3)Cl1B—Ca5x3.215 (3)
Ca5—O7viii2.983 (3)Cl1B—Ca4ii3.228 (3)
Ca5—P3vi3.0980 (12)Cl1B—Ca1viii3.248 (3)
O3—Ca1—O12i87.37 (11)O1viii—Ca5—Cl1A127.32 (10)
O3—Ca1—O4i87.35 (11)O10viii—Ca5—Cl1A76.06 (9)
O12i—Ca1—O4i133.32 (10)O11ix—Ca5—Cl1A96.86 (9)
O3—Ca1—O175.44 (10)O6vi—Ca5—Cl1A70.57 (9)
O12i—Ca1—O1140.05 (11)O2vi—Ca5—Cl1B143.19 (10)
O4i—Ca1—O182.37 (11)O1viii—Ca5—Cl1B76.22 (9)
O3—Ca1—O10ii75.42 (10)O10viii—Ca5—Cl1B127.64 (10)
O12i—Ca1—O10ii82.34 (11)O11ix—Ca5—Cl1B70.00 (9)
O4i—Ca1—O10ii140.07 (11)O6vi—Ca5—Cl1B96.39 (9)
O1—Ca1—O10ii58.67 (9)Cl1A—Ca5—Cl1B55.02 (6)
O3—Ca1—Cl1Bi142.96 (10)O2vi—Ca5—O7viii104.61 (9)
O12i—Ca1—Cl1Bi128.02 (9)O1viii—Ca5—O7viii68.29 (10)
O4i—Ca1—Cl1Bi75.83 (9)O10viii—Ca5—O7viii68.29 (10)
O1—Ca1—Cl1Bi69.83 (9)O11ix—Ca5—O7viii150.61 (10)
O10ii—Ca1—Cl1Bi96.62 (9)O6vi—Ca5—O7viii150.55 (10)
O3—Ca1—Cl1Ai143.83 (10)Cl1A—Ca5—O7viii99.02 (8)
O12i—Ca1—Cl1Ai76.56 (9)Cl1B—Ca5—O7viii99.63 (8)
O4i—Ca1—Cl1Ai127.08 (9)O2vi—Ca5—P3vi70.31 (7)
O1—Ca1—Cl1Ai96.39 (9)O1viii—Ca5—P3vi110.86 (8)
O10ii—Ca1—Cl1Ai70.51 (9)O10viii—Ca5—P3vi110.82 (8)
Cl1Bi—Ca1—Cl1Ai55.01 (6)O11ix—Ca5—P3vi29.45 (7)
O3—Ca1—O9i104.53 (9)O6vi—Ca5—P3vi29.48 (7)
O12i—Ca1—O9i68.33 (10)Cl1A—Ca5—P3vi85.46 (6)
O4i—Ca1—O9i68.32 (10)Cl1B—Ca5—P3vi84.87 (6)
O1—Ca1—O9i150.59 (10)O7viii—Ca5—P3vi174.93 (6)
O10ii—Ca1—O9i150.58 (10)O2vi—Ca5—Cl1Bx134.07 (10)
Cl1Bi—Ca1—O9i99.54 (8)O1viii—Ca5—Cl1Bx64.37 (9)
Cl1Ai—Ca1—O9i99.31 (8)O10viii—Ca5—Cl1Bx138.43 (9)
O3—Ca1—P170.40 (8)O11ix—Ca5—Cl1Bx66.00 (8)
O12i—Ca1—P1110.82 (8)O6vi—Ca5—Cl1Bx102.92 (8)
O4i—Ca1—P1110.80 (8)Cl1A—Ca5—Cl1Bx67.50 (8)
O1—Ca1—P129.44 (7)Cl1B—Ca5—Cl1Bx12.50 (9)
O10ii—Ca1—P129.48 (7)O7viii—Ca5—Cl1Bx97.78 (8)
Cl1Bi—Ca1—P184.92 (6)P3vi—Ca5—Cl1Bx86.10 (5)
Cl1Ai—Ca1—P185.20 (6)O2vi—Ca5—Cl1Avii133.77 (10)
O9i—Ca1—P1174.93 (6)O1viii—Ca5—Cl1Avii138.63 (9)
O3—Ca1—Cl1Aiii133.56 (10)O10viii—Ca5—Cl1Avii64.69 (9)
O12i—Ca1—Cl1Aiii64.25 (9)O11ix—Ca5—Cl1Avii102.31 (8)
O4i—Ca1—Cl1Aiii138.96 (9)O6vi—Ca5—Cl1Avii65.46 (8)
O1—Ca1—Cl1Aiii102.59 (9)Cl1A—Ca5—Cl1Avii12.45 (10)
O10ii—Ca1—Cl1Aiii65.44 (8)Cl1B—Ca5—Cl1Avii67.45 (8)
Cl1Bi—Ca1—Cl1Aiii68.29 (8)O7viii—Ca5—Cl1Avii98.37 (8)
Cl1Ai—Ca1—Cl1Aiii13.28 (9)P3vi—Ca5—Cl1Avii85.49 (5)
O9i—Ca1—Cl1Aiii98.20 (8)Cl1Bx—Ca5—Cl1Avii79.94 (6)
P1—Ca1—Cl1Aiii85.65 (5)O2vi—Ca5—P1vi22.55 (7)
O3—Ca1—Cl1Biv134.30 (10)O1viii—Ca5—P1vi78.94 (8)
O12i—Ca1—Cl1Biv138.19 (9)O10viii—Ca5—P1vi78.85 (8)
O4i—Ca1—Cl1Biv64.85 (9)O11ix—Ca5—P1vi94.96 (7)
O1—Ca1—Cl1Biv65.90 (8)O6vi—Ca5—P1vi94.91 (7)
O10ii—Ca1—Cl1Biv102.52 (9)Cl1A—Ca5—P1vi152.39 (7)
Cl1Bi—Ca1—Cl1Biv11.65 (10)Cl1B—Ca5—P1vi152.36 (7)
Cl1Ai—Ca1—Cl1Biv66.65 (8)O7viii—Ca5—P1vi82.06 (6)
O9i—Ca1—Cl1Biv98.03 (8)P3vi—Ca5—P1vi92.86 (3)
P1—Ca1—Cl1Biv85.85 (5)Cl1Bx—Ca5—P1vi139.97 (6)
Cl1Aiii—Ca1—Cl1Biv79.94 (6)Cl1Avii—Ca5—P1vi139.95 (6)
O3—Ca1—P222.52 (7)P1—O1—Ca5iv138.83 (18)
O12i—Ca1—P278.83 (8)P1—O1—Ca196.53 (15)
O4i—Ca1—P278.89 (8)Ca5iv—O1—Ca1119.36 (12)
O1—Ca1—P295.05 (7)P1—O1—Ca291.07 (13)
O10ii—Ca1—P294.97 (7)Ca5iv—O1—Ca2103.05 (11)
Cl1Bi—Ca1—P2151.95 (7)Ca1—O1—Ca296.75 (10)
Cl1Ai—Ca1—P2152.81 (6)P1—O2—Ca5ix122.84 (16)
O9i—Ca1—P282.01 (6)P1—O2—Ca3ii105.23 (16)
P1—Ca1—P292.92 (3)Ca5ix—O2—Ca3ii114.66 (13)
Cl1Aiii—Ca1—P2139.55 (6)P1—O2—Ca2105.07 (16)
Cl1Biv—Ca1—P2140.37 (6)Ca5ix—O2—Ca2114.47 (13)
O8—Ca2—O777.70 (11)Ca3ii—O2—Ca289.04 (10)
O8—Ca2—O977.62 (11)P2—O3—Ca1122.89 (16)
O7—Ca2—O977.67 (11)P2—O3—Ca3ii105.21 (16)
O8—Ca2—O5126.45 (10)Ca1—O3—Ca3ii114.56 (13)
O7—Ca2—O5150.05 (10)P2—O3—Ca2105.18 (16)
O9—Ca2—O589.82 (11)Ca1—O3—Ca2114.43 (13)
O8—Ca2—O3150.00 (10)Ca3ii—O3—Ca289.02 (10)
O7—Ca2—O389.72 (11)P2—O4—Ca1i138.91 (18)
O9—Ca2—O3126.55 (10)P2—O4—Ca4ii96.46 (15)
O5—Ca2—O375.95 (10)Ca1i—O4—Ca4ii119.29 (12)
O8—Ca2—O289.71 (11)P2—O4—Ca291.14 (13)
O7—Ca2—O2126.51 (10)Ca1i—O4—Ca2103.06 (11)
O9—Ca2—O2149.96 (10)Ca4ii—O4—Ca296.79 (10)
O5—Ca2—O275.87 (10)P3—O5—Ca4ii122.91 (16)
O3—Ca2—O275.96 (10)P3—O5—Ca3ii105.29 (16)
O8—Ca2—O670.87 (10)Ca4ii—O5—Ca3ii114.56 (13)
O7—Ca2—O6145.50 (11)P3—O5—Ca2105.13 (16)
O9—Ca2—O681.98 (10)Ca4ii—O5—Ca2114.35 (13)
O5—Ca2—O655.80 (9)Ca3ii—O5—Ca289.05 (10)
O3—Ca2—O6124.73 (10)P3—O6—Ca4ix138.84 (18)
O2—Ca2—O668.09 (9)P3—O6—Ca5ix96.40 (15)
O8—Ca2—O4145.59 (11)Ca4ix—O6—Ca5ix119.32 (13)
O7—Ca2—O482.02 (10)P3—O6—Ca291.12 (14)
O9—Ca2—O471.03 (10)Ca4ix—O6—Ca2103.20 (11)
O5—Ca2—O468.14 (9)Ca5ix—O6—Ca296.86 (10)
O3—Ca2—O455.75 (9)P2i—O7—Ca2133.9 (2)
O2—Ca2—O4124.65 (10)P2i—O7—Ca3133.1 (2)
O6—Ca2—O4117.10 (9)Ca2—O7—Ca387.72 (10)
O8—Ca2—O182.00 (10)P2i—O7—Ca5iv98.50 (13)
O7—Ca2—O170.93 (10)Ca2—O7—Ca5iv96.35 (10)
O9—Ca2—O1145.49 (10)Ca3—O7—Ca5iv96.23 (10)
O5—Ca2—O1124.64 (10)P1xi—O8—Ca2133.93 (19)
O3—Ca2—O168.11 (9)P1xi—O8—Ca3133.15 (19)
O2—Ca2—O155.81 (9)Ca2—O8—Ca387.72 (10)
O6—Ca2—O1117.05 (9)P1xi—O8—Ca4ix98.41 (13)
O4—Ca2—O1117.03 (9)Ca2—O8—Ca4ix96.38 (10)
O8—Ca2—P399.35 (8)Ca3—O8—Ca4ix96.24 (10)
O7—Ca2—P3166.17 (8)P3vi—O9—Ca2133.75 (19)
O9—Ca2—P388.50 (8)P3vi—O9—Ca3133.37 (19)
O5—Ca2—P327.63 (7)Ca2—O9—Ca387.75 (10)
O3—Ca2—P398.81 (8)P3vi—O9—Ca1i98.34 (13)
O2—Ca2—P366.56 (7)Ca2—O9—Ca1i96.29 (10)
O6—Ca2—P328.49 (7)Ca3—O9—Ca1i96.25 (10)
O4—Ca2—P393.75 (7)P1v—O10—Ca5iv138.82 (18)
O1—Ca2—P3122.37 (7)P1v—O10—Ca1v96.45 (15)
O8—Ca2—P188.44 (8)Ca5iv—O10—Ca1v119.32 (13)
O7—Ca2—P199.37 (8)P1v—O10—Ca390.73 (13)
O9—Ca2—P1166.06 (8)Ca5iv—O10—Ca3103.68 (11)
O5—Ca2—P198.77 (8)Ca1v—O10—Ca396.55 (10)
O3—Ca2—P166.62 (7)P3v—O11—Ca4ix138.88 (17)
O2—Ca2—P127.67 (7)P3v—O11—Ca5vi96.54 (15)
O6—Ca2—P193.73 (7)Ca4ix—O11—Ca5vi119.24 (13)
O4—Ca2—P1122.37 (7)P3v—O11—Ca390.70 (13)
O1—Ca2—P128.45 (7)Ca4ix—O11—Ca3103.60 (11)
P3—Ca2—P194.02 (3)Ca5vi—O11—Ca396.57 (10)
O8—Ca2—P2166.19 (8)P2v—O12—Ca1i139.02 (18)
O7—Ca2—P288.49 (8)P2v—O12—Ca496.37 (15)
O9—Ca2—P299.47 (8)Ca1i—O12—Ca4119.31 (12)
O5—Ca2—P266.61 (7)P2v—O12—Ca390.60 (13)
O3—Ca2—P227.63 (7)Ca1i—O12—Ca3103.67 (11)
O2—Ca2—P298.78 (8)Ca4—O12—Ca396.44 (10)
O6—Ca2—P2122.41 (7)O1—P1—O10ii107.49 (16)
O4—Ca2—P228.45 (7)O1—P1—O8xii112.26 (18)
O1—Ca2—P293.73 (7)O10ii—P1—O8xii112.07 (18)
P3—Ca2—P294.03 (3)O1—P1—O2106.94 (18)
P1—Ca2—P294.03 (3)O10ii—P1—O2106.77 (18)
O9—Ca3—O776.92 (10)O8xii—P1—O2110.99 (16)
O9—Ca3—O876.87 (10)O1—P1—Ca154.03 (12)
O7—Ca3—O876.86 (10)O10ii—P1—Ca154.07 (12)
O9—Ca3—O2v149.97 (10)O8xii—P1—Ca1136.53 (12)
O7—Ca3—O2v126.58 (10)O2—P1—Ca1112.48 (11)
O8—Ca3—O2v89.84 (11)O1—P1—Ca3ii111.41 (12)
O9—Ca3—O5v89.78 (11)O10ii—P1—Ca3ii60.64 (11)
O7—Ca3—O5v150.06 (10)O8xii—P1—Ca3ii135.58 (13)
O8—Ca3—O5v126.53 (10)O2—P1—Ca3ii46.99 (12)
O2v—Ca3—O5v76.57 (10)Ca1—P1—Ca3ii78.13 (3)
O9—Ca3—O3v126.52 (11)O1—P1—Ca260.47 (11)
O7—Ca3—O3v89.83 (11)O10ii—P1—Ca2111.65 (12)
O8—Ca3—O3v150.09 (10)O8xii—P1—Ca2135.53 (13)
O2v—Ca3—O3v76.65 (10)O2—P1—Ca247.26 (12)
O5v—Ca3—O3v76.60 (10)Ca1—P1—Ca278.19 (3)
O9—Ca3—O10144.54 (11)Ca3ii—P1—Ca264.33 (3)
O7—Ca3—O1070.80 (10)O1—P1—Ca5ix122.18 (12)
O8—Ca3—O1081.81 (10)O10ii—P1—Ca5ix122.02 (12)
O2v—Ca3—O1056.07 (9)O8xii—P1—Ca5ix76.37 (11)
O5v—Ca3—O10125.65 (10)Ca1—P1—Ca5ix147.10 (4)
O3v—Ca3—O1068.46 (9)Ca3ii—P1—Ca5ix74.06 (3)
O9—Ca3—O1181.79 (10)Ca2—P1—Ca5ix74.15 (3)
O7—Ca3—O11144.54 (10)O1—P1—Ca4iii80.22 (12)
O8—Ca3—O1170.84 (10)O10ii—P1—Ca4iii80.33 (12)
O2v—Ca3—O1168.37 (9)O8xii—P1—Ca4iii56.24 (11)
O5v—Ca3—O1155.98 (9)O2—P1—Ca4iii167.23 (12)
O3v—Ca3—O11125.60 (10)Ca1—P1—Ca4iii80.29 (3)
O10—Ca3—O11117.36 (9)Ca3ii—P1—Ca4iii140.95 (4)
O9—Ca3—O1270.80 (10)Ca2—P1—Ca4iii140.65 (4)
O7—Ca3—O1281.74 (10)Ca5ix—P1—Ca4iii132.62 (3)
O8—Ca3—O12144.45 (10)O12ii—P2—O4107.62 (16)
O2v—Ca3—O12125.68 (10)O12ii—P2—O7i112.16 (18)
O5v—Ca3—O1268.50 (9)O4—P2—O7i111.94 (18)
O3v—Ca3—O1255.99 (9)O12ii—P2—O3106.98 (17)
O10—Ca3—O12117.33 (9)O4—P2—O3106.80 (18)
O11—Ca3—O12117.40 (9)O7i—P2—O3111.04 (16)
O9—Ca3—P1v165.42 (8)O12ii—P2—Ca4ii54.17 (12)
O7—Ca3—P1v99.42 (8)O4—P2—Ca4ii54.07 (12)
O8—Ca3—P1v88.57 (8)O7i—P2—Ca4ii136.45 (12)
O2v—Ca3—P1v27.79 (7)O3—P2—Ca4ii112.51 (11)
O5v—Ca3—P1v99.54 (8)O12ii—P2—Ca3ii60.82 (12)
O3v—Ca3—P1v67.05 (7)O4—P2—Ca3ii111.41 (12)
O10—Ca3—P1v28.63 (7)O7i—P2—Ca3ii135.86 (13)
O11—Ca3—P1v94.11 (7)O3—P2—Ca3ii47.03 (12)
O12—Ca3—P1v123.04 (7)Ca4ii—P2—Ca3ii78.19 (3)
O9—Ca3—P3v88.51 (8)O12ii—P2—Ca2111.84 (12)
O7—Ca3—P3v165.42 (8)O4—P2—Ca260.42 (12)
O8—Ca3—P3v99.44 (8)O7i—P2—Ca2135.31 (13)
O2v—Ca3—P3v66.97 (7)O3—P2—Ca247.19 (12)
O5v—Ca3—P3v27.72 (7)Ca4ii—P2—Ca278.21 (3)
O3v—Ca3—P3v99.53 (8)Ca3ii—P2—Ca264.31 (3)
O10—Ca3—P3v123.04 (7)O12ii—P2—Ca1122.09 (12)
O11—Ca3—P3v28.60 (7)O4—P2—Ca1122.06 (12)
O12—Ca3—P3v94.18 (7)O7i—P2—Ca176.45 (11)
P1v—Ca3—P3v94.54 (3)Ca4ii—P2—Ca1147.10 (4)
O9—Ca3—P2v99.37 (8)Ca3ii—P2—Ca174.03 (3)
O7—Ca3—P2v88.52 (8)Ca2—P2—Ca174.11 (3)
O8—Ca3—P2v165.37 (8)O12ii—P2—Ca5x80.24 (12)
O2v—Ca3—P2v99.61 (8)O4—P2—Ca5x80.22 (12)
O5v—Ca3—P2v67.04 (7)O7i—P2—Ca5x56.18 (11)
O3v—Ca3—P2v27.76 (7)O3—P2—Ca5x167.22 (12)
O10—Ca3—P2v94.16 (7)Ca4ii—P2—Ca5x80.26 (3)
O11—Ca3—P2v123.02 (7)Ca3ii—P2—Ca5x141.03 (4)
O12—Ca3—P2v28.58 (7)Ca2—P2—Ca5x140.59 (4)
P1v—Ca3—P2v94.60 (3)Ca1—P2—Ca5x132.63 (3)
P3v—Ca3—P2v94.55 (3)O11ii—P3—O6107.54 (16)
O5v—Ca4—O6vi87.35 (11)O11ii—P3—O9ix112.18 (18)
O5v—Ca4—O11vi87.35 (11)O6—P3—O9ix112.21 (18)
O6vi—Ca4—O11vi133.23 (10)O11ii—P3—O5106.83 (18)
O5v—Ca4—O4v75.44 (10)O6—P3—O5106.84 (18)
O6vi—Ca4—O4v140.11 (11)O9ix—P3—O5110.93 (16)
O11vi—Ca4—O4v82.39 (10)O11ii—P3—Ca5ix54.01 (12)
O5v—Ca4—O1275.49 (10)O6—P3—Ca5ix54.12 (12)
O6vi—Ca4—O1282.42 (10)O9ix—P3—Ca5ix136.55 (12)
O11vi—Ca4—O12140.11 (11)O5—P3—Ca5ix112.51 (11)
O4v—Ca4—O1258.68 (9)O11ii—P3—Ca3ii60.70 (12)
O5v—Ca4—Cl1Avii143.22 (10)O6—P3—Ca3ii111.38 (12)
O6vi—Ca4—Cl1Avii76.54 (9)O9ix—P3—Ca3ii135.62 (13)
O11vi—Ca4—Cl1Avii127.58 (10)O5—P3—Ca3ii46.98 (12)
O4v—Ca4—Cl1Avii96.05 (9)Ca5ix—P3—Ca3ii78.15 (3)
O12—Ca4—Cl1Avii69.80 (9)O11ii—P3—Ca2111.71 (12)
O5v—Ca4—Cl1Bvii143.65 (10)O6—P3—Ca260.39 (12)
O6vi—Ca4—Cl1Bvii127.49 (9)O9ix—P3—Ca2135.38 (13)
O11vi—Ca4—Cl1Bvii75.87 (9)O5—P3—Ca247.24 (12)
O4v—Ca4—Cl1Bvii70.59 (9)Ca5ix—P3—Ca278.26 (3)
O12—Ca4—Cl1Bvii97.01 (9)Ca3ii—P3—Ca264.34 (3)
Cl1Avii—Ca4—Cl1Bvii55.01 (6)O11ii—P3—Ca4ii122.08 (13)
O5v—Ca4—O8vi104.51 (9)O6—P3—Ca4ii122.06 (13)
O6vi—Ca4—O8vi68.18 (10)O9ix—P3—Ca4ii76.32 (11)
O11vi—Ca4—O8vi68.37 (10)Ca5ix—P3—Ca4ii147.12 (4)
O4v—Ca4—O8vi150.66 (11)Ca3ii—P3—Ca4ii74.05 (3)
O12—Ca4—O8vi150.50 (11)Ca2—P3—Ca4ii74.12 (3)
Cl1Avii—Ca4—O8vi99.84 (8)O11ii—P3—Ca1xiv80.25 (12)
Cl1Bvii—Ca4—O8vi98.93 (8)O6—P3—Ca1xiv80.30 (12)
O5v—Ca4—P2v70.41 (7)O9ix—P3—Ca1xiv56.34 (11)
O6vi—Ca4—P2v110.86 (8)O5—P3—Ca1xiv167.27 (12)
O11vi—Ca4—P2v110.85 (8)Ca5ix—P3—Ca1xiv80.22 (3)
O4v—Ca4—P2v29.47 (7)Ca3ii—P3—Ca1xiv140.92 (4)
O12—Ca4—P2v29.46 (7)Ca2—P3—Ca1xiv140.64 (4)
Cl1Avii—Ca4—P2v84.62 (6)Ca4ii—P3—Ca1xiv132.66 (3)
Cl1Bvii—Ca4—P2v85.60 (6)Cl1Avii—Cl1A—Ca5119.9 (4)
O8vi—Ca4—P2v174.92 (6)Cl1Avii—Cl1A—Ca4vii118.0 (4)
O5v—Ca4—Cl1Bv133.80 (10)Ca5—Cl1A—Ca4vii101.12 (8)
O6vi—Ca4—Cl1Bv138.68 (9)Cl1Avii—Cl1A—Ca1i113.8 (4)
O11vi—Ca4—Cl1Bv64.81 (9)Ca5—Cl1A—Ca1i100.46 (8)
O4v—Ca4—Cl1Bv65.36 (8)Ca4vii—Cl1A—Ca1i100.28 (8)
O12—Ca4—Cl1Bv102.15 (9)Cl1Avii—Cl1A—Ca1xiii52.9 (3)
Cl1Avii—Ca4—Cl1Bv67.19 (8)Ca5—Cl1A—Ca1xiii88.11 (7)
Cl1Bvii—Ca4—Cl1Bv12.21 (10)Ca4vii—Cl1A—Ca1xiii87.85 (7)
O8vi—Ca4—Cl1Bv98.56 (8)Ca1i—Cl1A—Ca1xiii166.72 (9)
P2v—Ca4—Cl1Bv85.39 (5)Cl1Avii—Cl1A—Ca449.3 (3)
O5v—Ca4—Cl1A134.14 (10)Ca5—Cl1A—Ca487.64 (7)
O6vi—Ca4—Cl1A64.38 (9)Ca4vii—Cl1A—Ca4167.28 (10)
O11vi—Ca4—Cl1A138.41 (9)Ca1i—Cl1A—Ca487.00 (7)
O4v—Ca4—Cl1A102.96 (9)Ca1xiii—Cl1A—Ca483.20 (6)
O12—Ca4—Cl1A66.01 (8)Cl1Avii—Cl1A—Ca5vii47.6 (3)
Cl1Avii—Ca4—Cl1A12.72 (10)Ca5—Cl1A—Ca5vii167.55 (10)
Cl1Bvii—Ca4—Cl1A67.70 (8)Ca4vii—Cl1A—Ca5vii87.27 (7)
O8vi—Ca4—Cl1A97.64 (8)Ca1i—Cl1A—Ca5vii86.89 (6)
P2v—Ca4—Cl1A86.18 (5)Ca1xiii—Cl1A—Ca5vii82.99 (6)
Cl1Bv—Ca4—Cl1A79.89 (6)Ca4—Cl1A—Ca5vii82.69 (6)
O5v—Ca4—P3v22.49 (7)Cl1Bx—Cl1B—Ca1i121.2 (4)
O6vi—Ca4—P3v78.85 (8)Cl1Bx—Cl1B—Ca4vii117.0 (4)
O11vi—Ca4—P3v78.84 (8)Ca1i—Cl1B—Ca4vii100.52 (8)
O4v—Ca4—P3v94.98 (7)Cl1Bx—Cl1B—Ca5114.8 (4)
O12—Ca4—P3v95.05 (7)Ca1i—Cl1B—Ca5100.18 (8)
Cl1Avii—Ca4—P3v152.52 (7)Ca4vii—Cl1B—Ca599.68 (8)
Cl1Bvii—Ca4—P3v152.24 (6)Cl1Bx—Cl1B—Ca5x52.7 (3)
O8vi—Ca4—P3v82.02 (6)Ca1i—Cl1B—Ca5x88.20 (7)
P2v—Ca4—P3v92.90 (3)Ca4vii—Cl1B—Ca5x87.76 (7)
Cl1Bv—Ca4—P3v140.03 (6)Ca5—Cl1B—Ca5x167.50 (9)
Cl1A—Ca4—P3v139.95 (6)Cl1Bx—Cl1B—Ca4ii50.8 (4)
O2vi—Ca5—O1viii87.45 (12)Ca1i—Cl1B—Ca4ii87.95 (7)
O2vi—Ca5—O10viii87.40 (12)Ca4vii—Cl1B—Ca4ii167.79 (10)
O1viii—Ca5—O10viii133.28 (10)Ca5—Cl1B—Ca4ii87.33 (7)
O2vi—Ca5—O11ix75.35 (10)Ca5x—Cl1B—Ca4ii83.69 (6)
O1viii—Ca5—O11ix82.42 (11)Cl1Bx—Cl1B—Ca1viii47.2 (3)
O10viii—Ca5—O11ix140.06 (11)Ca1i—Cl1B—Ca1viii168.35 (10)
O2vi—Ca5—O6vi75.32 (10)Ca4vii—Cl1B—Ca1viii87.17 (7)
O1viii—Ca5—O6vi140.13 (11)Ca5—Cl1B—Ca1viii87.00 (7)
O10viii—Ca5—O6vi82.35 (10)Ca5x—Cl1B—Ca1viii83.33 (6)
O11ix—Ca5—O6vi58.68 (9)Ca4ii—Cl1B—Ca1viii83.19 (6)
O2vi—Ca5—Cl1A143.63 (10)
Symmetry codes: (i) x+1, y+2, z; (ii) x, y+1, z; (iii) x+1, y+1, z; (iv) x+1, y, z; (v) x, y1, z; (vi) x+1, y1/2, z+1/2; (vii) x, y+1, z; (viii) x1, y, z; (ix) x+1, y+1/2, z+1/2; (x) x, y+2, z; (xi) x+2, y1/2, z+1/2; (xii) x+2, y+1/2, z+1/2; (xiii) x1, y1, z; (xiv) x, y+5/2, z+1/2.
(F_mono) top
Crystal data top
Ca5ClO12P3F(000) = 1032
Mr = 520.76Dx = 3.19 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.7107 Å
Hall symbol: -P 2ybcCell parameters from 1997 reflections
a = 9.6344 (3) Åθ = 2.4–27.2°
b = 6.7442 (2) ŵ = 3.23 mm1
c = 19.2656 (5) ÅT = 100 K
β = 119.994 (1)°Prism, colourless
V = 1084.16 (5) Å30.29 × 0.12 × 0.10 mm
Z = 4
Data collection top
BRUKER APPEX-II CCD
diffractometer
2213 independent reflections
Radiation source: fine-focus sealed tube1431 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.030
ω and phi scansθmax = 26.4°, θmin = 2.4°
Absorption correction: multi-scan
BRUKER SADABS
h = 1210
Tmin = 0.482, Tmax = 1k = 08
12807 measured reflectionsl = 023
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.038 w = 1/[σ2(Fo2) + (0.038P)2 + 5.3396P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.103(Δ/σ)max < 0.001
S = 1.15Δρmax = 1.01 e Å3
2213 reflectionsΔρmin = 0.6 e Å3
130 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0309 (12)
Crystal data top
Ca5ClO12P3V = 1084.16 (5) Å3
Mr = 520.76Z = 4
Monoclinic, P21/cMo Kα radiation
a = 9.6344 (3) ŵ = 3.23 mm1
b = 6.7442 (2) ÅT = 100 K
c = 19.2656 (5) Å0.29 × 0.12 × 0.10 mm
β = 119.994 (1)°
Data collection top
BRUKER APPEX-II CCD
diffractometer
2213 independent reflections
Absorption correction: multi-scan
BRUKER SADABS
1431 reflections with I > 2σ(I)
Tmin = 0.482, Tmax = 1Rint = 0.030
12807 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.038130 parameters
wR(F2) = 0.1030 restraints
S = 1.15Δρmax = 1.01 e Å3
2213 reflectionsΔρmin = 0.6 e Å3
Special details top

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ca10.74536 (9)1.25015 (12)0.00298 (4)0.0065 (2)
Ca20.66670 (9)0.99465 (10)0.16669 (5)0.0055 (2)
Ca30.66671 (10)0.50132 (11)0.16670 (5)0.0089 (2)
Ca40.26051 (9)0.24998 (12)0.12727 (4)0.0065 (2)
Ca50.00598 (9)0.75010 (12)0.13029 (4)0.0066 (2)
O10.9130 (3)1.0666 (4)0.13291 (17)0.0110 (2)
O20.8722 (3)1.2504 (4)0.23264 (17)0.0110 (2)
O30.5929 (3)1.2500 (4)0.06387 (17)0.0110 (2)
O40.3531 (3)1.0666 (4)0.04350 (17)0.0110 (2)
O50.5348 (3)1.2501 (4)0.20345 (17)0.0110 (2)
O60.7338 (3)1.0665 (4)0.32351 (17)0.0110 (2)
O70.6561 (3)0.7503 (4)0.07439 (17)0.0110 (2)
O80.8512 (3)0.7501 (4)0.25354 (17)0.0110 (2)
O90.4928 (3)0.7501 (4)0.17203 (17)0.0110 (2)
O100.9130 (3)0.4339 (4)0.13300 (17)0.0110 (2)
O110.7340 (3)0.4330 (4)0.32360 (17)0.0110 (2)
O120.3526 (3)0.4337 (4)0.04326 (17)0.0110 (2)
P10.96730 (11)1.24998 (16)0.18744 (6)0.0051 (2)
P20.40760 (11)1.25021 (15)0.01632 (6)0.0054 (2)
P30.62505 (11)1.25011 (15)0.29617 (6)0.0052 (2)
Cl1A0.0013 (3)0.5605 (3)0.00112 (13)0.0166 (4)0.497 (2)
Cl1B0.0016 (3)0.9442 (3)0.00126 (13)0.0166 (4)0.503 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0076 (4)0.0060 (4)0.0073 (4)0.0000 (3)0.0046 (3)0.0003 (3)
Ca20.0068 (4)0.0052 (4)0.0051 (4)0.0020 (3)0.0035 (3)0.0025 (3)
Ca30.0117 (4)0.0037 (4)0.0111 (4)0.0021 (3)0.0055 (4)0.0026 (3)
Ca40.0063 (4)0.0061 (4)0.0066 (4)0.0002 (3)0.0028 (3)0.0000 (3)
Ca50.0083 (4)0.0060 (4)0.0055 (4)0.0001 (3)0.0035 (3)0.0001 (3)
O10.0108 (4)0.0126 (5)0.0098 (4)0.0003 (3)0.0054 (4)0.0002 (3)
O20.0108 (4)0.0126 (5)0.0098 (4)0.0003 (3)0.0054 (4)0.0002 (3)
O30.0108 (4)0.0126 (5)0.0098 (4)0.0003 (3)0.0054 (4)0.0002 (3)
O40.0108 (4)0.0126 (5)0.0098 (4)0.0003 (3)0.0054 (4)0.0002 (3)
O50.0108 (4)0.0126 (5)0.0098 (4)0.0003 (3)0.0054 (4)0.0002 (3)
O60.0108 (4)0.0126 (5)0.0098 (4)0.0003 (3)0.0054 (4)0.0002 (3)
O70.0108 (4)0.0126 (5)0.0098 (4)0.0003 (3)0.0054 (4)0.0002 (3)
O80.0108 (4)0.0126 (5)0.0098 (4)0.0003 (3)0.0054 (4)0.0002 (3)
O90.0108 (4)0.0126 (5)0.0098 (4)0.0003 (3)0.0054 (4)0.0002 (3)
O100.0108 (4)0.0126 (5)0.0098 (4)0.0003 (3)0.0054 (4)0.0002 (3)
O110.0108 (4)0.0126 (5)0.0098 (4)0.0003 (3)0.0054 (4)0.0002 (3)
O120.0108 (4)0.0126 (5)0.0098 (4)0.0003 (3)0.0054 (4)0.0002 (3)
P10.0054 (5)0.0060 (5)0.0044 (5)0.0004 (4)0.0027 (4)0.0004 (4)
P20.0062 (4)0.0056 (5)0.0046 (5)0.0003 (4)0.0029 (4)0.0005 (4)
P30.0055 (4)0.0058 (5)0.0044 (4)0.0004 (4)0.0026 (4)0.0001 (4)
Cl1A0.0101 (6)0.0315 (11)0.0081 (6)0.0016 (9)0.0046 (5)0.0019 (9)
Cl1B0.0101 (6)0.0315 (11)0.0081 (6)0.0016 (9)0.0046 (5)0.0019 (9)
Geometric parameters (Å, º) top
Ca1—O32.292 (3)Ca5—Cl1Bx3.214 (2)
Ca1—O12i2.321 (3)Ca5—Cl1Avii3.260 (2)
Ca1—O4i2.327 (3)Ca5—P1vi3.3900 (12)
Ca1—O12.523 (3)O1—P11.536 (3)
Ca1—O10ii2.525 (3)O1—Ca5iii2.325 (3)
Ca1—Cl1Ai2.791 (2)O2—P11.548 (3)
Ca1—Cl1Bi2.810 (2)O2—Ca5ix2.292 (3)
Ca1—O9i2.983 (3)O2—Ca3ii2.425 (3)
Ca1—P13.0991 (12)O3—P21.547 (3)
Ca1—Cl1Biii3.226 (2)O3—Ca3ii2.428 (3)
Ca1—Cl1Aiv3.248 (2)O4—P21.536 (3)
Ca1—P23.3899 (12)O4—Ca1i2.327 (3)
Ca2—O82.388 (3)O4—Ca4ii2.524 (3)
Ca2—O72.389 (3)O5—P31.547 (3)
Ca2—O92.390 (3)O5—Ca4ii2.293 (3)
Ca2—O52.446 (3)O5—Ca3ii2.427 (3)
Ca2—O32.447 (3)O6—P31.535 (3)
Ca2—O22.448 (3)O6—Ca4ix2.325 (3)
Ca2—O62.798 (3)O6—Ca5ix2.526 (3)
Ca2—O42.798 (3)O7—P2i1.536 (3)
Ca2—O12.799 (3)O7—Ca5iii2.982 (3)
Ca2—P33.2175 (12)O8—P1xi1.537 (3)
Ca2—P13.2179 (12)O8—Ca4ix2.984 (3)
Ca2—P23.2194 (12)O9—P3vi1.536 (3)
Ca3—O82.409 (3)O9—Ca1i2.983 (3)
Ca3—O92.410 (3)O10—P1v1.537 (3)
Ca3—O72.410 (3)O10—Ca5iii2.324 (3)
Ca3—O2v2.425 (3)O10—Ca1v2.525 (3)
Ca3—O5v2.427 (3)O11—P3v1.532 (3)
Ca3—O3v2.428 (3)O11—Ca4ix2.327 (3)
Ca3—O102.793 (3)O11—Ca5vi2.523 (3)
Ca3—O112.795 (3)O12—P2v1.535 (3)
Ca3—O122.797 (3)O12—Ca1i2.321 (3)
Ca3—P3v3.2023 (12)P1—O8xii1.537 (3)
Ca3—P2v3.2035 (12)P1—O10ii1.537 (3)
Ca3—P1v3.2035 (12)P1—Ca3ii3.2035 (12)
Ca4—O5v2.293 (3)P1—Ca5ix3.3900 (12)
Ca4—O6vi2.325 (3)P2—O12ii1.535 (3)
Ca4—O11vi2.327 (3)P2—O7i1.536 (3)
Ca4—O4v2.524 (3)P2—Ca4ii3.0995 (12)
Ca4—O122.526 (3)P2—Ca3ii3.2035 (12)
Ca4—Cl1Bvii2.789 (2)P3—O11ii1.532 (3)
Ca4—Cl1Avii2.806 (2)P3—O9ix1.536 (3)
Ca4—O8vi2.984 (3)P3—Ca5ix3.0997 (12)
Ca4—P2v3.0995 (12)P3—Ca3ii3.2023 (12)
Ca4—Cl1A3.234 (2)P3—Ca4ii3.3907 (12)
Ca4—Cl1Bv3.242 (2)Cl1A—Cl1Avii0.817 (5)
Ca4—P3v3.3907 (12)Cl1A—Ca1i2.791 (2)
Ca5—O2vi2.292 (3)Cl1A—Ca4vii2.806 (2)
Ca5—O10viii2.324 (3)Cl1A—Ca1xiii3.248 (2)
Ca5—O1viii2.325 (3)Cl1A—Ca5vii3.260 (2)
Ca5—O11ix2.523 (3)Cl1B—Cl1Bx0.753 (4)
Ca5—O6vi2.526 (3)Cl1B—Ca4vii2.789 (2)
Ca5—Cl1A2.778 (2)Cl1B—Ca1i2.810 (2)
Ca5—Cl1B2.821 (2)Cl1B—Ca5x3.214 (2)
Ca5—O7viii2.982 (3)Cl1B—Ca1viii3.226 (2)
Ca5—P3vi3.0997 (12)Cl1B—Ca4ii3.242 (2)
O3—Ca1—O12i87.42 (10)O10viii—Ca5—Cl1A76.34 (9)
O3—Ca1—O4i87.39 (10)O1viii—Ca5—Cl1A127.45 (9)
O12i—Ca1—O4i133.33 (10)O11ix—Ca5—Cl1A96.26 (8)
O3—Ca1—O175.42 (10)O6vi—Ca5—Cl1A70.05 (8)
O12i—Ca1—O1140.10 (10)O2vi—Ca5—Cl1B143.43 (9)
O4i—Ca1—O182.35 (10)O10viii—Ca5—Cl1B127.51 (9)
O3—Ca1—O10ii75.42 (10)O1viii—Ca5—Cl1B75.89 (9)
O12i—Ca1—O10ii82.28 (10)O11ix—Ca5—Cl1B70.39 (8)
O4i—Ca1—O10ii140.16 (10)O6vi—Ca5—Cl1B96.86 (8)
O1—Ca1—O10ii58.78 (9)Cl1A—Ca5—Cl1B55.06 (6)
O3—Ca1—Cl1Ai143.88 (9)O2vi—Ca5—O7viii104.57 (9)
O12i—Ca1—Cl1Ai76.26 (9)O10viii—Ca5—O7viii68.26 (9)
O4i—Ca1—Cl1Ai127.09 (9)O1viii—Ca5—O7viii68.24 (9)
O1—Ca1—Cl1Ai96.75 (8)O11ix—Ca5—O7viii150.62 (9)
O10ii—Ca1—Cl1Ai70.65 (8)O6vi—Ca5—O7viii150.59 (9)
O3—Ca1—Cl1Bi142.87 (9)Cl1A—Ca5—O7viii99.64 (7)
O12i—Ca1—Cl1Bi127.95 (9)Cl1B—Ca5—O7viii99.12 (7)
O4i—Ca1—Cl1Bi76.03 (8)O2vi—Ca5—P3vi70.34 (7)
O1—Ca1—Cl1Bi69.66 (8)O10viii—Ca5—P3vi110.89 (8)
O10ii—Ca1—Cl1Bi96.35 (8)O1viii—Ca5—P3vi110.88 (8)
Cl1Ai—Ca1—Cl1Bi55.05 (6)O11ix—Ca5—P3vi29.41 (7)
O3—Ca1—O9i104.53 (9)O6vi—Ca5—P3vi29.48 (7)
O12i—Ca1—O9i68.37 (9)Cl1A—Ca5—P3vi84.88 (5)
O4i—Ca1—O9i68.24 (9)Cl1B—Ca5—P3vi85.37 (5)
O1—Ca1—O9i150.50 (9)O7viii—Ca5—P3vi174.91 (6)
O10ii—Ca1—O9i150.56 (9)O2vi—Ca5—Cl1Bx133.78 (9)
Cl1Ai—Ca1—O9i99.07 (7)O10viii—Ca5—Cl1Bx138.58 (8)
Cl1Bi—Ca1—O9i99.80 (7)O1viii—Ca5—Cl1Bx64.64 (8)
O3—Ca1—P170.39 (7)O11ix—Ca5—Cl1Bx65.50 (8)
O12i—Ca1—P1110.82 (8)O6vi—Ca5—Cl1Bx102.35 (8)
O4i—Ca1—P1110.84 (8)Cl1A—Ca5—Cl1Bx67.30 (7)
O1—Ca1—P129.49 (7)Cl1B—Ca5—Cl1Bx12.26 (8)
O10ii—Ca1—P129.54 (7)O7viii—Ca5—Cl1Bx98.34 (7)
Cl1Ai—Ca1—P185.46 (5)P3vi—Ca5—Cl1Bx85.53 (5)
Cl1Bi—Ca1—P184.65 (5)O2vi—Ca5—Cl1Avii134.05 (9)
O9i—Ca1—P1174.92 (6)O10viii—Ca5—Cl1Avii64.45 (8)
O3—Ca1—Cl1Biii134.29 (9)O1viii—Ca5—Cl1Avii138.41 (8)
O12i—Ca1—Cl1Biii138.17 (9)O11ix—Ca5—Cl1Avii102.69 (8)
O4i—Ca1—Cl1Biii64.59 (8)O6vi—Ca5—Cl1Avii65.84 (8)
O1—Ca1—Cl1Biii66.06 (8)Cl1A—Ca5—Cl1Avii12.60 (9)
O10ii—Ca1—Cl1Biii102.84 (8)Cl1B—Ca5—Cl1Avii67.64 (7)
Cl1Ai—Ca1—Cl1Biii66.99 (7)O7viii—Ca5—Cl1Avii97.94 (7)
Cl1Bi—Ca1—Cl1Biii11.98 (8)P3vi—Ca5—Cl1Avii85.95 (5)
O9i—Ca1—Cl1Biii97.76 (7)Cl1Bx—Ca5—Cl1Avii79.90 (6)
P1—Ca1—Cl1Biii86.09 (5)O2vi—Ca5—P1vi22.56 (7)
O3—Ca1—Cl1Aiv133.62 (9)O10viii—Ca5—P1vi78.88 (7)
O12i—Ca1—Cl1Aiv64.48 (8)O1viii—Ca5—P1vi78.95 (7)
O4i—Ca1—Cl1Aiv138.84 (9)O11ix—Ca5—P1vi95.03 (7)
O1—Ca1—Cl1Aiv102.37 (8)O6vi—Ca5—P1vi94.99 (7)
O10ii—Ca1—Cl1Aiv65.29 (8)Cl1A—Ca5—P1vi152.45 (6)
Cl1Ai—Ca1—Cl1Aiv12.91 (9)Cl1B—Ca5—P1vi152.27 (6)
Cl1Bi—Ca1—Cl1Aiv67.93 (7)O7viii—Ca5—P1vi82.00 (6)
O9i—Ca1—Cl1Aiv98.46 (7)P3vi—Ca5—P1vi92.90 (3)
P1—Ca1—Cl1Aiv85.44 (5)Cl1Bx—Ca5—P1vi140.02 (5)
Cl1Biii—Ca1—Cl1Aiv79.89 (6)Cl1Avii—Ca5—P1vi139.94 (5)
O3—Ca1—P222.54 (7)P1—O1—Ca5iii138.68 (17)
O12i—Ca1—P278.90 (7)P1—O1—Ca196.53 (14)
O4i—Ca1—P278.89 (7)Ca5iii—O1—Ca1119.44 (12)
O1—Ca1—P295.01 (7)P1—O1—Ca291.09 (13)
O10ii—Ca1—P294.99 (7)Ca5iii—O1—Ca2103.10 (10)
Cl1Ai—Ca1—P2152.68 (6)Ca1—O1—Ca296.85 (9)
Cl1Bi—Ca1—P2152.04 (6)P1—O2—Ca5ix122.82 (16)
O9i—Ca1—P281.99 (6)P1—O2—Ca3ii105.33 (15)
P1—Ca1—P292.94 (3)Ca5ix—O2—Ca3ii114.71 (12)
Cl1Biii—Ca1—P2140.20 (5)P1—O2—Ca2105.03 (15)
Cl1Aiv—Ca1—P2139.77 (5)Ca5ix—O2—Ca2114.38 (12)
O8—Ca2—O777.58 (10)Ca3ii—O2—Ca289.04 (10)
O8—Ca2—O977.63 (10)P2—O3—Ca1122.83 (16)
O7—Ca2—O977.64 (10)P2—O3—Ca3ii105.26 (14)
O8—Ca2—O5126.57 (10)Ca1—O3—Ca3ii114.59 (12)
O7—Ca2—O5150.02 (10)P2—O3—Ca2105.20 (14)
O9—Ca2—O589.80 (10)Ca1—O3—Ca2114.41 (12)
O8—Ca2—O3150.03 (10)Ca3ii—O3—Ca289.01 (10)
O7—Ca2—O389.77 (10)P2—O4—Ca1i138.76 (17)
O9—Ca2—O3126.47 (10)P2—O4—Ca4ii96.52 (14)
O5—Ca2—O375.88 (9)Ca1i—O4—Ca4ii119.32 (12)
O8—Ca2—O289.85 (10)P2—O4—Ca291.18 (13)
O7—Ca2—O2126.51 (10)Ca1i—O4—Ca2103.10 (10)
O9—Ca2—O2150.04 (10)Ca4ii—O4—Ca296.87 (9)
O5—Ca2—O275.88 (9)P3—O5—Ca4ii122.81 (16)
O3—Ca2—O275.90 (10)P3—O5—Ca3ii105.23 (15)
O8—Ca2—O670.97 (9)Ca4ii—O5—Ca3ii114.69 (12)
O7—Ca2—O6145.49 (10)P3—O5—Ca2105.11 (14)
O9—Ca2—O682.03 (9)Ca4ii—O5—Ca2114.44 (12)
O5—Ca2—O655.84 (9)Ca3ii—O5—Ca289.05 (10)
O3—Ca2—O6124.68 (9)P3—O6—Ca4ix138.90 (17)
O2—Ca2—O668.12 (9)P3—O6—Ca5ix96.45 (14)
O8—Ca2—O4145.48 (10)Ca4ix—O6—Ca5ix119.30 (12)
O7—Ca2—O482.08 (9)P3—O6—Ca291.12 (13)
O9—Ca2—O470.92 (9)Ca4ix—O6—Ca2103.12 (10)
O5—Ca2—O468.06 (9)Ca5ix—O6—Ca296.78 (9)
O3—Ca2—O455.79 (9)P2i—O7—Ca2133.83 (17)
O2—Ca2—O4124.62 (9)P2i—O7—Ca3133.12 (17)
O6—Ca2—O4117.03 (9)Ca2—O7—Ca387.77 (10)
O8—Ca2—O182.06 (9)P2i—O7—Ca5iii98.48 (13)
O7—Ca2—O170.87 (9)Ca2—O7—Ca5iii96.40 (9)
O9—Ca2—O1145.48 (10)Ca3—O7—Ca5iii96.31 (9)
O5—Ca2—O1124.67 (9)P1xi—O8—Ca2133.77 (17)
O3—Ca2—O168.08 (9)P1xi—O8—Ca3133.23 (17)
O2—Ca2—O155.87 (9)Ca2—O8—Ca387.83 (10)
O6—Ca2—O1117.13 (9)P1xi—O8—Ca4ix98.36 (13)
O4—Ca2—O1117.02 (9)Ca2—O8—Ca4ix96.37 (9)
O8—Ca2—P399.45 (7)Ca3—O8—Ca4ix96.28 (9)
O7—Ca2—P3166.16 (8)P3vi—O9—Ca2133.73 (17)
O9—Ca2—P388.52 (7)P3vi—O9—Ca3133.26 (17)
O5—Ca2—P327.66 (7)Ca2—O9—Ca387.77 (10)
O3—Ca2—P398.76 (7)P3vi—O9—Ca1i98.43 (13)
O2—Ca2—P366.57 (7)Ca2—O9—Ca1i96.40 (9)
O6—Ca2—P328.49 (6)Ca3—O9—Ca1i96.30 (9)
O4—Ca2—P393.69 (6)P1v—O10—Ca5iii138.78 (17)
O1—Ca2—P3122.43 (7)P1v—O10—Ca1v96.41 (14)
O8—Ca2—P188.51 (7)Ca5iii—O10—Ca1v119.40 (12)
O7—Ca2—P199.36 (7)P1v—O10—Ca390.66 (13)
O9—Ca2—P1166.14 (8)Ca5iii—O10—Ca3103.74 (10)
O5—Ca2—P198.79 (7)Ca1v—O10—Ca396.55 (9)
O3—Ca2—P166.61 (7)P3v—O11—Ca4ix138.78 (17)
O2—Ca2—P127.68 (7)P3v—O11—Ca5vi96.66 (14)
O6—Ca2—P193.75 (6)Ca4ix—O11—Ca5vi119.29 (12)
O4—Ca2—P1122.40 (7)P3v—O11—Ca390.64 (13)
O1—Ca2—P128.50 (6)Ca4ix—O11—Ca3103.55 (10)
P3—Ca2—P194.04 (3)Ca5vi—O11—Ca396.54 (9)
O8—Ca2—P2166.10 (8)P2v—O12—Ca1i138.90 (17)
O7—Ca2—P288.52 (7)P2v—O12—Ca496.44 (14)
O9—Ca2—P299.39 (7)Ca1i—O12—Ca4119.40 (12)
O5—Ca2—P266.56 (7)P2v—O12—Ca390.53 (12)
O3—Ca2—P227.62 (7)Ca1i—O12—Ca3103.66 (10)
O2—Ca2—P298.74 (7)Ca4—O12—Ca396.46 (9)
O6—Ca2—P2122.39 (6)O1—P1—O8xii112.29 (16)
O4—Ca2—P228.48 (6)O1—P1—O10ii107.44 (15)
O1—Ca2—P293.67 (6)O8xii—P1—O10ii112.17 (16)
P3—Ca2—P294.01 (3)O1—P1—O2106.94 (16)
P1—Ca2—P294.02 (3)O8xii—P1—O2111.00 (16)
O8—Ca3—O976.86 (10)O10ii—P1—O2106.69 (16)
O8—Ca3—O776.80 (10)O1—P1—Ca153.98 (11)
O9—Ca3—O776.85 (10)O8xii—P1—Ca1136.55 (12)
O8—Ca3—O2v89.80 (10)O10ii—P1—Ca154.05 (11)
O9—Ca3—O2v150.05 (10)O2—P1—Ca1112.46 (11)
O7—Ca3—O2v126.51 (10)O1—P1—Ca3ii111.30 (11)
O8—Ca3—O5v126.59 (10)O8xii—P1—Ca3ii135.65 (12)
O9—Ca3—O5v89.82 (10)O10ii—P1—Ca3ii60.66 (11)
O7—Ca3—O5v150.05 (10)O2—P1—Ca3ii46.90 (11)
O2v—Ca3—O5v76.67 (10)Ca1—P1—Ca3ii78.13 (3)
O8—Ca3—O3v150.06 (10)O1—P1—Ca260.41 (11)
O9—Ca3—O3v126.49 (10)O8xii—P1—Ca2135.45 (12)
O7—Ca3—O3v89.83 (10)O10ii—P1—Ca2111.65 (11)
O2v—Ca3—O3v76.69 (10)O2—P1—Ca247.29 (11)
O5v—Ca3—O3v76.60 (10)Ca1—P1—Ca278.20 (3)
O8—Ca3—O1081.79 (9)Ca3ii—P1—Ca264.30 (3)
O9—Ca3—O10144.40 (10)O1—P1—Ca5ix122.16 (12)
O7—Ca3—O1070.70 (9)O8xii—P1—Ca5ix76.38 (11)
O2v—Ca3—O1056.10 (9)O10ii—P1—Ca5ix122.02 (12)
O5v—Ca3—O10125.74 (9)Ca1—P1—Ca5ix147.08 (4)
O3v—Ca3—O1068.46 (9)Ca3ii—P1—Ca5ix74.03 (3)
O8—Ca3—O1170.85 (9)Ca2—P1—Ca5ix74.12 (3)
O9—Ca3—O1181.88 (9)O1—P1—Ca4iv80.28 (11)
O7—Ca3—O11144.50 (10)O8xii—P1—Ca4iv56.27 (11)
O2v—Ca3—O1168.36 (9)O10ii—P1—Ca4iv80.33 (11)
O5v—Ca3—O1156.04 (9)O2—P1—Ca4iv167.27 (12)
O3v—Ca3—O11125.63 (9)Ca1—P1—Ca4iv80.27 (3)
O10—Ca3—O11117.39 (9)Ca3ii—P1—Ca4iv140.96 (4)
O8—Ca3—O12144.40 (10)Ca2—P1—Ca4iv140.65 (4)
O9—Ca3—O1270.72 (9)Ca5ix—P1—Ca4iv132.65 (3)
O7—Ca3—O1281.80 (9)O12ii—P2—O7i112.16 (16)
O2v—Ca3—O12125.77 (9)O12ii—P2—O4107.46 (15)
O5v—Ca3—O1268.43 (9)O7i—P2—O4112.10 (16)
O3v—Ca3—O1256.05 (9)O12ii—P2—O3106.96 (16)
O10—Ca3—O12117.36 (9)O7i—P2—O3111.12 (16)
O11—Ca3—O12117.39 (9)O4—P2—O3106.74 (16)
O8—Ca3—P3v99.43 (7)O12ii—P2—Ca4ii54.07 (11)
O9—Ca3—P3v88.54 (7)O7i—P2—Ca4ii136.42 (12)
O7—Ca3—P3v165.38 (8)O4—P2—Ca4ii53.99 (11)
O2v—Ca3—P3v67.06 (7)O3—P2—Ca4ii112.46 (11)
O5v—Ca3—P3v27.79 (7)O12ii—P2—Ca3ii60.83 (11)
O3v—Ca3—P3v99.60 (7)O7i—P2—Ca3ii135.86 (12)
O10—Ca3—P3v123.15 (7)O4—P2—Ca3ii111.26 (11)
O11—Ca3—P3v28.59 (6)O3—P2—Ca3ii46.98 (11)
O12—Ca3—P3v94.15 (6)Ca4ii—P2—Ca3ii78.16 (3)
O8—Ca3—P2v165.32 (8)O12ii—P2—Ca2111.77 (11)
O9—Ca3—P2v99.36 (7)O7i—P2—Ca2135.39 (12)
O7—Ca3—P2v88.54 (7)O4—P2—Ca260.34 (11)
O2v—Ca3—P2v99.66 (7)O3—P2—Ca247.18 (11)
O5v—Ca3—P2v67.03 (7)Ca4ii—P2—Ca278.19 (3)
O3v—Ca3—P2v27.76 (7)Ca3ii—P2—Ca264.28 (3)
O10—Ca3—P2v94.14 (6)O12ii—P2—Ca1122.16 (12)
O11—Ca3—P2v123.06 (7)O7i—P2—Ca176.49 (11)
O12—Ca3—P2v28.64 (6)O4—P2—Ca1122.06 (12)
P3v—Ca3—P2v94.61 (3)Ca4ii—P2—Ca1147.09 (4)
O8—Ca3—P1v88.56 (7)Ca3ii—P2—Ca174.04 (3)
O9—Ca3—P1v165.40 (8)Ca2—P2—Ca174.11 (3)
O7—Ca3—P1v99.38 (7)O12ii—P2—Ca5x80.19 (11)
O2v—Ca3—P1v27.77 (7)O7i—P2—Ca5x56.19 (11)
O5v—Ca3—P1v99.61 (7)O4—P2—Ca5x80.30 (11)
O3v—Ca3—P1v67.05 (7)O3—P2—Ca5x167.31 (12)
O10—Ca3—P1v28.68 (6)Ca4ii—P2—Ca5x80.24 (3)
O11—Ca3—P1v94.10 (6)Ca3ii—P2—Ca5x141.00 (4)
O12—Ca3—P1v123.10 (7)Ca2—P2—Ca5x140.59 (4)
P3v—Ca3—P1v94.61 (3)Ca1—P2—Ca5x132.68 (3)
P2v—Ca3—P1v94.60 (3)O11ii—P3—O6107.40 (16)
O5v—Ca4—O6vi87.36 (10)O11ii—P3—O9ix112.18 (16)
O5v—Ca4—O11vi87.44 (10)O6—P3—O9ix112.14 (16)
O6vi—Ca4—O11vi133.33 (10)O11ii—P3—O5106.92 (16)
O5v—Ca4—O4v75.34 (10)O6—P3—O5106.82 (16)
O6vi—Ca4—O4v140.07 (10)O9ix—P3—O5111.07 (16)
O11vi—Ca4—O4v82.33 (10)O11ii—P3—Ca5ix53.93 (11)
O5v—Ca4—O1275.43 (10)O6—P3—Ca5ix54.08 (11)
O6vi—Ca4—O1282.33 (10)O9ix—P3—Ca5ix136.47 (12)
O11vi—Ca4—O12140.11 (10)O5—P3—Ca5ix112.46 (11)
O4v—Ca4—O1258.73 (9)O11ii—P3—Ca3ii60.78 (11)
O5v—Ca4—Cl1Bvii143.16 (9)O6—P3—Ca3ii111.37 (11)
O6vi—Ca4—Cl1Bvii127.93 (9)O9ix—P3—Ca3ii135.73 (12)
O11vi—Ca4—Cl1Bvii75.60 (9)O5—P3—Ca3ii46.98 (11)
O4v—Ca4—Cl1Bvii70.20 (8)Ca5ix—P3—Ca3ii78.13 (3)
O12—Ca4—Cl1Bvii96.92 (8)O11ii—P3—Ca2111.66 (11)
O5v—Ca4—Cl1Avii143.54 (9)O6—P3—Ca260.39 (11)
O6vi—Ca4—Cl1Avii76.65 (8)O9ix—P3—Ca2135.46 (12)
O11vi—Ca4—Cl1Avii127.18 (9)O5—P3—Ca247.23 (11)
O4v—Ca4—Cl1Avii96.24 (8)Ca5ix—P3—Ca278.19 (3)
O12—Ca4—Cl1Avii70.16 (8)Ca3ii—P3—Ca264.32 (3)
Cl1Bvii—Ca4—Cl1Avii55.10 (6)O11ii—P3—Ca4ii122.23 (12)
O5v—Ca4—O8vi104.54 (9)O6—P3—Ca4ii122.06 (12)
O6vi—Ca4—O8vi68.28 (9)O9ix—P3—Ca4ii76.43 (11)
O11vi—Ca4—O8vi68.35 (9)Ca5ix—P3—Ca4ii147.10 (4)
O4v—Ca4—O8vi150.59 (9)Ca3ii—P3—Ca4ii74.08 (3)
O12—Ca4—O8vi150.52 (9)Ca2—P3—Ca4ii74.14 (3)
Cl1Bvii—Ca4—O8vi99.23 (8)O11ii—P3—Ca1xiv80.23 (11)
Cl1Avii—Ca4—O8vi99.62 (8)O6—P3—Ca1xiv80.25 (11)
O5v—Ca4—P2v70.34 (7)O9ix—P3—Ca1xiv56.22 (11)
O6vi—Ca4—P2v110.79 (8)O5—P3—Ca1xiv167.29 (12)
O11vi—Ca4—P2v110.83 (8)Ca5ix—P3—Ca1xiv80.25 (3)
O4v—Ca4—P2v29.49 (7)Ca3ii—P3—Ca1xiv140.97 (4)
O12—Ca4—P2v29.49 (7)Ca2—P3—Ca1xiv140.59 (4)
Cl1Bvii—Ca4—P2v85.31 (6)Ca4ii—P3—Ca1xiv132.65 (3)
Cl1Avii—Ca4—P2v84.91 (5)Cl1Avii—Cl1A—Ca5119.6 (3)
O8vi—Ca4—P2v174.88 (6)Cl1Avii—Cl1A—Ca1i117.4 (3)
O5v—Ca4—Cl1A133.67 (9)Ca5—Cl1A—Ca1i101.07 (7)
O6vi—Ca4—Cl1A64.15 (8)Cl1Avii—Cl1A—Ca4vii114.7 (3)
O11vi—Ca4—Cl1A138.79 (8)Ca5—Cl1A—Ca4vii100.66 (8)
O4v—Ca4—Cl1A102.93 (8)Ca1i—Cl1A—Ca4vii100.38 (7)
O12—Ca4—Cl1A65.63 (8)Cl1Avii—Cl1A—Ca452.0 (3)
Cl1Bvii—Ca4—Cl1A68.37 (6)Ca5—Cl1A—Ca487.95 (6)
Cl1Avii—Ca4—Cl1A13.27 (8)Ca1i—Cl1A—Ca487.70 (6)
O8vi—Ca4—Cl1A97.93 (7)Ca4vii—Cl1A—Ca4166.73 (8)
P2v—Ca4—Cl1A85.93 (5)Cl1Avii—Cl1A—Ca1xiii49.7 (3)
O5v—Ca4—Cl1Bv134.22 (9)Ca5—Cl1A—Ca1xiii87.66 (6)
O6vi—Ca4—Cl1Bv138.25 (9)Ca1i—Cl1A—Ca1xiii167.09 (9)
O11vi—Ca4—Cl1Bv64.99 (8)Ca4vii—Cl1A—Ca1xiii87.16 (6)
O4v—Ca4—Cl1Bv65.74 (8)Ca4—Cl1A—Ca1xiii83.09 (6)
O12—Ca4—Cl1Bv102.22 (8)Cl1Avii—Cl1A—Ca5vii47.8 (3)
Cl1Bvii—Ca4—Cl1Bv11.49 (9)Ca5—Cl1A—Ca5vii167.40 (9)
Cl1Avii—Ca4—Cl1Bv66.59 (6)Ca1i—Cl1A—Ca5vii87.22 (6)
O8vi—Ca4—Cl1Bv98.34 (7)Ca4vii—Cl1A—Ca5vii86.97 (6)
P2v—Ca4—Cl1Bv85.62 (5)Ca4—Cl1A—Ca5vii82.89 (6)
Cl1A—Ca4—Cl1Bv79.86 (6)Ca1xiii—Cl1A—Ca5vii82.69 (5)
O5v—Ca4—P3v22.55 (7)Cl1Bx—Cl1B—Ca4vii121.0 (4)
O6vi—Ca4—P3v78.84 (7)Cl1Bx—Cl1B—Ca1i117.3 (4)
O11vi—Ca4—P3v78.92 (7)Ca4vii—Cl1B—Ca1i100.33 (7)
O4v—Ca4—P3v94.95 (7)Cl1Bx—Cl1B—Ca5115.1 (4)
O12—Ca4—P3v95.03 (7)Ca4vii—Cl1B—Ca5100.04 (7)
Cl1Bvii—Ca4—P3v151.90 (6)Ca1i—Cl1B—Ca599.54 (7)
Cl1Avii—Ca4—P3v152.76 (6)Cl1Bx—Cl1B—Ca5x52.7 (3)
O8vi—Ca4—P3v81.98 (6)Ca4vii—Cl1B—Ca5x88.15 (6)
P2v—Ca4—P3v92.89 (3)Ca1i—Cl1B—Ca5x87.82 (7)
Cl1A—Ca4—P3v139.57 (5)Ca5—Cl1B—Ca5x167.74 (8)
Cl1Bv—Ca4—P3v140.43 (5)Cl1Bx—Cl1B—Ca1viii50.7 (3)
O2vi—Ca5—O10viii87.49 (10)Ca4vii—Cl1B—Ca1viii87.94 (6)
O2vi—Ca5—O1viii87.43 (10)Ca1i—Cl1B—Ca1viii168.02 (8)
O10viii—Ca5—O1viii133.23 (10)Ca5—Cl1B—Ca1viii87.40 (7)
O2vi—Ca5—O11ix75.37 (10)Ca5x—Cl1B—Ca1viii83.77 (6)
O10viii—Ca5—O11ix140.09 (10)Cl1Bx—Cl1B—Ca4ii47.5 (3)
O1viii—Ca5—O11ix82.48 (10)Ca4vii—Cl1B—Ca4ii168.51 (9)
O2vi—Ca5—O6vi75.41 (10)Ca1i—Cl1B—Ca4ii87.26 (6)
O10viii—Ca5—O6vi82.42 (10)Ca5—Cl1B—Ca4ii87.05 (6)
O1viii—Ca5—O6vi140.15 (10)Ca5x—Cl1B—Ca4ii83.50 (6)
O11ix—Ca5—O6vi58.64 (9)Ca1viii—Cl1B—Ca4ii83.33 (6)
O2vi—Ca5—Cl1A143.35 (9)
Symmetry codes: (i) x+1, y+2, z; (ii) x, y+1, z; (iii) x+1, y, z; (iv) x+1, y+1, z; (v) x, y1, z; (vi) x+1, y1/2, z+1/2; (vii) x, y+1, z; (viii) x1, y, z; (ix) x+1, y+1/2, z+1/2; (x) x, y+2, z; (xi) x+2, y1/2, z+1/2; (xii) x+2, y+1/2, z+1/2; (xiii) x1, y1, z; (xiv) x, y+5/2, z+1/2.
(A_mono) top
Crystal data top
Ca5ClO12P3F(000) = 1032
Mr = 520.76Dx = 3.193 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.7107 Å
Hall symbol: -P 2ybcCell parameters from 1895 reflections
a = 9.6307 (4) Åθ = 3.9–26.3°
b = 6.7425 (3) ŵ = 3.23 mm1
c = 19.2602 (7) ÅT = 100 K
β = 119.969 (1)°Prism, colourless
V = 1083.44 (8) Å30.17 × 0.07 × 0.05 mm
Z = 4
Data collection top
BRUKER APPEX-II CCD
diffractometer
2212 independent reflections
Radiation source: fine-focus sealed tube1285 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.037
ω and phi scansθmax = 26.4°, θmin = 2.4°
Absorption correction: multi-scan
BRUKER SADABS
h = 1210
Tmin = 0.870, Tmax = 1k = 08
17423 measured reflectionsl = 024
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.036 w = 1/[σ2(Fo2) + (0.0339P)2 + 3.8081P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.093(Δ/σ)max = 0.028
S = 1.16Δρmax = 1.12 e Å3
2212 reflectionsΔρmin = 0.59 e Å3
129 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0050 (5)
Crystal data top
Ca5ClO12P3V = 1083.44 (8) Å3
Mr = 520.76Z = 4
Monoclinic, P21/cMo Kα radiation
a = 9.6307 (4) ŵ = 3.23 mm1
b = 6.7425 (3) ÅT = 100 K
c = 19.2602 (7) Å0.17 × 0.07 × 0.05 mm
β = 119.969 (1)°
Data collection top
BRUKER APPEX-II CCD
diffractometer
2212 independent reflections
Absorption correction: multi-scan
BRUKER SADABS
1285 reflections with I > 2σ(I)
Tmin = 0.870, Tmax = 1Rint = 0.037
17423 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.036129 parameters
wR(F2) = 0.0930 restraints
S = 1.16Δρmax = 1.12 e Å3
2212 reflectionsΔρmin = 0.59 e Å3
Special details top

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ca10.74558 (9)1.25031 (15)0.00306 (4)0.00627 (19)
Ca20.66668 (11)0.99382 (11)0.16668 (5)0.0039 (2)
Ca30.66681 (12)0.50051 (12)0.16671 (6)0.0099 (3)
Ca40.26056 (9)0.25019 (15)0.12720 (4)0.00611 (19)
Ca50.00609 (9)0.75017 (15)0.13023 (4)0.00605 (19)
O10.9134 (4)1.0674 (5)0.1330 (2)0.0105 (2)
O20.8718 (3)1.2510 (5)0.23242 (16)0.0105 (2)
O30.5928 (3)1.2503 (5)0.06390 (16)0.0105 (2)
O40.3532 (4)1.0668 (5)0.0436 (2)0.0105 (2)
O50.5348 (3)1.2506 (5)0.20342 (16)0.0105 (2)
O60.7333 (4)1.0664 (5)0.3233 (2)0.0105 (2)
O70.6561 (3)0.7502 (5)0.07448 (16)0.0105 (2)
O80.8512 (3)0.7496 (5)0.25353 (16)0.0105 (2)
O90.4931 (3)0.7497 (5)0.17198 (16)0.0105 (2)
O100.9132 (4)0.4338 (5)0.1332 (2)0.0105 (2)
O110.7336 (4)0.4334 (5)0.3235 (2)0.0105 (2)
O120.3533 (4)0.4334 (5)0.0434 (2)0.0105 (2)
P10.96710 (11)1.2504 (2)0.18742 (6)0.0048 (2)
P20.40780 (11)1.2499 (2)0.01641 (6)0.0050 (2)
P30.62501 (11)1.25039 (19)0.29613 (6)0.0046 (2)
Cl1A0.0031 (3)0.5623 (4)0.00021 (17)0.0141 (4)0.490 (3)
Cl1B0.0028 (3)0.9460 (4)0.00000 (18)0.0141 (4)0.510 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0067 (4)0.0054 (4)0.0077 (4)0.0005 (4)0.0043 (3)0.0010 (5)
Ca20.0040 (5)0.0047 (5)0.0038 (5)0.0029 (3)0.0026 (4)0.0003 (4)
Ca30.0132 (5)0.0024 (5)0.0135 (6)0.0031 (4)0.0063 (5)0.0007 (4)
Ca40.0059 (4)0.0052 (4)0.0068 (4)0.0007 (4)0.0029 (3)0.0002 (5)
Ca50.0066 (4)0.0055 (4)0.0059 (4)0.0001 (4)0.0029 (3)0.0002 (4)
O10.0099 (4)0.0113 (4)0.0104 (4)0.0001 (5)0.0051 (3)0.0005 (5)
O20.0099 (4)0.0113 (4)0.0104 (4)0.0001 (5)0.0051 (3)0.0005 (5)
O30.0099 (4)0.0113 (4)0.0104 (4)0.0001 (5)0.0051 (3)0.0005 (5)
O40.0099 (4)0.0113 (4)0.0104 (4)0.0001 (5)0.0051 (3)0.0005 (5)
O50.0099 (4)0.0113 (4)0.0104 (4)0.0001 (5)0.0051 (3)0.0005 (5)
O60.0099 (4)0.0113 (4)0.0104 (4)0.0001 (5)0.0051 (3)0.0005 (5)
O70.0099 (4)0.0113 (4)0.0104 (4)0.0001 (5)0.0051 (3)0.0005 (5)
O80.0099 (4)0.0113 (4)0.0104 (4)0.0001 (5)0.0051 (3)0.0005 (5)
O90.0099 (4)0.0113 (4)0.0104 (4)0.0001 (5)0.0051 (3)0.0005 (5)
O100.0099 (4)0.0113 (4)0.0104 (4)0.0001 (5)0.0051 (3)0.0005 (5)
O110.0099 (4)0.0113 (4)0.0104 (4)0.0001 (5)0.0051 (3)0.0005 (5)
O120.0099 (4)0.0113 (4)0.0104 (4)0.0001 (5)0.0051 (3)0.0005 (5)
P10.0045 (4)0.0049 (4)0.0054 (5)0.0006 (5)0.0028 (4)0.0004 (6)
P20.0047 (4)0.0055 (4)0.0047 (5)0.0002 (5)0.0023 (4)0.0006 (6)
P30.0047 (4)0.0047 (4)0.0050 (4)0.0007 (5)0.0029 (4)0.0002 (6)
Cl1A0.0080 (6)0.0252 (9)0.0095 (6)0.0006 (12)0.0047 (5)0.0002 (13)
Cl1B0.0080 (6)0.0252 (9)0.0095 (6)0.0006 (12)0.0047 (5)0.0002 (13)
Geometric parameters (Å, º) top
Ca1—O32.294 (3)Ca5—Cl1Bx3.226 (3)
Ca1—O12i2.325 (3)Ca5—Cl1Avii3.246 (3)
Ca1—O4i2.330 (3)Ca5—P1vi3.3906 (12)
Ca1—O12.522 (4)O1—P11.532 (3)
Ca1—O10ii2.525 (4)O1—Ca5iii2.329 (3)
Ca1—Cl1Ai2.758 (3)O2—P11.546 (3)
Ca1—Cl1Bi2.835 (3)O2—Ca5ix2.296 (3)
Ca1—O9i2.984 (3)O2—Ca3ii2.415 (3)
Ca1—P13.0970 (12)O3—P21.543 (3)
Ca1—Cl1Biii3.198 (3)O3—Ca3ii2.422 (3)
Ca1—Cl1Aiv3.274 (3)O4—P21.534 (3)
Ca1—P23.3889 (12)O4—Ca1i2.330 (3)
Ca2—O72.384 (3)O4—Ca4ii2.520 (3)
Ca2—O92.384 (3)O5—P31.547 (3)
Ca2—O82.387 (3)O5—Ca4ii2.293 (3)
Ca2—O32.451 (3)O5—Ca3ii2.420 (3)
Ca2—O22.452 (3)O6—P31.534 (3)
Ca2—O52.452 (3)O6—Ca4ix2.324 (3)
Ca2—O62.796 (4)O6—Ca5ix2.528 (3)
Ca2—O42.798 (4)O7—P2i1.538 (3)
Ca2—O12.802 (3)O7—Ca5iii2.983 (3)
Ca2—P23.2196 (14)O8—P1xi1.538 (3)
Ca2—P13.2201 (14)O8—Ca4ix2.984 (3)
Ca2—P33.2202 (13)O9—P3vi1.539 (3)
Ca3—O92.409 (3)O9—Ca1i2.984 (3)
Ca3—O82.409 (3)O10—P1v1.532 (3)
Ca3—O72.412 (3)O10—Ca5iii2.325 (3)
Ca3—O2v2.415 (3)O10—Ca1v2.525 (4)
Ca3—O5v2.420 (3)O11—P3v1.531 (3)
Ca3—O3v2.422 (3)O11—Ca4ix2.326 (3)
Ca3—O102.790 (3)O11—Ca5vi2.525 (3)
Ca3—O122.792 (4)O12—P2v1.533 (3)
Ca3—O112.793 (4)O12—Ca1i2.325 (3)
Ca3—P1v3.1960 (14)P1—O10ii1.532 (3)
Ca3—P3v3.1972 (14)P1—O8xii1.538 (3)
Ca3—P2v3.2004 (14)P1—Ca3ii3.1960 (14)
Ca4—O5v2.293 (3)P1—Ca5ix3.3906 (12)
Ca4—O6vi2.324 (3)P2—O12ii1.533 (3)
Ca4—O11vi2.326 (3)P2—O7i1.538 (3)
Ca4—O4v2.520 (3)P2—Ca4ii3.0963 (11)
Ca4—O122.524 (3)P2—Ca3ii3.2004 (14)
Ca4—Cl1Bvii2.800 (3)P3—O11ii1.531 (3)
Ca4—Cl1Avii2.800 (3)P3—O9ix1.539 (3)
Ca4—O8vi2.984 (3)P3—Ca5ix3.0983 (12)
Ca4—P2v3.0963 (11)P3—Ca3ii3.1972 (14)
Ca4—Cl1Bv3.230 (3)P3—Ca4ii3.3906 (12)
Ca4—Cl1A3.240 (3)Cl1A—Cl1Avii0.842 (5)
Ca4—P3v3.3906 (12)Cl1A—Ca1i2.758 (3)
Ca5—O2vi2.296 (3)Cl1A—Ca4vii2.800 (3)
Ca5—O10viii2.325 (3)Cl1A—Ca5vii3.246 (3)
Ca5—O1viii2.329 (3)Cl1A—Ca1xiii3.274 (3)
Ca5—O11ix2.525 (3)Cl1B—Cl1Bx0.730 (5)
Ca5—O6vi2.528 (3)Cl1B—Ca4vii2.800 (3)
Ca5—Cl1A2.794 (3)Cl1B—Ca1i2.835 (3)
Ca5—Cl1B2.798 (3)Cl1B—Ca1viii3.198 (3)
Ca5—O7viii2.983 (3)Cl1B—Ca5x3.226 (3)
Ca5—P3vi3.0983 (12)Cl1B—Ca4ii3.230 (3)
O3—Ca1—O12i87.29 (12)O10viii—Ca5—Cl1A76.95 (10)
O3—Ca1—O4i87.41 (12)O1viii—Ca5—Cl1A127.22 (11)
O12i—Ca1—O4i133.10 (10)O11ix—Ca5—Cl1A95.84 (9)
O3—Ca1—O175.49 (11)O6vi—Ca5—Cl1A70.06 (10)
O12i—Ca1—O1140.10 (12)O2vi—Ca5—Cl1B143.16 (11)
O4i—Ca1—O182.52 (12)O10viii—Ca5—Cl1B127.96 (11)
O3—Ca1—O10ii75.42 (11)O1viii—Ca5—Cl1B75.35 (10)
O12i—Ca1—O10ii82.45 (12)O11ix—Ca5—Cl1B70.46 (10)
O4i—Ca1—O10ii140.17 (12)O6vi—Ca5—Cl1B97.41 (10)
O1—Ca1—O10ii58.63 (9)Cl1A—Ca5—Cl1B55.13 (6)
O3—Ca1—Cl1Ai143.68 (11)O2vi—Ca5—O7viii104.55 (9)
O12i—Ca1—Cl1Ai76.50 (10)O10viii—Ca5—O7viii68.26 (11)
O4i—Ca1—Cl1Ai127.23 (10)O1viii—Ca5—O7viii68.34 (11)
O1—Ca1—Cl1Ai96.44 (10)O11ix—Ca5—O7viii150.61 (11)
O10ii—Ca1—Cl1Ai70.42 (10)O6vi—Ca5—O7viii150.57 (11)
O3—Ca1—Cl1Bi143.21 (11)Cl1A—Ca5—O7viii100.00 (8)
O12i—Ca1—Cl1Bi127.91 (10)Cl1B—Ca5—O7viii98.87 (8)
O4i—Ca1—Cl1Bi75.88 (10)O2vi—Ca5—P3vi70.26 (7)
O1—Ca1—Cl1Bi70.06 (10)O10viii—Ca5—P3vi110.88 (9)
O10ii—Ca1—Cl1Bi96.73 (10)O1viii—Ca5—P3vi110.74 (9)
Cl1Ai—Ca1—Cl1Bi55.09 (6)O11ix—Ca5—P3vi29.40 (8)
O3—Ca1—O9i104.38 (9)O6vi—Ca5—P3vi29.49 (8)
O12i—Ca1—O9i68.21 (11)Cl1A—Ca5—P3vi84.64 (6)
O4i—Ca1—O9i68.19 (11)Cl1B—Ca5—P3vi85.68 (6)
O1—Ca1—O9i150.63 (11)O7viii—Ca5—P3vi174.81 (6)
O10ii—Ca1—O9i150.58 (11)O2vi—Ca5—Cl1Bx133.99 (11)
Cl1Ai—Ca1—O9i99.42 (8)O10viii—Ca5—Cl1Bx138.35 (11)
Cl1Bi—Ca1—O9i99.46 (9)O1viii—Ca5—Cl1Bx65.16 (10)
O3—Ca1—P170.40 (7)O11ix—Ca5—Cl1Bx65.54 (10)
O12i—Ca1—P1110.88 (10)O6vi—Ca5—Cl1Bx102.06 (9)
O4i—Ca1—P1110.93 (10)Cl1A—Ca5—Cl1Bx66.38 (8)
O1—Ca1—P129.43 (8)Cl1B—Ca5—Cl1Bx11.30 (10)
O10ii—Ca1—P129.45 (8)O7viii—Ca5—Cl1Bx98.60 (8)
Cl1Ai—Ca1—P185.20 (7)P3vi—Ca5—Cl1Bx85.37 (6)
Cl1Bi—Ca1—P185.14 (7)O2vi—Ca5—Cl1Avii133.90 (11)
O9i—Ca1—P1174.79 (6)O10viii—Ca5—Cl1Avii63.97 (10)
O3—Ca1—Cl1Biii134.01 (10)O1viii—Ca5—Cl1Avii138.73 (11)
O12i—Ca1—Cl1Biii138.58 (10)O11ix—Ca5—Cl1Avii103.24 (9)
O4i—Ca1—Cl1Biii64.61 (10)O6vi—Ca5—Cl1Avii66.07 (9)
O1—Ca1—Cl1Biii65.71 (9)Cl1A—Ca5—Cl1Avii13.55 (10)
O10ii—Ca1—Cl1Biii102.59 (9)Cl1B—Ca5—Cl1Avii68.63 (8)
Cl1Ai—Ca1—Cl1Biii67.17 (8)O7viii—Ca5—Cl1Avii97.60 (8)
Cl1Bi—Ca1—Cl1Biii12.08 (9)P3vi—Ca5—Cl1Avii86.35 (5)
O9i—Ca1—Cl1Biii98.18 (8)Cl1Bx—Ca5—Cl1Avii79.90 (5)
P1—Ca1—Cl1Biii85.81 (6)O2vi—Ca5—P1vi22.56 (7)
O3—Ca1—Cl1Aiv133.90 (10)O10viii—Ca5—P1vi78.83 (9)
O12i—Ca1—Cl1Aiv64.67 (10)O1viii—Ca5—P1vi78.88 (9)
O4i—Ca1—Cl1Aiv138.57 (10)O11ix—Ca5—P1vi94.93 (8)
O1—Ca1—Cl1Aiv102.46 (9)O6vi—Ca5—P1vi94.88 (8)
O10ii—Ca1—Cl1Aiv65.64 (9)Cl1A—Ca5—P1vi152.89 (7)
Cl1Ai—Ca1—Cl1Aiv12.73 (10)Cl1B—Ca5—P1vi151.75 (7)
Cl1Bi—Ca1—Cl1Aiv67.82 (8)O7viii—Ca5—P1vi81.98 (6)
O9i—Ca1—Cl1Aiv98.25 (8)P3vi—Ca5—P1vi92.82 (3)
P1—Ca1—Cl1Aiv85.72 (6)Cl1Bx—Ca5—P1vi140.45 (6)
Cl1Biii—Ca1—Cl1Aiv79.90 (5)Cl1Avii—Ca5—P1vi139.51 (6)
O3—Ca1—P222.50 (7)P1—O1—Ca5iii138.9 (2)
O12i—Ca1—P278.80 (9)P1—O1—Ca196.59 (15)
O4i—Ca1—P278.84 (8)Ca5iii—O1—Ca1119.29 (14)
O1—Ca1—P295.04 (8)P1—O1—Ca291.16 (15)
O10ii—Ca1—P295.00 (8)Ca5iii—O1—Ca2102.83 (11)
Cl1Ai—Ca1—P2152.68 (7)Ca1—O1—Ca296.84 (11)
Cl1Bi—Ca1—P2152.02 (6)P1—O2—Ca5ix122.68 (15)
O9i—Ca1—P281.89 (6)P1—O2—Ca3ii105.48 (16)
P1—Ca1—P292.90 (3)Ca5ix—O2—Ca3ii114.81 (13)
Cl1Biii—Ca1—P2139.98 (6)P1—O2—Ca2105.04 (16)
Cl1Aiv—Ca1—P2139.98 (6)Ca5ix—O2—Ca2114.22 (13)
O7—Ca2—O977.66 (11)Ca3ii—O2—Ca289.16 (9)
O7—Ca2—O877.67 (10)P2—O3—Ca1122.84 (15)
O9—Ca2—O877.67 (11)P2—O3—Ca3ii105.49 (16)
O7—Ca2—O389.86 (11)Ca1—O3—Ca3ii114.56 (13)
O9—Ca2—O3126.49 (10)P2—O3—Ca2105.14 (16)
O8—Ca2—O3150.09 (10)Ca1—O3—Ca2114.26 (13)
O7—Ca2—O2126.55 (10)Ca3ii—O3—Ca289.03 (9)
O9—Ca2—O2150.13 (10)P2—O4—Ca1i138.6 (2)
O8—Ca2—O290.01 (11)P2—O4—Ca4ii96.57 (15)
O3—Ca2—O275.65 (10)Ca1i—O4—Ca4ii119.36 (13)
O7—Ca2—O5150.04 (10)P2—O4—Ca291.25 (15)
O9—Ca2—O589.98 (12)Ca1i—O4—Ca2103.02 (12)
O8—Ca2—O5126.63 (10)Ca4ii—O4—Ca296.99 (12)
O3—Ca2—O575.61 (10)P3—O5—Ca4ii122.85 (15)
O2—Ca2—O575.60 (10)P3—O5—Ca3ii105.30 (16)
O7—Ca2—O6145.67 (11)Ca4ii—O5—Ca3ii114.78 (13)
O9—Ca2—O682.09 (10)P3—O5—Ca2105.02 (16)
O8—Ca2—O671.06 (10)Ca4ii—O5—Ca2114.30 (13)
O3—Ca2—O6124.43 (10)Ca3ii—O5—Ca289.06 (9)
O2—Ca2—O668.14 (9)P3—O6—Ca4ix139.05 (19)
O5—Ca2—O655.78 (10)P3—O6—Ca5ix96.30 (15)
O7—Ca2—O482.17 (10)Ca4ix—O6—Ca5ix119.13 (14)
O9—Ca2—O471.00 (10)P3—O6—Ca291.32 (16)
O8—Ca2—O4145.66 (11)Ca4ix—O6—Ca2103.13 (12)
O3—Ca2—O455.71 (9)Ca5ix—O6—Ca296.88 (11)
O2—Ca2—O4124.28 (10)P2i—O7—Ca2133.8 (2)
O5—Ca2—O467.96 (10)P2i—O7—Ca3133.1 (2)
O6—Ca2—O4116.87 (10)Ca2—O7—Ca387.83 (9)
O7—Ca2—O171.04 (10)P2i—O7—Ca5iii98.49 (12)
O9—Ca2—O1145.68 (11)Ca2—O7—Ca5iii96.43 (10)
O8—Ca2—O182.16 (10)Ca3—O7—Ca5iii96.32 (10)
O3—Ca2—O168.05 (10)P1xi—O8—Ca2133.6 (2)
O2—Ca2—O155.73 (10)P1xi—O8—Ca3133.4 (2)
O5—Ca2—O1124.29 (10)Ca2—O8—Ca387.81 (9)
O6—Ca2—O1117.04 (11)P1xi—O8—Ca4ix98.35 (12)
O4—Ca2—O1117.01 (10)Ca2—O8—Ca4ix96.31 (10)
O7—Ca2—P288.53 (8)Ca3—O8—Ca4ix96.36 (10)
O9—Ca2—P299.44 (8)P3vi—O9—Ca2133.5 (2)
O8—Ca2—P2166.19 (8)P3vi—O9—Ca3133.3 (2)
O3—Ca2—P227.56 (7)Ca2—O9—Ca387.89 (9)
O2—Ca2—P298.47 (8)P3vi—O9—Ca1i98.34 (13)
O5—Ca2—P266.45 (7)Ca2—O9—Ca1i96.46 (10)
O6—Ca2—P2122.22 (7)Ca3—O9—Ca1i96.41 (10)
O4—Ca2—P228.44 (7)P1v—O10—Ca5iii138.9 (2)
O1—Ca2—P293.59 (8)P1v—O10—Ca1v96.43 (15)
O7—Ca2—P199.43 (8)Ca5iii—O10—Ca1v119.23 (14)
O9—Ca2—P1166.25 (8)P1v—O10—Ca390.56 (15)
O8—Ca2—P188.58 (8)Ca5iii—O10—Ca3103.88 (12)
O3—Ca2—P166.52 (7)Ca1v—O10—Ca396.46 (11)
O2—Ca2—P127.62 (7)P3v—O11—Ca4ix138.94 (19)
O5—Ca2—P198.50 (8)P3v—O11—Ca5vi96.55 (15)
O6—Ca2—P193.70 (7)Ca4ix—O11—Ca5vi119.20 (14)
O4—Ca2—P1122.23 (7)P3v—O11—Ca390.52 (16)
O1—Ca2—P128.40 (7)Ca4ix—O11—Ca3103.76 (12)
P2—Ca2—P193.88 (3)Ca5vi—O11—Ca396.45 (11)
O7—Ca2—P3166.31 (8)P2v—O12—Ca1i138.9 (2)
O9—Ca2—P388.65 (8)P2v—O12—Ca496.46 (15)
O8—Ca2—P399.50 (8)Ca1i—O12—Ca4119.18 (13)
O3—Ca2—P398.51 (8)P2v—O12—Ca390.65 (15)
O2—Ca2—P366.43 (7)Ca1i—O12—Ca3103.88 (12)
O5—Ca2—P327.64 (7)Ca4—O12—Ca396.50 (12)
O6—Ca2—P328.45 (7)O10ii—P1—O1107.49 (15)
O4—Ca2—P393.57 (7)O10ii—P1—O8xii112.30 (19)
O1—Ca2—P3122.15 (8)O1—P1—O8xii111.94 (19)
P2—Ca2—P393.89 (3)O10ii—P1—O2106.65 (19)
P1—Ca2—P393.85 (3)O1—P1—O2107.05 (19)
O9—Ca3—O876.77 (11)O8xii—P1—O2111.11 (15)
O9—Ca3—O776.66 (10)O10ii—P1—Ca154.12 (13)
O8—Ca3—O776.70 (10)O1—P1—Ca153.98 (13)
O9—Ca3—O2v150.10 (10)O8xii—P1—Ca1136.50 (11)
O8—Ca3—O2v89.76 (12)O2—P1—Ca1112.39 (11)
O7—Ca3—O2v126.52 (10)O10ii—P1—Ca3ii60.79 (13)
O9—Ca3—O5v89.77 (12)O1—P1—Ca3ii111.37 (13)
O8—Ca3—O5v126.55 (10)O8xii—P1—Ca3ii135.90 (14)
O7—Ca3—O5v150.00 (10)O2—P1—Ca3ii46.74 (12)
O2v—Ca3—O5v76.88 (10)Ca1—P1—Ca3ii78.16 (3)
O9—Ca3—O3v126.39 (11)O10ii—P1—Ca2111.83 (13)
O8—Ca3—O3v150.12 (10)O1—P1—Ca260.44 (13)
O7—Ca3—O3v89.84 (11)O8xii—P1—Ca2135.19 (14)
O2v—Ca3—O3v76.88 (10)O2—P1—Ca247.34 (13)
O5v—Ca3—O3v76.75 (10)Ca1—P1—Ca278.23 (3)
O9—Ca3—O10144.22 (11)Ca3ii—P1—Ca264.34 (3)
O8—Ca3—O1081.69 (10)O10ii—P1—Ca5ix122.08 (14)
O7—Ca3—O1070.75 (10)O1—P1—Ca5ix122.20 (14)
O2v—Ca3—O1056.07 (10)O8xii—P1—Ca5ix76.36 (11)
O5v—Ca3—O10125.98 (10)Ca1—P1—Ca5ix147.14 (4)
O3v—Ca3—O1068.63 (10)Ca3ii—P1—Ca5ix74.06 (3)
O9—Ca3—O1270.74 (10)Ca2—P1—Ca5ix74.16 (3)
O8—Ca3—O12144.32 (11)O10ii—P1—Ca4iv80.29 (13)
O7—Ca3—O1281.76 (10)O1—P1—Ca4iv80.12 (13)
O2v—Ca3—O12125.90 (11)O8xii—P1—Ca4iv56.27 (10)
O5v—Ca3—O1268.46 (10)O2—P1—Ca4iv167.37 (11)
O3v—Ca3—O1255.95 (10)Ca1—P1—Ca4iv80.23 (3)
O10—Ca3—O12117.42 (11)Ca3ii—P1—Ca4iv141.05 (5)
O9—Ca3—O1181.78 (10)Ca2—P1—Ca4iv140.51 (5)
O8—Ca3—O1170.77 (10)Ca5ix—P1—Ca4iv132.62 (3)
O7—Ca3—O11144.25 (11)O12ii—P2—O4107.45 (15)
O2v—Ca3—O1168.53 (10)O12ii—P2—O7i112.1 (2)
O5v—Ca3—O1156.07 (10)O4—P2—O7i112.2 (2)
O3v—Ca3—O11125.88 (10)O12ii—P2—O3106.68 (19)
O10—Ca3—O11117.47 (11)O4—P2—O3106.86 (19)
O12—Ca3—O11117.42 (10)O7i—P2—O3111.22 (15)
O9—Ca3—P1v165.25 (9)O12ii—P2—Ca4ii54.08 (13)
O8—Ca3—P1v88.50 (8)O4—P2—Ca4ii53.95 (13)
O7—Ca3—P1v99.39 (8)O7i—P2—Ca4ii136.34 (11)
O2v—Ca3—P1v27.78 (7)O3—P2—Ca4ii112.45 (11)
O5v—Ca3—P1v99.85 (8)O12ii—P2—Ca3ii60.74 (14)
O3v—Ca3—P1v67.23 (7)O4—P2—Ca3ii111.18 (14)
O10—Ca3—P1v28.65 (7)O7i—P2—Ca3ii135.86 (14)
O12—Ca3—P1v123.18 (8)O3—P2—Ca3ii46.82 (12)
O11—Ca3—P1v94.27 (7)Ca4ii—P2—Ca3ii78.15 (3)
O9—Ca3—P3v88.54 (8)O12ii—P2—Ca2111.75 (14)
O8—Ca3—P3v99.37 (8)O4—P2—Ca260.31 (14)
O7—Ca3—P3v165.18 (8)O7i—P2—Ca2135.45 (14)
O2v—Ca3—P3v67.18 (7)O3—P2—Ca247.29 (12)
O5v—Ca3—P3v27.82 (7)Ca4ii—P2—Ca278.25 (3)
O3v—Ca3—P3v99.77 (8)Ca3ii—P2—Ca264.30 (3)
O10—Ca3—P3v123.26 (8)O12ii—P2—Ca1121.97 (13)
O12—Ca3—P3v94.23 (7)O4—P2—Ca1122.19 (13)
O11—Ca3—P3v28.60 (7)O7i—P2—Ca176.55 (11)
P1v—Ca3—P3v94.75 (4)Ca4ii—P2—Ca1147.11 (4)
O9—Ca3—P2v99.35 (8)Ca3ii—P2—Ca173.99 (3)
O8—Ca3—P2v165.26 (8)Ca2—P2—Ca174.15 (3)
O7—Ca3—P2v88.57 (8)O12ii—P2—Ca5x80.30 (14)
O2v—Ca3—P2v99.78 (8)O4—P2—Ca5x80.29 (14)
O5v—Ca3—P2v67.10 (7)O7i—P2—Ca5x56.15 (10)
O3v—Ca3—P2v27.69 (7)O3—P2—Ca5x167.36 (11)
O10—Ca3—P2v94.26 (8)Ca4ii—P2—Ca5x80.19 (3)
O12—Ca3—P2v28.61 (7)Ca3ii—P2—Ca5x141.01 (4)
O11—Ca3—P2v123.16 (8)Ca2—P2—Ca5x140.55 (4)
P1v—Ca3—P2v94.71 (4)Ca1—P2—Ca5x132.70 (3)
P3v—Ca3—P2v94.70 (4)O11ii—P3—O6107.67 (15)
O5v—Ca4—O6vi87.18 (12)O11ii—P3—O9ix112.24 (19)
O5v—Ca4—O11vi87.39 (12)O6—P3—O9ix111.91 (19)
O6vi—Ca4—O11vi133.19 (10)O11ii—P3—O5106.87 (19)
O5v—Ca4—O4v75.38 (11)O6—P3—O5106.78 (19)
O6vi—Ca4—O4v140.14 (11)O9ix—P3—O5111.07 (15)
O11vi—Ca4—O4v82.28 (11)O11ii—P3—Ca5ix54.06 (13)
O5v—Ca4—O1275.31 (11)O6—P3—Ca5ix54.21 (13)
O6vi—Ca4—O1282.44 (11)O9ix—P3—Ca5ix136.41 (11)
O11vi—Ca4—O12140.01 (11)O5—P3—Ca5ix112.52 (11)
O4v—Ca4—O1258.71 (9)O11ii—P3—Ca3ii60.87 (14)
O5v—Ca4—Cl1Bvii142.68 (11)O6—P3—Ca3ii111.32 (13)
O6vi—Ca4—Cl1Bvii128.48 (10)O9ix—P3—Ca3ii135.94 (14)
O11vi—Ca4—Cl1Bvii75.72 (10)O5—P3—Ca3ii46.88 (12)
O4v—Ca4—Cl1Bvii69.59 (10)Ca5ix—P3—Ca3ii78.17 (3)
O12—Ca4—Cl1Bvii96.55 (10)O11ii—P3—Ca2111.85 (13)
O5v—Ca4—Cl1Avii144.18 (10)O6—P3—Ca260.23 (14)
O6vi—Ca4—Cl1Avii76.80 (10)O9ix—P3—Ca2135.25 (14)
O11vi—Ca4—Cl1Avii126.76 (10)O5—P3—Ca247.34 (12)
O4v—Ca4—Cl1Avii96.73 (10)Ca5ix—P3—Ca278.25 (3)
O12—Ca4—Cl1Avii71.00 (9)Ca3ii—P3—Ca264.33 (3)
Cl1Bvii—Ca4—Cl1Avii55.03 (6)O11ii—P3—Ca4ii122.18 (14)
O5v—Ca4—O8vi104.49 (9)O6—P3—Ca4ii121.88 (14)
O6vi—Ca4—O8vi68.32 (11)O9ix—P3—Ca4ii76.46 (11)
O11vi—Ca4—O8vi68.25 (11)Ca5ix—P3—Ca4ii147.13 (4)
O4v—Ca4—O8vi150.45 (11)Ca3ii—P3—Ca4ii74.05 (3)
O12—Ca4—O8vi150.67 (11)Ca2—P3—Ca4ii74.12 (3)
Cl1Bvii—Ca4—O8vi99.78 (8)O11ii—P3—Ca1xiv80.21 (14)
Cl1Avii—Ca4—O8vi99.04 (8)O6—P3—Ca1xiv80.25 (14)
O5v—Ca4—P2v70.35 (7)O9ix—P3—Ca1xiv56.26 (11)
O6vi—Ca4—P2v110.89 (9)O5—P3—Ca1xiv167.33 (11)
O11vi—Ca4—P2v110.76 (9)Ca5ix—P3—Ca1xiv80.15 (3)
O4v—Ca4—P2v29.48 (8)Ca3ii—P3—Ca1xiv141.06 (4)
O12—Ca4—P2v29.47 (8)Ca2—P3—Ca1xiv140.44 (4)
Cl1Bvii—Ca4—P2v84.71 (6)Ca4ii—P3—Ca1xiv132.72 (3)
Cl1Avii—Ca4—P2v85.61 (6)Cl1Avii—Cl1A—Ca1i121.1 (4)
O8vi—Ca4—P2v174.84 (6)Cl1Avii—Cl1A—Ca5115.4 (4)
O5v—Ca4—Cl1Bv134.70 (10)Ca1i—Cl1A—Ca5101.34 (9)
O6vi—Ca4—Cl1Bv138.00 (10)Cl1Avii—Cl1A—Ca4vii114.4 (4)
O11vi—Ca4—Cl1Bv64.93 (10)Ca1i—Cl1A—Ca4vii101.26 (9)
O4v—Ca4—Cl1Bv66.31 (9)Ca5—Cl1A—Ca4vii100.34 (8)
O12—Ca4—Cl1Bv102.74 (10)Cl1Avii—Cl1A—Ca451.9 (4)
Cl1Bvii—Ca4—Cl1Bv11.26 (10)Ca1i—Cl1A—Ca488.02 (7)
Cl1Avii—Ca4—Cl1Bv66.25 (8)Ca5—Cl1A—Ca487.50 (8)
O8vi—Ca4—Cl1Bv97.73 (8)Ca4vii—Cl1A—Ca4166.31 (10)
P2v—Ca4—Cl1Bv86.18 (5)Cl1Avii—Cl1A—Ca5vii51.0 (3)
O5v—Ca4—Cl1A133.22 (10)Ca1i—Cl1A—Ca5vii87.98 (7)
O6vi—Ca4—Cl1A64.34 (10)Ca5—Cl1A—Ca5vii166.45 (10)
O11vi—Ca4—Cl1A139.26 (10)Ca4vii—Cl1A—Ca5vii87.28 (8)
O4v—Ca4—Cl1A102.60 (9)Ca4—Cl1A—Ca5vii82.96 (6)
O12—Ca4—Cl1A65.24 (9)Cl1Avii—Cl1A—Ca1xiii46.2 (3)
Cl1Bvii—Ca4—Cl1A68.69 (8)Ca1i—Cl1A—Ca1xiii167.27 (10)
Cl1Avii—Ca4—Cl1A13.69 (10)Ca5—Cl1A—Ca1xiii86.84 (7)
O8vi—Ca4—Cl1A98.49 (8)Ca4vii—Cl1A—Ca1xiii86.66 (7)
P2v—Ca4—Cl1A85.48 (5)Ca4—Cl1A—Ca1xiii82.55 (6)
Cl1Bv—Ca4—Cl1A79.93 (5)Ca5vii—Cl1A—Ca1xiii82.41 (6)
O5v—Ca4—P3v22.54 (7)Cl1Bx—Cl1B—Ca4vii120.3 (5)
O6vi—Ca4—P3v78.69 (9)Cl1Bx—Cl1B—Ca5120.1 (5)
O11vi—Ca4—P3v78.84 (9)Ca4vii—Cl1B—Ca5100.26 (8)
O4v—Ca4—P3v94.94 (8)Cl1Bx—Cl1B—Ca1i113.6 (4)
O12—Ca4—P3v94.93 (8)Ca4vii—Cl1B—Ca1i99.40 (9)
Cl1Bvii—Ca4—P3v151.67 (7)Ca5—Cl1B—Ca1i99.36 (9)
Cl1Avii—Ca4—P3v153.07 (7)Cl1Bx—Cl1B—Ca1viii54.3 (4)
O8vi—Ca4—P3v81.95 (6)Ca4vii—Cl1B—Ca1viii88.30 (8)
P2v—Ca4—P3v92.89 (3)Ca5—Cl1B—Ca1viii88.30 (7)
Cl1Bv—Ca4—P3v140.56 (6)Ca1i—Cl1B—Ca1viii167.92 (9)
Cl1A—Ca4—P3v139.38 (6)Cl1Bx—Cl1B—Ca5x48.6 (4)
O2vi—Ca5—O10viii87.47 (13)Ca4vii—Cl1B—Ca5x87.69 (8)
O2vi—Ca5—O1viii87.29 (13)Ca5—Cl1B—Ca5x168.70 (10)
O10viii—Ca5—O1viii133.28 (10)Ca1i—Cl1B—Ca5x87.12 (7)
O2vi—Ca5—O11ix75.25 (11)Ca1viii—Cl1B—Ca5x83.89 (7)
O10viii—Ca5—O11ix140.06 (12)Cl1Bx—Cl1B—Ca4ii48.5 (4)
O1viii—Ca5—O11ix82.36 (11)Ca4vii—Cl1B—Ca4ii168.74 (10)
O2vi—Ca5—O6vi75.32 (11)Ca5—Cl1B—Ca4ii87.65 (8)
O10viii—Ca5—O6vi82.40 (11)Ca1i—Cl1B—Ca4ii87.08 (7)
O1viii—Ca5—O6vi140.01 (12)Ca1viii—Cl1B—Ca4ii83.90 (7)
O11ix—Ca5—O6vi58.64 (9)Ca5x—Cl1B—Ca4ii83.42 (6)
O2vi—Ca5—Cl1A143.49 (10)
Symmetry codes: (i) x+1, y+2, z; (ii) x, y+1, z; (iii) x+1, y, z; (iv) x+1, y+1, z; (v) x, y1, z; (vi) x+1, y1/2, z+1/2; (vii) x, y+1, z; (viii) x1, y, z; (ix) x+1, y+1/2, z+1/2; (x) x, y+2, z; (xi) x+2, y1/2, z+1/2; (xii) x+2, y+1/2, z+1/2; (xiii) x1, y1, z; (xiv) x, y+5/2, z+1/2.
(1400l) top
Crystal data top
3(O4P)·0.54(Cl)·0.46(OH)·5(Ca)Dx = 3.176 Mg m3
Mr = 512.32Mo Kα radiation, λ = 0.7107 Å
Trigonal, P63/mCell parameters from 1952 reflections
Hall symbol: -P 6cθ = 3.9–26.3°
a = 9.5377 (3) ŵ = 3.16 mm1
c = 6.7999 (5) ÅT = 100 K
V = 535.70 (5) Å3Prism, colourless
Z = 20.48 × 0.11 × 0.06 mm
F(000) = 509
Data collection top
BRUKER APPEX-II CCD
diffractometer
485 independent reflections
Radiation source: fine-focus sealed tube456 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.044
ω and phi scansθmax = 28.3°, θmin = 2.5°
Absorption correction: multi-scan
BRUKER SADABS
h = 1212
Tmin = 0.685, Tmax = 1k = 1212
2425 measured reflectionsl = 99
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.027Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.064H atoms treated by a mixture of independent and constrained refinement
S = 1.18 w = 1/[σ2(Fo2) + (0.0265P)2 + 1.1517P]
where P = (Fo2 + 2Fc2)/3
485 reflections(Δ/σ)max < 0.001
47 parametersΔρmax = 0.87 e Å3
15 restraintsΔρmin = 0.86 e Å3
Crystal data top
3(O4P)·0.54(Cl)·0.46(OH)·5(Ca)Z = 2
Mr = 512.32Mo Kα radiation
Trigonal, P63/mµ = 3.16 mm1
a = 9.5377 (3) ÅT = 100 K
c = 6.7999 (5) Å0.48 × 0.11 × 0.06 mm
V = 535.70 (5) Å3
Data collection top
BRUKER APPEX-II CCD
diffractometer
485 independent reflections
Absorption correction: multi-scan
BRUKER SADABS
456 reflections with I > 2σ(I)
Tmin = 0.685, Tmax = 1Rint = 0.044
2425 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.02715 restraints
wR(F2) = 0.064H atoms treated by a mixture of independent and constrained refinement
S = 1.18Δρmax = 0.87 e Å3
485 reflectionsΔρmin = 0.86 e Å3
47 parameters
Special details top

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ca10.33330.66671.00259 (11)0.00759 (19)
Ca20.74382 (8)0.74544 (8)0.250.01107 (19)
P10.59634 (9)0.62795 (9)0.750.00513 (19)
O20.4093 (3)0.5341 (3)0.750.0144 (5)
O30.6482 (2)0.7356 (2)0.5677 (3)0.0205 (4)
O40.6639 (3)0.5117 (3)0.750.0087 (4)
Cl1110.4609 (7)0.0140.272 (4)
O1110.128 (3)0.010 (2)0.150 (7)
H11100.012*0.300 (13)
O1A110.250.0117 (15)0.155 (11)
H1A110.106 (3)0.014*0.078 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0094 (2)0.0094 (2)0.0040 (4)0.00471 (12)00
Ca20.0173 (3)0.0158 (3)0.0048 (3)0.0117 (3)00
P10.0074 (4)0.0056 (3)0.0041 (4)0.0046 (3)00
O20.0083 (10)0.0112 (11)0.0250 (13)0.0059 (9)00
O30.0381 (11)0.0176 (8)0.0166 (9)0.0222 (8)0.0177 (8)0.0114 (7)
O40.0120 (10)0.0089 (10)0.0090 (11)0.0080 (9)00
Cl10.0080.0080.0260.00400
O10.003 (2)0.003 (2)0.024 (4)0.0015 (11)00
O1A0.0052 (18)0.0052 (18)0.025 (3)0.0026 (9)00
Geometric parameters (Å, º) top
Ca1—O4i2.4021 (16)P1—O21.545 (2)
Ca1—O4ii2.4021 (16)P1—Ca2xiii3.1073 (10)
Ca1—O4iii2.4021 (16)P1—Ca1viii3.2102 (7)
Ca1—O2iv2.4473 (17)P1—Ca2ix3.4139 (10)
Ca1—O2v2.4473 (17)P1—Ca2xii3.4187 (10)
Ca1—O22.4473 (17)O2—Ca2ix2.312 (2)
Ca1—O3vi2.776 (2)O2—Ca1viii2.4473 (17)
Ca1—O3vii2.776 (2)O3—Ca2xiii2.5458 (19)
Ca1—O3viii2.776 (2)O3—Ca1viii2.776 (2)
Ca1—P1v3.2102 (7)O4—Ca1xiv2.4021 (16)
Ca1—P1iv3.2102 (8)O4—Ca1iii2.4021 (16)
Ca1—P13.2102 (7)O4—Ca2xii2.832 (2)
Ca2—O2ix2.312 (2)Cl1—Cl1xv0.532 (9)
Ca2—O3x2.3283 (18)Cl1—Ca2xvi2.827 (2)
Ca2—O32.3283 (18)Cl1—Ca2xvii2.827 (2)
Ca2—O1A2.4357 (7)Cl1—Ca2xv3.130 (3)
Ca2—O3xi2.5458 (19)Cl1—Ca2xiii3.130 (3)
Ca2—O3xii2.5458 (19)Cl1—Ca2xii3.130 (3)
Ca2—O1x2.572 (6)O1—O1x1.65 (4)
Ca2—O12.572 (6)O1—O1xviii1.75 (4)
Ca2—Cl12.827 (2)O1—Ca2xvi2.572 (6)
Ca2—Cl1x2.827 (2)O1—Ca2xvii2.572 (6)
Ca2—O4xiii2.832 (2)O1—H10.873 (18)
Ca2—P1xii3.1073 (10)O1—H1A0.16 (3)
Ca2—H1A2.626 (8)O1A—Ca2xvi2.4357 (7)
P1—O3viii1.5259 (18)O1A—Ca2xvii2.4357 (7)
P1—O31.5259 (18)O1A—H1A0.98 (2)
P1—O41.536 (2)
O4i—Ca1—O4ii76.36 (6)O2ix—Ca2—P1xii69.80 (6)
O4i—Ca1—O4iii76.36 (6)O3x—Ca2—P1xii109.10 (5)
O4ii—Ca1—O4iii76.36 (6)O3—Ca2—P1xii109.10 (5)
O4i—Ca1—O2iv90.84 (5)O1A—Ca2—P1xii83.03 (2)
O4ii—Ca1—O2iv151.98 (8)O3xi—Ca2—P1xii29.22 (4)
O4iii—Ca1—O2iv125.25 (7)O3xii—Ca2—P1xii29.22 (4)
O4i—Ca1—O2v125.25 (7)O1x—Ca2—P1xii83.41 (3)
O4ii—Ca1—O2v90.84 (5)O1—Ca2—P1xii83.41 (3)
O4iii—Ca1—O2v151.98 (8)Cl1—Ca2—P1xii84.00 (2)
O2iv—Ca1—O2v76.18 (6)Cl1x—Ca2—P1xii84.00 (2)
O4i—Ca1—O2151.98 (8)O4xiii—Ca2—P1xii174.03 (5)
O4ii—Ca1—O2125.25 (7)O2ix—Ca2—H1A145.6 (3)
O4iii—Ca1—O290.84 (5)O3x—Ca2—H1A81.7 (4)
O2iv—Ca1—O276.18 (6)O3—Ca2—H1A123.3 (4)
O2v—Ca1—O276.18 (6)O1A—Ca2—H1A22.0 (4)
O4i—Ca1—O3vi69.94 (6)O3xi—Ca2—H1A71.89 (19)
O4ii—Ca1—O3vi83.94 (6)O3xii—Ca2—H1A93.1 (2)
O4iii—Ca1—O3vi144.11 (6)O1x—Ca2—H1A40.7 (6)
O2iv—Ca1—O3vi68.19 (7)O1—Ca2—H1A3.2 (6)
O2v—Ca1—O3vi55.73 (6)Cl1—Ca2—H1A52.5 (4)
O2—Ca1—O3vi124.90 (6)Cl1x—Ca2—H1A8.5 (4)
O4i—Ca1—O3vii83.94 (7)O4xiii—Ca2—H1A101.98 (6)
O4ii—Ca1—O3vii144.11 (6)P1xii—Ca2—H1A83.54 (3)
O4iii—Ca1—O3vii69.94 (6)O3viii—P1—O3108.69 (15)
O2iv—Ca1—O3vii55.73 (6)O3viii—P1—O4111.96 (8)
O2v—Ca1—O3vii124.90 (6)O3—P1—O4111.96 (8)
O2—Ca1—O3vii68.19 (7)O3viii—P1—O2106.37 (10)
O3vi—Ca1—O3vii117.10 (2)O3—P1—O2106.37 (10)
O4i—Ca1—O3viii144.11 (6)O4—P1—O2111.18 (13)
O4ii—Ca1—O3viii69.94 (6)O3viii—P1—Ca2xiii54.53 (7)
O4iii—Ca1—O3viii83.94 (6)O3—P1—Ca2xiii54.53 (7)
O2iv—Ca1—O3viii124.90 (6)O4—P1—Ca2xiii135.36 (10)
O2v—Ca1—O3viii68.19 (7)O2—P1—Ca2xiii113.46 (9)
O2—Ca1—O3viii55.73 (6)O3viii—P1—Ca1viii111.49 (7)
O3vi—Ca1—O3viii117.10 (2)O3—P1—Ca1viii59.80 (8)
O3vii—Ca1—O3viii117.10 (2)O4—P1—Ca1viii135.80 (6)
O4i—Ca1—P1v98.30 (5)O2—P1—Ca1viii47.49 (6)
O4ii—Ca1—P1v90.41 (5)Ca2xiii—P1—Ca1viii78.690 (19)
O4iii—Ca1—P1v166.54 (5)O3viii—P1—Ca159.80 (8)
O2iv—Ca1—P1v66.55 (5)O3—P1—Ca1111.49 (7)
O2v—Ca1—P1v27.74 (5)O4—P1—Ca1135.80 (6)
O2—Ca1—P1v99.01 (5)O2—P1—Ca147.49 (6)
O3vi—Ca1—P1v28.36 (4)Ca2xiii—P1—Ca178.690 (19)
O3vii—Ca1—P1v122.28 (4)Ca1viii—P1—Ca164.69 (3)
O3viii—Ca1—P1v93.99 (4)O3viii—P1—Ca2ix121.42 (9)
O4i—Ca1—P1iv90.41 (5)O3—P1—Ca2ix121.42 (9)
O4ii—Ca1—P1iv166.54 (5)O4—P1—Ca2ix76.68 (9)
O4iii—Ca1—P1iv98.30 (5)Ca2xiii—P1—Ca2ix147.96 (3)
O2iv—Ca1—P1iv27.74 (5)Ca1viii—P1—Ca2ix74.353 (18)
O2v—Ca1—P1iv99.01 (5)Ca1—P1—Ca2ix74.353 (18)
O2—Ca1—P1iv66.55 (5)O3viii—P1—Ca2xii81.29 (8)
O3vi—Ca1—P1iv93.99 (4)O3—P1—Ca2xii81.29 (8)
O3vii—Ca1—P1iv28.36 (4)O4—P1—Ca2xii54.97 (9)
O3viii—Ca1—P1iv122.28 (4)O2—P1—Ca2xii166.14 (9)
P1v—Ca1—P1iv94.048 (18)Ca2xiii—P1—Ca2xii80.39 (3)
O4i—Ca1—P1166.54 (5)Ca1viii—P1—Ca2xii141.032 (18)
O4ii—Ca1—P198.30 (5)Ca1—P1—Ca2xii141.032 (18)
O4iii—Ca1—P190.41 (5)Ca2ix—P1—Ca2xii131.65 (3)
O2iv—Ca1—P199.01 (5)P1—O2—Ca2ix123.27 (13)
O2v—Ca1—P166.55 (5)P1—O2—Ca1104.77 (9)
O2—Ca1—P127.74 (5)Ca2ix—O2—Ca1114.60 (7)
O3vi—Ca1—P1122.28 (4)P1—O2—Ca1viii104.77 (9)
O3vii—Ca1—P193.99 (4)Ca2ix—O2—Ca1viii114.60 (7)
O3viii—Ca1—P128.36 (4)Ca1—O2—Ca1viii89.15 (8)
P1v—Ca1—P194.048 (19)P1—O3—Ca2140.32 (10)
P1iv—Ca1—P194.048 (18)P1—O3—Ca2xiii96.25 (9)
O2ix—Ca2—O3x86.83 (5)Ca2—O3—Ca2xiii118.13 (7)
O2ix—Ca2—O386.83 (5)P1—O3—Ca1viii91.84 (9)
O3x—Ca2—O3136.18 (11)Ca2—O3—Ca1viii101.85 (8)
O2ix—Ca2—O1A152.84 (6)Ca2xiii—O3—Ca1viii97.57 (6)
O3x—Ca2—O1A102.57 (5)P1—O4—Ca1xiv131.95 (6)
O3—Ca2—O1A102.57 (5)P1—O4—Ca1iii131.95 (6)
O2ix—Ca2—O3xi74.33 (7)Ca1xiv—O4—Ca1iii88.91 (7)
O3x—Ca2—O3xi80.78 (4)P1—O4—Ca2xii98.67 (10)
O3—Ca2—O3xi138.02 (7)Ca1xiv—O4—Ca2xii98.43 (7)
O1A—Ca2—O3xi82.02 (5)Ca1iii—O4—Ca2xii98.43 (7)
O2ix—Ca2—O3xii74.33 (7)Cl1xv—Cl1—Ca2120.49 (8)
O3x—Ca2—O3xii138.02 (7)Cl1xv—Cl1—Ca2xvi120.49 (8)
O3—Ca2—O3xii80.78 (4)Ca2—Cl1—Ca2xvi96.54 (10)
O1A—Ca2—O3xii82.02 (5)Cl1xv—Cl1—Ca2xvii120.49 (7)
O3xi—Ca2—O3xii58.29 (8)Ca2—Cl1—Ca2xvii96.54 (10)
O2ix—Ca2—O1x147.4 (2)Ca2xvi—Cl1—Ca2xvii96.54 (10)
O3x—Ca2—O1x120.3 (4)Cl1xv—Cl1—Ca2xv51.09 (6)
O3—Ca2—O1x84.7 (4)Ca2—Cl1—Ca2xv171.58 (14)
O1A—Ca2—O1x18.8 (4)Ca2xvi—Cl1—Ca2xv89.048 (19)
O3xi—Ca2—O1x91.4 (2)Ca2xvii—Cl1—Ca2xv89.048 (19)
O3xii—Ca2—O1x73.26 (17)Cl1xv—Cl1—Ca2xiii51.09 (7)
O2ix—Ca2—O1147.4 (2)Ca2—Cl1—Ca2xiii89.048 (19)
O3x—Ca2—O184.7 (4)Ca2xvi—Cl1—Ca2xiii89.048 (19)
O3—Ca2—O1120.3 (4)Ca2xvii—Cl1—Ca2xiii171.58 (14)
O1A—Ca2—O118.8 (4)Ca2xv—Cl1—Ca2xiii84.74 (9)
O3xi—Ca2—O173.26 (17)Cl1xv—Cl1—Ca2xii51.09 (6)
O3xii—Ca2—O191.4 (2)Ca2—Cl1—Ca2xii89.048 (19)
O1x—Ca2—O137.5 (7)Ca2xvi—Cl1—Ca2xii171.58 (14)
O2ix—Ca2—Cl1140.06 (7)Ca2xvii—Cl1—Ca2xii89.048 (19)
O3x—Ca2—Cl1131.17 (9)Ca2xv—Cl1—Ca2xii84.74 (9)
O3—Ca2—Cl173.55 (9)Ca2xiii—Cl1—Ca2xii84.74 (9)
O1A—Ca2—Cl130.49 (8)O1x—O1—O1xviii180.000 (12)
O3xi—Ca2—Cl197.33 (6)O1x—O1—Ca2xvi71.2 (4)
O3xii—Ca2—Cl168.49 (5)O1xviii—O1—Ca2xvi108.8 (4)
O1x—Ca2—Cl111.7 (3)O1x—O1—Ca2xvii71.2 (4)
O1—Ca2—Cl149.3 (4)O1xviii—O1—Ca2xvii108.8 (4)
O2ix—Ca2—Cl1x140.06 (7)Ca2xvi—O1—Ca2xvii110.2 (4)
O3x—Ca2—Cl1x73.55 (9)O1x—O1—Ca271.2 (4)
O3—Ca2—Cl1x131.17 (9)O1xviii—O1—Ca2108.8 (4)
O1A—Ca2—Cl1x30.49 (8)Ca2xvi—O1—Ca2110.2 (4)
O3xi—Ca2—Cl1x68.49 (5)Ca2xvii—O1—Ca2110.2 (4)
O3xii—Ca2—Cl1x97.33 (6)O1x—O1—H1180.000 (4)
O1x—Ca2—Cl1x49.3 (4)Ca2xvi—O1—H1108.8 (4)
O1—Ca2—Cl1x11.7 (3)Ca2xvii—O1—H1108.8 (4)
Cl1—Ca2—Cl1x60.98 (16)Ca2—O1—H1108.8 (4)
O2ix—Ca2—O4xiii104.22 (7)O1x—O1—H1A180.00 (5)
O3x—Ca2—O4xiii69.87 (5)Ca2xvi—O1—H1A108.8 (4)
O3—Ca2—O4xiii69.87 (5)Ca2xvii—O1—H1A108.8 (4)
O1A—Ca2—O4xiii102.94 (5)Ca2—O1—H1A108.8 (4)
O3xi—Ca2—O4xiii150.63 (4)Ca2—O1A—Ca2xvi120
O3xii—Ca2—O4xiii150.63 (4)Ca2—O1A—Ca2xvii120
O1x—Ca2—O4xiii102.24 (5)Ca2xvi—O1A—Ca2xvii120
O1—Ca2—O4xiii102.24 (5)Ca2—O1A—H1A90.000 (8)
Cl1—Ca2—O4xiii101.12 (4)Ca2xvi—O1A—H1A90.000 (2)
Cl1x—Ca2—O4xiii101.12 (4)Ca2xvii—O1A—H1A90.000 (7)
O4i—Ca1—P1—O3viii65.7 (2)Cl1x—Ca2—O3—P1134.00 (17)
O4ii—Ca1—P1—O3viii0.10 (9)O4xiii—Ca2—O3—P1138.7 (2)
O4iii—Ca1—P1—O3viii76.38 (9)P1xii—Ca2—O3—P135.0 (2)
O2iv—Ca1—P1—O3viii157.79 (10)O2ix—Ca2—O3—Ca2xiii179.25 (10)
O2v—Ca1—P1—O3viii87.20 (9)O3x—Ca2—O3—Ca2xiii98.65 (15)
O2—Ca1—P1—O3viii167.40 (12)O1A—Ca2—O3—Ca2xiii25.01 (9)
O3vi—Ca1—P1—O3viii87.95 (4)O3xi—Ca2—O3—Ca2xiii117.03 (6)
O3vii—Ca1—P1—O3viii146.30 (9)O3xii—Ca2—O3—Ca2xiii104.63 (5)
P1v—Ca1—P1—O3viii90.91 (8)O1x—Ca2—O3—Ca2xiii30.77 (14)
P1iv—Ca1—P1—O3viii174.73 (8)O1—Ca2—O3—Ca2xiii18.37 (19)
O4i—Ca1—P1—O3165.4 (2)Cl1—Ca2—O3—Ca2xiii34.47 (8)
O4ii—Ca1—P1—O399.84 (10)Cl1x—Ca2—O3—Ca2xiii12.93 (13)
O4iii—Ca1—P1—O3176.12 (10)O4xiii—Ca2—O3—Ca2xiii74.35 (9)
O2iv—Ca1—P1—O358.05 (11)P1xii—Ca2—O3—Ca2xiii111.90 (7)
O2v—Ca1—P1—O312.54 (10)O2ix—Ca2—O3—Ca1viii75.39 (7)
O2—Ca1—P1—O392.86 (12)O3x—Ca2—O3—Ca1viii6.70 (15)
O3vi—Ca1—P1—O311.79 (13)O1A—Ca2—O3—Ca1viii130.37 (4)
O3vii—Ca1—P1—O3113.96 (10)O3xi—Ca2—O3—Ca1viii137.61 (11)
O3viii—Ca1—P1—O399.74 (16)O3xii—Ca2—O3—Ca1viii150.01 (6)
P1v—Ca1—P1—O38.83 (9)O1x—Ca2—O3—Ca1viii136.13 (12)
P1iv—Ca1—P1—O385.53 (9)O1—Ca2—O3—Ca1viii123.73 (16)
O4i—Ca1—P1—O425.61 (19)Cl1—Ca2—O3—Ca1viii139.83 (6)
O4ii—Ca1—P1—O491.17 (13)Cl1x—Ca2—O3—Ca1viii118.29 (7)
O4iii—Ca1—P1—O414.89 (15)O4xiii—Ca2—O3—Ca1viii31.01 (5)
O2iv—Ca1—P1—O4110.94 (12)P1xii—Ca2—O3—Ca1viii142.74 (4)
O2v—Ca1—P1—O4178.47 (12)O3viii—P1—O4—Ca1xiv170.83 (14)
O2—Ca1—P1—O476.13 (14)O3—P1—O4—Ca1xiv48.5 (2)
O3vi—Ca1—P1—O4179.22 (11)O2—P1—O4—Ca1xiv70.34 (14)
O3vii—Ca1—P1—O455.03 (11)Ca2xiii—P1—O4—Ca1xiv109.66 (14)
O3viii—Ca1—P1—O491.27 (13)Ca1viii—P1—O4—Ca1xiv20.2 (2)
P1v—Ca1—P1—O4177.82 (11)Ca1—P1—O4—Ca1xiv120.47 (8)
P1iv—Ca1—P1—O483.46 (11)Ca2ix—P1—O4—Ca1xiv70.34 (14)
O4i—Ca1—P1—O2101.7 (2)Ca2xii—P1—O4—Ca1xiv109.66 (14)
O4ii—Ca1—P1—O2167.30 (10)O3viii—P1—O4—Ca1iii48.5 (2)
O4iii—Ca1—P1—O291.02 (10)O3—P1—O4—Ca1iii170.83 (14)
O2iv—Ca1—P1—O234.81 (11)O2—P1—O4—Ca1iii70.34 (14)
O2v—Ca1—P1—O2105.40 (13)Ca2xiii—P1—O4—Ca1iii109.66 (14)
O3vi—Ca1—P1—O2104.65 (10)Ca1viii—P1—O4—Ca1iii120.47 (8)
O3vii—Ca1—P1—O221.10 (9)Ca1—P1—O4—Ca1iii20.2 (2)
O3viii—Ca1—P1—O2167.40 (12)Ca2ix—P1—O4—Ca1iii70.34 (14)
P1v—Ca1—P1—O2101.69 (9)Ca2xii—P1—O4—Ca1iii109.66 (14)
P1iv—Ca1—P1—O27.33 (8)O3viii—P1—O4—Ca2xii61.18 (10)
O4i—Ca1—P1—Ca2xiii121.0 (2)O3—P1—O4—Ca2xii61.18 (10)
O4ii—Ca1—P1—Ca2xiii55.47 (5)O2—P1—O4—Ca2xii180
O4iii—Ca1—P1—Ca2xiii131.74 (5)Ca2xiii—P1—O4—Ca2xii0
O2iv—Ca1—P1—Ca2xiii102.42 (5)Ca1viii—P1—O4—Ca2xii129.87 (8)
O2v—Ca1—P1—Ca2xiii31.83 (5)Ca1—P1—O4—Ca2xii129.87 (8)
O2—Ca1—P1—Ca2xiii137.24 (9)Ca2ix—P1—O4—Ca2xii180
O3vi—Ca1—P1—Ca2xiii32.59 (5)O2ix—Ca2—Cl1—Cl1xv45.32 (10)
O3vii—Ca1—P1—Ca2xiii158.34 (4)O3x—Ca2—Cl1—Cl1xv156.25 (7)
O3viii—Ca1—P1—Ca2xiii55.37 (8)O3—Ca2—Cl1—Cl1xv18.43 (5)
P1v—Ca1—P1—Ca2xiii35.545 (16)O1A—Ca2—Cl1—Cl1xv180.000 (2)
P1iv—Ca1—P1—Ca2xiii129.901 (15)O3xi—Ca2—Cl1—Cl1xv119.61 (4)
O4i—Ca1—P1—Ca1viii156.3 (2)O3xii—Ca2—Cl1—Cl1xv67.95 (5)
O4ii—Ca1—P1—Ca1viii138.19 (5)O1x—Ca2—Cl1—Cl1xv180.000 (2)
O4iii—Ca1—P1—Ca1viii145.53 (5)O1—Ca2—Cl1—Cl1xv180.000 (2)
O2iv—Ca1—P1—Ca1viii19.70 (5)Cl1x—Ca2—Cl1—Cl1xv180.000 (2)
O2v—Ca1—P1—Ca1viii50.89 (5)O4xiii—Ca2—Cl1—Cl1xv83.35 (3)
O2—Ca1—P1—Ca1viii54.51 (8)P1xii—Ca2—Cl1—Cl1xv93.547 (13)
O3vi—Ca1—P1—Ca1viii50.14 (5)O2ix—Ca2—Cl1—Ca2xvi176.63 (8)
O3vii—Ca1—P1—Ca1viii75.61 (4)O3x—Ca2—Cl1—Ca2xvi24.94 (11)
O3viii—Ca1—P1—Ca1viii138.09 (8)O3—Ca2—Cl1—Ca2xvi112.88 (8)
P1v—Ca1—P1—Ca1viii47.178 (11)O1A—Ca2—Cl1—Ca2xvi48.69 (7)
P1iv—Ca1—P1—Ca1viii47.178 (11)O3xi—Ca2—Cl1—Ca2xvi109.08 (7)
O4i—Ca1—P1—Ca2ix76.5 (2)O3xii—Ca2—Cl1—Ca2xvi160.74 (11)
O4ii—Ca1—P1—Ca2ix142.03 (5)O1x—Ca2—Cl1—Ca2xvi48.69 (7)
O4iii—Ca1—P1—Ca2ix65.75 (5)O1—Ca2—Cl1—Ca2xvi48.69 (7)
O2iv—Ca1—P1—Ca2ix60.08 (5)Cl1x—Ca2—Cl1—Ca2xvi48.69 (7)
O2v—Ca1—P1—Ca2ix130.67 (5)O4xiii—Ca2—Cl1—Ca2xvi47.96 (9)
O2—Ca1—P1—Ca2ix25.27 (8)P1xii—Ca2—Cl1—Ca2xvi135.14 (7)
O3vi—Ca1—P1—Ca2ix129.92 (5)O2ix—Ca2—Cl1—Ca2xvii85.99 (15)
O3vii—Ca1—P1—Ca2ix4.17 (4)O3x—Ca2—Cl1—Ca2xvii72.44 (8)
O3viii—Ca1—P1—Ca2ix142.13 (8)O3—Ca2—Cl1—Ca2xvii149.74 (9)
P1v—Ca1—P1—Ca2ix126.960 (16)O1A—Ca2—Cl1—Ca2xvii48.69 (7)
P1iv—Ca1—P1—Ca2ix32.604 (15)O3xi—Ca2—Cl1—Ca2xvii11.70 (9)
O4i—Ca1—P1—Ca2xii62.2 (2)O3xii—Ca2—Cl1—Ca2xvii63.36 (6)
O4ii—Ca1—P1—Ca2xii3.34 (6)O1x—Ca2—Cl1—Ca2xvii48.69 (7)
O4iii—Ca1—P1—Ca2xii72.93 (6)O1—Ca2—Cl1—Ca2xvii48.69 (7)
O2iv—Ca1—P1—Ca2xii161.23 (6)Cl1x—Ca2—Cl1—Ca2xvii48.69 (7)
O2v—Ca1—P1—Ca2xii90.64 (6)O4xiii—Ca2—Cl1—Ca2xvii145.34 (6)
O2—Ca1—P1—Ca2xii163.95 (10)P1xii—Ca2—Cl1—Ca2xvii37.76 (6)
O3vi—Ca1—P1—Ca2xii91.40 (6)O2ix—Ca2—Cl1—Ca2xiii87.70 (8)
O3vii—Ca1—P1—Ca2xii142.85 (5)O3x—Ca2—Cl1—Ca2xiii113.88 (10)
O3viii—Ca1—P1—Ca2xii3.44 (8)O3—Ca2—Cl1—Ca2xiii23.95 (6)
P1v—Ca1—P1—Ca2xii94.35 (5)O1A—Ca2—Cl1—Ca2xiii137.62 (5)
P1iv—Ca1—P1—Ca2xii171.29 (4)O3xi—Ca2—Cl1—Ca2xiii161.99 (6)
O3viii—P1—O2—Ca2ix122.13 (8)O3xii—Ca2—Cl1—Ca2xiii110.33 (9)
O3—P1—O2—Ca2ix122.13 (8)O1x—Ca2—Cl1—Ca2xiii137.62 (5)
O4—P1—O2—Ca2ix0O1—Ca2—Cl1—Ca2xiii137.62 (5)
Ca2xiii—P1—O2—Ca2ix180Cl1x—Ca2—Cl1—Ca2xiii137.62 (5)
Ca1viii—P1—O2—Ca2ix133.46 (6)O4xiii—Ca2—Cl1—Ca2xiii40.97 (7)
Ca1—P1—O2—Ca2ix133.46 (6)P1xii—Ca2—Cl1—Ca2xiii135.92 (6)
Ca2xii—P1—O2—Ca2ix0O2ix—Ca2—Cl1—Ca2xii2.94 (14)
O3viii—P1—O2—Ca111.33 (11)O3x—Ca2—Cl1—Ca2xii161.37 (7)
O3—P1—O2—Ca1104.41 (8)O3—Ca2—Cl1—Ca2xii60.80 (7)
O4—P1—O2—Ca1133.46 (6)O1A—Ca2—Cl1—Ca2xii137.62 (5)
Ca2xiii—P1—O2—Ca146.54 (6)O3xi—Ca2—Cl1—Ca2xii77.23 (7)
Ca1viii—P1—O2—Ca193.07 (12)O3xii—Ca2—Cl1—Ca2xii25.57 (5)
Ca2ix—P1—O2—Ca1133.46 (6)O1x—Ca2—Cl1—Ca2xii137.62 (5)
Ca2xii—P1—O2—Ca1133.46 (6)O1—Ca2—Cl1—Ca2xii137.62 (5)
O3viii—P1—O2—Ca1viii104.41 (8)Cl1x—Ca2—Cl1—Ca2xii137.62 (5)
O3—P1—O2—Ca1viii11.33 (11)O4xiii—Ca2—Cl1—Ca2xii125.73 (4)
O4—P1—O2—Ca1viii133.46 (6)P1xii—Ca2—Cl1—Ca2xii51.17 (4)
Ca2xiii—P1—O2—Ca1viii46.54 (6)O2ix—Ca2—O1—O1x122.1 (5)
Ca1—P1—O2—Ca1viii93.07 (12)O3x—Ca2—O1—O1x162.28 (5)
Ca2ix—P1—O2—Ca1viii133.46 (6)O3—Ca2—O1—O1x20.55 (10)
Ca2xii—P1—O2—Ca1viii133.46 (6)O1A—Ca2—O1—O1x0.000 (5)
O4i—Ca1—O2—P1150.97 (11)O3xi—Ca2—O1—O1x115.78 (11)
O4ii—Ca1—O2—P115.45 (12)O3xii—Ca2—O1—O1x59.61 (4)
O4iii—Ca1—O2—P189.29 (9)Cl1—Ca2—O1—O1x0.000 (3)
O2iv—Ca1—O2—P1144.50 (10)Cl1x—Ca2—O1—O1x180.000 (6)
O2v—Ca1—O2—P165.62 (12)O4xiii—Ca2—O1—O1x94.23 (8)
O3vi—Ca1—O2—P194.15 (9)P1xii—Ca2—O1—O1x87.75 (5)
O3vii—Ca1—O2—P1157.24 (10)O2ix—Ca2—O1—O1xviii57.9 (5)
O3viii—Ca1—O2—P17.20 (7)O3x—Ca2—O1—O1xviii17.72 (5)
P1v—Ca1—O2—P181.50 (7)O3—Ca2—O1—O1xviii159.45 (9)
P1iv—Ca1—O2—P1172.02 (9)O1A—Ca2—O1—O1xviii180.000 (5)
O4i—Ca1—O2—Ca2ix12.84 (17)O3xi—Ca2—O1—O1xviii64.22 (11)
O4ii—Ca1—O2—Ca2ix122.68 (9)O3xii—Ca2—O1—O1xviii120.39 (4)
O4iii—Ca1—O2—Ca2ix48.84 (9)O1x—Ca2—O1—O1xviii180.000 (3)
O2iv—Ca1—O2—Ca2ix77.37 (12)Cl1—Ca2—O1—O1xviii180.000 (3)
O2v—Ca1—O2—Ca2ix156.25 (10)Cl1x—Ca2—O1—O1xviii0.000 (3)
O3vi—Ca1—O2—Ca2ix127.72 (6)O4xiii—Ca2—O1—O1xviii85.77 (8)
O3vii—Ca1—O2—Ca2ix19.11 (7)P1xii—Ca2—O1—O1xviii92.25 (4)
O3viii—Ca1—O2—Ca2ix130.92 (9)O2ix—Ca2—O1—Ca2xvi177.04 (8)
P1v—Ca1—O2—Ca2ix140.37 (6)O3x—Ca2—O1—Ca2xvi101.4 (5)
P1iv—Ca1—O2—Ca2ix49.85 (7)O3—Ca2—O1—Ca2xvi40.3 (5)
P1—Ca1—O2—Ca2ix138.13 (12)O1A—Ca2—O1—Ca2xvi60.9 (5)
O4i—Ca1—O2—Ca1viii103.97 (12)O3xi—Ca2—O1—Ca2xvi176.7 (6)
O4ii—Ca1—O2—Ca1viii120.51 (7)O3xii—Ca2—O1—Ca2xvi120.5 (5)
O4iii—Ca1—O2—Ca1viii165.65 (8)O1x—Ca2—O1—Ca2xvi60.9 (5)
O2iv—Ca1—O2—Ca1viii39.44 (9)Cl1—Ca2—O1—Ca2xvi60.9 (5)
O2v—Ca1—O2—Ca1viii39.44 (9)Cl1x—Ca2—O1—Ca2xvi119.1 (5)
O3vi—Ca1—O2—Ca1viii10.91 (10)O4xiii—Ca2—O1—Ca2xvi33.3 (5)
O3vii—Ca1—O2—Ca1viii97.70 (7)P1xii—Ca2—O1—Ca2xvi148.6 (5)
O3viii—Ca1—O2—Ca1viii112.26 (9)O2ix—Ca2—O1—Ca2xvii61.2 (10)
P1v—Ca1—O2—Ca1viii23.56 (6)O3x—Ca2—O1—Ca2xvii136.8 (5)
P1iv—Ca1—O2—Ca1viii66.96 (5)O3—Ca2—O1—Ca2xvii81.4 (4)
P1—Ca1—O2—Ca1viii105.06 (11)O1A—Ca2—O1—Ca2xvii60.9 (5)
O3viii—P1—O3—Ca2144.35 (11)O3xi—Ca2—O1—Ca2xvii54.9 (4)
O4—P1—O3—Ca220.1 (2)O3xii—Ca2—O1—Ca2xvii1.3 (5)
O2—P1—O3—Ca2101.5 (2)O1x—Ca2—O1—Ca2xvii60.9 (5)
Ca2xiii—P1—O3—Ca2151.0 (2)Cl1—Ca2—O1—Ca2xvii60.9 (5)
Ca1viii—P1—O3—Ca2111.1 (2)Cl1x—Ca2—O1—Ca2xvii119.1 (5)
Ca1—P1—O3—Ca2151.60 (16)O4xiii—Ca2—O1—Ca2xvii155.1 (4)
Ca2ix—P1—O3—Ca267.3 (2)P1xii—Ca2—O1—Ca2xvii26.9 (4)
Ca2xii—P1—O3—Ca266.68 (18)O2ix—Ca2—O1A—Ca2xvi180
O3viii—P1—O3—Ca2xiii6.70 (16)O3x—Ca2—O1A—Ca2xvi71.91 (5)
O4—P1—O3—Ca2xiii130.90 (10)O3—Ca2—O1A—Ca2xvi71.91 (5)
O2—P1—O3—Ca2xiii107.47 (10)O3xi—Ca2—O1A—Ca2xvi150.54 (4)
Ca1viii—P1—O3—Ca2xiii97.82 (7)O3xii—Ca2—O1A—Ca2xvi150.54 (4)
Ca1—P1—O3—Ca2xiii57.36 (8)O1x—Ca2—O1A—Ca2xvi90
Ca2ix—P1—O3—Ca2xiii141.67 (5)O1—Ca2—O1A—Ca2xvi90
Ca2xii—P1—O3—Ca2xiii84.37 (6)Cl1—Ca2—O1A—Ca2xvi90
O3viii—P1—O3—Ca1viii104.52 (12)Cl1x—Ca2—O1A—Ca2xvi90
O4—P1—O3—Ca1viii131.28 (9)O4xiii—Ca2—O1A—Ca2xvi0
O2—P1—O3—Ca1viii9.65 (10)P1xii—Ca2—O1A—Ca2xvi180
Ca2xiii—P1—O3—Ca1viii97.82 (7)O2ix—Ca2—O1A—Ca2xvii0
Ca1—P1—O3—Ca1viii40.47 (7)O3x—Ca2—O1A—Ca2xvii108.09 (5)
Ca2ix—P1—O3—Ca1viii43.84 (8)O3—Ca2—O1A—Ca2xvii108.09 (5)
Ca2xii—P1—O3—Ca1viii177.81 (5)O3xi—Ca2—O1A—Ca2xvii29.46 (4)
O2ix—Ca2—O3—P132.3 (2)O3xii—Ca2—O1A—Ca2xvii29.46 (4)
O3x—Ca2—O3—P1114.42 (17)O1x—Ca2—O1A—Ca2xvii90
O1A—Ca2—O3—P1121.91 (19)O1—Ca2—O1A—Ca2xvii90
O3xi—Ca2—O3—P129.9 (3)Cl1—Ca2—O1A—Ca2xvii90
O3xii—Ca2—O3—P142.3 (2)Cl1x—Ca2—O1A—Ca2xvii90
O1x—Ca2—O3—P1116.2 (2)O4xiii—Ca2—O1A—Ca2xvii180
O1—Ca2—O3—P1128.6 (2)P1xii—Ca2—O1A—Ca2xvii0
Cl1—Ca2—O3—P1112.5 (2)
Symmetry codes: (i) xy, x, z+2; (ii) y, x+y+1, z+2; (iii) x+1, y+1, z+2; (iv) x+y, x+1, z; (v) y+1, xy+1, z; (vi) y+1, xy+1, z+3/2; (vii) x+y, x+1, z+3/2; (viii) x, y, z+3/2; (ix) x+1, y+1, z+1; (x) x, y, z+1/2; (xi) xy+1, x, z1/2; (xii) xy+1, x, z+1; (xiii) y, x+y+1, z+1; (xiv) x+1, y+1, z1/2; (xv) x+2, y+2, z+1; (xvi) x+y+1, x+2, z; (xvii) y+2, xy+1, z; (xviii) x+2, y+2, z.
(1400r) top
Crystal data top
3(O4P)·0.54(Cl)·0.46(OH)·5(Ca)Dx = 3.164 Mg m3
Mr = 512.32Mo Kα radiation, λ = 0.7107 Å
Trigonal, P63/mCell parameters from 1183 reflections
Hall symbol: -P 6cθ = 2.5–26.1°
a = 9.5439 (2) ŵ = 3.14 mm1
c = 6.8174 (3) ÅT = 293 K
V = 537.78 (3) Å3Prism, colourless
Z = 20.23 × 0.09 × 0.07 mm
F(000) = 508.8
Data collection top
BRUKER APPEX-II CCD
diffractometer
402 independent reflections
Radiation source: fine-focus sealed tube367 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.031
ω and phi scansθmax = 26.4°, θmin = 2.5°
Absorption correction: multi-scan
BRUKER SADABS
h = 1111
Tmin = 0.343, Tmax = 0.430k = 1111
2996 measured reflectionsl = 88
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.028Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.069H atoms treated by a mixture of independent and constrained refinement
S = 1.20 w = 1/[σ2(Fo2) + (0.0285P)2 + 1.0863P]
where P = (Fo2 + 2Fc2)/3
402 reflections(Δ/σ)max < 0.001
46 parametersΔρmax = 0.74 e Å3
14 restraintsΔρmin = 0.54 e Å3
Crystal data top
3(O4P)·0.54(Cl)·0.46(OH)·5(Ca)Z = 2
Mr = 512.32Mo Kα radiation
Trigonal, P63/mµ = 3.14 mm1
a = 9.5439 (2) ÅT = 293 K
c = 6.8174 (3) Å0.23 × 0.09 × 0.07 mm
V = 537.78 (3) Å3
Data collection top
BRUKER APPEX-II CCD
diffractometer
402 independent reflections
Absorption correction: multi-scan
BRUKER SADABS
367 reflections with I > 2σ(I)
Tmin = 0.343, Tmax = 0.430Rint = 0.031
2996 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.02814 restraints
wR(F2) = 0.069H atoms treated by a mixture of independent and constrained refinement
S = 1.20Δρmax = 0.74 e Å3
402 reflectionsΔρmin = 0.54 e Å3
46 parameters
Special details top

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ca10.66670.33330.99736 (14)0.0117 (3)
Ca20.74331 (11)0.74629 (10)0.250.0163 (3)
P10.59691 (11)0.62804 (11)0.750.0078 (3)
O20.4102 (3)0.5343 (4)0.750.0202 (7)
O30.6487 (3)0.7356 (3)0.5687 (3)0.0272 (6)
O40.6640 (4)0.5117 (3)0.750.0139 (6)
Cl1110.4608 (18)0.032 (4)0.27
O1110.135 (3)0.031 (5)0.15
H11100.038*0.3
O1A110.250.031 (5)0.16
H1A110.106 (3)0.037*0.08
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0143 (4)0.0143 (4)0.0064 (5)0.00716 (18)00
Ca20.0243 (5)0.0214 (5)0.0093 (4)0.0159 (4)00
P10.0100 (5)0.0086 (5)0.0068 (5)0.0061 (4)00
O20.0107 (14)0.0172 (15)0.0345 (18)0.0082 (12)00
O30.0492 (15)0.0237 (12)0.0214 (12)0.0278 (11)0.0203 (12)0.0136 (10)
O40.0195 (14)0.0153 (14)0.0131 (14)0.0135 (12)00
Cl10.0158 (10)0.0158 (10)0.065 (14)0.0079 (5)00
O10.015 (3)0.015 (3)0.065 (15)0.0073 (13)00
O1A0.0145 (19)0.0145 (19)0.064 (14)0.0073 (10)00
Geometric parameters (Å, º) top
Ca1—O4i2.406 (2)P1—O41.534 (3)
Ca1—O4ii2.406 (2)P1—O21.543 (3)
Ca1—O42.406 (2)P1—Ca2xiii3.1202 (13)
Ca1—O2iii2.455 (2)P1—Ca1xv3.2184 (9)
Ca1—O2iv2.455 (2)P1—Ca1v3.2184 (9)
Ca1—O2v2.455 (2)P1—Ca2xi3.4045 (12)
Ca1—O3vi2.784 (3)P1—Ca2ix3.4214 (13)
Ca1—O3vii2.784 (3)O2—Ca2ix2.322 (3)
Ca1—O3viii2.784 (3)O2—Ca1xv2.455 (2)
Ca1—P1iii3.2184 (9)O2—Ca1v2.455 (2)
Ca1—P1iv3.2184 (9)O3—Ca2xiii2.555 (2)
Ca1—P1v3.2184 (9)O3—Ca1xv2.784 (3)
Ca2—O2ix2.322 (3)O4—Ca1xiv2.406 (2)
Ca2—O3x2.336 (2)O4—Ca2xi2.822 (3)
Ca2—O32.336 (2)Cl1—Cl1xvi0.53 (2)
Ca2—O1A2.4358 (9)Cl1—Ca2xvii2.828 (6)
Ca2—O3xi2.555 (2)Cl1—Ca2xviii2.828 (6)
Ca2—O3xii2.555 (2)Cl1—Ca2xvi3.134 (8)
Ca2—O1x2.559 (6)Cl1—Ca2xi3.134 (8)
Ca2—O12.559 (6)Cl1—Ca2xiii3.134 (8)
Ca2—O4xiii2.822 (3)O1—O1x1.57 (4)
Ca2—Cl12.828 (6)O1—O1xix1.84 (4)
Ca2—Cl1x2.828 (6)O1—Ca2xvii2.559 (6)
Ca2—P1xi3.1202 (12)O1—Ca2xviii2.559 (6)
P1—O3xiv1.522 (2)O1A—Ca2xvii2.4357 (9)
P1—O31.522 (2)O1A—Ca2xviii2.4358 (9)
O4i—Ca1—O4ii76.28 (7)O4xiii—Ca2—Cl1101.42 (6)
O4i—Ca1—O476.28 (7)O2ix—Ca2—Cl1x139.83 (16)
O4ii—Ca1—O476.28 (7)O3x—Ca2—Cl1x73.4 (2)
O4i—Ca1—O2iii90.91 (7)O3—Ca2—Cl1x131.3 (2)
O4ii—Ca1—O2iii152.15 (9)O1A—Ca2—Cl1x30.5 (2)
O4—Ca1—O2iii125.13 (9)O3xi—Ca2—Cl1x97.01 (12)
O4i—Ca1—O2iv125.13 (9)O3xii—Ca2—Cl1x68.31 (10)
O4ii—Ca1—O2iv90.91 (7)O1x—Ca2—Cl1x48.4 (5)
O4—Ca1—O2iv152.15 (10)O1—Ca2—Cl1x12.7 (4)
O2iii—Ca1—O2iv76.21 (8)O4xiii—Ca2—Cl1x101.42 (6)
O4i—Ca1—O2v152.15 (10)Cl1—Ca2—Cl1x61.1 (4)
O4ii—Ca1—O2v125.13 (9)O2ix—Ca2—P1xi69.80 (7)
O4—Ca1—O2v90.91 (7)O3x—Ca2—P1xi108.66 (6)
O2iii—Ca1—O2v76.21 (8)O3—Ca2—P1xi108.66 (6)
O2iv—Ca1—O2v76.21 (8)O1A—Ca2—P1xi82.73 (3)
O4i—Ca1—O3vi70.10 (8)O3xi—Ca2—P1xi29.00 (5)
O4ii—Ca1—O3vi84.08 (8)O3xii—Ca2—P1xi29.00 (5)
O4—Ca1—O3vi144.21 (7)O1x—Ca2—P1xi83.08 (3)
O2iii—Ca1—O3vi68.23 (8)O1—Ca2—P1xi83.08 (3)
O2iv—Ca1—O3vi55.47 (8)O4xiii—Ca2—P1xi173.98 (6)
O2v—Ca1—O3vi124.74 (7)Cl1—Ca2—P1xi83.74 (3)
O4i—Ca1—O3vii84.08 (8)Cl1x—Ca2—P1xi83.74 (3)
O4ii—Ca1—O3vii144.21 (7)O3xiv—P1—O3108.52 (19)
O4—Ca1—O3vii70.10 (8)O3xiv—P1—O4112.07 (10)
O2iii—Ca1—O3vii55.47 (8)O3—P1—O4112.07 (10)
O2iv—Ca1—O3vii124.74 (8)O3xiv—P1—O2106.41 (12)
O2v—Ca1—O3vii68.23 (9)O3—P1—O2106.41 (12)
O3vi—Ca1—O3vii117.01 (3)O4—P1—O2111.04 (16)
O4i—Ca1—O3viii144.21 (7)O3xiv—P1—Ca2xiii54.45 (9)
O4ii—Ca1—O3viii70.10 (8)O3—P1—Ca2xiii54.45 (9)
O4—Ca1—O3viii84.08 (8)O4—P1—Ca2xiii135.51 (12)
O2iii—Ca1—O3viii124.74 (7)O2—P1—Ca2xiii113.45 (12)
O2iv—Ca1—O3viii68.23 (8)O3xiv—P1—Ca1xv111.48 (9)
O2v—Ca1—O3viii55.47 (8)O3—P1—Ca1xv59.82 (10)
O3vi—Ca1—O3viii117.01 (3)O4—P1—Ca1xv135.71 (8)
O3vii—Ca1—O3viii117.01 (3)O2—P1—Ca1xv47.49 (8)
O4i—Ca1—P1iii90.49 (6)Ca2xiii—P1—Ca1xv78.68 (2)
O4ii—Ca1—P1iii166.52 (6)O3xiv—P1—Ca1v59.82 (10)
O4—Ca1—P1iii98.31 (6)O3—P1—Ca1v111.48 (9)
O2iii—Ca1—P1iii27.61 (7)O4—P1—Ca1v135.71 (8)
O2iv—Ca1—P1iii98.97 (6)O2—P1—Ca1v47.49 (8)
O2v—Ca1—P1iii66.66 (7)Ca2xiii—P1—Ca1v78.68 (2)
O3vi—Ca1—P1iii93.95 (5)Ca1xv—P1—Ca1v64.71 (3)
O3vii—Ca1—P1iii28.22 (5)O3xiv—P1—Ca2xi81.28 (11)
O3viii—Ca1—P1iii122.12 (5)O3—P1—Ca2xi81.28 (11)
O4i—Ca1—P1iv98.31 (6)O4—P1—Ca2xi55.07 (11)
O4ii—Ca1—P1iv90.49 (6)O2—P1—Ca2xi166.11 (12)
O4—Ca1—P1iv166.52 (6)Ca2xiii—P1—Ca2xi80.44 (4)
O2iii—Ca1—P1iv66.66 (7)Ca1xv—P1—Ca2xi141.04 (2)
O2iv—Ca1—P1iv27.61 (7)Ca1v—P1—Ca2xi141.04 (2)
O2v—Ca1—P1iv98.97 (6)O3xiv—P1—Ca2ix121.52 (11)
O3vi—Ca1—P1iv28.22 (5)O3—P1—Ca2ix121.52 (11)
O3vii—Ca1—P1iv122.12 (5)O4—P1—Ca2ix76.45 (12)
O3viii—Ca1—P1iv93.95 (5)Ca2xiii—P1—Ca2ix148.04 (4)
P1iii—Ca1—P1iv94.04 (2)Ca1xv—P1—Ca2ix74.43 (2)
O4i—Ca1—P1v166.52 (6)Ca1v—P1—Ca2ix74.43 (2)
O4ii—Ca1—P1v98.31 (6)Ca2xi—P1—Ca2ix131.52 (4)
O4—Ca1—P1v90.49 (6)P1—O2—Ca2ix123.25 (16)
O2iii—Ca1—P1v98.97 (6)P1—O2—Ca1xv104.90 (11)
O2iv—Ca1—P1v66.66 (7)Ca2ix—O2—Ca1xv114.51 (9)
O2v—Ca1—P1v27.61 (7)P1—O2—Ca1v104.90 (11)
O3vi—Ca1—P1v122.12 (5)Ca2ix—O2—Ca1v114.51 (9)
O3vii—Ca1—P1v93.95 (5)Ca1xv—O2—Ca1v89.11 (10)
O3viii—Ca1—P1v28.22 (5)P1—O3—Ca2140.60 (12)
P1iii—Ca1—P1v94.04 (2)P1—O3—Ca2xiii96.56 (11)
P1iv—Ca1—P1v94.04 (2)Ca2—O3—Ca2xiii117.80 (9)
O2ix—Ca2—O3x86.70 (7)P1—O3—Ca1xv91.96 (12)
O2ix—Ca2—O386.70 (7)Ca2—O3—Ca1xv101.32 (10)
O3x—Ca2—O3136.99 (14)Ca2xiii—O3—Ca1xv97.56 (7)
O2ix—Ca2—O1A152.53 (8)P1—O4—Ca1xiv131.94 (7)
O3x—Ca2—O1A102.59 (7)P1—O4—Ca1131.94 (7)
O3—Ca2—O1A102.59 (7)Ca1xiv—O4—Ca189.02 (9)
O2ix—Ca2—O3xi74.29 (8)P1—O4—Ca2xi98.47 (13)
O3x—Ca2—O3xi137.37 (9)Ca1xiv—O4—Ca2xi98.50 (8)
O3—Ca2—O3xi80.55 (5)Ca1—O4—Ca2xi98.50 (8)
O1A—Ca2—O3xi81.74 (6)Cl1xvi—Cl1—Ca2120.5 (2)
O2ix—Ca2—O3xii74.29 (8)Cl1xvi—Cl1—Ca2xvii120.5 (2)
O3x—Ca2—O3xii80.55 (5)Ca2—Cl1—Ca2xvii96.5 (3)
O3—Ca2—O3xii137.37 (9)Cl1xvi—Cl1—Ca2xviii120.5 (2)
O1A—Ca2—O3xii81.74 (6)Ca2—Cl1—Ca2xviii96.5 (3)
O3xi—Ca2—O3xii57.84 (10)Ca2xvii—Cl1—Ca2xviii96.5 (3)
O2ix—Ca2—O1x147.6 (2)Cl1xvi—Cl1—Ca2xvi51.02 (16)
O3x—Ca2—O1x119.5 (4)Ca2—Cl1—Ca2xvi171.6 (4)
O3—Ca2—O1x85.6 (4)Ca2xvii—Cl1—Ca2xvi89.14 (4)
O1A—Ca2—O1x17.8 (4)Ca2xviii—Cl1—Ca2xvi89.14 (4)
O3xi—Ca2—O1x73.45 (19)Cl1xvi—Cl1—Ca2xi51.02 (17)
O3xii—Ca2—O1x90.6 (2)Ca2—Cl1—Ca2xi89.14 (4)
O2ix—Ca2—O1147.6 (2)Ca2xvii—Cl1—Ca2xi89.14 (4)
O3x—Ca2—O185.6 (4)Ca2xviii—Cl1—Ca2xi171.6 (4)
O3—Ca2—O1119.5 (4)Ca2xvi—Cl1—Ca2xi84.6 (3)
O1A—Ca2—O117.8 (4)Cl1xvi—Cl1—Ca2xiii51.02 (18)
O3xi—Ca2—O190.6 (2)Ca2—Cl1—Ca2xiii89.14 (4)
O3xii—Ca2—O173.45 (19)Ca2xvii—Cl1—Ca2xiii171.6 (4)
O1x—Ca2—O135.7 (8)Ca2xviii—Cl1—Ca2xiii89.14 (4)
O2ix—Ca2—O4xiii104.18 (9)Ca2xvi—Cl1—Ca2xiii84.6 (3)
O3x—Ca2—O4xiii70.31 (6)Ca2xi—Cl1—Ca2xiii84.6 (3)
O3—Ca2—O4xiii70.31 (6)O1x—O1—O1xix180.000 (12)
O1A—Ca2—O4xiii103.29 (6)O1x—O1—Ca2xvii72.2 (4)
O3xi—Ca2—O4xiii150.85 (5)O1xix—O1—Ca2xvii107.8 (4)
O3xii—Ca2—O4xiii150.85 (5)O1x—O1—Ca272.2 (4)
O1x—Ca2—O4xiii102.64 (7)O1xix—O1—Ca2107.8 (4)
O1—Ca2—O4xiii102.64 (7)Ca2xvii—O1—Ca2111.1 (4)
O2ix—Ca2—Cl1139.83 (16)O1x—O1—Ca2xviii72.2 (4)
O3x—Ca2—Cl1131.3 (2)O1xix—O1—Ca2xviii107.8 (4)
O3—Ca2—Cl173.4 (2)Ca2xvii—O1—Ca2xviii111.1 (4)
O1A—Ca2—Cl130.5 (2)Ca2—O1—Ca2xviii111.1 (4)
O3xi—Ca2—Cl168.31 (10)Ca2—O1A—Ca2xvii120
O3xii—Ca2—Cl197.01 (12)Ca2—O1A—Ca2xviii120
O1x—Ca2—Cl112.7 (4)Ca2xvii—O1A—Ca2xviii120
O1—Ca2—Cl148.4 (5)
O3xiv—P1—O2—Ca2ix122.20 (10)O3vi—Ca1—O4—Ca2xi79.27 (13)
O3—P1—O2—Ca2ix122.20 (10)O3vii—Ca1—O4—Ca2xi29.62 (6)
O4—P1—O2—Ca2ix0O3viii—Ca1—O4—Ca2xi151.16 (7)
Ca2xiii—P1—O2—Ca2ix180P1iii—Ca1—O4—Ca2xi29.49 (6)
Ca1xv—P1—O2—Ca2ix133.45 (7)P1iv—Ca1—O4—Ca2xi126.6 (3)
Ca1v—P1—O2—Ca2ix133.45 (7)P1v—Ca1—O4—Ca2xi123.64 (5)
Ca2xi—P1—O2—Ca2ix0O2ix—Ca2—Cl1—Cl1xvi45.7 (2)
O3xiv—P1—O2—Ca1xv104.34 (10)O3x—Ca2—Cl1—Cl1xvi156.88 (11)
O3—P1—O2—Ca1xv11.25 (14)O3—Ca2—Cl1—Cl1xvi17.91 (6)
O4—P1—O2—Ca1xv133.45 (7)O1A—Ca2—Cl1—Cl1xvi180.000 (2)
Ca2xiii—P1—O2—Ca1xv46.55 (7)O3xi—Ca2—Cl1—Cl1xvi68.31 (10)
Ca1v—P1—O2—Ca1xv93.10 (15)O3xii—Ca2—Cl1—Cl1xvi119.55 (6)
Ca2xi—P1—O2—Ca1xv133.45 (7)O1x—Ca2—Cl1—Cl1xvi180
Ca2ix—P1—O2—Ca1xv133.45 (7)O1—Ca2—Cl1—Cl1xvi180.000 (4)
O3xiv—P1—O2—Ca1v11.25 (14)O4xiii—Ca2—Cl1—Cl1xvi83.15 (6)
O3—P1—O2—Ca1v104.34 (10)Cl1x—Ca2—Cl1—Cl1xvi180.000 (3)
O4—P1—O2—Ca1v133.45 (7)P1xi—Ca2—Cl1—Cl1xvi93.71 (3)
Ca2xiii—P1—O2—Ca1v46.55 (7)O2ix—Ca2—Cl1—Ca2xvii85.7 (4)
Ca1xv—P1—O2—Ca1v93.10 (15)O3x—Ca2—Cl1—Ca2xvii71.76 (13)
Ca2xi—P1—O2—Ca1v133.45 (7)O3—Ca2—Cl1—Ca2xvii149.3 (2)
Ca2ix—P1—O2—Ca1v133.45 (7)O1A—Ca2—Cl1—Ca2xvii48.64 (18)
O3xiv—P1—O3—Ca2144.86 (14)O3xi—Ca2—Cl1—Ca2xvii63.05 (12)
O4—P1—O3—Ca220.6 (3)O3xii—Ca2—Cl1—Ca2xvii11.8 (2)
O2—P1—O3—Ca2101.0 (3)O1x—Ca2—Cl1—Ca2xvii48.64 (18)
Ca2xiii—P1—O3—Ca2151.6 (3)O1—Ca2—Cl1—Ca2xvii48.64 (18)
Ca1xv—P1—O3—Ca2110.6 (3)O4xiii—Ca2—Cl1—Ca2xvii145.49 (14)
Ca1v—P1—O3—Ca2151.1 (2)Cl1x—Ca2—Cl1—Ca2xvii48.64 (18)
Ca2xi—P1—O3—Ca267.2 (2)P1xi—Ca2—Cl1—Ca2xvii37.65 (16)
Ca2ix—P1—O3—Ca266.7 (3)O2ix—Ca2—Cl1—Ca2xviii177.01 (10)
O3xiv—P1—O3—Ca2xiii6.7 (2)O3x—Ca2—Cl1—Ca2xviii25.5 (3)
O4—P1—O3—Ca2xiii131.03 (12)O3—Ca2—Cl1—Ca2xviii113.45 (17)
O2—P1—O3—Ca2xiii107.42 (13)O1A—Ca2—Cl1—Ca2xviii48.64 (18)
Ca1xv—P1—O3—Ca2xiii97.85 (8)O3xi—Ca2—Cl1—Ca2xviii160.3 (3)
Ca1v—P1—O3—Ca2xiii57.29 (11)O3xii—Ca2—Cl1—Ca2xviii109.09 (16)
Ca2xi—P1—O3—Ca2xiii84.44 (8)O1x—Ca2—Cl1—Ca2xviii48.64 (18)
Ca2ix—P1—O3—Ca2xiii141.72 (6)O1—Ca2—Cl1—Ca2xviii48.64 (18)
O3xiv—P1—O3—Ca1xv104.59 (15)O4xiii—Ca2—Cl1—Ca2xviii48.2 (2)
O4—P1—O3—Ca1xv131.12 (12)Cl1x—Ca2—Cl1—Ca2xviii48.64 (18)
O2—P1—O3—Ca1xv9.57 (12)P1xi—Ca2—Cl1—Ca2xviii134.9 (2)
Ca2xiii—P1—O3—Ca1xv97.85 (8)O2ix—Ca2—Cl1—Ca2xi3.3 (3)
Ca1v—P1—O3—Ca1xv40.56 (9)O3x—Ca2—Cl1—Ca2xi160.80 (10)
Ca2xi—P1—O3—Ca1xv177.72 (6)O3—Ca2—Cl1—Ca2xi60.23 (16)
Ca2ix—P1—O3—Ca1xv43.87 (10)O1A—Ca2—Cl1—Ca2xi137.68 (13)
O2ix—Ca2—O3—P131.9 (3)O3xi—Ca2—Cl1—Ca2xi25.99 (8)
O3x—Ca2—O3—P1113.5 (2)O3xii—Ca2—Cl1—Ca2xi77.23 (16)
O1A—Ca2—O3—P1122.0 (2)O1x—Ca2—Cl1—Ca2xi137.68 (13)
O3xi—Ca2—O3—P142.7 (3)O1—Ca2—Cl1—Ca2xi137.68 (13)
O3xii—Ca2—O3—P130.5 (4)O4xiii—Ca2—Cl1—Ca2xi125.47 (9)
O1x—Ca2—O3—P1116.6 (3)Cl1x—Ca2—Cl1—Ca2xi137.68 (13)
O1—Ca2—O3—P1128.1 (3)P1xi—Ca2—Cl1—Ca2xi51.39 (10)
O4xiii—Ca2—O3—P1138.2 (3)O2ix—Ca2—Cl1—Ca2xiii87.97 (11)
Cl1—Ca2—O3—P1112.8 (3)O3x—Ca2—Cl1—Ca2xiii114.6 (2)
Cl1x—Ca2—O3—P1133.8 (2)O3—Ca2—Cl1—Ca2xiii24.41 (12)
P1xi—Ca2—O3—P135.5 (3)O1A—Ca2—Cl1—Ca2xiii137.68 (13)
O2ix—Ca2—O3—Ca2xiii179.60 (12)O3xi—Ca2—Cl1—Ca2xiii110.6 (2)
O3x—Ca2—O3—Ca2xiii98.80 (19)O3xii—Ca2—Cl1—Ca2xiii161.87 (12)
O1A—Ca2—O3—Ca2xiii25.74 (12)O1x—Ca2—Cl1—Ca2xiii137.68 (13)
O3xi—Ca2—O3—Ca2xiii104.99 (6)O1—Ca2—Cl1—Ca2xiii137.68 (13)
O3xii—Ca2—O3—Ca2xiii117.19 (7)O4xiii—Ca2—Cl1—Ca2xiii40.84 (17)
O1x—Ca2—O3—Ca2xiii31.06 (16)Cl1x—Ca2—Cl1—Ca2xiii137.68 (13)
O1—Ca2—O3—Ca2xiii19.6 (2)P1xi—Ca2—Cl1—Ca2xiii136.03 (15)
O4xiii—Ca2—O3—Ca2xiii74.06 (11)O2ix—Ca2—O1—O1x120.5 (6)
Cl1—Ca2—O3—Ca2xiii34.95 (12)O3x—Ca2—O1—O1x162.81 (6)
Cl1x—Ca2—O3—Ca2xiii13.94 (19)O3—Ca2—O1—O1x19.79 (10)
P1xi—Ca2—O3—Ca2xiii112.22 (9)O1A—Ca2—O1—O1x0.000 (5)
O2ix—Ca2—O3—Ca1xv75.49 (8)O3xi—Ca2—O1—O1x59.71 (5)
O3x—Ca2—O3—Ca1xv6.11 (19)O3xii—Ca2—O1—O1x115.75 (12)
O1A—Ca2—O3—Ca1xv130.65 (5)O4xiii—Ca2—O1—O1x94.14 (9)
O3xi—Ca2—O3—Ca1xv150.09 (7)Cl1—Ca2—O1—O1x0.000 (3)
O3xii—Ca2—O3—Ca1xv137.90 (14)Cl1x—Ca2—O1—O1x180.000 (6)
O1x—Ca2—O3—Ca1xv135.97 (13)P1xi—Ca2—O1—O1x87.76 (5)
O1—Ca2—O3—Ca1xv124.55 (17)O2ix—Ca2—O1—O1xix59.5 (6)
O4xiii—Ca2—O3—Ca1xv30.85 (7)O3x—Ca2—O1—O1xix17.19 (6)
Cl1—Ca2—O3—Ca1xv139.86 (9)O3—Ca2—O1—O1xix160.21 (10)
Cl1x—Ca2—O3—Ca1xv118.85 (13)O1A—Ca2—O1—O1xix180.000 (5)
P1xi—Ca2—O3—Ca1xv142.87 (5)O3xi—Ca2—O1—O1xix120.29 (5)
O3xiv—P1—O4—Ca1xiv170.69 (18)O3xii—Ca2—O1—O1xix64.25 (12)
O3—P1—O4—Ca1xiv48.4 (3)O1x—Ca2—O1—O1xix180.000 (3)
O2—P1—O4—Ca1xiv70.45 (18)O4xiii—Ca2—O1—O1xix85.86 (9)
Ca2xiii—P1—O4—Ca1xiv109.55 (18)Cl1—Ca2—O1—O1xix180.000 (3)
Ca1xv—P1—O4—Ca1xiv20.4 (3)Cl1x—Ca2—O1—O1xix0.000 (6)
Ca1v—P1—O4—Ca1xiv120.48 (10)P1xi—Ca2—O1—O1xix92.24 (5)
Ca2xi—P1—O4—Ca1xiv109.55 (18)O2ix—Ca2—O1—Ca2xvii58.4 (11)
Ca2ix—P1—O4—Ca1xiv70.45 (18)O3x—Ca2—O1—Ca2xvii135.1 (5)
O3xiv—P1—O4—Ca148.4 (3)O3—Ca2—O1—Ca2xvii81.9 (4)
O3—P1—O4—Ca1170.69 (18)O1A—Ca2—O1—Ca2xvii62.1 (5)
O2—P1—O4—Ca170.45 (18)O3xi—Ca2—O1—Ca2xvii2.4 (5)
Ca2xiii—P1—O4—Ca1109.55 (18)O3xii—Ca2—O1—Ca2xvii53.7 (4)
Ca1xv—P1—O4—Ca1120.48 (10)O1x—Ca2—O1—Ca2xvii62.1 (5)
Ca1v—P1—O4—Ca120.4 (3)O4xiii—Ca2—O1—Ca2xvii156.2 (4)
Ca2xi—P1—O4—Ca1109.55 (18)Cl1—Ca2—O1—Ca2xvii62.1 (5)
Ca2ix—P1—O4—Ca170.45 (18)Cl1x—Ca2—O1—Ca2xvii117.9 (5)
O3xiv—P1—O4—Ca2xi61.15 (13)P1xi—Ca2—O1—Ca2xvii25.7 (5)
O3—P1—O4—Ca2xi61.15 (13)O2ix—Ca2—O1—Ca2xviii177.45 (9)
O2—P1—O4—Ca2xi180O3x—Ca2—O1—Ca2xviii100.7 (5)
Ca2xiii—P1—O4—Ca2xi0O3—Ca2—O1—Ca2xviii42.3 (6)
Ca1xv—P1—O4—Ca2xi129.97 (10)O1A—Ca2—O1—Ca2xviii62.1 (5)
Ca1v—P1—O4—Ca2xi129.97 (10)O3xi—Ca2—O1—Ca2xviii121.8 (5)
Ca2ix—P1—O4—Ca2xi180O3xii—Ca2—O1—Ca2xviii177.8 (6)
O4i—Ca1—O4—P1168.5 (3)O1x—Ca2—O1—Ca2xviii62.1 (5)
O4ii—Ca1—O4—P1112.5 (3)O4xiii—Ca2—O1—Ca2xviii32.1 (6)
O2iii—Ca1—O4—P187.2 (2)Cl1—Ca2—O1—Ca2xviii62.1 (5)
O2iv—Ca1—O4—P147.8 (3)Cl1x—Ca2—O1—Ca2xviii117.9 (5)
O2v—Ca1—O4—P113.5 (2)P1xi—Ca2—O1—Ca2xviii149.8 (6)
O3vi—Ca1—O4—P1171.19 (14)O2ix—Ca2—O1A—Ca2xvii0
O3vii—Ca1—O4—P179.9 (2)O3x—Ca2—O1A—Ca2xvii107.58 (6)
O3viii—Ca1—O4—P141.6 (2)O3—Ca2—O1A—Ca2xvii107.58 (6)
P1iii—Ca1—O4—P180.0 (2)O3xi—Ca2—O1A—Ca2xvii29.25 (5)
P1iv—Ca1—O4—P1123.8 (2)O3xii—Ca2—O1A—Ca2xvii29.25 (5)
P1v—Ca1—O4—P114.1 (2)O1x—Ca2—O1A—Ca2xvii90
O4i—Ca1—O4—Ca1xiv39.47 (11)O1—Ca2—O1A—Ca2xvii90
O4ii—Ca1—O4—Ca1xiv39.47 (11)O4xiii—Ca2—O1A—Ca2xvii180
O2iii—Ca1—O4—Ca1xiv120.75 (9)Cl1—Ca2—O1A—Ca2xvii90
O2iv—Ca1—O4—Ca1xiv104.21 (15)Cl1x—Ca2—O1A—Ca2xvii90
O2v—Ca1—O4—Ca1xiv165.52 (9)P1xi—Ca2—O1A—Ca2xvii0
O3vi—Ca1—O4—Ca1xiv19.18 (18)O2ix—Ca2—O1A—Ca2xviii180
O3vii—Ca1—O4—Ca1xiv128.07 (10)O3x—Ca2—O1A—Ca2xviii72.42 (6)
O3viii—Ca1—O4—Ca1xiv110.39 (8)O3—Ca2—O1A—Ca2xviii72.42 (6)
P1iii—Ca1—O4—Ca1xiv127.94 (7)O3xi—Ca2—O1A—Ca2xviii150.75 (5)
P1iv—Ca1—O4—Ca1xiv28.2 (3)O3xii—Ca2—O1A—Ca2xviii150.75 (5)
P1v—Ca1—O4—Ca1xiv137.91 (7)O1x—Ca2—O1A—Ca2xviii90
O4i—Ca1—O4—Ca2xi58.97 (10)O1—Ca2—O1A—Ca2xviii90
O4ii—Ca1—O4—Ca2xi137.92 (8)O4xiii—Ca2—O1A—Ca2xviii0
O2iii—Ca1—O4—Ca2xi22.30 (11)Cl1—Ca2—O1A—Ca2xviii90
O2iv—Ca1—O4—Ca2xi157.35 (13)Cl1x—Ca2—O1A—Ca2xviii90
O2v—Ca1—O4—Ca2xi96.03 (8)P1xi—Ca2—O1A—Ca2xviii180
Symmetry codes: (i) x+y+1, x+1, z; (ii) y+1, xy, z; (iii) xy+1, x, z+2; (iv) y, x+y, z+2; (v) x+1, y+1, z+2; (vi) y, x+y, z+1/2; (vii) xy+1, x, z+1/2; (viii) x+1, y+1, z+1/2; (ix) x+1, y+1, z+1; (x) x, y, z+1/2; (xi) xy+1, x, z+1; (xii) xy+1, x, z1/2; (xiii) y, x+y+1, z+1; (xiv) x, y, z+3/2; (xv) x+1, y+1, z1/2; (xvi) x+2, y+2, z+1; (xvii) y+2, xy+1, z; (xviii) x+y+1, x+2, z; (xix) x+2, y+2, z.
(1450l) top
Crystal data top
3(O4P)·0.44(Cl)·0.56(OH)·5(Ca)Dx = 3.193 Mg m3
Mr = 510.42Mo Kα radiation, λ = 0.7107 Å
Trigonal, P63/mCell parameters from 2987 reflections
Hall symbol: -P 6cθ = 2.4–27.4°
a = 9.4815 (2) ŵ = 3.16 mm1
c = 6.8200 (3) ÅT = 100 K
V = 530.97 (3) Å3Prism, colourless
Z = 20.11 × 0.08 × 0.04 mm
F(000) = 507.2
Data collection top
BRUKER APPEX-II CCD
diffractometer
588 independent reflections
Radiation source: fine-focus sealed tube552 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.024
ω and phi scansθmax = 30.6°, θmin = 2.5°
Absorption correction: multi-scan
BRUKER SADABS
h = 1313
Tmin = 0.815, Tmax = 1k = 1313
2999 measured reflectionsl = 99
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.034Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.075H atoms treated by a mixture of independent and constrained refinement
S = 1.13 w = 1/[σ2(Fo2) + (0.0229P)2 + 2.4011P]
where P = (Fo2 + 2Fc2)/3
588 reflections(Δ/σ)max < 0.001
47 parametersΔρmax = 1.45 e Å3
15 restraintsΔρmin = 0.92 e Å3
Crystal data top
3(O4P)·0.44(Cl)·0.56(OH)·5(Ca)Z = 2
Mr = 510.42Mo Kα radiation
Trigonal, P63/mµ = 3.16 mm1
a = 9.4815 (2) ÅT = 100 K
c = 6.8200 (3) Å0.11 × 0.08 × 0.04 mm
V = 530.97 (3) Å3
Data collection top
BRUKER APPEX-II CCD
diffractometer
588 independent reflections
Absorption correction: multi-scan
BRUKER SADABS
552 reflections with I > 2σ(I)
Tmin = 0.815, Tmax = 1Rint = 0.024
2999 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03415 restraints
wR(F2) = 0.075H atoms treated by a mixture of independent and constrained refinement
S = 1.13Δρmax = 1.45 e Å3
588 reflectionsΔρmin = 0.92 e Å3
47 parameters
Special details top

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ca10.33330.66671.00217 (12)0.00778 (19)
Ca20.74372 (10)0.74879 (9)0.250.01253 (19)
P10.59806 (10)0.62892 (10)0.750.00514 (18)
O20.4105 (3)0.5338 (3)0.750.0182 (6)
O30.6484 (3)0.7363 (3)0.5680 (3)0.0241 (5)
O40.6671 (3)0.5130 (3)0.750.0082 (4)
Cl1110.4685 (9)0.0140.220 (4)
O1110.129 (3)0.017 (2)0.152 (8)
H11100.021*0.303 (16)
O1A110.250.0162 (15)0.257 (14)
H1A110.106 (3)0.019*0.129 (7)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0093 (2)0.0093 (2)0.0047 (4)0.00465 (12)00
Ca20.0203 (4)0.0175 (4)0.0061 (3)0.0142 (3)00
P10.0071 (4)0.0059 (4)0.0045 (4)0.0049 (3)00
O20.0081 (12)0.0131 (13)0.0356 (17)0.0069 (10)00
O30.0470 (14)0.0211 (10)0.0178 (10)0.0273 (10)0.0211 (10)0.0139 (8)
O40.0109 (11)0.0080 (11)0.0092 (11)0.0072 (9)00
Cl10.0080.0080.0260.00400
O10.011 (2)0.011 (2)0.029 (4)0.0057 (12)00
O1A0.0105 (17)0.0105 (17)0.028 (3)0.0052 (9)00
Geometric parameters (Å, º) top
Ca1—O4i2.3982 (18)P1—O41.535 (2)
Ca1—O4ii2.3982 (18)P1—O21.540 (3)
Ca1—O4iii2.3982 (18)P1—Ca2xiii3.1089 (11)
Ca1—O2iv2.450 (2)P1—Ca1viii3.2069 (8)
Ca1—O2v2.450 (2)P1—Ca2xi3.3539 (11)
Ca1—O22.450 (2)P1—Ca2ix3.4236 (11)
Ca1—O3vi2.760 (3)O2—Ca2ix2.323 (3)
Ca1—O3vii2.760 (3)O2—Ca1viii2.450 (2)
Ca1—O3viii2.760 (3)O3—Ca2xiii2.552 (2)
Ca1—P1v3.2069 (8)O3—Ca1viii2.760 (3)
Ca1—P1iv3.2069 (8)O4—Ca1xv2.3982 (18)
Ca1—P13.2069 (8)O4—Ca1iii2.3982 (18)
Ca2—O2ix2.323 (3)O4—Ca2xi2.766 (3)
Ca2—O3x2.330 (2)Cl1—Cl1xiv0.430 (12)
Ca2—O32.330 (2)Cl1—Ca2xvi2.830 (3)
Ca2—O1A2.4063 (8)Cl1—Ca2xvii2.830 (3)
Ca2—O1x2.543 (6)Cl1—Ca2xiv3.078 (4)
Ca2—O12.543 (6)Cl1—Ca2xi3.078 (4)
Ca2—O3xi2.552 (2)Cl1—Ca2xiii3.078 (4)
Ca2—O3xii2.552 (2)O1—O1x1.65 (4)
Ca2—O4xiii2.766 (3)O1—Ca2xvi2.543 (6)
Ca2—Cl12.830 (3)O1—Ca2xvii2.543 (6)
Ca2—Cl1x2.830 (3)O1—H10.881 (18)
Ca2—Cl1xiv3.078 (4)O1—H1A0.16 (3)
Ca2—H1A2.599 (8)O1A—Ca2xvi2.4063 (8)
P1—O3viii1.523 (2)O1A—Ca2xvii2.4063 (8)
P1—O31.523 (2)O1A—H1A0.98 (2)
O4i—Ca1—O4ii75.81 (6)O4xiii—Ca2—Cl1x102.07 (5)
O4i—Ca1—O4iii75.81 (6)Cl1—Ca2—Cl1x63.5 (2)
O4ii—Ca1—O4iii75.81 (6)O2ix—Ca2—Cl1xiv133.66 (8)
O4i—Ca1—O2iv91.39 (6)O3x—Ca2—Cl1xiv139.12 (10)
O4ii—Ca1—O2iv152.83 (9)O3—Ca2—Cl1xiv66.09 (11)
O4iii—Ca1—O2iv124.76 (8)O1A—Ca2—Cl1xiv38.59 (9)
O4i—Ca1—O2v124.76 (8)O1x—Ca2—Cl1xiv19.7 (4)
O4ii—Ca1—O2v91.39 (6)O1—Ca2—Cl1xiv57.5 (4)
O4iii—Ca1—O2v152.83 (9)O3xi—Ca2—Cl1xiv65.56 (6)
O2iv—Ca1—O2v76.17 (7)O3xii—Ca2—Cl1xiv101.12 (7)
O4i—Ca1—O2152.83 (9)O4xiii—Ca2—Cl1xiv101.08 (4)
O4ii—Ca1—O2124.76 (8)Cl1—Ca2—Cl1xiv6.8 (2)
O4iii—Ca1—O291.39 (6)Cl1x—Ca2—Cl1xiv70.35 (2)
O2iv—Ca1—O276.17 (7)O2ix—Ca2—H1A144.9 (3)
O2v—Ca1—O276.17 (7)O3x—Ca2—H1A81.7 (4)
O4i—Ca1—O3vi69.66 (7)O3—Ca2—H1A124.0 (4)
O4ii—Ca1—O3vi84.80 (7)O1A—Ca2—H1A22.2 (4)
O4iii—Ca1—O3vi143.61 (7)O1x—Ca2—H1A41.1 (6)
O2iv—Ca1—O3vi68.20 (8)O1—Ca2—H1A3.3 (6)
O2v—Ca1—O3vi55.62 (8)O3xi—Ca2—H1A93.0 (2)
O2—Ca1—O3vi124.80 (7)O3xii—Ca2—H1A71.66 (19)
O4i—Ca1—O3vii84.80 (8)O4xiii—Ca2—H1A103.16 (7)
O4ii—Ca1—O3vii143.61 (7)Cl1—Ca2—H1A54.0 (4)
O4iii—Ca1—O3vii69.66 (7)Cl1x—Ca2—H1A9.5 (4)
O2iv—Ca1—O3vii55.62 (8)Cl1xiv—Ca2—H1A60.8 (4)
O2v—Ca1—O3vii124.80 (7)O3viii—P1—O3109.18 (18)
O2—Ca1—O3vii68.20 (8)O3viii—P1—O4112.05 (9)
O3vi—Ca1—O3vii117.06 (3)O3—P1—O4112.05 (9)
O4i—Ca1—O3viii143.61 (7)O3viii—P1—O2106.01 (12)
O4ii—Ca1—O3viii69.66 (7)O3—P1—O2106.01 (12)
O4iii—Ca1—O3viii84.80 (7)O4—P1—O2111.18 (15)
O2iv—Ca1—O3viii124.80 (7)O3viii—P1—Ca2xiii54.71 (9)
O2v—Ca1—O3viii68.20 (8)O3—P1—Ca2xiii54.71 (9)
O2—Ca1—O3viii55.62 (8)O4—P1—Ca2xiii134.87 (11)
O3vi—Ca1—O3viii117.06 (3)O2—P1—Ca2xiii113.94 (11)
O3vii—Ca1—O3viii117.06 (3)O3viii—P1—Ca159.30 (10)
O4i—Ca1—P1v97.98 (6)O3—P1—Ca1111.33 (9)
O4ii—Ca1—P1v91.27 (5)O4—P1—Ca1135.86 (7)
O4iii—Ca1—P1v166.64 (5)O2—P1—Ca147.66 (7)
O2iv—Ca1—P1v66.50 (6)Ca2xiii—P1—Ca178.96 (2)
O2v—Ca1—P1v27.68 (6)O3viii—P1—Ca1viii111.33 (9)
O2—Ca1—P1v98.92 (6)O3—P1—Ca1viii59.30 (10)
O3vi—Ca1—P1v28.32 (4)O4—P1—Ca1viii135.86 (7)
O3vii—Ca1—P1v122.11 (5)O2—P1—Ca1viii47.66 (7)
O3viii—Ca1—P1v93.99 (5)Ca2xiii—P1—Ca1viii78.96 (2)
O4i—Ca1—P1iv91.27 (5)Ca1—P1—Ca1viii64.86 (3)
O4ii—Ca1—P1iv166.64 (5)O3viii—P1—Ca2xi81.79 (10)
O4iii—Ca1—P1iv97.98 (6)O3—P1—Ca2xi81.79 (10)
O2iv—Ca1—P1iv27.68 (6)O4—P1—Ca2xi54.66 (10)
O2v—Ca1—P1iv98.92 (6)O2—P1—Ca2xi165.84 (11)
O2—Ca1—P1iv66.50 (6)Ca2xiii—P1—Ca2xi80.22 (3)
O3vi—Ca1—P1iv93.99 (5)Ca1—P1—Ca2xi141.03 (2)
O3vii—Ca1—P1iv28.32 (4)Ca1viii—P1—Ca2xi141.03 (2)
O3viii—Ca1—P1iv122.11 (5)O3viii—P1—Ca2ix121.05 (11)
P1v—Ca1—P1iv93.93 (2)O3—P1—Ca2ix121.05 (11)
O4i—Ca1—P1166.64 (5)O4—P1—Ca2ix76.72 (10)
O4ii—Ca1—P197.98 (6)Ca2xiii—P1—Ca2ix148.40 (3)
O4iii—Ca1—P191.27 (5)Ca1—P1—Ca2ix74.48 (2)
O2iv—Ca1—P198.92 (6)Ca1viii—P1—Ca2ix74.48 (2)
O2v—Ca1—P166.50 (6)Ca2xi—P1—Ca2ix131.38 (3)
O2—Ca1—P127.68 (7)P1—O2—Ca2ix123.51 (15)
O3vi—Ca1—P1122.11 (5)P1—O2—Ca1104.66 (11)
O3vii—Ca1—P193.99 (5)Ca2ix—O2—Ca1114.54 (9)
O3viii—Ca1—P128.32 (4)P1—O2—Ca1viii104.66 (11)
P1v—Ca1—P193.93 (2)Ca2ix—O2—Ca1viii114.54 (9)
P1iv—Ca1—P193.93 (2)Ca1—O2—Ca1viii89.16 (9)
O2ix—Ca2—O3x86.38 (6)P1—O3—Ca2140.96 (12)
O2ix—Ca2—O386.38 (6)P1—O3—Ca2xiii96.15 (11)
O3x—Ca2—O3137.17 (13)Ca2—O3—Ca2xiii117.41 (9)
O2ix—Ca2—O1A152.04 (7)P1—O3—Ca1viii92.38 (11)
O3x—Ca2—O1A102.97 (7)Ca2—O3—Ca1viii101.34 (9)
O3—Ca2—O1A102.97 (7)Ca2xiii—O3—Ca1viii98.15 (7)
O2ix—Ca2—O1x146.7 (2)P1—O4—Ca1xv131.21 (7)
O3x—Ca2—O1x120.9 (4)P1—O4—Ca1iii131.21 (7)
O3—Ca2—O1x84.9 (4)Ca1xv—O4—Ca1iii89.62 (8)
O1A—Ca2—O1x18.9 (4)P1—O4—Ca2xi98.42 (12)
O2ix—Ca2—O1146.7 (2)Ca1xv—O4—Ca2xi99.43 (7)
O3x—Ca2—O184.9 (4)Ca1iii—O4—Ca2xi99.43 (7)
O3—Ca2—O1120.9 (4)Cl1xiv—Cl1—Ca2121.77 (11)
O1A—Ca2—O118.9 (4)Cl1xiv—Cl1—Ca2xvi121.77 (10)
O1x—Ca2—O137.8 (8)Ca2—Cl1—Ca2xvi94.83 (14)
O2ix—Ca2—O3xi73.77 (8)Cl1xiv—Cl1—Ca2xvii121.77 (11)
O3x—Ca2—O3xi137.11 (8)Ca2—Cl1—Ca2xvii94.83 (14)
O3—Ca2—O3xi80.06 (4)Ca2xvi—Cl1—Ca2xvii94.83 (14)
O1A—Ca2—O3xi81.88 (6)Cl1xiv—Cl1—Ca2xiv51.41 (8)
O1x—Ca2—O3xi73.08 (18)Ca2—Cl1—Ca2xiv173.2 (2)
O1—Ca2—O3xi91.4 (2)Ca2xvi—Cl1—Ca2xiv89.77 (2)
O2ix—Ca2—O3xii73.77 (8)Ca2xvii—Cl1—Ca2xiv89.77 (2)
O3x—Ca2—O3xii80.06 (4)Cl1xiv—Cl1—Ca2xi51.41 (9)
O3—Ca2—O3xii137.11 (8)Ca2—Cl1—Ca2xi89.77 (2)
O1A—Ca2—O3xii81.88 (6)Ca2xvi—Cl1—Ca2xi89.77 (2)
O1x—Ca2—O3xii91.4 (2)Ca2xvii—Cl1—Ca2xi173.2 (2)
O1—Ca2—O3xii73.08 (18)Ca2xiv—Cl1—Ca2xi85.21 (13)
O3xi—Ca2—O3xii58.18 (9)Cl1xiv—Cl1—Ca2xiii51.41 (10)
O2ix—Ca2—O4xiii103.73 (9)Ca2—Cl1—Ca2xiii89.77 (2)
O3x—Ca2—O4xiii70.47 (6)Ca2xvi—Cl1—Ca2xiii173.2 (2)
O3—Ca2—O4xiii70.47 (6)Ca2xvii—Cl1—Ca2xiii89.77 (2)
O1A—Ca2—O4xiii104.23 (6)Ca2xiv—Cl1—Ca2xiii85.21 (13)
O1x—Ca2—O4xiii103.45 (6)Ca2xi—Cl1—Ca2xiii85.21 (13)
O1—Ca2—O4xiii103.45 (6)O1x—O1—Ca2xvi71.1 (4)
O3xi—Ca2—O4xiii150.53 (5)O1x—O1—Ca271.1 (4)
O3xii—Ca2—O4xiii150.53 (5)Ca2xvi—O1—Ca2110.0 (4)
O2ix—Ca2—Cl1138.67 (9)O1x—O1—Ca2xvii71.1 (4)
O3x—Ca2—Cl1132.91 (12)Ca2xvi—O1—Ca2xvii110.0 (4)
O3—Ca2—Cl172.58 (12)Ca2—O1—Ca2xvii110.0 (4)
O1A—Ca2—Cl131.77 (11)O1x—O1—H1180.000 (4)
O1x—Ca2—Cl112.9 (4)Ca2xvi—O1—H1108.9 (4)
O1—Ca2—Cl150.7 (4)Ca2—O1—H1108.9 (4)
O3xi—Ca2—Cl167.91 (7)Ca2xvii—O1—H1108.9 (4)
O3xii—Ca2—Cl197.81 (8)O1x—O1—H1A180.00 (5)
O4xiii—Ca2—Cl1102.07 (5)Ca2xvi—O1—H1A108.9 (4)
O2ix—Ca2—Cl1x138.67 (9)Ca2—O1—H1A108.9 (4)
O3x—Ca2—Cl1x72.58 (12)Ca2xvii—O1—H1A108.9 (4)
O3—Ca2—Cl1x132.91 (12)Ca2—O1A—Ca2xvi120
O1A—Ca2—Cl1x31.77 (11)Ca2—O1A—Ca2xvii120
O1x—Ca2—Cl1x50.7 (4)Ca2xvi—O1A—Ca2xvii120
O1—Ca2—Cl1x12.9 (4)Ca2—O1A—H1A90.000 (8)
O3xi—Ca2—Cl1x97.81 (8)Ca2xvi—O1A—H1A90.000 (6)
O3xii—Ca2—Cl1x67.91 (7)Ca2xvii—O1A—H1A90.000 (2)
O4i—Ca1—P1—O3viii62.0 (3)O1A—Ca2—O3—P1120.5 (2)
O4ii—Ca1—P1—O3viii0.72 (11)O1x—Ca2—O3—P1115.0 (3)
O4iii—Ca1—P1—O3viii76.57 (11)O1—Ca2—O3—P1126.9 (3)
O2iv—Ca1—P1—O3viii157.92 (12)O3xi—Ca2—O3—P141.3 (3)
O2v—Ca1—P1—O3viii87.32 (11)O3xii—Ca2—O3—P128.5 (4)
O2—Ca1—P1—O3viii167.16 (14)O4xiii—Ca2—O3—P1138.8 (3)
O3vi—Ca1—P1—O3viii88.13 (5)Cl1—Ca2—O3—P1111.1 (3)
O3vii—Ca1—P1—O3viii146.27 (11)Cl1x—Ca2—O3—P1132.8 (2)
P1v—Ca1—P1—O3viii91.11 (10)Cl1xiv—Ca2—O3—P1108.9 (3)
P1iv—Ca1—P1—O3viii174.66 (10)O2ix—Ca2—O3—Ca2xiii179.04 (12)
O4i—Ca1—P1—O3162.3 (3)O3x—Ca2—O3—Ca2xiii100.24 (18)
O4ii—Ca1—P1—O3100.99 (12)O1A—Ca2—O3—Ca2xiii25.71 (11)
O4iii—Ca1—P1—O3176.85 (13)O1x—Ca2—O3—Ca2xiii31.22 (15)
O2iv—Ca1—P1—O357.65 (13)O1—Ca2—O3—Ca2xiii19.3 (2)
O2v—Ca1—P1—O312.96 (13)O3xi—Ca2—O3—Ca2xiii104.90 (6)
O2—Ca1—P1—O392.57 (15)O3xii—Ca2—O3—Ca2xiii117.71 (7)
O3vi—Ca1—P1—O312.15 (16)O4xiii—Ca2—O3—Ca2xiii75.01 (10)
O3vii—Ca1—P1—O3113.45 (12)Cl1—Ca2—O3—Ca2xiii35.09 (9)
O3viii—Ca1—P1—O3100.3 (2)Cl1x—Ca2—O3—Ca2xiii13.44 (17)
P1v—Ca1—P1—O39.16 (11)Cl1xiv—Ca2—O3—Ca2xiii37.34 (9)
P1iv—Ca1—P1—O385.06 (11)O2ix—Ca2—O3—Ca1viii75.48 (8)
O4i—Ca1—P1—O428.9 (2)O3x—Ca2—O3—Ca1viii5.24 (19)
O4ii—Ca1—P1—O490.15 (15)O1A—Ca2—O3—Ca1viii131.19 (5)
O4iii—Ca1—P1—O414.30 (17)O1x—Ca2—O3—Ca1viii136.70 (13)
O2iv—Ca1—P1—O4111.21 (13)O1—Ca2—O3—Ca1viii124.78 (16)
O2v—Ca1—P1—O4178.19 (13)O3xi—Ca2—O3—Ca1viii149.62 (7)
O2—Ca1—P1—O476.28 (16)O3xii—Ca2—O3—Ca1viii136.81 (14)
O3vi—Ca1—P1—O4179.00 (13)O4xiii—Ca2—O3—Ca1viii30.47 (6)
O3vii—Ca1—P1—O455.40 (13)Cl1—Ca2—O3—Ca1viii140.57 (7)
O3viii—Ca1—P1—O490.87 (15)Cl1x—Ca2—O3—Ca1viii118.92 (9)
P1v—Ca1—P1—O4178.02 (12)Cl1xiv—Ca2—O3—Ca1viii142.82 (7)
P1iv—Ca1—P1—O483.79 (12)O3viii—P1—O4—Ca1xv172.04 (17)
O4i—Ca1—P1—O2105.2 (3)O3—P1—O4—Ca1xv48.9 (2)
O4ii—Ca1—P1—O2166.43 (12)O2—P1—O4—Ca1xv69.52 (16)
O4iii—Ca1—P1—O290.58 (12)Ca2xiii—P1—O4—Ca1xv110.48 (16)
O2iv—Ca1—P1—O234.92 (13)Ca1—P1—O4—Ca1xv119.88 (8)
O2v—Ca1—P1—O2105.53 (16)Ca1viii—P1—O4—Ca1xv19.2 (2)
O3vi—Ca1—P1—O2104.72 (12)Ca2xi—P1—O4—Ca1xv110.48 (16)
O3vii—Ca1—P1—O220.88 (11)Ca2ix—P1—O4—Ca1xv69.52 (16)
O3viii—Ca1—P1—O2167.16 (14)O3viii—P1—O4—Ca1iii48.9 (2)
P1v—Ca1—P1—O2101.73 (10)O3—P1—O4—Ca1iii172.04 (17)
P1iv—Ca1—P1—O27.51 (10)O2—P1—O4—Ca1iii69.52 (16)
O4i—Ca1—P1—Ca2xiii117.3 (3)Ca2xiii—P1—O4—Ca1iii110.48 (16)
O4ii—Ca1—P1—Ca2xiii56.07 (5)Ca1—P1—O4—Ca1iii19.2 (2)
O4iii—Ca1—P1—Ca2xiii131.92 (5)Ca1viii—P1—O4—Ca1iii119.88 (8)
O2iv—Ca1—P1—Ca2xiii102.58 (6)Ca2xi—P1—O4—Ca1iii110.48 (16)
O2v—Ca1—P1—Ca2xiii31.97 (6)Ca2ix—P1—O4—Ca1iii69.52 (16)
O2—Ca1—P1—Ca2xiii137.50 (11)O3viii—P1—O4—Ca2xi61.56 (12)
O3vi—Ca1—P1—Ca2xiii32.78 (6)O3—P1—O4—Ca2xi61.56 (12)
O3vii—Ca1—P1—Ca2xiii158.38 (5)O2—P1—O4—Ca2xi180
O3viii—Ca1—P1—Ca2xiii55.35 (10)Ca2xiii—P1—O4—Ca2xi0
P1v—Ca1—P1—Ca2xiii35.766 (18)Ca1—P1—O4—Ca2xi129.64 (9)
P1iv—Ca1—P1—Ca2xiii129.990 (16)Ca1viii—P1—O4—Ca2xi129.64 (9)
O4i—Ca1—P1—Ca1viii159.8 (3)Ca2ix—P1—O4—Ca2xi180
O4ii—Ca1—P1—Ca1viii138.95 (5)O2ix—Ca2—Cl1—Cl1xiv45.24 (13)
O4iii—Ca1—P1—Ca1viii145.20 (5)O3x—Ca2—Cl1—Cl1xiv156.84 (9)
O2iv—Ca1—P1—Ca1viii19.70 (6)O3—Ca2—Cl1—Cl1xiv17.57 (6)
O2v—Ca1—P1—Ca1viii50.91 (6)O1A—Ca2—Cl1—Cl1xiv180.000 (3)
O2—Ca1—P1—Ca1viii54.62 (10)O1x—Ca2—Cl1—Cl1xiv180.000 (4)
O3vi—Ca1—P1—Ca1viii50.10 (6)O1—Ca2—Cl1—Cl1xiv180.000 (3)
O3vii—Ca1—P1—Ca1viii75.50 (4)O3xi—Ca2—Cl1—Cl1xiv68.54 (7)
O3viii—Ca1—P1—Ca1viii138.22 (10)O3xii—Ca2—Cl1—Cl1xiv119.49 (5)
P1v—Ca1—P1—Ca1viii47.112 (11)O4xiii—Ca2—Cl1—Cl1xiv82.39 (4)
P1iv—Ca1—P1—Ca1viii47.112 (12)Cl1x—Ca2—Cl1—Cl1xiv180.000 (2)
O4i—Ca1—P1—Ca2xi58.4 (3)O2ix—Ca2—Cl1—Ca2xvi87.1 (2)
O4ii—Ca1—P1—Ca2xi2.83 (7)O3x—Ca2—Cl1—Ca2xvi70.80 (9)
O4iii—Ca1—P1—Ca2xi73.02 (7)O3—Ca2—Cl1—Ca2xvi149.93 (11)
O2iv—Ca1—P1—Ca2xi161.47 (7)O1A—Ca2—Cl1—Ca2xvi47.64 (9)
O2v—Ca1—P1—Ca2xi90.87 (7)O1x—Ca2—Cl1—Ca2xvi47.64 (9)
O2—Ca1—P1—Ca2xi163.61 (12)O1—Ca2—Cl1—Ca2xvi47.64 (9)
O3vi—Ca1—P1—Ca2xi91.68 (7)O3xi—Ca2—Cl1—Ca2xvi63.82 (7)
O3vii—Ca1—P1—Ca2xi142.72 (6)O3xii—Ca2—Cl1—Ca2xvi12.87 (11)
O3viii—Ca1—P1—Ca2xi3.55 (10)O4xiii—Ca2—Cl1—Ca2xvi145.25 (7)
P1v—Ca1—P1—Ca2xi94.66 (5)Cl1x—Ca2—Cl1—Ca2xvi47.64 (9)
P1iv—Ca1—P1—Ca2xi171.11 (5)Cl1xiv—Ca2—Cl1—Ca2xvi132.36 (9)
O4i—Ca1—P1—Ca2ix79.9 (3)O2ix—Ca2—Cl1—Ca2xvii177.60 (9)
O4ii—Ca1—P1—Ca2ix141.22 (5)O3x—Ca2—Cl1—Ca2xvii24.48 (15)
O4iii—Ca1—P1—Ca2ix65.36 (5)O3—Ca2—Cl1—Ca2xvii114.79 (10)
O2iv—Ca1—P1—Ca2ix60.14 (6)O1A—Ca2—Cl1—Ca2xvii47.64 (9)
O2v—Ca1—P1—Ca2ix130.75 (6)O1x—Ca2—Cl1—Ca2xvii47.64 (9)
O2—Ca1—P1—Ca2ix25.22 (10)O1—Ca2—Cl1—Ca2xvii47.64 (9)
O3vi—Ca1—P1—Ca2ix129.94 (6)O3xi—Ca2—Cl1—Ca2xvii159.10 (14)
O3vii—Ca1—P1—Ca2ix4.34 (4)O3xii—Ca2—Cl1—Ca2xvii108.15 (9)
O3viii—Ca1—P1—Ca2ix141.94 (10)O4xiii—Ca2—Cl1—Ca2xvii49.97 (11)
P1v—Ca1—P1—Ca2ix126.951 (17)Cl1x—Ca2—Cl1—Ca2xvii47.64 (9)
P1iv—Ca1—P1—Ca2ix32.726 (17)Cl1xiv—Ca2—Cl1—Ca2xvii132.36 (9)
O3viii—P1—O2—Ca2ix122.01 (9)O2ix—Ca2—Cl1—Ca2xi2.63 (18)
O3—P1—O2—Ca2ix122.01 (9)O3x—Ca2—Cl1—Ca2xi160.55 (9)
O4—P1—O2—Ca2ix0O3—Ca2—Cl1—Ca2xi60.18 (9)
Ca2xiii—P1—O2—Ca2ix180O1A—Ca2—Cl1—Ca2xi137.39 (7)
Ca1—P1—O2—Ca2ix133.49 (7)O1x—Ca2—Cl1—Ca2xi137.39 (7)
Ca1viii—P1—O2—Ca2ix133.49 (7)O1—Ca2—Cl1—Ca2xi137.39 (7)
Ca2xi—P1—O2—Ca2ix0O3xi—Ca2—Cl1—Ca2xi25.94 (6)
O3viii—P1—O2—Ca111.47 (13)O3xii—Ca2—Cl1—Ca2xi76.89 (9)
O3—P1—O2—Ca1104.50 (10)O4xiii—Ca2—Cl1—Ca2xi125.00 (6)
O4—P1—O2—Ca1133.49 (7)Cl1x—Ca2—Cl1—Ca2xi137.39 (7)
Ca2xiii—P1—O2—Ca146.51 (7)Cl1xiv—Ca2—Cl1—Ca2xi42.61 (7)
Ca1viii—P1—O2—Ca193.03 (14)O2ix—Ca2—Cl1—Ca2xiii87.84 (10)
Ca2xi—P1—O2—Ca1133.49 (7)O3x—Ca2—Cl1—Ca2xiii114.24 (13)
Ca2ix—P1—O2—Ca1133.49 (7)O3—Ca2—Cl1—Ca2xiii25.03 (8)
O3viii—P1—O2—Ca1viii104.50 (10)O1A—Ca2—Cl1—Ca2xiii137.39 (7)
O3—P1—O2—Ca1viii11.47 (13)O1x—Ca2—Cl1—Ca2xiii137.39 (7)
O4—P1—O2—Ca1viii133.49 (7)O1—Ca2—Cl1—Ca2xiii137.39 (7)
Ca2xiii—P1—O2—Ca1viii46.51 (7)O3xi—Ca2—Cl1—Ca2xiii111.15 (12)
Ca1—P1—O2—Ca1viii93.03 (14)O3xii—Ca2—Cl1—Ca2xiii162.10 (7)
Ca2xi—P1—O2—Ca1viii133.49 (7)O4xiii—Ca2—Cl1—Ca2xiii39.79 (9)
Ca2ix—P1—O2—Ca1viii133.49 (7)Cl1x—Ca2—Cl1—Ca2xiii137.39 (7)
O4i—Ca1—O2—P1150.76 (12)Cl1xiv—Ca2—Cl1—Ca2xiii42.61 (7)
O4ii—Ca1—O2—P116.42 (14)O2ix—Ca2—O1—O1x121.4 (5)
O4iii—Ca1—O2—P190.07 (11)O3x—Ca2—O1—O1x163.19 (6)
O2iv—Ca1—O2—P1144.38 (12)O3—Ca2—O1—O1x19.62 (10)
O2v—Ca1—O2—P165.50 (15)O1A—Ca2—O1—O1x0.000 (5)
O3vi—Ca1—O2—P193.94 (11)O3xi—Ca2—O1—O1x59.61 (5)
O3vii—Ca1—O2—P1157.48 (12)O3xii—Ca2—O1—O1x115.66 (12)
O3viii—Ca1—O2—P17.34 (8)O4xiii—Ca2—O1—O1x94.70 (10)
P1v—Ca1—O2—P181.40 (9)Cl1—Ca2—O1—O1x0.000 (3)
P1iv—Ca1—O2—P1171.83 (11)Cl1x—Ca2—O1—O1x180.000 (3)
O4i—Ca1—O2—Ca2ix12.4 (2)Cl1xiv—Ca2—O1—O1x0.000 (3)
O4ii—Ca1—O2—Ca2ix121.89 (10)O2ix—Ca2—O1—Ca2xvi60.7 (10)
O4iii—Ca1—O2—Ca2ix48.25 (10)O3x—Ca2—O1—Ca2xvi136.1 (5)
O2iv—Ca1—O2—Ca2ix77.30 (14)O3—Ca2—O1—Ca2xvi80.3 (4)
O2v—Ca1—O2—Ca2ix156.18 (12)O1A—Ca2—O1—Ca2xvi60.7 (5)
O3vi—Ca1—O2—Ca2ix127.74 (8)O1x—Ca2—O1—Ca2xvi60.7 (5)
O3vii—Ca1—O2—Ca2ix19.17 (8)O3xi—Ca2—O1—Ca2xvi1.1 (5)
O3viii—Ca1—O2—Ca2ix130.98 (11)O3xii—Ca2—O1—Ca2xvi54.9 (4)
P1v—Ca1—O2—Ca2ix140.28 (7)O4xiii—Ca2—O1—Ca2xvi155.4 (4)
P1iv—Ca1—O2—Ca2ix49.85 (8)Cl1—Ca2—O1—Ca2xvi60.7 (5)
P1—Ca1—O2—Ca2ix138.32 (15)Cl1x—Ca2—O1—Ca2xvi119.3 (5)
O4i—Ca1—O2—Ca1viii104.30 (14)Cl1xiv—Ca2—O1—Ca2xvi60.7 (5)
O4ii—Ca1—O2—Ca1viii121.36 (8)O2ix—Ca2—O1—Ca2xvii177.90 (8)
O4iii—Ca1—O2—Ca1viii164.99 (9)O3x—Ca2—O1—Ca2xvii102.5 (5)
O2iv—Ca1—O2—Ca1viii39.44 (9)O3—Ca2—O1—Ca2xvii41.1 (6)
O2v—Ca1—O2—Ca1viii39.44 (9)O1A—Ca2—O1—Ca2xvii60.7 (5)
O3vi—Ca1—O2—Ca1viii11.00 (12)O1x—Ca2—O1—Ca2xvii60.7 (5)
O3vii—Ca1—O2—Ca1viii97.58 (8)O3xi—Ca2—O1—Ca2xvii120.3 (5)
O3viii—Ca1—O2—Ca1viii112.28 (10)O3xii—Ca2—O1—Ca2xvii176.4 (6)
P1v—Ca1—O2—Ca1viii23.54 (8)O4xiii—Ca2—O1—Ca2xvii34.0 (6)
P1iv—Ca1—O2—Ca1viii66.89 (6)Cl1—Ca2—O1—Ca2xvii60.7 (5)
P1—Ca1—O2—Ca1viii104.94 (13)Cl1x—Ca2—O1—Ca2xvii119.3 (5)
O3viii—P1—O3—Ca2144.72 (14)Cl1xiv—Ca2—O1—Ca2xvii60.7 (5)
O4—P1—O3—Ca220.0 (3)O2ix—Ca2—O1A—Ca2xvi0
O2—P1—O3—Ca2101.5 (3)O3x—Ca2—O1A—Ca2xvi107.19 (6)
Ca2xiii—P1—O3—Ca2150.2 (3)O3—Ca2—O1A—Ca2xvi107.19 (6)
Ca1—P1—O3—Ca2151.7 (2)O1x—Ca2—O1A—Ca2xvi90
Ca1viii—P1—O3—Ca2111.3 (3)O1—Ca2—O1A—Ca2xvi90
Ca2xi—P1—O3—Ca266.4 (2)O3xi—Ca2—O1A—Ca2xvi29.41 (5)
Ca2ix—P1—O3—Ca267.4 (3)O3xii—Ca2—O1A—Ca2xvi29.41 (5)
O3viii—P1—O3—Ca2xiii5.5 (2)O4xiii—Ca2—O1A—Ca2xvi180
O4—P1—O3—Ca2xiii130.23 (11)Cl1—Ca2—O1A—Ca2xvi90
O2—P1—O3—Ca2xiii108.31 (12)Cl1x—Ca2—O1A—Ca2xvi90
Ca1—P1—O3—Ca2xiii58.12 (10)Cl1xiv—Ca2—O1A—Ca2xvi90
Ca1viii—P1—O3—Ca2xiii98.47 (8)O2ix—Ca2—O1A—Ca2xvii180
Ca2xi—P1—O3—Ca2xiii83.79 (8)O3x—Ca2—O1A—Ca2xvii72.81 (6)
Ca2ix—P1—O3—Ca2xiii142.37 (6)O3—Ca2—O1A—Ca2xvii72.81 (6)
O3viii—P1—O3—Ca1viii103.96 (15)O1x—Ca2—O1A—Ca2xvii90
O4—P1—O3—Ca1viii131.30 (11)O1—Ca2—O1A—Ca2xvii90
O2—P1—O3—Ca1viii9.84 (12)O3xi—Ca2—O1A—Ca2xvii150.59 (5)
Ca2xiii—P1—O3—Ca1viii98.47 (8)O3xii—Ca2—O1A—Ca2xvii150.59 (5)
Ca1—P1—O3—Ca1viii40.35 (9)O4xiii—Ca2—O1A—Ca2xvii0
Ca2xi—P1—O3—Ca1viii177.75 (6)Cl1—Ca2—O1A—Ca2xvii90
Ca2ix—P1—O3—Ca1viii43.90 (9)Cl1x—Ca2—O1A—Ca2xvii90
O2ix—Ca2—O3—P132.8 (3)Cl1xiv—Ca2—O1A—Ca2xvii90
O3x—Ca2—O3—P1113.6 (2)
Symmetry codes: (i) xy, x, z+2; (ii) y, x+y+1, z+2; (iii) x+1, y+1, z+2; (iv) x+y, x+1, z; (v) y+1, xy+1, z; (vi) y+1, xy+1, z+3/2; (vii) x+y, x+1, z+3/2; (viii) x, y, z+3/2; (ix) x+1, y+1, z+1; (x) x, y, z+1/2; (xi) xy+1, x, z+1; (xii) xy+1, x, z1/2; (xiii) y, x+y+1, z+1; (xiv) x+2, y+2, z+1; (xv) x+1, y+1, z1/2; (xvi) y+2, xy+1, z; (xvii) x+y+1, x+2, z.
(1450r) top
Crystal data top
3(O4P)·0.44(Cl)·0.56(OH)·5(Ca)Dx = 3.168 Mg m3
Mr = 510.42Mo Kα radiation, λ = 0.7107 Å
Trigonal, P63/mCell parameters from 2856 reflections
Hall symbol: -P 6cθ = 2.5–30.2°
a = 9.4894 (4) ŵ = 3.14 mm1
c = 6.8612 (7) ÅT = 293 K
V = 535.07 (6) Å3Prism, colourless
Z = 20.25 × 0.12 × 0.05 mm
F(000) = 507.2
Data collection top
BRUKER APPEX-II CCD
diffractometer
397 independent reflections
Radiation source: fine-focus sealed tube376 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.030
ω and phi scansθmax = 26.3°, θmin = 2.5°
Absorption correction: multi-scan
BRUKER SADABS
h = 1111
Tmin = 0.598, Tmax = 0.748k = 1111
5663 measured reflectionsl = 88
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.032Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.076H atoms treated by a mixture of independent and constrained refinement
S = 0.96 w = 1/[σ2(Fo2) + (0.031P)2 + 3.9033P]
where P = (Fo2 + 2Fc2)/3
397 reflections(Δ/σ)max < 0.001
44 parametersΔρmax = 0.89 e Å3
14 restraintsΔρmin = 1.03 e Å3
Crystal data top
3(O4P)·0.44(Cl)·0.56(OH)·5(Ca)Z = 2
Mr = 510.42Mo Kα radiation
Trigonal, P63/mµ = 3.14 mm1
a = 9.4894 (4) ÅT = 293 K
c = 6.8612 (7) Å0.25 × 0.12 × 0.05 mm
V = 535.07 (6) Å3
Data collection top
BRUKER APPEX-II CCD
diffractometer
397 independent reflections
Absorption correction: multi-scan
BRUKER SADABS
376 reflections with I > 2σ(I)
Tmin = 0.598, Tmax = 0.748Rint = 0.030
5663 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03214 restraints
wR(F2) = 0.076H atoms treated by a mixture of independent and constrained refinement
S = 0.96Δρmax = 0.89 e Å3
397 reflectionsΔρmin = 1.03 e Å3
44 parameters
Special details top

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ca10.66670.33330.99791 (17)0.0128 (3)
Ca20.74370 (13)0.75079 (13)0.250.0179 (3)
P10.59950 (13)0.62969 (13)0.750.0083 (3)
O20.4121 (4)0.5342 (4)0.750.0263 (9)
O30.6500 (4)0.7366 (3)0.5692 (4)0.0332 (8)
O40.6688 (4)0.5139 (4)0.750.0132 (7)
Cl1110.4697 (15)0.0390.22
O1110.136 (3)0.035 (2)0.15
H11100.041*0.3
O1A110.250.0356 (17)0.26
H1A110.107 (3)0.043*0.13
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0151 (4)0.0151 (4)0.0081 (5)0.00756 (19)00
Ca20.0287 (6)0.0233 (6)0.0101 (5)0.0191 (5)00
P10.0103 (6)0.0097 (5)0.0071 (6)0.0066 (4)00
O20.0127 (17)0.0185 (18)0.050 (3)0.0100 (15)00
O30.062 (2)0.0315 (15)0.0237 (14)0.0369 (15)0.0262 (15)0.0174 (13)
O40.0166 (16)0.0136 (16)0.0135 (16)0.0107 (14)00
Cl10.0360.0360.0440.01800
O10.029 (3)0.029 (3)0.045 (4)0.0147 (14)00
O1A0.0314 (19)0.0314 (19)0.044 (3)0.0157 (10)00
Geometric parameters (Å, º) top
Ca1—O4i2.407 (2)P1—O41.537 (3)
Ca1—O4ii2.407 (2)P1—O21.540 (4)
Ca1—O42.407 (2)P1—Ca2xiii3.1217 (15)
Ca1—O2iii2.464 (3)P1—Ca1xvi3.2219 (11)
Ca1—O2iv2.464 (3)P1—Ca1v3.2219 (11)
Ca1—O2v2.464 (3)P1—Ca2xii3.3270 (15)
Ca1—O3vi2.777 (3)P1—Ca2x3.4473 (15)
Ca1—O3vii2.777 (4)O2—Ca2x2.346 (4)
Ca1—O3viii2.777 (4)O2—Ca1xvi2.464 (3)
Ca1—P1iii3.2219 (11)O2—Ca1v2.464 (3)
Ca1—P1iv3.2219 (11)O3—Ca2xiii2.566 (3)
Ca1—P1v3.2219 (11)O3—Ca1xvi2.777 (3)
Ca2—O3ix2.342 (3)O4—Ca1xv2.407 (2)
Ca2—O32.342 (3)O4—Ca2xii2.740 (4)
Ca2—O2x2.346 (4)Cl1—Cl1xiv0.42 (2)
Ca2—O1A2.3992 (11)Cl1—Ca2xvii2.833 (5)
Ca2—O1ix2.524 (6)Cl1—Ca2xviii2.833 (5)
Ca2—O12.524 (6)Cl1—Ca2xiv3.075 (6)
Ca2—O3xi2.566 (3)Cl1—Ca2xiii3.075 (6)
Ca2—O3xii2.566 (3)Cl1—Ca2xii3.075 (6)
Ca2—O4xiii2.740 (4)O1—O1ix1.57 (4)
Ca2—Cl12.833 (6)O1—O1xix1.87 (4)
Ca2—Cl1ix2.833 (6)O1—Ca2xvii2.524 (6)
Ca2—Cl1xiv3.075 (6)O1—Ca2xviii2.524 (6)
P1—O3xv1.520 (3)O1A—Ca2xvii2.3992 (11)
P1—O31.520 (3)O1A—Ca2xviii2.3992 (11)
O4i—Ca1—O4ii75.58 (9)O4xiii—Ca2—Cl1102.63 (7)
O4i—Ca1—O475.58 (9)O3ix—Ca2—Cl1ix72.15 (19)
O4ii—Ca1—O475.58 (9)O3—Ca2—Cl1ix133.49 (18)
O4i—Ca1—O2iii153.44 (11)O2x—Ca2—Cl1ix138.20 (14)
O4ii—Ca1—O2iii91.70 (8)O1A—Ca2—Cl1ix32.14 (17)
O4—Ca1—O2iii124.34 (11)O1ix—Ca2—Cl1ix50.2 (5)
O4i—Ca1—O2iv91.70 (8)O1—Ca2—Cl1ix14.1 (4)
O4ii—Ca1—O2iv124.34 (10)O3xi—Ca2—Cl1ix67.50 (10)
O4—Ca1—O2iv153.44 (11)O3xii—Ca2—Cl1ix97.56 (12)
O2iii—Ca1—O2iv76.15 (9)O4xiii—Ca2—Cl1ix102.63 (7)
O4i—Ca1—O2v124.34 (10)Cl1—Ca2—Cl1ix64.3 (3)
O4ii—Ca1—O2v153.44 (11)O3ix—Ca2—Cl1xiv139.52 (16)
O4—Ca1—O2v91.70 (8)O3—Ca2—Cl1xiv65.86 (17)
O2iii—Ca1—O2v76.15 (9)O2x—Ca2—Cl1xiv133.39 (12)
O2iv—Ca1—O2v76.15 (9)O1A—Ca2—Cl1xiv38.72 (15)
O4i—Ca1—O3vi85.28 (10)O1ix—Ca2—Cl1xiv20.7 (5)
O4ii—Ca1—O3vi69.63 (9)O1—Ca2—Cl1xiv56.8 (4)
O4—Ca1—O3vi143.51 (9)O3xi—Ca2—Cl1xiv100.76 (11)
O2iii—Ca1—O3vi68.35 (11)O3xii—Ca2—Cl1xiv65.29 (8)
O2iv—Ca1—O3vi55.27 (10)O4xiii—Ca2—Cl1xiv101.62 (6)
O2v—Ca1—O3vi124.58 (9)Cl1—Ca2—Cl1xiv6.6 (3)
O4i—Ca1—O3vii143.51 (9)Cl1ix—Ca2—Cl1xiv70.86 (4)
O4ii—Ca1—O3vii85.28 (10)O3xv—P1—O3109.3 (2)
O4—Ca1—O3vii69.63 (9)O3xv—P1—O4111.87 (12)
O2iii—Ca1—O3vii55.27 (10)O3—P1—O4111.87 (12)
O2iv—Ca1—O3vii124.58 (9)O3xv—P1—O2106.15 (16)
O2v—Ca1—O3vii68.35 (11)O3—P1—O2106.15 (16)
O3vi—Ca1—O3vii116.96 (4)O4—P1—O2111.1 (2)
O4i—Ca1—O3viii69.63 (9)O3xv—P1—Ca2xiii54.81 (12)
O4ii—Ca1—O3viii143.51 (9)O3—P1—Ca2xiii54.81 (12)
O4—Ca1—O3viii85.28 (10)O4—P1—Ca2xiii134.79 (14)
O2iii—Ca1—O3viii124.58 (9)O2—P1—Ca2xiii114.09 (14)
O2iv—Ca1—O3viii68.35 (11)O3xv—P1—Ca1xvi111.58 (12)
O2v—Ca1—O3viii55.27 (10)O3—P1—Ca1xvi59.45 (14)
O3vi—Ca1—O3viii116.96 (4)O4—P1—Ca1xvi135.79 (9)
O3vii—Ca1—O3viii116.96 (4)O2—P1—Ca1xvi47.67 (10)
O4i—Ca1—P1iii166.72 (7)Ca2xiii—P1—Ca1xvi79.10 (3)
O4ii—Ca1—P1iii91.71 (7)O3xv—P1—Ca1v59.45 (14)
O4—Ca1—P1iii97.75 (7)O3—P1—Ca1v111.58 (12)
O2iii—Ca1—P1iii27.52 (8)O4—P1—Ca1v135.79 (9)
O2iv—Ca1—P1iii98.81 (7)O2—P1—Ca1v47.67 (10)
O2v—Ca1—P1iii66.60 (8)Ca2xiii—P1—Ca1v79.10 (3)
O3vi—Ca1—P1iii94.03 (6)Ca1xvi—P1—Ca1v64.94 (4)
O3vii—Ca1—P1iii28.13 (6)O3xv—P1—Ca2xii81.68 (14)
O3viii—Ca1—P1iii121.87 (6)O3—P1—Ca2xii81.68 (14)
O4i—Ca1—P1iv91.71 (7)O4—P1—Ca2xii54.61 (13)
O4ii—Ca1—P1iv97.75 (7)O2—P1—Ca2xii165.74 (15)
O4—Ca1—P1iv166.72 (7)Ca2xiii—P1—Ca2xii80.17 (5)
O2iii—Ca1—P1iv66.60 (8)Ca1xvi—P1—Ca2xii141.07 (3)
O2iv—Ca1—P1iv27.52 (8)Ca1v—P1—Ca2xii141.07 (3)
O2v—Ca1—P1iv98.81 (7)O3xv—P1—Ca2x121.08 (14)
O3vi—Ca1—P1iv28.13 (6)O3—P1—Ca2x121.08 (14)
O3vii—Ca1—P1iv121.87 (6)O4—P1—Ca2x76.64 (13)
O3viii—Ca1—P1iv94.03 (6)Ca2xiii—P1—Ca2x148.57 (4)
P1iii—Ca1—P1iv93.88 (3)Ca1xvi—P1—Ca2x74.49 (3)
O4i—Ca1—P1v97.75 (7)Ca1v—P1—Ca2x74.49 (3)
O4ii—Ca1—P1v166.72 (7)Ca2xii—P1—Ca2x131.26 (5)
O4—Ca1—P1v91.71 (7)P1—O2—Ca2x123.7 (2)
O2iii—Ca1—P1v98.81 (7)P1—O2—Ca1xvi104.81 (14)
O2iv—Ca1—P1v66.60 (8)Ca2x—O2—Ca1xvi114.27 (11)
O2v—Ca1—P1v27.52 (8)P1—O2—Ca1v104.81 (14)
O3vi—Ca1—P1v121.87 (6)Ca2x—O2—Ca1v114.27 (11)
O3vii—Ca1—P1v94.03 (6)Ca1xvi—O2—Ca1v89.19 (12)
O3viii—Ca1—P1v28.13 (6)P1—O3—Ca2141.72 (15)
P1iii—Ca1—P1v93.88 (3)P1—O3—Ca2xiii96.24 (15)
P1iv—Ca1—P1v93.88 (3)Ca2—O3—Ca2xiii116.97 (12)
O3ix—Ca2—O3138.47 (18)P1—O3—Ca1xvi92.42 (15)
O3ix—Ca2—O2x86.07 (8)Ca2—O3—Ca1xvi100.57 (12)
O3—Ca2—O2x86.07 (8)Ca2xiii—O3—Ca1xvi98.16 (9)
O3ix—Ca2—O1A103.02 (9)P1—O4—Ca1xv130.88 (9)
O3—Ca2—O1A103.02 (9)P1—O4—Ca1130.88 (9)
O2x—Ca2—O1A151.69 (10)Ca1xv—O4—Ca189.92 (11)
O3ix—Ca2—O1ix120.3 (4)P1—O4—Ca2xii98.17 (15)
O3—Ca2—O1ix85.7 (4)Ca1xv—O4—Ca2xii99.97 (10)
O2x—Ca2—O1ix146.8 (2)Ca1—O4—Ca2xii99.97 (10)
O1A—Ca2—O1ix18.1 (4)Cl1xiv—Cl1—Ca2122.14 (18)
O3ix—Ca2—O185.7 (4)Cl1xiv—Cl1—Ca2xvii122.14 (17)
O3—Ca2—O1120.3 (4)Ca2—Cl1—Ca2xvii94.3 (2)
O2x—Ca2—O1146.8 (2)Cl1xiv—Cl1—Ca2xviii122.14 (17)
O1A—Ca2—O118.1 (4)Ca2—Cl1—Ca2xviii94.3 (2)
O1ix—Ca2—O136.1 (8)Ca2xvii—Cl1—Ca2xviii94.3 (2)
O3ix—Ca2—O3xi79.50 (6)Cl1xiv—Cl1—Ca2xiv51.28 (14)
O3—Ca2—O3xi136.18 (11)Ca2—Cl1—Ca2xiv173.4 (3)
O2x—Ca2—O3xi73.82 (11)Ca2xvii—Cl1—Ca2xiv90.14 (3)
O1A—Ca2—O3xi81.48 (8)Ca2xviii—Cl1—Ca2xiv90.14 (3)
O1ix—Ca2—O3xi90.5 (2)Cl1xiv—Cl1—Ca2xiii51.28 (16)
O1—Ca2—O3xi73.10 (19)Ca2—Cl1—Ca2xiii90.14 (3)
O3ix—Ca2—O3xii136.18 (11)Ca2xvii—Cl1—Ca2xiii173.4 (3)
O3—Ca2—O3xii79.50 (6)Ca2xviii—Cl1—Ca2xiii90.14 (3)
O2x—Ca2—O3xii73.82 (11)Ca2xiv—Cl1—Ca2xiii85.0 (2)
O1A—Ca2—O3xii81.48 (8)Cl1xiv—Cl1—Ca2xii51.28 (15)
O1ix—Ca2—O3xii73.10 (19)Ca2—Cl1—Ca2xii90.14 (3)
O1—Ca2—O3xii90.5 (2)Ca2xvii—Cl1—Ca2xii90.14 (3)
O3xi—Ca2—O3xii57.81 (12)Ca2xviii—Cl1—Ca2xii173.4 (3)
O3ix—Ca2—O4xiii71.18 (8)Ca2xiv—Cl1—Ca2xii85.0 (2)
O3—Ca2—O4xiii71.18 (8)Ca2xiii—Cl1—Ca2xii85.0 (2)
O2x—Ca2—O4xiii103.35 (11)O1ix—O1—O1xix180.000 (12)
O1A—Ca2—O4xiii104.96 (7)O1ix—O1—Ca2xvii71.9 (4)
O1ix—Ca2—O4xiii104.21 (8)O1xix—O1—Ca2xvii108.1 (4)
O1—Ca2—O4xiii104.21 (8)O1ix—O1—Ca271.9 (4)
O3xi—Ca2—O4xiii150.67 (6)O1xix—O1—Ca2108.1 (4)
O3xii—Ca2—O4xiii150.67 (6)Ca2xvii—O1—Ca2110.8 (4)
O3ix—Ca2—Cl1133.49 (18)O1ix—O1—Ca2xviii71.9 (4)
O3—Ca2—Cl172.15 (19)O1xix—O1—Ca2xviii108.1 (4)
O2x—Ca2—Cl1138.20 (14)Ca2xvii—O1—Ca2xviii110.8 (4)
O1A—Ca2—Cl132.14 (17)Ca2—O1—Ca2xviii110.8 (4)
O1ix—Ca2—Cl114.1 (4)Ca2—O1A—Ca2xvii120
O1—Ca2—Cl150.2 (5)Ca2—O1A—Ca2xviii120
O3xi—Ca2—Cl197.56 (12)Ca2xvii—O1A—Ca2xviii120
O3xii—Ca2—Cl167.50 (10)
O3xv—P1—O2—Ca2x121.85 (12)O3vi—Ca1—O4—Ca2xii78.73 (16)
O3—P1—O2—Ca2x121.85 (12)O3vii—Ca1—O4—Ca2xii29.42 (8)
O4—P1—O2—Ca2x0O3viii—Ca1—O4—Ca2xii150.48 (8)
Ca2xiii—P1—O2—Ca2x180P1iii—Ca1—O4—Ca2xii28.92 (7)
Ca1xvi—P1—O2—Ca2x133.43 (9)P1iv—Ca1—O4—Ca2xii122.0 (3)
Ca1v—P1—O2—Ca2x133.43 (9)P1v—Ca1—O4—Ca2xii123.08 (6)
Ca2xii—P1—O2—Ca2x0O3ix—Ca2—Cl1—Cl1xiv157.83 (13)
O3xv—P1—O2—Ca1xvi104.72 (13)O3—Ca2—Cl1—Cl1xiv16.72 (8)
O3—P1—O2—Ca1xvi11.58 (17)O2x—Ca2—Cl1—Cl1xiv45.36 (18)
O4—P1—O2—Ca1xvi133.43 (9)O1A—Ca2—Cl1—Cl1xiv180.000 (2)
Ca2xiii—P1—O2—Ca1xvi46.57 (9)O1ix—Ca2—Cl1—Cl1xiv180.000 (2)
Ca1v—P1—O2—Ca1xvi93.14 (18)O1—Ca2—Cl1—Cl1xiv180.000 (3)
Ca2xii—P1—O2—Ca1xvi133.43 (9)O3xi—Ca2—Cl1—Cl1xiv119.50 (7)
Ca2x—P1—O2—Ca1xvi133.43 (9)O3xii—Ca2—Cl1—Cl1xiv69.04 (10)
O3xv—P1—O2—Ca1v11.58 (17)O4xiii—Ca2—Cl1—Cl1xiv81.91 (5)
O3—P1—O2—Ca1v104.72 (13)Cl1ix—Ca2—Cl1—Cl1xiv180.000 (3)
O4—P1—O2—Ca1v133.43 (9)O3ix—Ca2—Cl1—Ca2xvii69.51 (13)
Ca2xiii—P1—O2—Ca1v46.57 (9)O3—Ca2—Cl1—Ca2xvii149.37 (17)
Ca1xvi—P1—O2—Ca1v93.14 (18)O2x—Ca2—Cl1—Ca2xvii87.3 (3)
Ca2xii—P1—O2—Ca1v133.43 (9)O1A—Ca2—Cl1—Ca2xvii47.34 (14)
Ca2x—P1—O2—Ca1v133.43 (9)O1ix—Ca2—Cl1—Ca2xvii47.34 (14)
O3xv—P1—O3—Ca2145.32 (19)O1—Ca2—Cl1—Ca2xvii47.34 (14)
O4—P1—O3—Ca220.8 (4)O3xi—Ca2—Cl1—Ca2xvii13.16 (17)
O2—P1—O3—Ca2100.6 (3)O3xii—Ca2—Cl1—Ca2xvii63.61 (10)
Ca2xiii—P1—O3—Ca2151.0 (4)O4xiii—Ca2—Cl1—Ca2xvii145.43 (11)
Ca1xvi—P1—O3—Ca2110.5 (4)Cl1ix—Ca2—Cl1—Ca2xvii47.34 (14)
Ca1v—P1—O3—Ca2150.8 (3)Cl1xiv—Ca2—Cl1—Ca2xvii132.66 (14)
Ca2xii—P1—O3—Ca267.2 (3)O3ix—Ca2—Cl1—Ca2xviii25.2 (2)
Ca2x—P1—O3—Ca266.4 (4)O3—Ca2—Cl1—Ca2xviii115.94 (14)
O3xv—P1—O3—Ca2xiii5.7 (3)O2x—Ca2—Cl1—Ca2xviii178.01 (12)
O4—P1—O3—Ca2xiii130.22 (14)O1A—Ca2—Cl1—Ca2xviii47.34 (14)
O2—P1—O3—Ca2xiii108.40 (16)O1ix—Ca2—Cl1—Ca2xviii47.34 (14)
Ca1xvi—P1—O3—Ca2xiii98.49 (10)O1—Ca2—Cl1—Ca2xviii47.34 (14)
Ca1v—P1—O3—Ca2xiii58.15 (14)O3xi—Ca2—Cl1—Ca2xviii107.85 (13)
Ca2xii—P1—O3—Ca2xiii83.81 (10)O3xii—Ca2—Cl1—Ca2xviii158.3 (2)
Ca2x—P1—O3—Ca2xiii142.56 (8)O4xiii—Ca2—Cl1—Ca2xviii50.75 (18)
O3xv—P1—O3—Ca1xvi104.2 (2)Cl1ix—Ca2—Cl1—Ca2xviii47.34 (14)
O4—P1—O3—Ca1xvi131.29 (14)Cl1xiv—Ca2—Cl1—Ca2xviii132.66 (14)
O2—P1—O3—Ca1xvi9.92 (16)O3ix—Ca2—Cl1—Ca2xiii115.3 (2)
Ca2xiii—P1—O3—Ca1xvi98.49 (10)O3—Ca2—Cl1—Ca2xiii25.79 (12)
Ca1v—P1—O3—Ca1xvi40.33 (12)O2x—Ca2—Cl1—Ca2xiii87.87 (12)
Ca2xii—P1—O3—Ca1xvi177.71 (8)O1A—Ca2—Cl1—Ca2xiii137.49 (11)
Ca2x—P1—O3—Ca1xvi44.08 (12)O1ix—Ca2—Cl1—Ca2xiii137.49 (11)
O3ix—Ca2—O3—P1111.9 (3)O1—Ca2—Cl1—Ca2xiii137.49 (11)
O2x—Ca2—O3—P132.3 (4)O3xi—Ca2—Cl1—Ca2xiii162.01 (11)
O1A—Ca2—O3—P1120.5 (3)O3xii—Ca2—Cl1—Ca2xiii111.55 (19)
O1ix—Ca2—O3—P1115.5 (4)O4xiii—Ca2—Cl1—Ca2xiii39.40 (15)
O1—Ca2—O3—P1126.3 (4)Cl1ix—Ca2—Cl1—Ca2xiii137.49 (11)
O3xi—Ca2—O3—P129.3 (5)Cl1xiv—Ca2—Cl1—Ca2xiii42.51 (11)
O3xii—Ca2—O3—P141.9 (4)O3ix—Ca2—Cl1—Ca2xii159.66 (12)
O4xiii—Ca2—O3—P1137.9 (4)O3—Ca2—Cl1—Ca2xii59.23 (14)
Cl1—Ca2—O3—P1111.5 (4)O2x—Ca2—Cl1—Ca2xii2.8 (3)
Cl1ix—Ca2—O3—P1132.4 (3)O1A—Ca2—Cl1—Ca2xii137.49 (11)
Cl1xiv—Ca2—O3—P1109.4 (4)O1ix—Ca2—Cl1—Ca2xii137.49 (11)
O3ix—Ca2—O3—Ca2xiii100.8 (2)O1—Ca2—Cl1—Ca2xii137.49 (11)
O2x—Ca2—O3—Ca2xiii179.63 (15)O3xi—Ca2—Cl1—Ca2xii76.99 (14)
O1A—Ca2—O3—Ca2xiii26.77 (15)O3xii—Ca2—Cl1—Ca2xii26.54 (8)
O1ix—Ca2—O3—Ca2xiii31.78 (17)O4xiii—Ca2—Cl1—Ca2xii124.42 (8)
O1—Ca2—O3—Ca2xiii21.0 (2)Cl1ix—Ca2—Cl1—Ca2xii137.49 (11)
O3xi—Ca2—O3—Ca2xiii117.99 (9)Cl1xiv—Ca2—Cl1—Ca2xii42.51 (11)
O3xii—Ca2—O3—Ca2xiii105.37 (8)O3ix—Ca2—O1—O1ix164.06 (7)
O4xiii—Ca2—O3—Ca2xiii74.84 (14)O3—Ca2—O1—O1ix18.48 (12)
Cl1—Ca2—O3—Ca2xiii35.80 (13)O2x—Ca2—O1—O1ix119.9 (6)
Cl1ix—Ca2—O3—Ca2xiii14.9 (2)O1A—Ca2—O1—O1ix0.000 (5)
Cl1xiv—Ca2—O3—Ca2xiii37.87 (12)O3xi—Ca2—O1—O1ix115.61 (13)
O3ix—Ca2—O3—Ca1xvi4.1 (3)O3xii—Ca2—O1—O1ix59.64 (6)
O2x—Ca2—O3—Ca1xvi75.48 (10)O4xiii—Ca2—O1—O1ix94.74 (11)
O1A—Ca2—O3—Ca1xvi131.66 (7)Cl1—Ca2—O1—O1ix0
O1ix—Ca2—O3—Ca1xvi136.67 (13)Cl1ix—Ca2—O1—O1ix180.000 (5)
O1—Ca2—O3—Ca1xvi125.87 (17)Cl1xiv—Ca2—O1—O1ix0
O3xi—Ca2—O3—Ca1xvi137.12 (18)O3ix—Ca2—O1—O1xix15.94 (7)
O3xii—Ca2—O3—Ca1xvi149.74 (9)O3—Ca2—O1—O1xix161.52 (12)
O4xiii—Ca2—O3—Ca1xvi30.06 (8)O2x—Ca2—O1—O1xix60.1 (6)
Cl1—Ca2—O3—Ca1xvi140.69 (10)O1A—Ca2—O1—O1xix180.000 (5)
Cl1ix—Ca2—O3—Ca1xvi119.77 (13)O1ix—Ca2—O1—O1xix180.000 (3)
Cl1xiv—Ca2—O3—Ca1xvi142.76 (10)O3xi—Ca2—O1—O1xix64.39 (13)
O3xv—P1—O4—Ca1xv172.4 (2)O3xii—Ca2—O1—O1xix120.36 (6)
O3—P1—O4—Ca1xv49.3 (3)O4xiii—Ca2—O1—O1xix85.26 (10)
O2—P1—O4—Ca1xv69.2 (2)Cl1—Ca2—O1—O1xix180.000 (3)
Ca2xiii—P1—O4—Ca1xv110.8 (2)Cl1ix—Ca2—O1—O1xix0.000 (5)
Ca1xvi—P1—O4—Ca1xv18.8 (3)Cl1xiv—Ca2—O1—O1xix180.000 (2)
Ca1v—P1—O4—Ca1xv119.51 (10)O3ix—Ca2—O1—Ca2xvii134.2 (5)
Ca2xii—P1—O4—Ca1xv110.8 (2)O3—Ca2—O1—Ca2xvii80.2 (5)
Ca2x—P1—O4—Ca1xv69.2 (2)O2x—Ca2—O1—Ca2xvii58.2 (11)
O3xv—P1—O4—Ca149.3 (3)O1A—Ca2—O1—Ca2xvii61.8 (5)
O3—P1—O4—Ca1172.4 (2)O1ix—Ca2—O1—Ca2xvii61.8 (5)
O2—P1—O4—Ca169.2 (2)O3xi—Ca2—O1—Ca2xvii53.8 (4)
Ca2xiii—P1—O4—Ca1110.8 (2)O3xii—Ca2—O1—Ca2xvii2.1 (5)
Ca1xvi—P1—O4—Ca1119.51 (10)O4xiii—Ca2—O1—Ca2xvii156.5 (4)
Ca1v—P1—O4—Ca118.8 (3)Cl1—Ca2—O1—Ca2xvii61.8 (5)
Ca2xii—P1—O4—Ca1110.8 (2)Cl1ix—Ca2—O1—Ca2xvii118.2 (5)
Ca2x—P1—O4—Ca169.2 (2)Cl1xiv—Ca2—O1—Ca2xvii61.8 (5)
O3xv—P1—O4—Ca2xii61.54 (16)O3ix—Ca2—O1—Ca2xviii102.3 (5)
O3—P1—O4—Ca2xii61.54 (16)O3—Ca2—O1—Ca2xviii43.3 (6)
O2—P1—O4—Ca2xii180O2x—Ca2—O1—Ca2xviii178.31 (10)
Ca2xiii—P1—O4—Ca2xii0O1A—Ca2—O1—Ca2xviii61.8 (5)
Ca1xvi—P1—O4—Ca2xii129.66 (12)O1ix—Ca2—O1—Ca2xviii61.8 (5)
Ca1v—P1—O4—Ca2xii129.66 (11)O3xi—Ca2—O1—Ca2xviii177.4 (6)
Ca2x—P1—O4—Ca2xii180O3xii—Ca2—O1—Ca2xviii121.4 (5)
O4i—Ca1—O4—P1110.6 (3)O4xiii—Ca2—O1—Ca2xviii33.0 (6)
O4ii—Ca1—O4—P1170.9 (3)Cl1—Ca2—O1—Ca2xviii61.8 (5)
O2iii—Ca1—O4—P188.9 (3)Cl1ix—Ca2—O1—Ca2xviii118.2 (5)
O2iv—Ca1—O4—P147.0 (4)Cl1xiv—Ca2—O1—Ca2xviii61.8 (5)
O2v—Ca1—O4—P114.5 (2)O3ix—Ca2—O1A—Ca2xvii106.32 (8)
O3vi—Ca1—O4—P1171.21 (16)O3—Ca2—O1A—Ca2xvii106.32 (8)
O3vii—Ca1—O4—P180.6 (2)O2x—Ca2—O1A—Ca2xvii0
O3viii—Ca1—O4—P140.4 (2)O1ix—Ca2—O1A—Ca2xvii90
P1iii—Ca1—O4—P181.1 (2)O1—Ca2—O1A—Ca2xvii90
P1iv—Ca1—O4—P1127.9 (2)O3xi—Ca2—O1A—Ca2xvii29.26 (6)
P1v—Ca1—O4—P113.0 (2)O3xii—Ca2—O1A—Ca2xvii29.26 (6)
O4i—Ca1—O4—Ca1xv39.25 (13)O4xiii—Ca2—O1A—Ca2xvii180
O4ii—Ca1—O4—Ca1xv39.25 (13)Cl1—Ca2—O1A—Ca2xvii90
O2iii—Ca1—O4—Ca1xv121.29 (11)Cl1ix—Ca2—O1A—Ca2xvii90
O2iv—Ca1—O4—Ca1xv102.79 (19)Cl1xiv—Ca2—O1A—Ca2xvii90
O2v—Ca1—O4—Ca1xv164.36 (11)O3ix—Ca2—O1A—Ca2xviii73.68 (8)
O3vi—Ca1—O4—Ca1xv21.4 (2)O3—Ca2—O1A—Ca2xviii73.68 (8)
O3vii—Ca1—O4—Ca1xv129.52 (12)O2x—Ca2—O1A—Ca2xviii180
O3viii—Ca1—O4—Ca1xv109.41 (10)O1ix—Ca2—O1A—Ca2xviii90
P1iii—Ca1—O4—Ca1xv129.03 (8)O1—Ca2—O1A—Ca2xviii90
P1iv—Ca1—O4—Ca1xv21.9 (4)O3xi—Ca2—O1A—Ca2xviii150.74 (6)
P1v—Ca1—O4—Ca1xv136.82 (8)O3xii—Ca2—O1A—Ca2xviii150.74 (6)
O4i—Ca1—O4—Ca2xii139.36 (10)O4xiii—Ca2—O1A—Ca2xviii0
O4ii—Ca1—O4—Ca2xii60.85 (12)Cl1—Ca2—O1A—Ca2xviii90
O2iii—Ca1—O4—Ca2xii21.19 (13)Cl1ix—Ca2—O1A—Ca2xviii90
O2iv—Ca1—O4—Ca2xii157.10 (17)Cl1xiv—Ca2—O1A—Ca2xviii90
O2v—Ca1—O4—Ca2xii95.54 (10)
Symmetry codes: (i) y+1, xy, z; (ii) x+y+1, x+1, z; (iii) xy+1, x, z+2; (iv) y, x+y, z+2; (v) x+1, y+1, z+2; (vi) y, x+y, z+1/2; (vii) xy+1, x, z+1/2; (viii) x+1, y+1, z+1/2; (ix) x, y, z+1/2; (x) x+1, y+1, z+1; (xi) xy+1, x, z1/2; (xii) xy+1, x, z+1; (xiii) y, x+y+1, z+1; (xiv) x+2, y+2, z+1; (xv) x, y, z+3/2; (xvi) x+1, y+1, z1/2; (xvii) y+2, xy+1, z; (xviii) x+y+1, x+2, z; (xix) x+2, y+2, z.
(1475l) top
Crystal data top
3(O4P)·0.29(Cl)·0.71(OH)·5(Ca)Dx = 3.192 Mg m3
Mr = 507.86Mo Kα radiation, λ = 0.7107 Å
Trigonal, P63/mCell parameters from 2894 reflections
Hall symbol: -P 6cθ = 3.9–27.4°
a = 9.431 (5) ŵ = 3.14 mm1
c = 6.860 (5) ÅT = 100 K
V = 528.4 (6) Å3Prism, colourless
Z = 20.11 × 0.08 × 0.04 mm
F(000) = 504.8
Data collection top
BRUKER APPEX-II CCD
diffractometer
588 independent reflections
Radiation source: fine-focus sealed tube542 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.019
ω and phi scansθmax = 30.6°, θmin = 2.5°
Absorption correction: multi-scan
BRUKER SADABS
h = 1313
Tmin = 0.672, Tmax = 1k = 1313
10188 measured reflectionsl = 99
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.037Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.085H atoms treated by a mixture of independent and constrained refinement
S = 1.22 w = 1/[σ2(Fo2) + (0.0235P)2 + 2.7715P]
where P = (Fo2 + 2Fc2)/3
588 reflections(Δ/σ)max = 0.001
48 parametersΔρmax = 1.67 e Å3
15 restraintsΔρmin = 1.18 e Å3
Crystal data top
3(O4P)·0.29(Cl)·0.71(OH)·5(Ca)Z = 2
Mr = 507.86Mo Kα radiation
Trigonal, P63/mµ = 3.14 mm1
a = 9.431 (5) ÅT = 100 K
c = 6.860 (5) Å0.11 × 0.08 × 0.04 mm
V = 528.4 (6) Å3
Data collection top
BRUKER APPEX-II CCD
diffractometer
588 independent reflections
Absorption correction: multi-scan
BRUKER SADABS
542 reflections with I > 2σ(I)
Tmin = 0.672, Tmax = 1Rint = 0.019
10188 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03715 restraints
wR(F2) = 0.085H atoms treated by a mixture of independent and constrained refinement
S = 1.22Δρmax = 1.67 e Å3
588 reflectionsΔρmin = 1.18 e Å3
48 parameters
Special details top

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ca10.33330.66671.00178 (14)0.0082 (2)
Ca20.74445 (12)0.75333 (11)0.250.0122 (2)
P10.60061 (12)0.63047 (12)0.750.0046 (2)
O20.4118 (4)0.5332 (4)0.750.0236 (8)
O30.6502 (4)0.7377 (3)0.5690 (4)0.0298 (7)
O40.6715 (4)0.5148 (3)0.750.0070 (5)
Cl1110.480 (2)0.0140.143 (4)
O1110.160 (4)0.021 (2)0.188 (10)
H1110.030 (5)0.025*0.188 (10)
O1A110.250.0185 (15)0.34 (2)
H1A110.106 (3)0.022*0.168 (10)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0093 (3)0.0093 (3)0.0059 (4)0.00465 (14)00
Ca20.0223 (4)0.0155 (4)0.0058 (4)0.0147 (4)00
P10.0064 (4)0.0055 (4)0.0033 (4)0.0041 (3)00
O20.0075 (14)0.0111 (15)0.054 (3)0.0061 (12)00
O30.064 (2)0.0271 (13)0.0179 (12)0.0373 (14)0.0269 (13)0.0170 (10)
O40.0084 (12)0.0078 (12)0.0076 (12)0.0062 (10)00
Cl10.0080.0080.0260.00400
O10.017 (2)0.017 (2)0.028 (4)0.0087 (12)00
O1A0.0142 (17)0.0142 (17)0.027 (3)0.0071 (8)00
Geometric parameters (Å, º) top
Ca1—O4i2.398 (2)P1—O41.538 (3)
Ca1—O4ii2.398 (2)P1—O21.542 (4)
Ca1—O4iii2.398 (2)P1—Ca2xiii3.110 (2)
Ca1—O2iv2.459 (3)P1—Ca1viii3.2115 (17)
Ca1—O2v2.459 (3)P1—Ca2xi3.280 (2)
Ca1—O22.459 (3)P1—Ca2x3.451 (2)
Ca1—O3vi2.759 (4)O2—Ca2x2.343 (4)
Ca1—O3vii2.759 (4)O2—Ca1viii2.459 (3)
Ca1—O3viii2.759 (4)O3—Ca2xiii2.557 (3)
Ca1—P1v3.2115 (17)O3—Ca1viii2.759 (4)
Ca1—P1iv3.2115 (17)O4—Ca1xv2.398 (2)
Ca1—P13.2115 (17)O4—Ca1iii2.398 (2)
Ca2—O3ix2.339 (3)O4—Ca2xi2.692 (3)
Ca2—O32.339 (3)Cl1—Cl1xiv0.28 (3)
Ca2—O2x2.343 (4)Cl1—Ca2xvi2.845 (8)
Ca2—O1A2.3693 (16)Cl1—Ca2xvii2.845 (8)
Ca2—O1ix2.448 (8)Cl1—Ca2xiv3.009 (9)
Ca2—O12.448 (8)Cl1—Ca2xi3.009 (9)
Ca2—O3xi2.557 (3)Cl1—Ca2xiii3.009 (9)
Ca2—O3xii2.557 (3)O1—O1ix1.23 (6)
Ca2—O4xiii2.692 (3)O1—Ca2xvi2.448 (8)
Ca2—Cl12.845 (8)O1—Ca2xvii2.448 (8)
Ca2—Cl1ix2.845 (8)O1—H10.89 (2)
Ca2—Cl1xiv3.009 (9)O1—H1A0.37 (4)
Ca2—H1A2.566 (8)O1A—Ca2xvi2.3693 (16)
P1—O3viii1.520 (3)O1A—Ca2xvii2.3693 (16)
P1—O31.520 (3)O1A—H1A0.99 (2)
O4i—Ca1—O4ii75.17 (9)O4xiii—Ca2—Cl1ix103.20 (7)
O4i—Ca1—O4iii75.17 (9)Cl1—Ca2—Cl1ix67.2 (5)
O4ii—Ca1—O4iii75.17 (9)O3ix—Ca2—Cl1xiv139.3 (2)
O4i—Ca1—O2iv92.10 (9)O3—Ca2—Cl1xiv66.7 (2)
O4ii—Ca1—O2iv153.91 (10)O2x—Ca2—Cl1xiv133.65 (16)
O4iii—Ca1—O2iv124.14 (10)O1A—Ca2—Cl1xiv38.1 (2)
O4i—Ca1—O2v124.14 (10)O1ix—Ca2—Cl1xiv23.5 (7)
O4ii—Ca1—O2v92.10 (9)O1—Ca2—Cl1xiv52.6 (7)
O4iii—Ca1—O2v153.91 (10)O3xi—Ca2—Cl1xiv65.52 (10)
O2iv—Ca1—O2v76.12 (10)O3xii—Ca2—Cl1xiv100.62 (13)
O4i—Ca1—O2153.91 (10)O4xiii—Ca2—Cl1xiv102.47 (6)
O4ii—Ca1—O2124.14 (10)Cl1—Ca2—Cl1xiv4.5 (4)
O4iii—Ca1—O292.10 (9)Cl1ix—Ca2—Cl1xiv71.67 (6)
O2iv—Ca1—O276.12 (10)O3ix—Ca2—H1A81.5 (4)
O2v—Ca1—O276.12 (10)O3—Ca2—H1A124.8 (4)
O4i—Ca1—O3vi69.28 (8)O2x—Ca2—H1A144.1 (3)
O4ii—Ca1—O3vi86.00 (9)O1A—Ca2—H1A22.6 (4)
O4iii—Ca1—O3vi142.99 (8)O1ix—Ca2—H1A37.1 (8)
O2iv—Ca1—O3vi68.10 (10)O1—Ca2—H1A8.0 (8)
O2v—Ca1—O3vi55.53 (9)O3xi—Ca2—H1A92.9 (2)
O2—Ca1—O3vi124.62 (9)O3xii—Ca2—H1A71.26 (19)
O4i—Ca1—O3vii86.00 (9)O4xiii—Ca2—H1A104.67 (8)
O4ii—Ca1—O3vii142.99 (8)Cl1—Ca2—H1A56.2 (5)
O4iii—Ca1—O3vii69.28 (8)Cl1ix—Ca2—H1A11.0 (5)
O2iv—Ca1—O3vii55.53 (9)Cl1xiv—Ca2—H1A60.6 (5)
O2v—Ca1—O3vii124.62 (9)O3viii—P1—O3109.5 (2)
O2—Ca1—O3vii68.10 (10)O3viii—P1—O4111.93 (11)
O3vi—Ca1—O3vii116.97 (3)O3—P1—O4111.93 (11)
O4i—Ca1—O3viii142.99 (8)O3viii—P1—O2105.99 (16)
O4ii—Ca1—O3viii69.28 (8)O3—P1—O2105.99 (16)
O4iii—Ca1—O3viii86.00 (9)O4—P1—O2111.11 (18)
O2iv—Ca1—O3viii124.62 (9)O3viii—P1—Ca2xiii54.86 (11)
O2v—Ca1—O3viii68.10 (10)O3—P1—Ca2xiii54.86 (11)
O2—Ca1—O3viii55.53 (9)O4—P1—Ca2xiii134.23 (12)
O3vi—Ca1—O3viii116.97 (3)O2—P1—Ca2xiii114.66 (13)
O3vii—Ca1—O3viii116.97 (3)O3viii—P1—Ca1viii111.43 (11)
O4i—Ca1—P1v97.48 (7)O3—P1—Ca1viii59.12 (13)
O4ii—Ca1—P1v92.40 (7)O4—P1—Ca1viii135.89 (8)
O4iii—Ca1—P1v166.75 (6)O2—P1—Ca1viii47.87 (9)
O2iv—Ca1—P1v66.34 (8)Ca2xiii—P1—Ca1viii79.39 (3)
O2v—Ca1—P1v27.71 (8)O3viii—P1—Ca159.12 (14)
O2—Ca1—P1v98.82 (8)O3—P1—Ca1111.43 (11)
O3vi—Ca1—P1v28.21 (5)O4—P1—Ca1135.89 (8)
O3vii—Ca1—P1v121.86 (6)O2—P1—Ca147.87 (9)
O3viii—Ca1—P1v93.97 (6)Ca2xiii—P1—Ca179.39 (3)
O4i—Ca1—P1iv92.40 (7)Ca1viii—P1—Ca165.07 (6)
O4ii—Ca1—P1iv166.75 (6)O3viii—P1—Ca2xi81.97 (13)
O4iii—Ca1—P1iv97.48 (7)O3—P1—Ca2xi81.97 (13)
O2iv—Ca1—P1iv27.71 (8)O4—P1—Ca2xi54.37 (11)
O2v—Ca1—P1iv98.82 (8)O2—P1—Ca2xi165.47 (14)
O2—Ca1—P1iv66.34 (8)Ca2xiii—P1—Ca2xi79.87 (4)
O3vi—Ca1—P1iv93.97 (6)Ca1viii—P1—Ca2xi141.03 (3)
O3vii—Ca1—P1iv28.21 (5)Ca1—P1—Ca2xi141.03 (3)
O3viii—Ca1—P1iv121.86 (6)O3viii—P1—Ca2x120.86 (14)
P1v—Ca1—P1iv93.79 (4)O3—P1—Ca2x120.86 (14)
O4i—Ca1—P1166.75 (6)O4—P1—Ca2x76.86 (12)
O4ii—Ca1—P197.48 (7)Ca2xiii—P1—Ca2x148.91 (4)
O4iii—Ca1—P192.40 (7)Ca1viii—P1—Ca2x74.51 (2)
O2iv—Ca1—P198.82 (8)Ca1—P1—Ca2x74.51 (2)
O2v—Ca1—P166.34 (8)Ca2xi—P1—Ca2x131.23 (4)
O2—Ca1—P127.71 (8)P1—O2—Ca2x124.02 (18)
O3vi—Ca1—P1121.86 (6)P1—O2—Ca1104.42 (13)
O3vii—Ca1—P193.97 (6)Ca2x—O2—Ca1114.42 (10)
O3viii—Ca1—P128.21 (5)P1—O2—Ca1viii104.42 (13)
P1v—Ca1—P193.79 (4)Ca2x—O2—Ca1viii114.42 (10)
P1iv—Ca1—P193.79 (4)Ca1—O2—Ca1viii89.23 (12)
O3ix—Ca2—O3138.68 (18)P1—O3—Ca2141.91 (14)
O3ix—Ca2—O2x85.83 (8)P1—O3—Ca2xiii96.06 (14)
O3—Ca2—O2x85.83 (8)Ca2—O3—Ca2xiii116.66 (11)
O3ix—Ca2—O1A103.28 (9)P1—O3—Ca1viii92.67 (15)
O3—Ca2—O1A103.28 (9)Ca2—O3—Ca1viii100.48 (12)
O2x—Ca2—O1A151.25 (9)Ca2xiii—O3—Ca1viii98.77 (8)
O3ix—Ca2—O1ix117.2 (7)P1—O4—Ca1xv130.24 (8)
O3—Ca2—O1ix89.3 (7)P1—O4—Ca1iii130.24 (8)
O2x—Ca2—O1ix148.1 (3)Ca1xv—O4—Ca1iii90.46 (11)
O1A—Ca2—O1ix14.5 (7)P1—O4—Ca2xi97.96 (13)
O3ix—Ca2—O189.3 (7)Ca1xv—O4—Ca2xi100.85 (8)
O3—Ca2—O1117.2 (7)Ca1iii—O4—Ca2xi100.85 (8)
O2x—Ca2—O1148.1 (3)Cl1xiv—Cl1—Ca2123.6 (3)
O1A—Ca2—O114.5 (7)Cl1xiv—Cl1—Ca2xvi123.6 (2)
O1ix—Ca2—O129.1 (14)Ca2—Cl1—Ca2xvi92.3 (3)
O3ix—Ca2—O3xi135.94 (10)Cl1xiv—Cl1—Ca2xvii123.6 (2)
O3—Ca2—O3xi79.05 (7)Ca2—Cl1—Ca2xvii92.3 (3)
O2x—Ca2—O3xi73.35 (10)Ca2xvi—Cl1—Ca2xvii92.3 (3)
O1A—Ca2—O3xi81.60 (8)Cl1xiv—Cl1—Ca2xiv51.94 (19)
O1ix—Ca2—O3xi74.7 (3)Ca2—Cl1—Ca2xiv175.5 (4)
O1—Ca2—O3xi88.9 (4)Ca2xvi—Cl1—Ca2xiv90.77 (5)
O3ix—Ca2—O3xii79.05 (7)Ca2xvii—Cl1—Ca2xiv90.77 (5)
O3—Ca2—O3xii135.94 (10)Cl1xiv—Cl1—Ca2xi51.9 (2)
O2x—Ca2—O3xii73.35 (10)Ca2—Cl1—Ca2xi90.77 (5)
O1A—Ca2—O3xii81.60 (8)Ca2xvi—Cl1—Ca2xi90.77 (5)
O1ix—Ca2—O3xii88.9 (4)Ca2xvii—Cl1—Ca2xi175.5 (4)
O1—Ca2—O3xii74.7 (3)Ca2xiv—Cl1—Ca2xi86.0 (3)
O3xi—Ca2—O3xii58.09 (12)Cl1xiv—Cl1—Ca2xiii51.9 (2)
O3ix—Ca2—O4xiii71.31 (8)Ca2—Cl1—Ca2xiii90.77 (5)
O3—Ca2—O4xiii71.31 (8)Ca2xvi—Cl1—Ca2xiii175.5 (4)
O2x—Ca2—O4xiii102.84 (10)Ca2xvii—Cl1—Ca2xiii90.77 (5)
O1A—Ca2—O4xiii105.91 (7)Ca2xiv—Cl1—Ca2xiii86.0 (3)
O1ix—Ca2—O4xiii105.39 (8)Ca2xi—Cl1—Ca2xiii86.0 (3)
O1—Ca2—O4xiii105.39 (8)O1ix—O1—Ca2xvi75.5 (7)
O3xi—Ca2—O4xiii150.34 (6)O1ix—O1—Ca275.5 (7)
O3xii—Ca2—O4xiii150.34 (6)Ca2xvi—O1—Ca2113.9 (5)
O3ix—Ca2—Cl1135.2 (2)O1ix—O1—Ca2xvii75.5 (7)
O3—Ca2—Cl170.9 (2)Ca2xvi—O1—Ca2xvii113.9 (5)
O2x—Ca2—Cl1136.90 (17)Ca2—O1—Ca2xvii113.9 (5)
O1A—Ca2—Cl133.6 (2)O1ix—O1—H1180.000 (17)
O1ix—Ca2—Cl119.1 (7)Ca2xvi—O1—H1104.5 (7)
O1—Ca2—Cl148.1 (8)Ca2—O1—H1104.5 (7)
O3xi—Ca2—Cl167.02 (11)Ca2xvii—O1—H1104.5 (7)
O3xii—Ca2—Cl198.45 (14)O1ix—O1—H1A180.00 (3)
O4xiii—Ca2—Cl1103.20 (7)Ca2xvi—O1—H1A104.5 (7)
O3ix—Ca2—Cl1ix70.9 (2)Ca2—O1—H1A104.5 (7)
O3—Ca2—Cl1ix135.2 (2)Ca2xvii—O1—H1A104.5 (7)
O2x—Ca2—Cl1ix136.90 (17)Ca2—O1A—Ca2xvi120
O1A—Ca2—Cl1ix33.6 (2)Ca2—O1A—Ca2xvii120
O1ix—Ca2—Cl1ix48.1 (8)Ca2xvi—O1A—Ca2xvii120
O1—Ca2—Cl1ix19.1 (7)Ca2—O1A—H1A90.000 (8)
O3xi—Ca2—Cl1ix98.45 (14)Ca2xvi—O1A—H1A90.000 (6)
O3xii—Ca2—Cl1ix67.02 (11)Ca2xvii—O1A—H1A90.000 (2)
O4i—Ca1—P1—O3viii56.9 (3)O1A—Ca2—O3—P1119.5 (3)
O4ii—Ca1—P1—O3viii1.59 (13)O1ix—Ca2—O3—P1115.6 (4)
O4iii—Ca1—P1—O3viii76.94 (14)O1—Ca2—O3—P1124.0 (4)
O2iv—Ca1—P1—O3viii157.97 (14)O3xi—Ca2—O3—P141.0 (4)
O2v—Ca1—P1—O3viii87.42 (14)O3xii—Ca2—O3—P127.9 (5)
O2—Ca1—P1—O3viii166.87 (18)O4xiii—Ca2—O3—P1137.9 (4)
O3vi—Ca1—P1—O3viii88.34 (7)Cl1—Ca2—O3—P1110.3 (4)
O3vii—Ca1—P1—O3viii146.32 (13)Cl1ix—Ca2—O3—P1132.0 (3)
P1v—Ca1—P1—O3viii91.34 (13)Cl1xiv—Ca2—O3—P1108.9 (4)
P1iv—Ca1—P1—O3viii174.60 (12)O3ix—Ca2—O3—Ca2xiii102.0 (2)
O4i—Ca1—P1—O3157.5 (3)O2x—Ca2—O3—Ca2xiii179.15 (15)
O4ii—Ca1—P1—O3102.19 (16)O1A—Ca2—O3—Ca2xiii26.77 (14)
O4iii—Ca1—P1—O3177.54 (16)O1ix—Ca2—O3—Ca2xiii30.7 (2)
O2iv—Ca1—P1—O357.37 (17)O1—Ca2—O3—Ca2xiii22.3 (3)
O2v—Ca1—P1—O313.18 (16)O3xi—Ca2—O3—Ca2xiii105.31 (7)
O2—Ca1—P1—O392.53 (19)O3xii—Ca2—O3—Ca2xiii118.38 (8)
O3vi—Ca1—P1—O312.3 (2)O4xiii—Ca2—O3—Ca2xiii75.80 (13)
O3vii—Ca1—P1—O3113.08 (16)Cl1—Ca2—O3—Ca2xiii36.04 (13)
O3viii—Ca1—P1—O3100.6 (3)Cl1ix—Ca2—O3—Ca2xiii14.3 (2)
P1v—Ca1—P1—O39.26 (15)Cl1xiv—Ca2—O3—Ca2xiii37.41 (13)
P1iv—Ca1—P1—O384.80 (15)O3ix—Ca2—O3—Ca1viii3.4 (2)
O4i—Ca1—P1—O433.6 (2)O2x—Ca2—O3—Ca1viii75.40 (10)
O4ii—Ca1—P1—O488.89 (17)O1A—Ca2—O3—Ca1viii132.22 (6)
O4iii—Ca1—P1—O413.54 (19)O1ix—Ca2—O3—Ca1viii136.2 (2)
O2iv—Ca1—P1—O4111.55 (16)O1—Ca2—O3—Ca1viii127.8 (2)
O2v—Ca1—P1—O4177.91 (15)O3xi—Ca2—O3—Ca1viii149.23 (9)
O2—Ca1—P1—O476.39 (19)O3xii—Ca2—O3—Ca1viii136.17 (17)
O3vi—Ca1—P1—O4178.82 (15)O4xiii—Ca2—O3—Ca1viii29.66 (8)
O3vii—Ca1—P1—O455.84 (15)Cl1—Ca2—O3—Ca1viii141.49 (10)
O3viii—Ca1—P1—O490.48 (18)Cl1ix—Ca2—O3—Ca1viii119.75 (16)
P1v—Ca1—P1—O4178.18 (14)Cl1xiv—Ca2—O3—Ca1viii142.86 (11)
P1iv—Ca1—P1—O484.12 (14)O3viii—P1—O4—Ca1xv173.3 (2)
O4i—Ca1—P1—O2110.0 (3)O3—P1—O4—Ca1xv49.8 (3)
O4ii—Ca1—P1—O2165.28 (14)O2—P1—O4—Ca1xv68.44 (17)
O4iii—Ca1—P1—O289.93 (14)Ca2xiii—P1—O4—Ca1xv111.56 (17)
O2iv—Ca1—P1—O235.16 (15)Ca1viii—P1—O4—Ca1xv17.9 (3)
O2v—Ca1—P1—O2105.70 (19)Ca1—P1—O4—Ca1xv119.04 (10)
O3vi—Ca1—P1—O2104.79 (15)Ca2xi—P1—O4—Ca1xv111.56 (17)
O3vii—Ca1—P1—O220.55 (13)Ca2x—P1—O4—Ca1xv68.44 (17)
O3viii—Ca1—P1—O2166.87 (18)O3viii—P1—O4—Ca1iii49.8 (3)
P1v—Ca1—P1—O2101.79 (13)O3—P1—O4—Ca1iii173.3 (2)
P1iv—Ca1—P1—O27.73 (12)O2—P1—O4—Ca1iii68.44 (17)
O4i—Ca1—P1—Ca2xiii112.1 (3)Ca2xiii—P1—O4—Ca1iii111.56 (17)
O4ii—Ca1—P1—Ca2xiii56.83 (6)Ca1viii—P1—O4—Ca1iii119.04 (10)
O4iii—Ca1—P1—Ca2xiii132.17 (6)Ca1—P1—O4—Ca1iii17.9 (3)
O2iv—Ca1—P1—Ca2xiii102.73 (8)Ca2xi—P1—O4—Ca1iii111.56 (17)
O2v—Ca1—P1—Ca2xiii32.19 (7)Ca2x—P1—O4—Ca1iii68.44 (17)
O2—Ca1—P1—Ca2xiii137.89 (13)O3viii—P1—O4—Ca2xi61.72 (16)
O3vi—Ca1—P1—Ca2xiii33.10 (7)O3—P1—O4—Ca2xi61.72 (16)
O3vii—Ca1—P1—Ca2xiii158.44 (6)O2—P1—O4—Ca2xi180
O3viii—Ca1—P1—Ca2xiii55.24 (12)Ca2xiii—P1—O4—Ca2xi0
P1v—Ca1—P1—Ca2xiii36.10 (3)Ca1viii—P1—O4—Ca2xi129.41 (10)
P1iv—Ca1—P1—Ca2xiii130.16 (3)Ca1—P1—O4—Ca2xi129.41 (10)
O4i—Ca1—P1—Ca1viii164.7 (3)Ca2x—P1—O4—Ca2xi180
O4ii—Ca1—P1—Ca1viii139.96 (6)O3ix—Ca2—Cl1—Cl1xiv157.68 (14)
O4iii—Ca1—P1—Ca1viii144.69 (6)O3—Ca2—Cl1—Cl1xiv16.45 (7)
O2iv—Ca1—P1—Ca1viii19.60 (8)O2x—Ca2—Cl1—Cl1xiv44.7 (2)
O2v—Ca1—P1—Ca1viii50.94 (7)O1A—Ca2—Cl1—Cl1xiv180.000 (6)
O2—Ca1—P1—Ca1viii54.76 (12)O1ix—Ca2—Cl1—Cl1xiv180.000 (5)
O3vi—Ca1—P1—Ca1viii50.03 (7)O1—Ca2—Cl1—Cl1xiv180.000 (6)
O3vii—Ca1—P1—Ca1viii75.31 (5)O3xi—Ca2—Cl1—Cl1xiv69.43 (11)
O3viii—Ca1—P1—Ca1viii138.37 (12)O3xii—Ca2—Cl1—Cl1xiv119.38 (7)
P1v—Ca1—P1—Ca1viii47.03 (2)O4xiii—Ca2—Cl1—Cl1xiv81.03 (6)
P1iv—Ca1—P1—Ca1viii47.03 (2)Cl1ix—Ca2—Cl1—Cl1xiv180.000 (6)
O4i—Ca1—P1—Ca2xi53.2 (3)O3ix—Ca2—Cl1—Ca2xvi68.52 (14)
O4ii—Ca1—P1—Ca2xi2.09 (8)O3—Ca2—Cl1—Ca2xvi150.2 (2)
O4iii—Ca1—P1—Ca2xi73.26 (8)O2x—Ca2—Cl1—Ca2xvi89.0 (4)
O2iv—Ca1—P1—Ca2xi161.65 (9)O1A—Ca2—Cl1—Ca2xvi46.21 (18)
O2v—Ca1—P1—Ca2xi91.11 (9)O1ix—Ca2—Cl1—Ca2xvi46.21 (18)
O2—Ca1—P1—Ca2xi163.19 (14)O1—Ca2—Cl1—Ca2xvi46.21 (18)
O3vi—Ca1—P1—Ca2xi92.02 (9)O3xi—Ca2—Cl1—Ca2xvi64.36 (11)
O3vii—Ca1—P1—Ca2xi142.64 (7)O3xii—Ca2—Cl1—Ca2xvi14.4 (2)
O3viii—Ca1—P1—Ca2xi3.68 (12)O4xiii—Ca2—Cl1—Ca2xvi145.18 (13)
P1v—Ca1—P1—Ca2xi95.02 (7)Cl1ix—Ca2—Cl1—Ca2xvi46.21 (18)
P1iv—Ca1—P1—Ca2xi170.92 (5)Cl1xiv—Ca2—Cl1—Ca2xvi133.79 (18)
O4i—Ca1—P1—Ca2x84.9 (3)O3ix—Ca2—Cl1—Ca2xvii23.9 (3)
O4ii—Ca1—P1—Ca2x140.23 (6)O3—Ca2—Cl1—Ca2xvii117.34 (17)
O4iii—Ca1—P1—Ca2x64.88 (7)O2x—Ca2—Cl1—Ca2xvii178.54 (10)
O2iv—Ca1—P1—Ca2x60.22 (8)O1A—Ca2—Cl1—Ca2xvii46.21 (18)
O2v—Ca1—P1—Ca2x130.76 (7)O1ix—Ca2—Cl1—Ca2xvii46.21 (18)
O2—Ca1—P1—Ca2x25.06 (12)O1—Ca2—Cl1—Ca2xvii46.21 (18)
O3vi—Ca1—P1—Ca2x129.85 (7)O3xi—Ca2—Cl1—Ca2xvii156.8 (3)
O3vii—Ca1—P1—Ca2x4.51 (5)O3xii—Ca2—Cl1—Ca2xvii106.83 (16)
O3viii—Ca1—P1—Ca2x141.81 (12)O4xiii—Ca2—Cl1—Ca2xvii52.8 (2)
P1v—Ca1—P1—Ca2x126.85 (3)Cl1ix—Ca2—Cl1—Ca2xvii46.21 (18)
P1iv—Ca1—P1—Ca2x32.79 (2)Cl1xiv—Ca2—Cl1—Ca2xvii133.79 (18)
O3viii—P1—O2—Ca2x121.82 (11)O3ix—Ca2—Cl1—Ca2xi159.32 (13)
O3—P1—O2—Ca2x121.82 (11)O3—Ca2—Cl1—Ca2xi59.45 (19)
O4—P1—O2—Ca2x0O2x—Ca2—Cl1—Ca2xi1.8 (3)
Ca2xiii—P1—O2—Ca2x180O1A—Ca2—Cl1—Ca2xi137.01 (15)
Ca1viii—P1—O2—Ca2x133.52 (9)O1ix—Ca2—Cl1—Ca2xi137.01 (15)
Ca1—P1—O2—Ca2x133.52 (9)O1—Ca2—Cl1—Ca2xi137.01 (15)
Ca2xi—P1—O2—Ca2x0O3xi—Ca2—Cl1—Ca2xi26.44 (9)
O3viii—P1—O2—Ca111.70 (16)O3xii—Ca2—Cl1—Ca2xi76.38 (19)
O3—P1—O2—Ca1104.67 (12)O4xiii—Ca2—Cl1—Ca2xi124.03 (11)
O4—P1—O2—Ca1133.52 (9)Cl1ix—Ca2—Cl1—Ca2xi137.01 (15)
Ca2xiii—P1—O2—Ca146.48 (9)Cl1xiv—Ca2—Cl1—Ca2xi42.99 (16)
Ca1viii—P1—O2—Ca192.97 (17)O3ix—Ca2—Cl1—Ca2xiii114.7 (3)
Ca2xi—P1—O2—Ca1133.52 (9)O3—Ca2—Cl1—Ca2xiii26.54 (15)
Ca2x—P1—O2—Ca1133.52 (9)O2x—Ca2—Cl1—Ca2xiii87.74 (12)
O3viii—P1—O2—Ca1viii104.67 (12)O1A—Ca2—Cl1—Ca2xiii137.01 (15)
O3—P1—O2—Ca1viii11.70 (16)O1ix—Ca2—Cl1—Ca2xiii137.01 (15)
O4—P1—O2—Ca1viii133.52 (9)O1—Ca2—Cl1—Ca2xiii137.01 (15)
Ca2xiii—P1—O2—Ca1viii46.48 (9)O3xi—Ca2—Cl1—Ca2xiii112.4 (3)
Ca1—P1—O2—Ca1viii92.97 (17)O3xii—Ca2—Cl1—Ca2xiii162.37 (14)
Ca2xi—P1—O2—Ca1viii133.52 (9)O4xiii—Ca2—Cl1—Ca2xiii38.0 (2)
Ca2x—P1—O2—Ca1viii133.52 (9)Cl1ix—Ca2—Cl1—Ca2xiii137.01 (15)
O4i—Ca1—O2—P1150.66 (15)Cl1xiv—Ca2—Cl1—Ca2xiii42.99 (16)
O4ii—Ca1—O2—P117.72 (17)O3ix—Ca2—O1—O1ix164.47 (7)
O4iii—Ca1—O2—P191.18 (13)O3—Ca2—O1—O1ix17.52 (13)
O2iv—Ca1—O2—P1144.11 (14)O2x—Ca2—O1—O1ix114.6 (10)
O2v—Ca1—O2—P165.27 (18)O1A—Ca2—O1—O1ix0.000 (9)
O3vi—Ca1—O2—P193.73 (13)O3xi—Ca2—O1—O1ix59.56 (6)
O3vii—Ca1—O2—P1157.83 (14)O3xii—Ca2—O1—O1ix116.69 (18)
O3viii—Ca1—O2—P17.48 (10)O4xiii—Ca2—O1—O1ix94.09 (19)
P1v—Ca1—O2—P181.29 (11)Cl1—Ca2—O1—O1ix0.0000 (10)
P1iv—Ca1—O2—P1171.58 (14)Cl1ix—Ca2—O1—O1ix180.000 (7)
O4i—Ca1—O2—Ca2x12.0 (2)Cl1xiv—Ca2—O1—O1ix0.000 (5)
O4ii—Ca1—O2—Ca2x120.97 (12)O3ix—Ca2—O1—Ca2xvi129.0 (10)
O4iii—Ca1—O2—Ca2x47.51 (12)O3—Ca2—O1—Ca2xvi84.0 (9)
O2iv—Ca1—O2—Ca2x77.20 (17)O2x—Ca2—O1—Ca2xvi48 (2)
O2v—Ca1—O2—Ca2x156.04 (14)O1A—Ca2—O1—Ca2xvi66.5 (10)
O3vi—Ca1—O2—Ca2x127.58 (10)O1ix—Ca2—O1—Ca2xvi66.5 (10)
O3vii—Ca1—O2—Ca2x19.14 (9)O3xi—Ca2—O1—Ca2xvi7.0 (10)
O3viii—Ca1—O2—Ca2x131.20 (13)O3xii—Ca2—O1—Ca2xvi50.2 (8)
P1v—Ca1—O2—Ca2x140.03 (9)O4xiii—Ca2—O1—Ca2xvi160.6 (8)
P1iv—Ca1—O2—Ca2x49.74 (9)Cl1—Ca2—O1—Ca2xvi66.5 (10)
P1—Ca1—O2—Ca2x138.69 (18)Cl1ix—Ca2—O1—Ca2xvi113.5 (10)
O4i—Ca1—O2—Ca1viii104.65 (17)Cl1xiv—Ca2—O1—Ca2xvi66.5 (10)
O4ii—Ca1—O2—Ca1viii122.41 (9)O3ix—Ca2—O1—Ca2xvii98.0 (10)
O4iii—Ca1—O2—Ca1viii164.13 (10)O3—Ca2—O1—Ca2xvii49.0 (11)
O2iv—Ca1—O2—Ca1viii39.42 (3)O2x—Ca2—O1—Ca2xvii178.91 (9)
O2v—Ca1—O2—Ca1viii39.42 (3)O1A—Ca2—O1—Ca2xvii66.5 (10)
O3vi—Ca1—O2—Ca1viii10.96 (15)O1ix—Ca2—O1—Ca2xvii66.5 (10)
O3vii—Ca1—O2—Ca1viii97.48 (10)O3xi—Ca2—O1—Ca2xvii126.1 (10)
O3viii—Ca1—O2—Ca1viii112.18 (13)O3xii—Ca2—O1—Ca2xvii176.8 (11)
P1v—Ca1—O2—Ca1viii23.41 (9)O4xiii—Ca2—O1—Ca2xvii27.6 (12)
P1iv—Ca1—O2—Ca1viii66.88 (7)Cl1—Ca2—O1—Ca2xvii66.5 (10)
P1—Ca1—O2—Ca1viii104.69 (16)Cl1ix—Ca2—O1—Ca2xvii113.5 (10)
O3viii—P1—O3—Ca2145.37 (19)Cl1xiv—Ca2—O1—Ca2xvii66.5 (10)
O4—P1—O3—Ca220.6 (4)O3ix—Ca2—O1A—Ca2xvi105.96 (7)
O2—P1—O3—Ca2100.7 (3)O3—Ca2—O1A—Ca2xvi105.96 (7)
Ca2xiii—P1—O3—Ca2150.1 (4)O2x—Ca2—O1A—Ca2xvi0
Ca1viii—P1—O3—Ca2110.8 (4)O1ix—Ca2—O1A—Ca2xvi90
Ca1—P1—O3—Ca2151.1 (3)O1—Ca2—O1A—Ca2xvi90
Ca2xi—P1—O3—Ca266.9 (3)O3xi—Ca2—O1A—Ca2xvi29.39 (6)
Ca2x—P1—O3—Ca266.8 (4)O3xii—Ca2—O1A—Ca2xvi29.39 (6)
O3viii—P1—O3—Ca2xiii4.7 (3)O4xiii—Ca2—O1A—Ca2xvi180
O4—P1—O3—Ca2xiii129.51 (13)Cl1—Ca2—O1A—Ca2xvi90
O2—P1—O3—Ca2xiii109.21 (15)Cl1ix—Ca2—O1A—Ca2xvi90
Ca1viii—P1—O3—Ca2xiii99.12 (10)Cl1xiv—Ca2—O1A—Ca2xvi90
Ca1—P1—O3—Ca2xiii58.79 (14)O3ix—Ca2—O1A—Ca2xvii74.04 (7)
Ca2xi—P1—O3—Ca2xiii83.22 (10)O3—Ca2—O1A—Ca2xvii74.04 (7)
Ca2x—P1—O3—Ca2xiii143.07 (7)O2x—Ca2—O1A—Ca2xvii180
O3viii—P1—O3—Ca1viii103.85 (19)O1ix—Ca2—O1A—Ca2xvii90
O4—P1—O3—Ca1viii131.38 (12)O1—Ca2—O1A—Ca2xvii90
O2—P1—O3—Ca1viii10.09 (15)O3xi—Ca2—O1A—Ca2xvii150.61 (6)
Ca2xiii—P1—O3—Ca1viii99.12 (10)O3xii—Ca2—O1A—Ca2xvii150.61 (6)
Ca1—P1—O3—Ca1viii40.33 (11)O4xiii—Ca2—O1A—Ca2xvii0
Ca2xi—P1—O3—Ca1viii177.66 (8)Cl1—Ca2—O1A—Ca2xvii90
Ca2x—P1—O3—Ca1viii43.95 (11)Cl1ix—Ca2—O1A—Ca2xvii90
O3ix—Ca2—O3—P1111.7 (3)Cl1xiv—Ca2—O1A—Ca2xvii90
O2x—Ca2—O3—P132.8 (3)
Symmetry codes: (i) xy, x, z+2; (ii) y, x+y+1, z+2; (iii) x+1, y+1, z+2; (iv) x+y, x+1, z; (v) y+1, xy+1, z; (vi) y+1, xy+1, z+3/2; (vii) x+y, x+1, z+3/2; (viii) x, y, z+3/2; (ix) x, y, z+1/2; (x) x+1, y+1, z+1; (xi) xy+1, x, z+1; (xii) xy+1, x, z1/2; (xiii) y, x+y+1, z+1; (xiv) x+2, y+2, z+1; (xv) x+1, y+1, z1/2; (xvi) y+2, xy+1, z; (xvii) x+y+1, x+2, z.
(1475r) top
Crystal data top
3(O4P)·0.28(Cl)·0.72(OH)·5(Ca)Dx = 3.184 Mg m3
Mr = 507.8Mo Kα radiation, λ = 0.7107 Å
Trigonal, P63/mCell parameters from 1989 reflections
Hall symbol: -P 6cθ = 2.5–26.4°
a = 9.4284 (8) ŵ = 3.13 mm1
c = 6.8756 (7) ÅT = 293 K
V = 529.32 (12) Å3Prism, colourless
Z = 20.29 × 0.09 × 0.03 mm
F(000) = 504.8
Data collection top
BRUKER APPEX-II CCD
diffractometer
393 independent reflections
Radiation source: fine-focus sealed tube351 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.038
ω and phi scansθmax = 26.3°, θmin = 2.5°
Absorption correction: multi-scan
BRUKER SADABS
h = 1111
Tmin = 0.772, Tmax = 1k = 1111
2393 measured reflectionsl = 88
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.033Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.081H atoms treated by a mixture of independent and constrained refinement
S = 1.07 w = 1/[σ2(Fo2) + (0.0408P)2 + 1.7689P]
where P = (Fo2 + 2Fc2)/3
393 reflections(Δ/σ)max < 0.001
47 parametersΔρmax = 0.84 e Å3
32 restraintsΔρmin = 0.60 e Å3
Crystal data top
3(O4P)·0.28(Cl)·0.72(OH)·5(Ca)Z = 2
Mr = 507.8Mo Kα radiation
Trigonal, P63/mµ = 3.13 mm1
a = 9.4284 (8) ÅT = 293 K
c = 6.8756 (7) Å0.29 × 0.09 × 0.03 mm
V = 529.32 (12) Å3
Data collection top
BRUKER APPEX-II CCD
diffractometer
393 independent reflections
Absorption correction: multi-scan
BRUKER SADABS
351 reflections with I > 2σ(I)
Tmin = 0.772, Tmax = 1Rint = 0.038
2393 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03332 restraints
wR(F2) = 0.081H atoms treated by a mixture of independent and constrained refinement
S = 1.07Δρmax = 0.84 e Å3
393 reflectionsΔρmin = 0.60 e Å3
47 parameters
Special details top

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ca10.66670.33330.99827 (18)0.0125 (3)
Ca20.74514 (12)0.75420 (11)0.250.0163 (3)
P10.60124 (12)0.63086 (13)0.750.0075 (3)
O20.4133 (4)0.5345 (4)0.750.0296 (10)
O30.6512 (4)0.7377 (3)0.5700 (4)0.0351 (8)
O40.6714 (4)0.5148 (4)0.750.0114 (7)
Cl1110.473 (3)0.029 (3)0.14
O1110.173 (4)0.028 (3)0.19
H1110.044 (5)0.034*0.19
O1A110.250.029 (3)0.34
H1A110.107 (3)0.034*0.17
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0135 (4)0.0135 (4)0.0103 (6)0.00677 (19)00
Ca20.0260 (6)0.0183 (5)0.0120 (6)0.0166 (4)00
P10.0085 (6)0.0071 (5)0.0082 (6)0.0048 (4)00
O20.0111 (16)0.0167 (17)0.064 (3)0.0089 (15)00
O30.069 (2)0.0331 (15)0.0242 (16)0.0415 (15)0.0296 (15)0.0195 (13)
O40.0140 (15)0.0122 (15)0.0109 (17)0.0088 (13)00
Cl10.029 (2)0.029 (2)0.029 (8)0.0145 (10)00
O10.028 (3)0.028 (3)0.029 (8)0.0141 (13)00
O1A0.028 (2)0.028 (2)0.029 (7)0.0141 (11)00
Geometric parameters (Å, º) top
Ca1—O4i2.402 (2)P1—O21.535 (4)
Ca1—O4ii2.402 (2)P1—O41.535 (3)
Ca1—O42.402 (2)P1—Ca2xiii3.1068 (14)
Ca1—O2iii2.461 (3)P1—Ca1xvi3.2160 (11)
Ca1—O2iv2.461 (3)P1—Ca1v3.2160 (11)
Ca1—O2v2.461 (3)P1—Ca2xi3.2714 (14)
Ca1—O3vi2.769 (3)P1—Ca2x3.4625 (14)
Ca1—O3vii2.769 (4)O2—Ca2x2.361 (4)
Ca1—O3viii2.769 (3)O2—Ca1v2.461 (3)
Ca1—P1iii3.2160 (11)O2—Ca1xvi2.461 (3)
Ca1—P1iv3.2160 (11)O3—Ca2xiii2.556 (3)
Ca1—P1v3.2160 (11)O3—Ca1xvi2.769 (3)
Ca2—O3ix2.347 (3)O4—Ca1xv2.402 (2)
Ca2—O32.347 (3)O4—Ca2xi2.693 (3)
Ca2—O2x2.361 (4)Cl1—Cl1xiv0.37 (4)
Ca2—O1A2.3614 (10)Cl1—Ca2xvii2.815 (11)
Ca2—O1ix2.420 (6)Cl1—Ca2xviii2.815 (11)
Ca2—O12.420 (6)Cl1—Ca2xiv3.034 (13)
Ca2—O3xi2.556 (3)Cl1—Ca2xiii3.034 (13)
Ca2—O3xii2.556 (3)Cl1—Ca2xi3.034 (13)
Ca2—O4xiii2.693 (3)O1—O1ix1.06 (6)
Ca2—Cl12.815 (11)O1—Ca2xvii2.420 (6)
Ca2—Cl1ix2.815 (11)O1—Ca2xviii2.420 (6)
Ca2—Cl1xiv3.034 (13)O1—H10.89 (2)
Ca2—H12.755 (18)O1—H1A0.45 (4)
Ca2—H1A2.557 (8)O1A—Ca2xvii2.3614 (10)
P1—O3xv1.515 (3)O1A—Ca2xviii2.3614 (10)
P1—O31.515 (3)O1A—H1A0.98 (2)
O4i—Ca1—O4ii75.06 (9)O3xi—Ca2—Cl1xiv65.23 (12)
O4i—Ca1—O475.06 (9)O3xii—Ca2—Cl1xiv100.91 (17)
O4ii—Ca1—O475.06 (9)O4xiii—Ca2—Cl1xiv102.46 (8)
O4i—Ca1—O2iii92.31 (8)Cl1—Ca2—Cl1xiv5.9 (7)
O4ii—Ca1—O2iii154.20 (11)Cl1ix—Ca2—Cl1xiv71.88 (5)
O4—Ca1—O2iii123.99 (10)O3ix—Ca2—H173.4 (6)
O4i—Ca1—O2iv123.99 (10)O3—Ca2—H1132.8 (6)
O4ii—Ca1—O2iv92.31 (8)O2x—Ca2—H1138.8 (4)
O4—Ca1—O2iv154.20 (11)O1A—Ca2—H131.0 (6)
O2iii—Ca1—O2iv76.00 (9)O1ix—Ca2—H143.6 (12)
O4i—Ca1—O2v154.20 (11)O1—Ca2—H118.4 (4)
O4ii—Ca1—O2v123.99 (10)O3xi—Ca2—H197.1 (3)
O4—Ca1—O2v92.31 (8)O3xii—Ca2—H167.9 (2)
O2iii—Ca1—O2v76.00 (9)O4xiii—Ca2—H1103.75 (11)
O2iv—Ca1—O2v76.00 (9)Cl1—Ca2—H164.0 (7)
O4i—Ca1—O3vi69.46 (9)Cl1ix—Ca2—H12.0 (8)
O4ii—Ca1—O3vi86.05 (9)Cl1xiv—Ca2—H169.9 (7)
O4—Ca1—O3vi143.07 (9)O3ix—Ca2—H1A81.5 (4)
O2iii—Ca1—O3vi68.35 (10)O3—Ca2—H1A124.9 (4)
O2iv—Ca1—O3vi55.17 (10)O2x—Ca2—H1A144.2 (3)
O2v—Ca1—O3vi124.37 (9)O1A—Ca2—H1A22.6 (4)
O4i—Ca1—O3vii86.05 (9)O1ix—Ca2—H1A35.2 (8)
O4ii—Ca1—O3vii143.07 (9)O1—Ca2—H1A10.0 (8)
O4—Ca1—O3vii69.46 (9)O3xi—Ca2—H1A92.8 (2)
O2iii—Ca1—O3vii55.17 (10)O3xii—Ca2—H1A71.21 (19)
O2iv—Ca1—O3vii124.37 (9)O4xiii—Ca2—H1A104.83 (8)
O2v—Ca1—O3vii68.35 (10)Cl1—Ca2—H1A55.5 (5)
O3vi—Ca1—O3vii116.90 (4)Cl1ix—Ca2—H1A10.4 (5)
O4i—Ca1—O3viii143.07 (9)Cl1xiv—Ca2—H1A61.5 (5)
O4ii—Ca1—O3viii69.46 (9)H1—Ca2—H1A8.4 (8)
O4—Ca1—O3viii86.05 (9)O3xv—P1—O3109.6 (2)
O2iii—Ca1—O3viii124.37 (9)O3xv—P1—O2106.07 (16)
O2iv—Ca1—O3viii68.35 (10)O3—P1—O2106.07 (16)
O2v—Ca1—O3viii55.17 (10)O3xv—P1—O4111.87 (12)
O3vi—Ca1—O3viii116.90 (4)O3—P1—O4111.87 (12)
O3vii—Ca1—O3viii116.90 (4)O2—P1—O4111.06 (19)
O4i—Ca1—P1iii92.49 (6)O3xv—P1—Ca2xiii54.90 (12)
O4ii—Ca1—P1iii166.71 (7)O3—P1—Ca2xiii54.90 (12)
O4—Ca1—P1iii97.52 (7)O2—P1—Ca2xiii114.54 (14)
O2iii—Ca1—P1iii27.48 (8)O4—P1—Ca2xiii134.40 (13)
O2iv—Ca1—P1iii98.63 (7)O3xv—P1—Ca1xvi111.68 (11)
O2v—Ca1—P1iii66.52 (8)O3—P1—Ca1xvi59.33 (14)
O3vi—Ca1—P1iii94.00 (6)O2—P1—Ca1xvi47.71 (9)
O3vii—Ca1—P1iii28.07 (6)O4—P1—Ca1xvi135.68 (8)
O3viii—Ca1—P1iii121.68 (6)Ca2xiii—P1—Ca1xvi79.50 (3)
O4i—Ca1—P1iv97.52 (7)O3xv—P1—Ca1v59.33 (14)
O4ii—Ca1—P1iv92.49 (6)O3—P1—Ca1v111.68 (11)
O4—Ca1—P1iv166.71 (7)O2—P1—Ca1v47.71 (9)
O2iii—Ca1—P1iv66.52 (8)O4—P1—Ca1v135.68 (8)
O2iv—Ca1—P1iv27.48 (8)Ca2xiii—P1—Ca1v79.50 (3)
O2v—Ca1—P1iv98.63 (7)Ca1xvi—P1—Ca1v65.12 (4)
O3vi—Ca1—P1iv28.07 (6)O3xv—P1—Ca2xi81.74 (14)
O3vii—Ca1—P1iv121.68 (6)O3—P1—Ca2xi81.74 (14)
O3viii—Ca1—P1iv94.00 (6)O2—P1—Ca2xi165.73 (14)
P1iii—Ca1—P1iv93.76 (3)O4—P1—Ca2xi54.68 (12)
O4i—Ca1—P1v166.71 (7)Ca2xiii—P1—Ca2xi79.72 (4)
O4ii—Ca1—P1v97.52 (7)Ca1xvi—P1—Ca2xi141.00 (3)
O4—Ca1—P1v92.49 (6)Ca1v—P1—Ca2xi141.00 (3)
O2iii—Ca1—P1v98.63 (7)O3xv—P1—Ca2x120.94 (14)
O2iv—Ca1—P1v66.52 (8)O3—P1—Ca2x120.94 (14)
O2v—Ca1—P1v27.48 (8)O4—P1—Ca2x76.66 (12)
O3vi—Ca1—P1v121.68 (6)Ca2xiii—P1—Ca2x148.94 (4)
O3vii—Ca1—P1v94.00 (6)Ca1xvi—P1—Ca2x74.43 (2)
O3viii—Ca1—P1v28.07 (6)Ca1v—P1—Ca2x74.43 (2)
P1iii—Ca1—P1v93.76 (3)Ca2xi—P1—Ca2x131.34 (4)
P1iv—Ca1—P1v93.76 (3)P1—O2—Ca2x124.06 (19)
O3ix—Ca2—O3139.16 (18)P1—O2—Ca1v104.80 (13)
O3ix—Ca2—O2x85.61 (8)Ca2x—O2—Ca1v113.98 (11)
O3—Ca2—O2x85.61 (8)P1—O2—Ca1xvi104.80 (13)
O3ix—Ca2—O1A103.30 (9)Ca2x—O2—Ca1xvi113.98 (11)
O3—Ca2—O1A103.30 (9)Ca1v—O2—Ca1xvi89.39 (12)
O2x—Ca2—O1A151.42 (9)P1—O3—Ca2142.31 (14)
O3ix—Ca2—O1ix115.4 (6)P1—O3—Ca2xiii96.10 (14)
O3—Ca2—O1ix91.1 (6)Ca2—O3—Ca2xiii116.46 (11)
O2x—Ca2—O1ix149.0 (3)P1—O3—Ca1xvi92.60 (15)
O1A—Ca2—O1ix12.6 (7)Ca2—O3—Ca1xvi100.14 (12)
O3ix—Ca2—O191.1 (6)Ca2xiii—O3—Ca1xvi98.74 (9)
O3—Ca2—O1115.4 (6)P1—O4—Ca1xv130.28 (8)
O2x—Ca2—O1149.0 (3)P1—O4—Ca1130.28 (8)
O1A—Ca2—O112.6 (7)Ca1xv—O4—Ca190.60 (11)
O1ix—Ca2—O125.2 (13)P1—O4—Ca2xi97.60 (14)
O3ix—Ca2—O3xi135.56 (10)Ca1xv—O4—Ca2xi100.90 (9)
O3—Ca2—O3xi78.84 (6)Ca1—O4—Ca2xi100.90 (9)
O2x—Ca2—O3xi73.57 (10)Cl1xiv—Cl1—Ca2123.0 (4)
O1A—Ca2—O3xi81.51 (8)Cl1xiv—Cl1—Ca2xvii123.0 (3)
O1ix—Ca2—O3xi75.5 (3)Ca2—Cl1—Ca2xvii93.2 (5)
O1—Ca2—O3xi87.8 (3)Cl1xiv—Cl1—Ca2xviii123.0 (4)
O3ix—Ca2—O3xii78.84 (6)Ca2—Cl1—Ca2xviii93.2 (5)
O3—Ca2—O3xii135.56 (10)Ca2xvii—Cl1—Ca2xviii93.2 (5)
O2x—Ca2—O3xii73.57 (10)Cl1xiv—Cl1—Ca2xiv51.1 (3)
O1A—Ca2—O3xii81.51 (8)Ca2—Cl1—Ca2xiv174.1 (6)
O1ix—Ca2—O3xii87.8 (3)Ca2xvii—Cl1—Ca2xiv90.88 (5)
O1—Ca2—O3xii75.5 (3)Ca2xviii—Cl1—Ca2xiv90.88 (5)
O3xi—Ca2—O3xii57.92 (12)Cl1xiv—Cl1—Ca2xiii51.1 (3)
O3ix—Ca2—O4xiii71.59 (8)Ca2—Cl1—Ca2xiii90.88 (5)
O3—Ca2—O4xiii71.59 (8)Ca2xvii—Cl1—Ca2xiii174.1 (6)
O2x—Ca2—O4xiii102.48 (11)Ca2xviii—Cl1—Ca2xiii90.88 (5)
O1A—Ca2—O4xiii106.09 (7)Ca2xiv—Cl1—Ca2xiii84.7 (4)
O1ix—Ca2—O4xiii105.69 (8)Cl1xiv—Cl1—Ca2xi51.1 (3)
O1—Ca2—O4xiii105.69 (8)Ca2—Cl1—Ca2xi90.88 (5)
O3xi—Ca2—O4xiii150.41 (7)Ca2xvii—Cl1—Ca2xi90.88 (5)
O3xii—Ca2—O4xiii150.41 (7)Ca2xviii—Cl1—Ca2xi174.1 (6)
O3ix—Ca2—Cl1134.7 (3)Ca2xiv—Cl1—Ca2xi84.7 (4)
O3—Ca2—Cl171.5 (3)Ca2xiii—Cl1—Ca2xi84.7 (4)
O2x—Ca2—Cl1137.5 (3)O1ix—O1—Ca2xvii77.4 (7)
O1A—Ca2—Cl133.0 (4)O1ix—O1—Ca277.4 (7)
O1ix—Ca2—Cl120.4 (8)Ca2xvii—O1—Ca2115.4 (5)
O1—Ca2—Cl145.6 (7)O1ix—O1—Ca2xviii77.4 (7)
O3xi—Ca2—Cl167.21 (14)Ca2xvii—O1—Ca2xviii115.4 (5)
O3xii—Ca2—Cl198.03 (19)Ca2—O1—Ca2xviii115.4 (5)
O4xiii—Ca2—Cl1103.45 (8)O1ix—O1—H1180.00 (3)
O3ix—Ca2—Cl1ix71.5 (3)Ca2xvii—O1—H1102.6 (7)
O3—Ca2—Cl1ix134.7 (3)Ca2—O1—H1102.6 (6)
O2x—Ca2—Cl1ix137.5 (3)Ca2xviii—O1—H1102.6 (7)
O1A—Ca2—Cl1ix33.0 (4)O1ix—O1—H1A180.00 (2)
O1ix—Ca2—Cl1ix45.6 (7)Ca2xvii—O1—H1A102.6 (7)
O1—Ca2—Cl1ix20.4 (8)Ca2—O1—H1A102.6 (7)
O3xi—Ca2—Cl1ix98.03 (19)Ca2xviii—O1—H1A102.6 (7)
O3xii—Ca2—Cl1ix67.21 (14)Ca2—O1A—Ca2xvii120
O4xiii—Ca2—Cl1ix103.45 (8)Ca2—O1A—Ca2xviii120
Cl1—Ca2—Cl1ix66.0 (7)Ca2xvii—O1A—Ca2xviii120
O3ix—Ca2—Cl1xiv140.1 (3)Ca2—O1A—H190.000 (9)
O3—Ca2—Cl1xiv65.8 (3)Ca2xvii—O1A—H190.000 (7)
O2x—Ca2—Cl1xiv133.1 (2)Ca2xviii—O1A—H190.0000 (10)
O1A—Ca2—Cl1xiv38.9 (3)Ca2—O1A—H1A90.000 (7)
O1ix—Ca2—Cl1xiv26.3 (7)Ca2xvii—O1A—H1A90.000 (6)
O1—Ca2—Cl1xiv51.5 (8)Ca2xviii—O1A—H1A90.0000 (10)
O3xv—P1—O2—Ca2x121.75 (11)P1v—Ca1—O4—Ca1xv136.21 (7)
O3—P1—O2—Ca2x121.75 (11)O4i—Ca1—O4—Ca2xi62.14 (12)
O4—P1—O2—Ca2x0O4ii—Ca1—O4—Ca2xi140.31 (10)
Ca2xiii—P1—O2—Ca2x180O2iii—Ca1—O4—Ca2xi20.42 (13)
Ca1xvi—P1—O2—Ca2x133.33 (9)O2iv—Ca1—O4—Ca2xi156.83 (17)
Ca1v—P1—O2—Ca2x133.33 (9)O2v—Ca1—O4—Ca2xi95.06 (10)
Ca2xi—P1—O2—Ca2x0O3vi—Ca1—O4—Ca2xi78.58 (15)
O3xv—P1—O2—Ca1v11.58 (16)O3vii—Ca1—O4—Ca2xi29.23 (7)
O3—P1—O2—Ca1v104.92 (12)O3viii—Ca1—O4—Ca2xi149.90 (8)
O4—P1—O2—Ca1v133.33 (9)P1iii—Ca1—O4—Ca2xi28.44 (7)
Ca2xiii—P1—O2—Ca1v46.67 (9)P1iv—Ca1—O4—Ca2xi119.4 (3)
Ca1xvi—P1—O2—Ca1v93.35 (17)P1v—Ca1—O4—Ca2xi122.56 (6)
Ca2xi—P1—O2—Ca1v133.33 (9)O3ix—Ca2—Cl1—Cl1xiv158.35 (18)
Ca2x—P1—O2—Ca1v133.33 (9)O3—Ca2—Cl1—Cl1xiv16.06 (8)
O3xv—P1—O2—Ca1xvi104.92 (12)O2x—Ca2—Cl1—Cl1xiv45.0 (3)
O3—P1—O2—Ca1xvi11.58 (16)O1A—Ca2—Cl1—Cl1xiv180.000 (11)
O4—P1—O2—Ca1xvi133.33 (9)O1ix—Ca2—Cl1—Cl1xiv180.000 (12)
Ca2xiii—P1—O2—Ca1xvi46.67 (9)O1—Ca2—Cl1—Cl1xiv180.000 (10)
Ca1v—P1—O2—Ca1xvi93.35 (17)O3xi—Ca2—Cl1—Cl1xiv69.30 (15)
Ca2xi—P1—O2—Ca1xvi133.33 (9)O3xii—Ca2—Cl1—Cl1xiv119.43 (8)
Ca2x—P1—O2—Ca1xvi133.33 (9)O4xiii—Ca2—Cl1—Cl1xiv81.08 (8)
O3xv—P1—O3—Ca2145.53 (19)Cl1ix—Ca2—Cl1—Cl1xiv180.000 (10)
O2—P1—O3—Ca2100.4 (3)O3ix—Ca2—Cl1—Ca2xvii68.34 (18)
O4—P1—O3—Ca220.9 (4)O3—Ca2—Cl1—Ca2xvii149.4 (3)
Ca2xiii—P1—O3—Ca2150.6 (4)O2x—Ca2—Cl1—Ca2xvii88.3 (6)
Ca1xvi—P1—O3—Ca2110.3 (4)O1A—Ca2—Cl1—Ca2xvii46.7 (3)
Ca1v—P1—O3—Ca2150.7 (3)O1ix—Ca2—Cl1—Ca2xvii46.7 (3)
Ca2xi—P1—O3—Ca267.4 (3)O1—Ca2—Cl1—Ca2xvii46.7 (3)
Ca2x—P1—O3—Ca266.3 (4)O3xi—Ca2—Cl1—Ca2xvii64.01 (15)
O3xv—P1—O3—Ca2xiii5.1 (3)O3xii—Ca2—Cl1—Ca2xvii13.9 (3)
O2—P1—O3—Ca2xiii109.02 (15)O4xiii—Ca2—Cl1—Ca2xvii145.61 (19)
O4—P1—O3—Ca2xiii129.75 (14)Cl1ix—Ca2—Cl1—Ca2xvii46.7 (3)
Ca1xvi—P1—O3—Ca2xiii99.08 (10)Cl1xiv—Ca2—Cl1—Ca2xvii133.3 (3)
Ca1v—P1—O3—Ca2xiii58.73 (14)O3ix—Ca2—Cl1—Ca2xviii25.0 (4)
Ca2xi—P1—O3—Ca2xiii83.21 (10)O3—Ca2—Cl1—Ca2xviii117.3 (2)
Ca2x—P1—O3—Ca2xiii143.07 (7)O2x—Ca2—Cl1—Ca2xviii178.33 (11)
O3xv—P1—O3—Ca1xvi104.2 (2)O1A—Ca2—Cl1—Ca2xviii46.7 (3)
O2—P1—O3—Ca1xvi9.94 (15)O1ix—Ca2—Cl1—Ca2xviii46.7 (3)
O4—P1—O3—Ca1xvi131.17 (13)O1—Ca2—Cl1—Ca2xviii46.7 (3)
Ca2xiii—P1—O3—Ca1xvi99.08 (10)O3xi—Ca2—Cl1—Ca2xviii157.4 (4)
Ca1v—P1—O3—Ca1xvi40.35 (12)O3xii—Ca2—Cl1—Ca2xviii107.3 (2)
Ca2xi—P1—O3—Ca1xvi177.71 (8)O4xiii—Ca2—Cl1—Ca2xviii52.2 (4)
Ca2x—P1—O3—Ca1xvi43.99 (11)Cl1ix—Ca2—Cl1—Ca2xviii46.7 (3)
O3ix—Ca2—O3—P1110.7 (3)Cl1xiv—Ca2—Cl1—Ca2xviii133.3 (3)
O2x—Ca2—O3—P132.6 (4)O3ix—Ca2—Cl1—Ca2xiii116.0 (4)
O1A—Ca2—O3—P1119.9 (3)O3—Ca2—Cl1—Ca2xiii26.3 (2)
O1ix—Ca2—O3—P1116.5 (4)O2x—Ca2—Cl1—Ca2xiii87.40 (12)
O1—Ca2—O3—P1123.6 (4)O1A—Ca2—Cl1—Ca2xiii137.6 (2)
O3xi—Ca2—O3—P141.5 (4)O1ix—Ca2—Cl1—Ca2xiii137.6 (2)
O3xii—Ca2—O3—P128.5 (5)O1—Ca2—Cl1—Ca2xiii137.6 (2)
O4xiii—Ca2—O3—P1137.3 (4)O3xi—Ca2—Cl1—Ca2xiii111.7 (4)
Cl1—Ca2—O3—P1111.0 (4)O3xii—Ca2—Cl1—Ca2xiii161.81 (19)
Cl1ix—Ca2—O3—P1131.8 (3)O4xiii—Ca2—Cl1—Ca2xiii38.7 (3)
Cl1xiv—Ca2—O3—P1109.2 (4)Cl1ix—Ca2—Cl1—Ca2xiii137.6 (2)
O3ix—Ca2—O3—Ca2xiii102.3 (2)Cl1xiv—Ca2—Cl1—Ca2xiii42.4 (2)
O2x—Ca2—O3—Ca2xiii179.59 (15)O3ix—Ca2—Cl1—Ca2xi159.27 (15)
O1A—Ca2—O3—Ca2xiii27.10 (15)O3—Ca2—Cl1—Ca2xi58.4 (3)
O1ix—Ca2—O3—Ca2xiii30.5 (2)O2x—Ca2—Cl1—Ca2xi2.6 (5)
O1—Ca2—O3—Ca2xiii23.4 (3)O1A—Ca2—Cl1—Ca2xi137.6 (2)
O3xi—Ca2—O3—Ca2xiii105.49 (8)O1ix—Ca2—Cl1—Ca2xi137.6 (2)
O3xii—Ca2—O3—Ca2xiii118.50 (8)O1—Ca2—Cl1—Ca2xi137.6 (2)
O4xiii—Ca2—O3—Ca2xiii75.70 (13)O3xi—Ca2—Cl1—Ca2xi26.92 (11)
Cl1—Ca2—O3—Ca2xiii36.00 (15)O3xii—Ca2—Cl1—Ca2xi77.1 (3)
Cl1ix—Ca2—O3—Ca2xiii15.2 (3)O4xiii—Ca2—Cl1—Ca2xi123.45 (15)
Cl1xiv—Ca2—O3—Ca2xiii37.80 (14)Cl1ix—Ca2—Cl1—Ca2xi137.6 (2)
O3ix—Ca2—O3—Ca1xvi2.9 (2)Cl1xiv—Ca2—Cl1—Ca2xi42.4 (2)
O2x—Ca2—O3—Ca1xvi75.26 (10)O3ix—Ca2—O1—O1ix164.79 (7)
O1A—Ca2—O3—Ca1xvi132.26 (7)O3—Ca2—O1—O1ix16.88 (12)
O1ix—Ca2—O3—Ca1xvi135.63 (19)O2x—Ca2—O1—O1ix111.8 (10)
O1—Ca2—O3—Ca1xvi128.5 (2)O1A—Ca2—O1—O1ix0.000 (11)
O3xi—Ca2—O3—Ca1xvi149.35 (9)O3xi—Ca2—O1—O1ix59.66 (6)
O3xii—Ca2—O3—Ca1xvi136.35 (17)O3xii—Ca2—O1—O1ix117.05 (17)
O4xiii—Ca2—O3—Ca1xvi29.46 (8)O4xiii—Ca2—O1—O1ix93.60 (19)
Cl1—Ca2—O3—Ca1xvi141.16 (13)Cl1—Ca2—O1—O1ix0.000 (6)
Cl1ix—Ca2—O3—Ca1xvi120.3 (2)Cl1ix—Ca2—O1—O1ix180.000 (9)
Cl1xiv—Ca2—O3—Ca1xvi142.95 (13)Cl1xiv—Ca2—O1—O1ix0.000 (3)
O3xv—P1—O4—Ca1xv173.0 (2)O3ix—Ca2—O1—Ca2xvii125.9 (10)
O3—P1—O4—Ca1xv49.6 (3)O3—Ca2—O1—Ca2xvii86.2 (9)
O2—P1—O4—Ca1xv68.70 (19)O2x—Ca2—O1—Ca2xvii43 (2)
Ca2xiii—P1—O4—Ca1xv111.30 (19)O1A—Ca2—O1—Ca2xvii69.3 (10)
Ca1xvi—P1—O4—Ca1xv18.3 (3)O1ix—Ca2—O1—Ca2xvii69.3 (10)
Ca1v—P1—O4—Ca1xv119.08 (9)O3xi—Ca2—O1—Ca2xvii9.6 (10)
Ca2xi—P1—O4—Ca1xv111.30 (19)O3xii—Ca2—O1—Ca2xvii47.7 (8)
Ca2x—P1—O4—Ca1xv68.70 (19)O4xiii—Ca2—O1—Ca2xvii162.9 (8)
O3xv—P1—O4—Ca149.6 (3)Cl1—Ca2—O1—Ca2xvii69.3 (10)
O3—P1—O4—Ca1173.0 (2)Cl1ix—Ca2—O1—Ca2xvii110.7 (10)
O2—P1—O4—Ca168.70 (19)Cl1xiv—Ca2—O1—Ca2xvii69.3 (10)
Ca2xiii—P1—O4—Ca1111.30 (19)O3ix—Ca2—O1—Ca2xviii95.5 (10)
Ca1xvi—P1—O4—Ca1119.08 (9)O3—Ca2—O1—Ca2xviii52.4 (11)
Ca1v—P1—O4—Ca118.3 (3)O2x—Ca2—O1—Ca2xviii178.87 (9)
Ca2xi—P1—O4—Ca1111.30 (19)O1A—Ca2—O1—Ca2xviii69.3 (10)
Ca2x—P1—O4—Ca168.70 (19)O1ix—Ca2—O1—Ca2xviii69.3 (10)
O3xv—P1—O4—Ca2xi61.70 (16)O3xi—Ca2—O1—Ca2xviii129.0 (10)
O3—P1—O4—Ca2xi61.70 (16)O3xii—Ca2—O1—Ca2xviii173.6 (11)
O2—P1—O4—Ca2xi180O4xiii—Ca2—O1—Ca2xviii24.3 (12)
Ca2xiii—P1—O4—Ca2xi0Cl1—Ca2—O1—Ca2xviii69.3 (10)
Ca1xvi—P1—O4—Ca2xi129.62 (11)Cl1ix—Ca2—O1—Ca2xviii110.7 (10)
Ca1v—P1—O4—Ca2xi129.62 (11)Cl1xiv—Ca2—O1—Ca2xviii69.3 (10)
Ca2x—P1—O4—Ca2xi180O3ix—Ca2—O1A—Ca2xvii105.64 (7)
O4i—Ca1—O4—P1172.0 (3)O3—Ca2—O1A—Ca2xvii105.64 (7)
O4ii—Ca1—O4—P1109.8 (3)O2x—Ca2—O1A—Ca2xvii0
O2iii—Ca1—O4—P189.4 (2)O1ix—Ca2—O1A—Ca2xvii90
O2iv—Ca1—O4—P147.0 (3)O1—Ca2—O1A—Ca2xvii90
O2v—Ca1—O4—P114.8 (2)O3xi—Ca2—O1A—Ca2xvii29.31 (6)
O3vi—Ca1—O4—P1171.56 (15)O3xii—Ca2—O1A—Ca2xvii29.31 (6)
O3vii—Ca1—O4—P180.6 (2)O4xiii—Ca2—O1A—Ca2xvii180
O3viii—Ca1—O4—P140.0 (2)Cl1—Ca2—O1A—Ca2xvii90
P1iii—Ca1—O4—P181.4 (2)Cl1ix—Ca2—O1A—Ca2xvii90
P1iv—Ca1—O4—P1130.7 (2)Cl1xiv—Ca2—O1A—Ca2xvii90
P1v—Ca1—O4—P112.7 (2)O3ix—Ca2—O1A—Ca2xviii74.36 (7)
O4i—Ca1—O4—Ca1xv39.09 (13)O3—Ca2—O1A—Ca2xviii74.36 (7)
O4ii—Ca1—O4—Ca1xv39.09 (13)O2x—Ca2—O1A—Ca2xviii180
O2iii—Ca1—O4—Ca1xv121.64 (10)O1ix—Ca2—O1A—Ca2xviii90
O2iv—Ca1—O4—Ca1xv101.95 (19)O1—Ca2—O1A—Ca2xviii90
O2v—Ca1—O4—Ca1xv163.72 (10)O3xi—Ca2—O1A—Ca2xviii150.69 (6)
O3vi—Ca1—O4—Ca1xv22.64 (19)O3xii—Ca2—O1A—Ca2xviii150.69 (6)
O3vii—Ca1—O4—Ca1xv130.45 (11)O4xiii—Ca2—O1A—Ca2xviii0
O3viii—Ca1—O4—Ca1xv108.88 (9)Cl1—Ca2—O1A—Ca2xviii90
P1iii—Ca1—O4—Ca1xv129.66 (7)Cl1ix—Ca2—O1A—Ca2xviii90
P1iv—Ca1—O4—Ca1xv18.2 (4)Cl1xiv—Ca2—O1A—Ca2xviii90
Symmetry codes: (i) x+y+1, x+1, z; (ii) y+1, xy, z; (iii) xy+1, x, z+2; (iv) y, x+y, z+2; (v) x+1, y+1, z+2; (vi) y, x+y, z+1/2; (vii) xy+1, x, z+1/2; (viii) x+1, y+1, z+1/2; (ix) x, y, z+1/2; (x) x+1, y+1, z+1; (xi) xy+1, x, z+1; (xii) xy+1, x, z1/2; (xiii) y, x+y+1, z+1; (xiv) x+2, y+2, z+1; (xv) x, y, z+3/2; (xvi) x+1, y+1, z1/2; (xvii) y+2, xy+1, z; (xviii) x+y+1, x+2, z.
(1480l) top
Crystal data top
3(O4P)·0.18(Cl)·0.82(OH)·5(Ca)Dx = 3.165 Mg m3
Mr = 505.67Mo Kα radiation, λ = 0.7107 Å
Trigonal, P63/mCell parameters from 1985 reflections
Hall symbol: -P 6cθ = 2.4–33.2°
a = 9.4139 (2) ŵ = 3.08 mm1
c = 6.8679 (2) ÅT = 100 K
V = 527.10 (2) Å3Prism, colourless
Z = 20.20 × 0.17 × 0.02 mm
F(000) = 503.2
Data collection top
BRUKER APPEX-II CCD
diffractometer
586 independent reflections
Radiation source: fine-focus sealed tube545 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.019
ω and phi scansθmax = 30.5°, θmin = 2.5°
Absorption correction: multi-scan
BRUKER SADABS
h = 1313
Tmin = 0.745, Tmax = 1k = 1313
2668 measured reflectionsl = 99
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.039Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.086H atoms treated by a mixture of independent and constrained refinement
S = 1.13 w = 1/[σ2(Fo2) + (0.0246P)2 + 3.2518P]
where P = (Fo2 + 2Fc2)/3
586 reflections(Δ/σ)max = 0.004
48 parametersΔρmax = 1.57 e Å3
15 restraintsΔρmin = 1.29 e Å3
Crystal data top
3(O4P)·0.18(Cl)·0.82(OH)·5(Ca)Z = 2
Mr = 505.67Mo Kα radiation
Trigonal, P63/mµ = 3.08 mm1
a = 9.4139 (2) ÅT = 100 K
c = 6.8679 (2) Å0.20 × 0.17 × 0.02 mm
V = 527.10 (2) Å3
Data collection top
BRUKER APPEX-II CCD
diffractometer
586 independent reflections
Absorption correction: multi-scan
BRUKER SADABS
545 reflections with I > 2σ(I)
Tmin = 0.745, Tmax = 1Rint = 0.019
2668 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.03915 restraints
wR(F2) = 0.086H atoms treated by a mixture of independent and constrained refinement
S = 1.13Δρmax = 1.57 e Å3
586 reflectionsΔρmin = 1.29 e Å3
48 parameters
Special details top

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ca10.33330.66671.00177 (15)0.0094 (2)
Ca20.74535 (12)0.75446 (11)0.250.0127 (2)
P10.60148 (12)0.63123 (12)0.750.0058 (2)
O20.4125 (4)0.5336 (4)0.750.0234 (9)
O30.6516 (4)0.7387 (3)0.5691 (4)0.0290 (7)
O40.6725 (4)0.5152 (4)0.750.0087 (5)
Cl1110.483 (4)0.0140.090 (4)
O1110.174 (4)0.023 (2)0.236 (13)
H1110.044 (5)0.027*0.236 (13)
O1A110.250.0194 (15)0.35 (3)
H1A110.107 (3)0.023*0.173 (13)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0110 (3)0.0110 (3)0.0060 (4)0.00552 (14)00
Ca20.0225 (5)0.0148 (4)0.0069 (4)0.0139 (4)00
P10.0079 (4)0.0067 (4)0.0042 (4)0.0048 (4)00
O20.0099 (14)0.0124 (15)0.051 (3)0.0081 (13)00
O30.060 (2)0.0265 (13)0.0178 (12)0.0347 (14)0.0241 (13)0.0157 (11)
O40.0089 (12)0.0100 (13)0.0096 (14)0.0066 (11)00
Cl10.0080.0080.0260.00400
O10.020 (2)0.020 (2)0.028 (4)0.0101 (11)00
O1A0.0158 (16)0.0158 (16)0.027 (3)0.0079 (8)00
Geometric parameters (Å, º) top
Ca1—O4i2.397 (2)P1—O41.540 (3)
Ca1—O4ii2.397 (2)P1—O21.541 (4)
Ca1—O4iii2.397 (2)P1—Ca2xiii3.0993 (13)
Ca1—O2iv2.459 (2)P1—Ca1viii3.2117 (10)
Ca1—O2v2.459 (2)P1—Ca2xii3.2641 (13)
Ca1—O22.459 (2)P1—Ca2x3.4625 (14)
Ca1—O3vi2.765 (3)O2—Ca2x2.352 (4)
Ca1—O3vii2.765 (3)O2—Ca1viii2.459 (2)
Ca1—O3viii2.765 (3)O3—Ca2xiii2.549 (3)
Ca1—P1v3.2117 (10)O3—Ca1viii2.765 (3)
Ca1—P1iv3.2117 (10)O4—Ca1xv2.397 (2)
Ca1—P13.2117 (10)O4—Ca1iii2.397 (2)
Ca2—O3ix2.340 (3)O4—Ca2xii2.680 (3)
Ca2—O32.340 (3)Cl1—Cl1xiv0.23 (5)
Ca2—O2x2.352 (4)Cl1—Ca2xvi2.849 (15)
Ca2—O1A2.3555 (10)Cl1—Ca2xvii2.849 (15)
Ca2—O1ix2.412 (7)Cl1—Ca2xiv2.984 (17)
Ca2—O12.412 (7)Cl1—Ca2xii2.984 (17)
Ca2—O3xi2.549 (3)Cl1—Ca2xiii2.984 (17)
Ca2—O3xii2.549 (3)O1—O1ix1.04 (6)
Ca2—O4xiii2.680 (3)O1—Ca2xvi2.412 (6)
Ca2—Cl12.849 (15)O1—Ca2xvii2.412 (6)
Ca2—Cl1ix2.849 (15)O1—H10.89 (2)
Ca2—Cl1xiv2.984 (17)O1—H1A0.47 (4)
Ca2—H12.747 (19)O1A—Ca2xvi2.3555 (10)
Ca2—H1A2.553 (8)O1A—Ca2xvii2.3555 (10)
P1—O3viii1.520 (3)O1A—H1A0.99 (2)
P1—O31.520 (3)
O4i—Ca1—O4ii75.01 (8)O3xi—Ca2—Cl1xiv100.6 (2)
O4i—Ca1—O4iii75.01 (8)O3xii—Ca2—Cl1xiv65.47 (15)
O4ii—Ca1—O4iii75.01 (8)O4xiii—Ca2—Cl1xiv102.75 (9)
O4i—Ca1—O2iv92.34 (8)Cl1—Ca2—Cl1xiv3.7 (9)
O4ii—Ca1—O2iv154.25 (10)Cl1ix—Ca2—Cl1xiv72.09 (4)
O4iii—Ca1—O2iv123.96 (10)O3ix—Ca2—H173.4 (6)
O4i—Ca1—O2v123.96 (10)O3—Ca2—H1132.7 (6)
O4ii—Ca1—O2v92.34 (8)O2x—Ca2—H1138.8 (5)
O4iii—Ca1—O2v154.25 (10)O1A—Ca2—H131.0 (7)
O2iv—Ca1—O2v76.03 (9)O1ix—Ca2—H143.4 (13)
O4i—Ca1—O2154.25 (11)O1—Ca2—H118.5 (4)
O4ii—Ca1—O2123.96 (10)O3xi—Ca2—H167.9 (3)
O4iii—Ca1—O292.34 (8)O3xii—Ca2—H197.2 (3)
O2iv—Ca1—O276.03 (9)O4xiii—Ca2—H1103.87 (11)
O2v—Ca1—O276.03 (9)Cl1—Ca2—H165.2 (8)
O4i—Ca1—O3vi69.14 (8)Cl1ix—Ca2—H13.2 (8)
O4ii—Ca1—O3vi86.30 (9)Cl1xiv—Ca2—H168.9 (8)
O4iii—Ca1—O3vi142.80 (8)O3ix—Ca2—H1A81.3 (4)
O2iv—Ca1—O3vi68.13 (10)O3—Ca2—H1A124.9 (4)
O2v—Ca1—O3vi55.51 (9)O2x—Ca2—H1A144.1 (3)
O2—Ca1—O3vi124.55 (9)O1A—Ca2—H1A22.7 (4)
O4i—Ca1—O3vii86.30 (9)O1ix—Ca2—H1A35.2 (8)
O4ii—Ca1—O3vii142.80 (9)O1—Ca2—H1A10.2 (8)
O4iii—Ca1—O3vii69.14 (8)O3xi—Ca2—H1A71.1 (2)
O2iv—Ca1—O3vii55.51 (9)O3xii—Ca2—H1A93.0 (2)
O2v—Ca1—O3vii124.55 (9)O4xiii—Ca2—H1A104.95 (8)
O2—Ca1—O3vii68.13 (10)Cl1—Ca2—H1A56.9 (6)
O3vi—Ca1—O3vii116.97 (4)Cl1ix—Ca2—H1A11.5 (6)
O4i—Ca1—O3viii142.80 (9)Cl1xiv—Ca2—H1A60.6 (6)
O4ii—Ca1—O3viii69.14 (8)H1—Ca2—H1A8.3 (8)
O4iii—Ca1—O3viii86.30 (9)O3viii—P1—O3109.6 (2)
O2iv—Ca1—O3viii124.55 (9)O3viii—P1—O4111.81 (12)
O2v—Ca1—O3viii68.13 (10)O3—P1—O4111.81 (12)
O2—Ca1—O3viii55.51 (9)O3viii—P1—O2106.19 (16)
O3vi—Ca1—O3viii116.97 (4)O3—P1—O2106.19 (16)
O3vii—Ca1—O3viii116.97 (4)O4—P1—O2110.98 (18)
O4i—Ca1—P1v97.35 (7)O3viii—P1—Ca2xiii54.89 (11)
O4ii—Ca1—P1v92.71 (6)O3—P1—Ca2xiii54.89 (11)
O4iii—Ca1—P1v166.78 (6)O4—P1—Ca2xiii134.18 (13)
O2iv—Ca1—P1v66.32 (8)O2—P1—Ca2xiii114.84 (13)
O2v—Ca1—P1v27.68 (8)O3viii—P1—Ca1viii111.68 (11)
O2—Ca1—P1v98.72 (7)O3—P1—Ca1viii59.32 (13)
O3vi—Ca1—P1v28.23 (5)O4—P1—Ca1viii135.75 (8)
O3vii—Ca1—P1v121.82 (6)O2—P1—Ca1viii47.86 (9)
O3viii—Ca1—P1v93.97 (6)Ca2xiii—P1—Ca1viii79.58 (3)
O4i—Ca1—P1iv92.71 (6)O3viii—P1—Ca159.32 (13)
O4ii—Ca1—P1iv166.78 (6)O3—P1—Ca1111.68 (11)
O4iii—Ca1—P1iv97.35 (7)O4—P1—Ca1135.75 (8)
O2iv—Ca1—P1iv27.68 (8)O2—P1—Ca147.86 (9)
O2v—Ca1—P1iv98.72 (7)Ca2xiii—P1—Ca179.58 (3)
O2—Ca1—P1iv66.32 (8)Ca1viii—P1—Ca165.15 (4)
O3vi—Ca1—P1iv93.97 (6)O3viii—P1—Ca2xii81.78 (13)
O3vii—Ca1—P1iv28.23 (5)O3—P1—Ca2xii81.78 (13)
O3viii—Ca1—P1iv121.82 (6)O4—P1—Ca2xii54.47 (12)
P1v—Ca1—P1iv93.74 (3)O2—P1—Ca2xii165.45 (14)
O4i—Ca1—P1166.78 (6)Ca2xiii—P1—Ca2xii79.71 (4)
O4ii—Ca1—P197.35 (7)Ca1viii—P1—Ca2xii141.03 (3)
O4iii—Ca1—P192.71 (6)Ca1—P1—Ca2xii141.03 (3)
O2iv—Ca1—P198.72 (7)O3viii—P1—Ca2x120.93 (14)
O2v—Ca1—P166.32 (8)O3—P1—Ca2x120.93 (14)
O2—Ca1—P127.68 (8)O4—P1—Ca2x76.84 (12)
O3vi—Ca1—P1121.82 (6)Ca2xiii—P1—Ca2x148.98 (4)
O3vii—Ca1—P193.97 (6)Ca1viii—P1—Ca2x74.39 (2)
O3viii—Ca1—P128.23 (5)Ca1—P1—Ca2x74.39 (2)
P1v—Ca1—P193.74 (3)Ca2xii—P1—Ca2x131.31 (4)
P1iv—Ca1—P193.74 (3)P1—O2—Ca2x124.28 (18)
O3ix—Ca2—O3139.06 (17)P1—O2—Ca1viii104.45 (13)
O3ix—Ca2—O2x85.76 (8)Ca2x—O2—Ca1viii114.18 (10)
O3—Ca2—O2x85.76 (8)P1—O2—Ca1104.45 (13)
O3ix—Ca2—O1A103.22 (9)Ca2x—O2—Ca1114.18 (10)
O3—Ca2—O1A103.22 (9)Ca1viii—O2—Ca189.35 (11)
O2x—Ca2—O1A151.37 (9)P1—O3—Ca2142.13 (14)
O3ix—Ca2—O1ix115.2 (7)P1—O3—Ca2xiii95.91 (14)
O3—Ca2—O1ix91.2 (7)Ca2—O3—Ca2xiii116.77 (11)
O2x—Ca2—O1ix149.0 (3)P1—O3—Ca1viii92.46 (14)
O1A—Ca2—O1ix12.5 (7)Ca2—O3—Ca1viii100.29 (12)
O3ix—Ca2—O191.2 (7)Ca2xiii—O3—Ca1viii98.90 (9)
O3—Ca2—O1115.2 (7)P1—O4—Ca1xv130.07 (8)
O2x—Ca2—O1149.0 (3)P1—O4—Ca1iii130.07 (8)
O1A—Ca2—O112.5 (7)Ca1xv—O4—Ca1iii90.66 (10)
O1ix—Ca2—O124.9 (14)P1—O4—Ca2xii97.66 (14)
O3ix—Ca2—O3xi78.74 (6)Ca1xv—O4—Ca2xii101.21 (9)
O3—Ca2—O3xi135.88 (10)Ca1iii—O4—Ca2xii101.21 (9)
O2x—Ca2—O3xi73.52 (10)Cl1xiv—Cl1—Ca2124.2 (5)
O1A—Ca2—O3xi81.56 (8)Cl1xiv—Cl1—Ca2xvi124.2 (4)
O1ix—Ca2—O3xi87.8 (4)Ca2—Cl1—Ca2xvi91.5 (6)
O1—Ca2—O3xi75.6 (3)Cl1xiv—Cl1—Ca2xvii124.2 (4)
O3ix—Ca2—O3xii135.88 (10)Ca2—Cl1—Ca2xvii91.5 (6)
O3—Ca2—O3xii78.74 (6)Ca2xvi—Cl1—Ca2xvii91.5 (6)
O2x—Ca2—O3xii73.52 (10)Cl1xiv—Cl1—Ca2xiv52.1 (4)
O1A—Ca2—O3xii81.56 (8)Ca2—Cl1—Ca2xiv176.3 (9)
O1ix—Ca2—O3xii75.6 (3)Ca2xvi—Cl1—Ca2xiv91.08 (5)
O1—Ca2—O3xii87.8 (4)Ca2xvii—Cl1—Ca2xiv91.08 (5)
O3xi—Ca2—O3xii58.33 (12)Cl1xiv—Cl1—Ca2xii52.1 (4)
O3ix—Ca2—O4xiii71.46 (8)Ca2—Cl1—Ca2xii91.08 (5)
O3—Ca2—O4xiii71.46 (8)Ca2xvi—Cl1—Ca2xii91.08 (5)
O2x—Ca2—O4xiii102.39 (11)Ca2xvii—Cl1—Ca2xii176.3 (9)
O1A—Ca2—O4xiii106.24 (7)Ca2xiv—Cl1—Ca2xii86.2 (6)
O1ix—Ca2—O4xiii105.85 (8)Cl1xiv—Cl1—Ca2xiii52.1 (4)
O1—Ca2—O4xiii105.85 (8)Ca2—Cl1—Ca2xiii91.08 (5)
O3xi—Ca2—O4xiii150.17 (6)Ca2xvi—Cl1—Ca2xiii176.3 (9)
O3xii—Ca2—O4xiii150.17 (6)Ca2xvii—Cl1—Ca2xiii91.08 (5)
O3ix—Ca2—Cl1135.7 (4)Ca2xiv—Cl1—Ca2xiii86.2 (6)
O3—Ca2—Cl170.3 (4)Ca2xii—Cl1—Ca2xiii86.2 (6)
O2x—Ca2—Cl1136.5 (3)O1ix—O1—Ca277.5 (7)
O1A—Ca2—Cl134.2 (5)O1ix—O1—Ca2xvi77.5 (7)
O1ix—Ca2—Cl121.8 (8)Ca2—O1—Ca2xvi115.5 (5)
O1—Ca2—Cl146.7 (8)O1ix—O1—Ca2xvii77.5 (7)
O3xi—Ca2—Cl198.8 (2)Ca2—O1—Ca2xvii115.5 (5)
O3xii—Ca2—Cl166.71 (17)Ca2xvi—O1—Ca2xvii115.5 (5)
O4xiii—Ca2—Cl1103.37 (9)O1ix—O1—H1180.000 (17)
O3ix—Ca2—Cl1ix70.3 (4)Ca2—O1—H1102.5 (7)
O3—Ca2—Cl1ix135.7 (4)Ca2xvi—O1—H1102.5 (7)
O2x—Ca2—Cl1ix136.5 (3)Ca2xvii—O1—H1102.5 (7)
O1A—Ca2—Cl1ix34.2 (5)O1ix—O1—H1A180.00 (2)
O1ix—Ca2—Cl1ix46.7 (8)Ca2—O1—H1A102.5 (7)
O1—Ca2—Cl1ix21.8 (8)Ca2xvi—O1—H1A102.5 (7)
O3xi—Ca2—Cl1ix66.71 (17)Ca2xvii—O1—H1A102.5 (7)
O3xii—Ca2—Cl1ix98.8 (2)Ca2—O1A—Ca2xvi120
O4xiii—Ca2—Cl1ix103.37 (9)Ca2—O1A—Ca2xvii120
Cl1—Ca2—Cl1ix68.4 (9)Ca2xvi—O1A—Ca2xvii120
O3ix—Ca2—Cl1xiv139.1 (4)Ca2—O1A—H190.000 (9)
O3—Ca2—Cl1xiv66.8 (4)Ca2xvi—O1A—H190.000 (8)
O2x—Ca2—Cl1xiv133.9 (3)Ca2xvii—O1A—H190.0000 (10)
O1A—Ca2—Cl1xiv37.9 (4)Ca2—O1A—H1A90.000 (8)
O1ix—Ca2—Cl1xiv25.4 (8)Ca2xvi—O1A—H1A90.000 (6)
O1—Ca2—Cl1xiv50.3 (8)Ca2xvii—O1A—H1A90.0000 (10)
O4i—Ca1—P1—O3viii55.5 (3)O1A—Ca2—O3—P1119.8 (3)
O4ii—Ca1—P1—O3viii1.78 (14)O1ix—Ca2—O3—P1116.5 (4)
O4iii—Ca1—P1—O3viii77.01 (14)O1—Ca2—O3—P1123.6 (4)
O2iv—Ca1—P1—O3viii158.03 (15)O3xi—Ca2—O3—P128.4 (5)
O2v—Ca1—P1—O3viii87.54 (14)O3xii—Ca2—O3—P141.4 (4)
O2—Ca1—P1—O3viii166.88 (18)O4xiii—Ca2—O3—P1137.2 (4)
O3vi—Ca1—P1—O3viii88.41 (6)Cl1—Ca2—O3—P1110.5 (4)
O3vii—Ca1—P1—O3viii146.27 (14)Cl1ix—Ca2—O3—P1132.5 (4)
P1v—Ca1—P1—O3viii91.44 (13)Cl1xiv—Ca2—O3—P1109.4 (4)
P1iv—Ca1—P1—O3viii174.56 (13)O3ix—Ca2—O3—Ca2xiii102.1 (2)
O4i—Ca1—P1—O3156.1 (3)O2x—Ca2—O3—Ca2xiii179.37 (15)
O4ii—Ca1—P1—O3102.34 (16)O1A—Ca2—O3—Ca2xiii26.91 (14)
O4iii—Ca1—P1—O3177.57 (16)O1ix—Ca2—O3—Ca2xiii30.3 (2)
O2iv—Ca1—P1—O357.48 (17)O1—Ca2—O3—Ca2xiii23.2 (3)
O2v—Ca1—P1—O313.01 (16)O3xi—Ca2—O3—Ca2xiii118.38 (8)
O2—Ca1—P1—O392.57 (19)O3xii—Ca2—O3—Ca2xiii105.34 (7)
O3vi—Ca1—P1—O312.1 (2)O4xiii—Ca2—O3—Ca2xiii76.05 (13)
O3vii—Ca1—P1—O3113.17 (15)Cl1—Ca2—O3—Ca2xiii36.25 (17)
O3viii—Ca1—P1—O3100.6 (3)Cl1ix—Ca2—O3—Ca2xiii14.3 (3)
P1v—Ca1—P1—O39.12 (15)Cl1xiv—Ca2—O3—Ca2xiii37.37 (17)
P1iv—Ca1—P1—O384.88 (14)O3ix—Ca2—O3—Ca1viii3.4 (2)
O4i—Ca1—P1—O435.0 (3)O2x—Ca2—O3—Ca1viii75.11 (10)
O4ii—Ca1—P1—O488.79 (17)O1A—Ca2—O3—Ca1viii132.43 (7)
O4iii—Ca1—P1—O413.6 (2)O1ix—Ca2—O3—Ca1viii135.79 (19)
O2iv—Ca1—P1—O4111.39 (16)O1—Ca2—O3—Ca1viii128.7 (2)
O2v—Ca1—P1—O4178.12 (16)O3xi—Ca2—O3—Ca1viii136.10 (17)
O2—Ca1—P1—O476.30 (19)O3xii—Ca2—O3—Ca1viii149.14 (9)
O3vi—Ca1—P1—O4178.99 (15)O4xiii—Ca2—O3—Ca1viii29.47 (8)
O3vii—Ca1—P1—O455.70 (15)Cl1—Ca2—O3—Ca1viii141.77 (15)
O3viii—Ca1—P1—O490.58 (18)Cl1ix—Ca2—O3—Ca1viii119.8 (3)
P1v—Ca1—P1—O4177.99 (14)Cl1xiv—Ca2—O3—Ca1viii142.89 (15)
P1iv—Ca1—P1—O483.99 (15)O3viii—P1—O4—Ca1xv173.3 (2)
O4i—Ca1—P1—O2111.3 (3)O3—P1—O4—Ca1xv50.0 (3)
O4ii—Ca1—P1—O2165.09 (14)O2—P1—O4—Ca1xv68.32 (18)
O4iii—Ca1—P1—O289.86 (14)Ca2xiii—P1—O4—Ca1xv111.68 (18)
O2iv—Ca1—P1—O235.09 (16)Ca1viii—P1—O4—Ca1xv17.8 (3)
O2v—Ca1—P1—O2105.58 (19)Ca1—P1—O4—Ca1xv118.82 (9)
O3vi—Ca1—P1—O2104.71 (15)Ca2xii—P1—O4—Ca1xv111.68 (18)
O3vii—Ca1—P1—O220.60 (14)Ca2x—P1—O4—Ca1xv68.32 (18)
O3viii—Ca1—P1—O2166.88 (18)O3viii—P1—O4—Ca1iii50.0 (3)
P1v—Ca1—P1—O2101.69 (13)O3—P1—O4—Ca1iii173.3 (2)
P1iv—Ca1—P1—O27.69 (12)O2—P1—O4—Ca1iii68.32 (18)
O4i—Ca1—P1—Ca2xiii110.7 (3)Ca2xiii—P1—O4—Ca1iii111.68 (18)
O4ii—Ca1—P1—Ca2xiii56.97 (6)Ca1viii—P1—O4—Ca1iii118.82 (9)
O4iii—Ca1—P1—Ca2xiii132.20 (7)Ca1—P1—O4—Ca1iii17.8 (3)
O2iv—Ca1—P1—Ca2xiii102.85 (8)Ca2xii—P1—O4—Ca1iii111.68 (18)
O2v—Ca1—P1—Ca2xiii32.36 (7)Ca2x—P1—O4—Ca1iii68.32 (18)
O2—Ca1—P1—Ca2xiii137.94 (13)O3viii—P1—O4—Ca2xii61.64 (16)
O3vi—Ca1—P1—Ca2xiii33.23 (7)O3—P1—O4—Ca2xii61.64 (16)
O3vii—Ca1—P1—Ca2xiii158.54 (6)O2—P1—O4—Ca2xii180
O3viii—Ca1—P1—Ca2xiii55.19 (12)Ca2xiii—P1—O4—Ca2xii0
P1v—Ca1—P1—Ca2xiii36.25 (2)Ca1viii—P1—O4—Ca2xii129.50 (10)
P1iv—Ca1—P1—Ca2xiii130.25 (2)Ca1—P1—O4—Ca2xii129.50 (10)
O4i—Ca1—P1—Ca1viii166.0 (3)Ca2x—P1—O4—Ca2xii180
O4ii—Ca1—P1—Ca1viii140.22 (6)O3ix—Ca2—Cl1—Cl1xiv157.73 (19)
O4iii—Ca1—P1—Ca1viii144.55 (7)O3—Ca2—Cl1—Cl1xiv16.32 (9)
O2iv—Ca1—P1—Ca1viii19.59 (8)O2x—Ca2—Cl1—Cl1xiv44.2 (4)
O2v—Ca1—P1—Ca1viii50.89 (7)O1A—Ca2—Cl1—Cl1xiv180.000 (16)
O2—Ca1—P1—Ca1viii54.69 (12)O1ix—Ca2—Cl1—Cl1xiv180.000 (15)
O3vi—Ca1—P1—Ca1viii50.02 (7)O1—Ca2—Cl1—Cl1xiv180.000 (16)
O3vii—Ca1—P1—Ca1viii75.29 (6)O3xi—Ca2—Cl1—Cl1xiv119.43 (10)
O3viii—Ca1—P1—Ca1viii138.44 (12)O3xii—Ca2—Cl1—Cl1xiv69.58 (18)
P1v—Ca1—P1—Ca1viii47.000 (15)O4xiii—Ca2—Cl1—Cl1xiv80.70 (10)
P1iv—Ca1—P1—Ca1viii47.000 (15)Cl1ix—Ca2—Cl1—Cl1xiv180.000 (18)
O4i—Ca1—P1—Ca2xii51.8 (3)O3ix—Ca2—Cl1—Ca2xvi68.02 (19)
O4ii—Ca1—P1—Ca2xii1.95 (8)O3—Ca2—Cl1—Ca2xvi150.6 (4)
O4iii—Ca1—P1—Ca2xii73.28 (8)O2x—Ca2—Cl1—Ca2xvi90.1 (7)
O2iv—Ca1—P1—Ca2xii161.77 (9)O1A—Ca2—Cl1—Ca2xvi45.8 (3)
O2v—Ca1—P1—Ca2xii91.28 (9)O1ix—Ca2—Cl1—Ca2xvi45.8 (3)
O2—Ca1—P1—Ca2xii163.14 (14)O1—Ca2—Cl1—Ca2xvi45.8 (3)
O3vi—Ca1—P1—Ca2xii92.15 (9)O3xi—Ca2—Cl1—Ca2xvi14.8 (4)
O3vii—Ca1—P1—Ca2xii142.54 (7)O3xii—Ca2—Cl1—Ca2xvi64.66 (17)
O3viii—Ca1—P1—Ca2xii3.74 (12)O4xiii—Ca2—Cl1—Ca2xvi145.1 (2)
P1v—Ca1—P1—Ca2xii95.17 (7)Cl1ix—Ca2—Cl1—Ca2xvi45.8 (3)
P1iv—Ca1—P1—Ca2xii170.83 (6)Cl1xiv—Ca2—Cl1—Ca2xvi134.2 (4)
O4i—Ca1—P1—Ca2x86.3 (3)O3ix—Ca2—Cl1—Ca2xvii23.5 (5)
O4ii—Ca1—P1—Ca2x140.06 (6)O3—Ca2—Cl1—Ca2xvii117.9 (3)
O4iii—Ca1—P1—Ca2x64.83 (6)O2x—Ca2—Cl1—Ca2xvii178.40 (11)
O2iv—Ca1—P1—Ca2x60.12 (8)O1A—Ca2—Cl1—Ca2xvii45.8 (3)
O2v—Ca1—P1—Ca2x130.61 (7)O1ix—Ca2—Cl1—Ca2xvii45.8 (3)
O2—Ca1—P1—Ca2x25.03 (12)O1—Ca2—Cl1—Ca2xvii45.8 (3)
O3vi—Ca1—P1—Ca2x129.74 (7)O3xi—Ca2—Cl1—Ca2xvii106.3 (3)
O3vii—Ca1—P1—Ca2x4.43 (6)O3xii—Ca2—Cl1—Ca2xvii156.2 (5)
O3viii—Ca1—P1—Ca2x141.85 (12)O4xiii—Ca2—Cl1—Ca2xvii53.5 (4)
P1v—Ca1—P1—Ca2x126.72 (2)Cl1ix—Ca2—Cl1—Ca2xvii45.8 (3)
P1iv—Ca1—P1—Ca2x32.72 (2)Cl1xiv—Ca2—Cl1—Ca2xvii134.2 (4)
O3viii—P1—O2—Ca2x121.71 (11)O3ix—Ca2—Cl1—Ca2xii159.13 (17)
O3—P1—O2—Ca2x121.71 (11)O3—Ca2—Cl1—Ca2xii59.5 (4)
O4—P1—O2—Ca2x0O2x—Ca2—Cl1—Ca2xii1.0 (6)
Ca2xiii—P1—O2—Ca2x180O1A—Ca2—Cl1—Ca2xii136.9 (3)
Ca1viii—P1—O2—Ca2x133.44 (8)O1ix—Ca2—Cl1—Ca2xii136.9 (3)
Ca1—P1—O2—Ca2x133.44 (8)O1—Ca2—Cl1—Ca2xii136.9 (3)
Ca2xii—P1—O2—Ca2x0O3xi—Ca2—Cl1—Ca2xii76.3 (4)
O3viii—P1—O2—Ca1viii104.84 (12)O3xii—Ca2—Cl1—Ca2xii26.45 (14)
O3—P1—O2—Ca1viii11.73 (16)O4xiii—Ca2—Cl1—Ca2xii123.8 (2)
O4—P1—O2—Ca1viii133.44 (8)Cl1ix—Ca2—Cl1—Ca2xii136.9 (3)
Ca2xiii—P1—O2—Ca1viii46.56 (8)Cl1xiv—Ca2—Cl1—Ca2xii43.1 (3)
Ca1—P1—O2—Ca1viii93.11 (17)O3ix—Ca2—Cl1—Ca2xiii114.6 (5)
Ca2xii—P1—O2—Ca1viii133.44 (8)O3—Ca2—Cl1—Ca2xiii26.8 (3)
Ca2x—P1—O2—Ca1viii133.44 (8)O2x—Ca2—Cl1—Ca2xiii87.29 (12)
O3viii—P1—O2—Ca111.73 (16)O1A—Ca2—Cl1—Ca2xiii136.9 (3)
O3—P1—O2—Ca1104.84 (12)O1ix—Ca2—Cl1—Ca2xiii136.9 (3)
O4—P1—O2—Ca1133.44 (8)O1—Ca2—Cl1—Ca2xiii136.9 (3)
Ca2xiii—P1—O2—Ca146.56 (8)O3xi—Ca2—Cl1—Ca2xiii162.6 (2)
Ca1viii—P1—O2—Ca193.11 (17)O3xii—Ca2—Cl1—Ca2xiii112.7 (5)
Ca2xii—P1—O2—Ca1133.44 (8)O4xiii—Ca2—Cl1—Ca2xiii37.6 (4)
Ca2x—P1—O2—Ca1133.44 (8)Cl1ix—Ca2—Cl1—Ca2xiii136.9 (3)
O4i—Ca1—O2—P1150.63 (17)Cl1xiv—Ca2—Cl1—Ca2xiii43.1 (3)
O4ii—Ca1—O2—P117.92 (17)O3ix—Ca2—O1—O1ix164.66 (7)
O4iii—Ca1—O2—P191.38 (13)O3—Ca2—O1—O1ix17.00 (12)
O2iv—Ca1—O2—P1144.16 (14)O2x—Ca2—O1—O1ix111.6 (11)
O2v—Ca1—O2—P165.37 (18)O1A—Ca2—O1—O1ix0.000 (12)
O3vi—Ca1—O2—P193.75 (13)O3xi—Ca2—O1—O1ix117.30 (17)
O3vii—Ca1—O2—P1157.77 (14)O3xii—Ca2—O1—O1ix59.48 (6)
O3viii—Ca1—O2—P17.49 (10)O4xiii—Ca2—O1—O1ix93.6 (2)
P1v—Ca1—O2—P181.35 (11)Cl1—Ca2—O1—O1ix0.000 (6)
P1iv—Ca1—O2—P1171.62 (14)Cl1ix—Ca2—O1—O1ix180.000 (9)
O4i—Ca1—O2—Ca2x11.7 (3)Cl1xiv—Ca2—O1—O1ix0.000 (6)
O4ii—Ca1—O2—Ca2x120.97 (12)O3ix—Ca2—O1—Ca2xvi125.8 (10)
O4iii—Ca1—O2—Ca2x47.50 (12)O3—Ca2—O1—Ca2xvi86.5 (9)
O2iv—Ca1—O2—Ca2x76.96 (17)O2x—Ca2—O1—Ca2xvi42 (2)
O2v—Ca1—O2—Ca2x155.75 (14)O1A—Ca2—O1—Ca2xvi69.5 (10)
O3vi—Ca1—O2—Ca2x127.36 (10)O1ix—Ca2—O1—Ca2xvi69.5 (10)
O3vii—Ca1—O2—Ca2x18.89 (10)O3xi—Ca2—O1—Ca2xvi47.8 (9)
O3viii—Ca1—O2—Ca2x131.40 (13)O3xii—Ca2—O1—Ca2xvi10.0 (10)
P1v—Ca1—O2—Ca2x139.77 (9)O4xiii—Ca2—O1—Ca2xvi163.1 (8)
P1iv—Ca1—O2—Ca2x49.50 (9)Cl1—Ca2—O1—Ca2xvi69.5 (10)
P1—Ca1—O2—Ca2x138.88 (18)Cl1ix—Ca2—O1—Ca2xvi110.5 (10)
O4i—Ca1—O2—Ca1viii104.61 (18)Cl1xiv—Ca2—O1—Ca2xvi69.5 (10)
O4ii—Ca1—O2—Ca1viii122.68 (9)O3ix—Ca2—O1—Ca2xvii95.1 (10)
O4iii—Ca1—O2—Ca1viii163.86 (10)O3—Ca2—O1—Ca2xvii52.5 (11)
O2iv—Ca1—O2—Ca1viii39.39 (3)O2x—Ca2—O1—Ca2xvii178.93 (9)
O2v—Ca1—O2—Ca1viii39.39 (3)O1A—Ca2—O1—Ca2xvii69.5 (10)
O3vi—Ca1—O2—Ca1viii11.01 (15)O1ix—Ca2—O1—Ca2xvii69.5 (10)
O3vii—Ca1—O2—Ca1viii97.46 (10)O3xi—Ca2—O1—Ca2xvii173.2 (12)
O3viii—Ca1—O2—Ca1viii112.25 (13)O3xii—Ca2—O1—Ca2xvii129.0 (10)
P1v—Ca1—O2—Ca1viii23.42 (9)O4xiii—Ca2—O1—Ca2xvii24.1 (12)
P1iv—Ca1—O2—Ca1viii66.86 (7)Cl1—Ca2—O1—Ca2xvii69.5 (10)
P1—Ca1—O2—Ca1viii104.76 (16)Cl1ix—Ca2—O1—Ca2xvii110.5 (10)
O3viii—P1—O3—Ca2145.55 (19)Cl1xiv—Ca2—O1—Ca2xvii69.5 (10)
O4—P1—O3—Ca221.0 (4)O3ix—Ca2—O1A—Ca2xvi105.77 (7)
O2—P1—O3—Ca2100.2 (3)O3—Ca2—O1A—Ca2xvi105.77 (7)
Ca2xiii—P1—O3—Ca2150.5 (4)O2x—Ca2—O1A—Ca2xvi0
Ca1viii—P1—O3—Ca2110.3 (4)O1ix—Ca2—O1A—Ca2xvi90
Ca1—P1—O3—Ca2150.6 (3)O1—Ca2—O1A—Ca2xvi90
Ca2xii—P1—O3—Ca267.4 (3)O3xi—Ca2—O1A—Ca2xvi29.52 (6)
Ca2x—P1—O3—Ca266.3 (4)O3xii—Ca2—O1A—Ca2xvi29.52 (6)
O3viii—P1—O3—Ca2xiii5.0 (3)O4xiii—Ca2—O1A—Ca2xvi180
O4—P1—O3—Ca2xiii129.51 (13)Cl1—Ca2—O1A—Ca2xvi90
O2—P1—O3—Ca2xiii109.31 (15)Cl1ix—Ca2—O1A—Ca2xvi90
Ca1viii—P1—O3—Ca2xiii99.21 (10)Cl1xiv—Ca2—O1A—Ca2xvi90
Ca1—P1—O3—Ca2xiii58.83 (14)O3ix—Ca2—O1A—Ca2xvii74.23 (7)
Ca2xii—P1—O3—Ca2xiii83.16 (10)O3—Ca2—O1A—Ca2xvii74.23 (7)
Ca2x—P1—O3—Ca2xiii143.13 (7)O2x—Ca2—O1A—Ca2xvii180
O3viii—P1—O3—Ca1viii104.18 (19)O1ix—Ca2—O1A—Ca2xvii90
O4—P1—O3—Ca1viii131.28 (13)O1—Ca2—O1A—Ca2xvii90
O2—P1—O3—Ca1viii10.10 (15)O3xi—Ca2—O1A—Ca2xvii150.48 (6)
Ca2xiii—P1—O3—Ca1viii99.21 (10)O3xii—Ca2—O1A—Ca2xvii150.48 (6)
Ca1—P1—O3—Ca1viii40.38 (11)O4xiii—Ca2—O1A—Ca2xvii0
Ca2xii—P1—O3—Ca1viii177.63 (8)Cl1—Ca2—O1A—Ca2xvii90
Ca2x—P1—O3—Ca1viii43.92 (11)Cl1ix—Ca2—O1A—Ca2xvii90
O3ix—Ca2—O3—P1111.1 (3)Cl1xiv—Ca2—O1A—Ca2xvii90
O2x—Ca2—O3—P132.6 (3)
Symmetry codes: (i) xy, x, z+2; (ii) y, x+y+1, z+2; (iii) x+1, y+1, z+2; (iv) x+y, x+1, z; (v) y+1, xy+1, z; (vi) y+1, xy+1, z+3/2; (vii) x+y, x+1, z+3/2; (viii) x, y, z+3/2; (ix) x, y, z+1/2; (x) x+1, y+1, z+1; (xi) xy+1, x, z1/2; (xii) xy+1, x, z+1; (xiii) y, x+y+1, z+1; (xiv) x+2, y+2, z+1; (xv) x+1, y+1, z1/2; (xvi) y+2, xy+1, z; (xvii) x+y+1, x+2, z.
(1480r) top
Crystal data top
3(O4P)·0.18(Cl)·0.82(OH)·5(Ca)Dx = 3.175 Mg m3
Mr = 505.80Mo Kα radiation, λ = 0.7107 Å
Trigonal, P63/mCell parameters from 1976 reflections
Hall symbol: -P 6cθ = 2.5–26.4°
a = 9.4230 (2) ŵ = 3.11 mm1
c = 6.8794 (3) ÅT = 293 K
V = 529.00 (3) Å3Prism, colourless
Z = 20.23 × 0.08 × 0.07 mm
F(000) = 503
Data collection top
BRUKER APPEX-II CCD
diffractometer
389 independent reflections
Radiation source: fine-focus sealed tube371 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.033
ω and phi scansθmax = 26.4°, θmin = 2.5°
Absorption correction: multi-scan
BRUKER SADABS
h = 1111
Tmin = 0.744, Tmax = 1k = 1111
5438 measured reflectionsl = 88
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.029Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.068H atoms treated by a mixture of independent and constrained refinement
S = 1.15 w = 1/[σ2(Fo2) + (0.0255P)2 + 1.942P]
where P = (Fo2 + 2Fc2)/3
389 reflections(Δ/σ)max = 0.001
47 parametersΔρmax = 0.77 e Å3
32 restraintsΔρmin = 0.57 e Å3
Crystal data top
3(O4P)·0.18(Cl)·0.82(OH)·5(Ca)Z = 2
Mr = 505.80Mo Kα radiation
Trigonal, P63/mµ = 3.11 mm1
a = 9.4230 (2) ÅT = 293 K
c = 6.8794 (3) Å0.23 × 0.08 × 0.07 mm
V = 529.00 (3) Å3
Data collection top
BRUKER APPEX-II CCD
diffractometer
389 independent reflections
Absorption correction: multi-scan
BRUKER SADABS
371 reflections with I > 2σ(I)
Tmin = 0.744, Tmax = 1Rint = 0.033
5438 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.02932 restraints
wR(F2) = 0.068H atoms treated by a mixture of independent and constrained refinement
S = 1.15Δρmax = 0.77 e Å3
389 reflectionsΔρmin = 0.57 e Å3
47 parameters
Special details top

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ca10.66670.33330.99825 (15)0.0118 (3)
Ca20.74568 (11)0.75472 (11)0.250.0146 (3)
P10.60169 (12)0.63108 (12)0.750.0067 (3)
O20.4140 (4)0.5347 (4)0.750.0267 (9)
O30.6523 (4)0.7384 (3)0.5696 (4)0.0320 (7)
O40.6720 (4)0.5149 (3)0.750.0115 (6)
Cl1110.474 (4)0.021 (3)0.09
O1110.168 (3)0.027 (3)0.24
H1110.038 (4)0.032*0.24
O1A110.250.025 (3)0.35
H1A110.107 (3)0.03*0.17
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0134 (3)0.0134 (3)0.0086 (5)0.00670 (17)00
Ca20.0235 (5)0.0169 (5)0.0095 (4)0.0148 (4)00
P10.0082 (5)0.0074 (5)0.0061 (5)0.0050 (4)00
O20.0098 (15)0.0150 (15)0.056 (2)0.0070 (13)00
O30.0646 (18)0.0307 (13)0.0199 (12)0.0382 (14)0.0246 (13)0.0162 (11)
O40.0130 (14)0.0110 (14)0.0138 (15)0.0085 (12)00
Cl10.020 (2)0.020 (2)0.022 (8)0.0101 (12)00
O10.028 (3)0.028 (3)0.025 (8)0.0140 (14)00
O1A0.024 (2)0.024 (2)0.026 (8)0.0122 (12)00
Geometric parameters (Å, º) top
Ca1—O4i2.400 (2)P1—O21.532 (3)
Ca1—O4ii2.400 (2)P1—O41.537 (3)
Ca1—O42.400 (2)P1—Ca2xiii3.1029 (13)
Ca1—O2iii2.463 (2)P1—Ca1xvi3.2178 (10)
Ca1—O2iv2.463 (2)P1—Ca1v3.2178 (10)
Ca1—O2v2.463 (2)P1—Ca2xii3.2650 (13)
Ca1—O3vi2.775 (3)P1—Ca2x3.4685 (13)
Ca1—O3vii2.775 (3)O2—Ca2x2.366 (3)
Ca1—O3viii2.775 (3)O2—Ca1xvi2.463 (2)
Ca1—P1iii3.2178 (10)O2—Ca1v2.463 (2)
Ca1—P1iv3.2178 (10)O3—Ca2xiii2.552 (3)
Ca1—P1v3.2178 (10)O3—Ca1xvi2.775 (3)
Ca2—O3ix2.345 (2)O4—Ca1xv2.400 (2)
Ca2—O32.345 (2)O4—Ca2xii2.689 (3)
Ca2—O1A2.3550 (9)Cl1—Cl1xiv0.35 (5)
Ca2—O2x2.366 (3)Cl1—Ca2xvii2.815 (14)
Ca2—O1ix2.421 (5)Cl1—Ca2xviii2.815 (14)
Ca2—O12.421 (5)Cl1—Ca2xiv3.024 (16)
Ca2—O3xi2.552 (3)Cl1—Ca2xii3.024 (16)
Ca2—O3xii2.552 (3)Cl1—Ca2xiii3.024 (16)
Ca2—O4xiii2.689 (3)O1—O1ix1.12 (4)
Ca2—Cl12.815 (14)O1—Ca2xvii2.421 (5)
Ca2—Cl1ix2.815 (14)O1—Ca2xviii2.421 (5)
Ca2—Cl1xiv3.024 (16)O1A—Ca2xvii2.3550 (9)
P1—O3xv1.519 (2)O1A—Ca2xviii2.3550 (9)
P1—O31.519 (2)
O4i—Ca1—O4ii74.96 (8)O3xi—Ca2—Cl198.2 (2)
O4i—Ca1—O474.96 (8)O3xii—Ca2—Cl167.01 (17)
O4ii—Ca1—O474.96 (8)O4xiii—Ca2—Cl1103.55 (9)
O4i—Ca1—O2iii92.42 (7)O3ix—Ca2—Cl1ix71.2 (4)
O4ii—Ca1—O2iii154.43 (10)O3—Ca2—Cl1ix134.8 (4)
O4—Ca1—O2iii123.82 (9)O1A—Ca2—Cl1ix33.2 (4)
O4i—Ca1—O2iv123.82 (9)O2x—Ca2—Cl1ix137.4 (3)
O4ii—Ca1—O2iv92.42 (7)O1ix—Ca2—Cl1ix46.7 (6)
O4—Ca1—O2iv154.43 (10)O1—Ca2—Cl1ix19.8 (7)
O2iii—Ca1—O2iv76.02 (8)O3xi—Ca2—Cl1ix67.01 (17)
O4i—Ca1—O2v154.43 (10)O3xii—Ca2—Cl1ix98.2 (2)
O4ii—Ca1—O2v123.82 (9)O4xiii—Ca2—Cl1ix103.55 (9)
O4—Ca1—O2v92.42 (7)Cl1—Ca2—Cl1ix66.5 (9)
O2iii—Ca1—O2v76.02 (8)O3ix—Ca2—Cl1xiv140.0 (4)
O2iv—Ca1—O2v76.02 (8)O3—Ca2—Cl1xiv65.8 (4)
O4i—Ca1—O3vi69.33 (8)O1A—Ca2—Cl1xiv38.9 (4)
O4ii—Ca1—O3vi86.19 (9)O2x—Ca2—Cl1xiv133.2 (3)
O4—Ca1—O3vi142.88 (8)O1ix—Ca2—Cl1xiv25.4 (6)
O2iii—Ca1—O3vi68.44 (9)O1—Ca2—Cl1xiv52.3 (7)
O2iv—Ca1—O3vi55.16 (9)O3xi—Ca2—Cl1xiv100.9 (2)
O2v—Ca1—O3vi124.43 (8)O3xii—Ca2—Cl1xiv65.13 (13)
O4i—Ca1—O3vii86.19 (9)O4xiii—Ca2—Cl1xiv102.60 (8)
O4ii—Ca1—O3vii142.88 (8)Cl1—Ca2—Cl1xiv5.6 (8)
O4—Ca1—O3vii69.33 (8)Cl1ix—Ca2—Cl1xiv72.08 (6)
O2iii—Ca1—O3vii55.16 (9)O3xv—P1—O3109.5 (2)
O2iv—Ca1—O3vii124.43 (8)O3xv—P1—O2106.24 (14)
O2v—Ca1—O3vii68.44 (9)O3—P1—O2106.24 (14)
O3vi—Ca1—O3vii116.94 (3)O3xv—P1—O4111.76 (11)
O4i—Ca1—O3viii142.88 (8)O3—P1—O4111.76 (11)
O4ii—Ca1—O3viii69.33 (8)O2—P1—O4111.02 (17)
O4—Ca1—O3viii86.19 (9)O3xv—P1—Ca2xiii54.88 (10)
O2iii—Ca1—O3viii124.43 (8)O3—P1—Ca2xiii54.88 (10)
O2iv—Ca1—O3viii68.44 (9)O2—P1—Ca2xiii114.62 (13)
O2v—Ca1—O3viii55.16 (9)O4—P1—Ca2xiii134.36 (12)
O3vi—Ca1—O3viii116.94 (3)O3xv—P1—Ca1xvi111.82 (10)
O3vii—Ca1—O3viii116.94 (3)O3—P1—Ca1xvi59.50 (12)
O4i—Ca1—P1iii92.64 (6)O2—P1—Ca1xvi47.72 (8)
O4ii—Ca1—P1iii166.70 (6)O4—P1—Ca1xvi135.65 (8)
O4—Ca1—P1iii97.46 (6)Ca2xiii—P1—Ca1xvi79.56 (2)
O2iii—Ca1—P1iii27.40 (7)O3xv—P1—Ca1v59.50 (12)
O2iv—Ca1—P1iii98.61 (7)O3—P1—Ca1v111.82 (10)
O2v—Ca1—P1iii66.60 (7)O2—P1—Ca1v47.72 (8)
O3vi—Ca1—P1iii94.00 (6)O4—P1—Ca1v135.65 (8)
O3vii—Ca1—P1iii28.14 (5)Ca2xiii—P1—Ca1v79.56 (2)
O3viii—Ca1—P1iii121.75 (6)Ca1xvi—P1—Ca1v65.13 (4)
O4i—Ca1—P1iv97.46 (6)O3xv—P1—Ca2xii81.55 (12)
O4ii—Ca1—P1iv92.64 (6)O3—P1—Ca2xii81.55 (12)
O4—Ca1—P1iv166.70 (6)O2—P1—Ca2xii165.76 (13)
O2iii—Ca1—P1iv66.60 (7)O4—P1—Ca2xii54.74 (11)
O2iv—Ca1—P1iv27.40 (7)Ca2xiii—P1—Ca2xii79.62 (4)
O2v—Ca1—P1iv98.61 (7)Ca1xvi—P1—Ca2xii140.99 (2)
O3vi—Ca1—P1iv28.14 (5)Ca1v—P1—Ca2xii140.99 (2)
O3vii—Ca1—P1iv121.75 (6)O3xv—P1—Ca2x121.03 (13)
O3viii—Ca1—P1iv94.00 (6)O3—P1—Ca2x121.03 (13)
P1iii—Ca1—P1iv93.75 (2)O4—P1—Ca2x76.72 (11)
O4i—Ca1—P1v166.70 (6)Ca2xiii—P1—Ca2x148.92 (4)
O4ii—Ca1—P1v97.46 (6)Ca1xvi—P1—Ca2x74.35 (2)
O4—Ca1—P1v92.64 (6)Ca1v—P1—Ca2x74.35 (2)
O2iii—Ca1—P1v98.61 (7)Ca2xii—P1—Ca2x131.46 (4)
O2iv—Ca1—P1v66.60 (7)P1—O2—Ca2x124.30 (18)
O2v—Ca1—P1v27.40 (7)P1—O2—Ca1xvi104.88 (12)
O3vi—Ca1—P1v121.75 (6)Ca2x—O2—Ca1xvi113.77 (10)
O3vii—Ca1—P1v94.00 (6)P1—O2—Ca1v104.88 (12)
O3viii—Ca1—P1v28.14 (5)Ca2x—O2—Ca1v113.77 (10)
P1iii—Ca1—P1v93.75 (2)Ca1xvi—O2—Ca1v89.35 (11)
P1iv—Ca1—P1v93.75 (2)P1—O3—Ca2142.39 (13)
O3ix—Ca2—O3139.37 (16)P1—O3—Ca2xiii95.98 (13)
O3ix—Ca2—O1A103.22 (8)Ca2—O3—Ca2xiii116.64 (10)
O3—Ca2—O1A103.22 (8)P1—O3—Ca1xvi92.36 (13)
O3ix—Ca2—O2x85.58 (7)Ca2—O3—Ca1xvi100.09 (11)
O3—Ca2—O2x85.58 (7)Ca2xiii—O3—Ca1xvi98.74 (8)
O1A—Ca2—O2x151.61 (8)P1—O4—Ca1xv130.16 (8)
O3ix—Ca2—O1ix116.1 (5)P1—O4—Ca1130.16 (8)
O3—Ca2—O1ix90.3 (5)Ca1xv—O4—Ca190.72 (10)
O1A—Ca2—O1ix13.4 (5)P1—O4—Ca2xii97.43 (13)
O2x—Ca2—O1ix148.8 (2)Ca1xv—O4—Ca2xii101.12 (8)
O3ix—Ca2—O190.3 (5)Ca1—O4—Ca2xii101.12 (8)
O3—Ca2—O1116.1 (5)Cl1xiv—Cl1—Ca2123.2 (5)
O1A—Ca2—O113.4 (5)Cl1xiv—Cl1—Ca2xvii123.2 (4)
O2x—Ca2—O1148.8 (2)Ca2—Cl1—Ca2xvii92.8 (6)
O1ix—Ca2—O126.8 (10)Cl1xiv—Cl1—Ca2xviii123.2 (4)
O3ix—Ca2—O3xi78.64 (5)Ca2—Cl1—Ca2xviii92.8 (6)
O3—Ca2—O3xi135.63 (9)Ca2xvii—Cl1—Ca2xviii92.8 (6)
O1A—Ca2—O3xi81.46 (7)Cl1xiv—Cl1—Ca2xiv51.1 (3)
O2x—Ca2—O3xi73.81 (10)Ca2—Cl1—Ca2xiv174.4 (8)
O1ix—Ca2—O3xi88.2 (3)Ca2xvii—Cl1—Ca2xiv91.03 (6)
O1—Ca2—O3xi75.1 (2)Ca2xviii—Cl1—Ca2xiv91.03 (6)
O3ix—Ca2—O3xii135.63 (9)Cl1xiv—Cl1—Ca2xii51.1 (4)
O3—Ca2—O3xii78.64 (5)Ca2—Cl1—Ca2xii91.03 (6)
O1A—Ca2—O3xii81.46 (7)Ca2xvii—Cl1—Ca2xii91.03 (6)
O2x—Ca2—O3xii73.81 (10)Ca2xviii—Cl1—Ca2xii174.4 (8)
O1ix—Ca2—O3xii75.1 (2)Ca2xiv—Cl1—Ca2xii84.8 (5)
O1—Ca2—O3xii88.2 (3)Cl1xiv—Cl1—Ca2xiii51.1 (4)
O3xi—Ca2—O3xii58.18 (11)Ca2—Cl1—Ca2xiii91.03 (6)
O3ix—Ca2—O4xiii71.65 (7)Ca2xvii—Cl1—Ca2xiii174.4 (8)
O3—Ca2—O4xiii71.65 (7)Ca2xviii—Cl1—Ca2xiii91.03 (6)
O1A—Ca2—O4xiii106.27 (7)Ca2xiv—Cl1—Ca2xiii84.8 (5)
O2x—Ca2—O4xiii102.12 (10)Ca2xii—Cl1—Ca2xiii84.8 (5)
O1ix—Ca2—O4xiii105.81 (7)O1ix—O1—Ca276.6 (5)
O1—Ca2—O4xiii105.81 (7)O1ix—O1—Ca2xvii76.6 (5)
O3xi—Ca2—O4xiii150.26 (6)Ca2—O1—Ca2xvii114.8 (4)
O3xii—Ca2—O4xiii150.26 (6)O1ix—O1—Ca2xviii76.6 (5)
O3ix—Ca2—Cl1134.8 (4)Ca2—O1—Ca2xviii114.8 (4)
O3—Ca2—Cl171.2 (4)Ca2xvii—O1—Ca2xviii114.8 (4)
O1A—Ca2—Cl133.2 (4)Ca2—O1A—Ca2xvii120
O2x—Ca2—Cl1137.4 (3)Ca2—O1A—Ca2xviii120
O1ix—Ca2—Cl119.8 (7)Ca2xvii—O1A—Ca2xviii120
O1—Ca2—Cl146.7 (6)
O3xv—P1—O2—Ca2x121.71 (10)P1v—Ca1—O4—Ca1xv136.07 (7)
O3—P1—O2—Ca2x121.71 (10)O4i—Ca1—O4—Ca2xii62.43 (11)
O4—P1—O2—Ca2x0O4ii—Ca1—O4—Ca2xii140.54 (9)
Ca2xiii—P1—O2—Ca2x180O2iii—Ca1—O4—Ca2xii20.25 (12)
Ca1xvi—P1—O2—Ca2x133.32 (8)O2iv—Ca1—O4—Ca2xii156.87 (16)
Ca1v—P1—O2—Ca2x133.32 (8)O2v—Ca1—O4—Ca2xii95.02 (9)
Ca2xii—P1—O2—Ca2x0O3vi—Ca1—O4—Ca2xii78.51 (14)
O3xv—P1—O2—Ca1xvi104.97 (11)O3vii—Ca1—O4—Ca2xii29.17 (7)
O3—P1—O2—Ca1xvi11.62 (15)O3viii—Ca1—O4—Ca2xii149.85 (7)
O4—P1—O2—Ca1xvi133.32 (8)P1iii—Ca1—O4—Ca2xii28.31 (7)
Ca2xiii—P1—O2—Ca1xvi46.68 (8)P1iv—Ca1—O4—Ca2xii118.9 (3)
Ca1v—P1—O2—Ca1xvi93.35 (16)P1v—Ca1—O4—Ca2xii122.45 (6)
Ca2xii—P1—O2—Ca1xvi133.32 (8)O3ix—Ca2—Cl1—Cl1xiv158.38 (17)
Ca2x—P1—O2—Ca1xvi133.32 (8)O3—Ca2—Cl1—Cl1xiv16.02 (8)
O3xv—P1—O2—Ca1v11.62 (15)O1A—Ca2—Cl1—Cl1xiv180.000 (12)
O3—P1—O2—Ca1v104.97 (11)O2x—Ca2—Cl1—Cl1xiv44.6 (4)
O4—P1—O2—Ca1v133.32 (8)O1ix—Ca2—Cl1—Cl1xiv180.000 (6)
Ca2xiii—P1—O2—Ca1v46.68 (8)O1—Ca2—Cl1—Cl1xiv180.000 (8)
Ca1xvi—P1—O2—Ca1v93.35 (16)O3xi—Ca2—Cl1—Cl1xiv119.54 (9)
Ca2xii—P1—O2—Ca1v133.32 (8)O3xii—Ca2—Cl1—Cl1xiv69.30 (17)
Ca2x—P1—O2—Ca1v133.32 (8)O4xiii—Ca2—Cl1—Cl1xiv80.92 (10)
O3xv—P1—O3—Ca2145.66 (18)Cl1ix—Ca2—Cl1—Cl1xiv180.000 (9)
O2—P1—O3—Ca2100.0 (3)O3ix—Ca2—Cl1—Ca2xvii68.1 (2)
O4—P1—O3—Ca221.3 (4)O3—Ca2—Cl1—Ca2xvii149.5 (4)
Ca2xiii—P1—O3—Ca2151.0 (4)O1A—Ca2—Cl1—Ca2xvii46.5 (3)
Ca1xvi—P1—O3—Ca2109.9 (3)O2x—Ca2—Cl1—Ca2xvii88.9 (7)
Ca1v—P1—O3—Ca2150.3 (3)O1ix—Ca2—Cl1—Ca2xvii46.5 (3)
Ca2xii—P1—O3—Ca267.8 (3)O1—Ca2—Cl1—Ca2xvii46.5 (3)
Ca2x—P1—O3—Ca266.0 (3)O3xi—Ca2—Cl1—Ca2xvii14.0 (4)
O3xv—P1—O3—Ca2xiii5.4 (2)O3xii—Ca2—Cl1—Ca2xvii64.20 (17)
O2—P1—O3—Ca2xiii109.00 (14)O4xiii—Ca2—Cl1—Ca2xvii145.6 (2)
O4—P1—O3—Ca2xiii129.77 (13)Cl1ix—Ca2—Cl1—Ca2xvii46.5 (3)
Ca1xvi—P1—O3—Ca2xiii99.05 (9)Cl1xiv—Ca2—Cl1—Ca2xvii133.5 (3)
Ca1v—P1—O3—Ca2xiii58.66 (13)O3ix—Ca2—Cl1—Ca2xviii24.9 (5)
Ca2xii—P1—O3—Ca2xiii83.21 (9)O3—Ca2—Cl1—Ca2xviii117.5 (3)
Ca2x—P1—O3—Ca2xiii143.02 (7)O1A—Ca2—Cl1—Ca2xviii46.5 (3)
O3xv—P1—O3—Ca1xvi104.40 (18)O2x—Ca2—Cl1—Ca2xviii178.11 (10)
O2—P1—O3—Ca1xvi9.96 (14)O1ix—Ca2—Cl1—Ca2xviii46.5 (3)
O4—P1—O3—Ca1xvi131.19 (12)O1—Ca2—Cl1—Ca2xviii46.5 (3)
Ca2xiii—P1—O3—Ca1xvi99.05 (9)O3xi—Ca2—Cl1—Ca2xviii107.0 (3)
Ca1v—P1—O3—Ca1xvi40.39 (10)O3xii—Ca2—Cl1—Ca2xviii157.2 (5)
Ca2xii—P1—O3—Ca1xvi177.74 (7)O4xiii—Ca2—Cl1—Ca2xviii52.6 (4)
Ca2x—P1—O3—Ca1xvi43.98 (10)Cl1ix—Ca2—Cl1—Ca2xviii46.5 (3)
O3ix—Ca2—O3—P1110.4 (3)Cl1xiv—Ca2—Cl1—Ca2xviii133.5 (3)
O1A—Ca2—O3—P1120.2 (3)O3ix—Ca2—Cl1—Ca2xii159.20 (16)
O2x—Ca2—O3—P132.4 (3)O3—Ca2—Cl1—Ca2xii58.4 (3)
O1ix—Ca2—O3—P1116.6 (3)O1A—Ca2—Cl1—Ca2xii137.6 (3)
O1—Ca2—O3—P1124.2 (3)O2x—Ca2—Cl1—Ca2xii2.2 (6)
O3xi—Ca2—O3—P128.9 (5)O1ix—Ca2—Cl1—Ca2xii137.6 (3)
O3xii—Ca2—O3—P141.9 (4)O1—Ca2—Cl1—Ca2xii137.6 (3)
O4xiii—Ca2—O3—P1136.8 (3)O3xi—Ca2—Cl1—Ca2xii77.1 (3)
Cl1—Ca2—O3—P1111.3 (3)O3xii—Ca2—Cl1—Ca2xii26.89 (12)
Cl1ix—Ca2—O3—P1132.2 (4)O4xiii—Ca2—Cl1—Ca2xii123.34 (18)
Cl1xiv—Ca2—O3—P1109.6 (3)Cl1ix—Ca2—Cl1—Ca2xii137.6 (3)
O3ix—Ca2—O3—Ca2xiii102.2 (2)Cl1xiv—Ca2—Cl1—Ca2xii42.4 (3)
O1A—Ca2—O3—Ca2xiii27.17 (13)O3ix—Ca2—Cl1—Ca2xiii116.0 (4)
O2x—Ca2—O3—Ca2xiii179.83 (14)O3—Ca2—Cl1—Ca2xiii26.4 (2)
O1ix—Ca2—O3—Ca2xiii30.74 (17)O1A—Ca2—Cl1—Ca2xiii137.6 (3)
O1—Ca2—O3—Ca2xiii23.2 (2)O2x—Ca2—Cl1—Ca2xiii87.02 (12)
O3xi—Ca2—O3—Ca2xiii118.44 (7)O1ix—Ca2—Cl1—Ca2xiii137.6 (3)
O3xii—Ca2—O3—Ca2xiii105.47 (7)O1—Ca2—Cl1—Ca2xiii137.6 (3)
O4xiii—Ca2—O3—Ca2xiii75.84 (12)O3xi—Ca2—Cl1—Ca2xiii162.0 (2)
Cl1—Ca2—O3—Ca2xiii36.11 (16)O3xii—Ca2—Cl1—Ca2xiii111.7 (4)
Cl1ix—Ca2—O3—Ca2xiii15.2 (3)O4xiii—Ca2—Cl1—Ca2xiii38.5 (4)
Cl1xiv—Ca2—O3—Ca2xiii37.81 (15)Cl1ix—Ca2—Cl1—Ca2xiii137.6 (3)
O3ix—Ca2—O3—Ca1xvi3.0 (2)Cl1xiv—Ca2—Cl1—Ca2xiii42.4 (3)
O1A—Ca2—O3—Ca1xvi132.36 (6)O3ix—Ca2—O1—O1ix164.86 (6)
O2x—Ca2—O3—Ca1xvi74.99 (9)O3—Ca2—O1—O1ix16.91 (11)
O1ix—Ca2—O3—Ca1xvi135.93 (15)O1A—Ca2—O1—O1ix0.000 (7)
O1—Ca2—O3—Ca1xvi128.38 (17)O2x—Ca2—O1—O1ix113.2 (8)
O3xi—Ca2—O3—Ca1xvi136.38 (16)O3xi—Ca2—O1—O1ix116.98 (13)
O3xii—Ca2—O3—Ca1xvi149.34 (8)O3xii—Ca2—O1—O1ix59.50 (6)
O4xiii—Ca2—O3—Ca1xvi29.34 (8)O4xiii—Ca2—O1—O1ix93.87 (15)
Cl1—Ca2—O3—Ca1xvi141.30 (14)Cl1—Ca2—O1—O1ix0.000 (4)
Cl1ix—Ca2—O3—Ca1xvi120.4 (2)Cl1ix—Ca2—O1—O1ix180.000 (6)
Cl1xiv—Ca2—O3—Ca1xvi142.99 (14)Cl1xiv—Ca2—O1—O1ix0.000 (2)
O3xv—P1—O4—Ca1xv172.97 (19)O3ix—Ca2—O1—Ca2xvii127.0 (7)
O3—P1—O4—Ca1xv49.8 (3)O3—Ca2—O1—Ca2xvii85.0 (7)
O2—P1—O4—Ca1xv68.61 (17)O1A—Ca2—O1—Ca2xvii68.1 (7)
Ca2xiii—P1—O4—Ca1xv111.39 (17)O2x—Ca2—O1—Ca2xvii45.2 (15)
Ca1xvi—P1—O4—Ca1xv18.3 (3)O1ix—Ca2—O1—Ca2xvii68.1 (7)
Ca1v—P1—O4—Ca1xv118.97 (9)O3xi—Ca2—O1—Ca2xvii48.9 (6)
Ca2xii—P1—O4—Ca1xv111.39 (17)O3xii—Ca2—O1—Ca2xvii8.6 (7)
Ca2x—P1—O4—Ca1xv68.61 (17)O4xiii—Ca2—O1—Ca2xvii162.0 (6)
O3xv—P1—O4—Ca149.8 (3)Cl1—Ca2—O1—Ca2xvii68.1 (7)
O3—P1—O4—Ca1172.97 (19)Cl1ix—Ca2—O1—Ca2xvii111.9 (7)
O2—P1—O4—Ca168.61 (17)Cl1xiv—Ca2—O1—Ca2xvii68.1 (7)
Ca2xiii—P1—O4—Ca1111.39 (17)O3ix—Ca2—O1—Ca2xviii96.8 (7)
Ca1xvi—P1—O4—Ca1118.97 (9)O3—Ca2—O1—Ca2xviii51.2 (8)
Ca1v—P1—O4—Ca118.3 (3)O1A—Ca2—O1—Ca2xviii68.1 (7)
Ca2xii—P1—O4—Ca1111.39 (17)O2x—Ca2—O1—Ca2xviii178.66 (8)
Ca2x—P1—O4—Ca168.61 (17)O1ix—Ca2—O1—Ca2xviii68.1 (7)
O3xv—P1—O4—Ca2xii61.58 (14)O3xi—Ca2—O1—Ca2xviii174.9 (8)
O3—P1—O4—Ca2xii61.58 (14)O3xii—Ca2—O1—Ca2xviii127.6 (7)
O2—P1—O4—Ca2xii180O4xiii—Ca2—O1—Ca2xviii25.8 (9)
Ca2xiii—P1—O4—Ca2xii0Cl1—Ca2—O1—Ca2xviii68.1 (7)
Ca1xvi—P1—O4—Ca2xii129.64 (10)Cl1ix—Ca2—O1—Ca2xviii111.9 (7)
Ca1v—P1—O4—Ca2xii129.64 (10)Cl1xiv—Ca2—O1—Ca2xviii68.1 (7)
Ca2x—P1—O4—Ca2xii180O3ix—Ca2—O1A—Ca2xvii105.57 (7)
O4i—Ca1—O4—P1172.2 (2)O3—Ca2—O1A—Ca2xvii105.57 (7)
O4ii—Ca1—O4—P1109.7 (3)O2x—Ca2—O1A—Ca2xvii0
O2iii—Ca1—O4—P189.5 (2)O1ix—Ca2—O1A—Ca2xvii90
O2iv—Ca1—O4—P147.1 (3)O1—Ca2—O1A—Ca2xvii90
O2v—Ca1—O4—P114.8 (2)O3xi—Ca2—O1A—Ca2xvii29.45 (6)
O3vi—Ca1—O4—P1171.70 (14)O3xii—Ca2—O1A—Ca2xvii29.45 (6)
O3vii—Ca1—O4—P180.62 (19)O4xiii—Ca2—O1A—Ca2xvii180
O3viii—Ca1—O4—P140.1 (2)Cl1—Ca2—O1A—Ca2xvii90
P1iii—Ca1—O4—P181.5 (2)Cl1ix—Ca2—O1A—Ca2xvii90
P1iv—Ca1—O4—P1131.3 (2)Cl1xiv—Ca2—O1A—Ca2xvii90
P1v—Ca1—O4—P112.7 (2)O3ix—Ca2—O1A—Ca2xviii74.43 (7)
O4i—Ca1—O4—Ca1xv39.06 (11)O3—Ca2—O1A—Ca2xviii74.43 (7)
O4ii—Ca1—O4—Ca1xv39.06 (11)O2x—Ca2—O1A—Ca2xviii180
O2iii—Ca1—O4—Ca1xv121.73 (9)O1ix—Ca2—O1A—Ca2xviii90
O2iv—Ca1—O4—Ca1xv101.65 (18)O1—Ca2—O1A—Ca2xviii90
O2v—Ca1—O4—Ca1xv163.50 (10)O3xi—Ca2—O1A—Ca2xviii150.55 (6)
O3vi—Ca1—O4—Ca1xv22.97 (18)O3xii—Ca2—O1A—Ca2xviii150.55 (6)
O3vii—Ca1—O4—Ca1xv130.65 (10)O4xiii—Ca2—O1A—Ca2xviii0
O3viii—Ca1—O4—Ca1xv108.66 (9)Cl1—Ca2—O1A—Ca2xviii90
P1iii—Ca1—O4—Ca1xv129.79 (7)Cl1ix—Ca2—O1A—Ca2xviii90
P1iv—Ca1—O4—Ca1xv17.4 (4)Cl1xiv—Ca2—O1A—Ca2xviii90
Symmetry codes: (i) x+y+1, x+1, z; (ii) y+1, xy, z; (iii) xy+1, x, z+2; (iv) y, x+y, z+2; (v) x+1, y+1, z+2; (vi) y, x+y, z+1/2; (vii) xy+1, x, z+1/2; (viii) x+1, y+1, z+1/2; (ix) x, y, z+1/2; (x) x+1, y+1, z+1; (xi) xy+1, x, z1/2; (xii) xy+1, x, z+1; (xiii) y, x+y+1, z+1; (xiv) x+2, y+2, z+1; (xv) x, y, z+3/2; (xvi) x+1, y+1, z1/2; (xvii) y+2, xy+1, z; (xviii) x+y+1, x+2, z.
(1500l) top
Crystal data top
Ca64(PO4)F(000) = 1232
Mr = 620.36Dx = 2.882 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.7107 Å
Hall symbol: -P 2ybcCell parameters from 3765 reflections
a = 12.8348 (6) Åθ = 2.8–26.4°
b = 9.0961 (4) ŵ = 2.77 mm1
c = 12.8365 (5) ÅT = 100 K
β = 107.434 (2)°Needle, colourless
V = 1429.78 (11) Å30.23 × 0.07 × 0.06 mm
Z = 4
Data collection top
BRUKER APPEX-II CCD
diffractometer
2916 independent reflections
Radiation source: fine-focus sealed tube2303 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.032
ω and phi scansθmax = 26.4°, θmin = 1.7°
Absorption correction: multi-scan
BRUKER SADABS
h = 1615
Tmin = 0.611, Tmax = 0.746k = 011
11763 measured reflectionsl = 016
Refinement top
Refinement on F2205 restraints
Least-squares matrix: fullPrimary atom site location: structure-invariant direct methods
R[F2 > 2σ(F2)] = 0.042Secondary atom site location: difference Fourier map
wR(F2) = 0.101 w = 1/[σ2(Fo2) + (0.0418P)2 + 6.137P]
where P = (Fo2 + 2Fc2)/3
S = 1.06(Δ/σ)max = 0.002
2916 reflectionsΔρmax = 0.93 e Å3
362 parametersΔρmin = 0.85 e Å3
Crystal data top
Ca64(PO4)V = 1429.78 (11) Å3
Mr = 620.36Z = 4
Monoclinic, P21/cMo Kα radiation
a = 12.8348 (6) ŵ = 2.77 mm1
b = 9.0961 (4) ÅT = 100 K
c = 12.8365 (5) Å0.23 × 0.07 × 0.06 mm
β = 107.434 (2)°
Data collection top
BRUKER APPEX-II CCD
diffractometer
2916 independent reflections
Absorption correction: multi-scan
BRUKER SADABS
2303 reflections with I > 2σ(I)
Tmin = 0.611, Tmax = 0.746Rint = 0.032
11763 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.042362 parameters
wR(F2) = 0.101205 restraints
S = 1.06Δρmax = 0.93 e Å3
2916 reflectionsΔρmin = 0.85 e Å3
Special details top

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ca10.79942 (15)0.75869 (16)0.68890 (11)0.0178 (4)0.710 (3)
Ca1B0.7475 (4)0.7386 (4)0.6915 (3)0.0178 (4)0.290 (3)
Ca20.92434 (9)0.42777 (11)0.81347 (7)0.0247 (3)
Ca30.94760 (7)0.28044 (11)0.54694 (7)0.0189 (2)
Ca50.6721 (3)0.3543 (4)0.3177 (2)0.0193 (6)0.710 (3)
Ca5B0.6769 (9)0.3847 (10)0.3422 (7)0.0193 (6)0.290 (3)
Ca60.55930 (7)0.72465 (10)0.42602 (7)0.0143 (2)
Ca40.68052 (8)0.08358 (10)0.53649 (7)0.0197 (2)
P10.84378 (9)0.61697 (12)0.97220 (8)0.0102 (2)
O10.8681 (3)0.6745 (4)0.8694 (2)0.0189 (7)
O20.8543 (5)0.4462 (6)0.9731 (4)0.0102 (13)0.710 (3)
O30.7327 (4)0.6552 (6)0.9837 (4)0.0163 (12)0.710 (3)
O40.9319 (4)0.6842 (6)1.0674 (4)0.0185 (13)0.710 (3)
O2B0.8847 (13)0.4611 (18)0.9847 (12)0.019 (4)0.290 (3)
O3B0.7202 (9)0.6257 (12)0.9523 (9)0.007 (2)0.290 (3)
O4B0.9032 (10)0.6957 (14)1.0822 (9)0.012 (3)0.290 (3)
P20.69970 (9)0.41361 (13)0.58422 (10)0.0175 (3)
O50.6282 (5)0.3099 (7)0.6211 (5)0.0180 (16)0.710 (3)
O60.6333 (5)0.5015 (6)0.4847 (4)0.0309 (12)0.710 (3)
O70.7579 (5)0.3257 (6)0.5138 (5)0.0260 (14)0.710 (3)
O80.7767 (6)0.4983 (7)0.6808 (6)0.0277 (18)0.710 (3)
O6B0.6289 (15)0.559 (2)0.5450 (15)0.0309 (12)0.213 (8)
O7B0.7778 (10)0.3012 (13)0.5494 (10)0.012 (3)0.290 (3)
O8B0.7812 (12)0.5083 (16)0.6554 (11)0.012 (3)*0.290 (3)
P30.89564 (9)0.41934 (12)0.28003 (8)0.0114 (2)
O90.7841 (5)0.4804 (7)0.2049 (5)0.0142 (15)0.710 (3)
O100.9432 (4)0.3135 (6)0.2109 (4)0.0221 (11)0.710 (3)
O110.9708 (3)0.5466 (5)0.3187 (3)0.0147 (9)0.710 (3)
O120.8668 (4)0.3296 (5)0.3667 (4)0.0139 (10)0.710 (3)
O9B0.7944 (12)0.5087 (16)0.2255 (11)0.012 (4)0.290 (3)
O10B0.9741 (9)0.3828 (13)0.2189 (8)0.013 (2)0.290 (3)
O11B0.9647 (9)0.5027 (12)0.3973 (8)0.020 (2)0.290 (3)
O12B0.8571 (8)0.2830 (12)0.3311 (8)0.009 (2)0.290 (3)
P40.53622 (10)0.60767 (12)0.16534 (8)0.0120 (2)
O130.4219 (3)0.6733 (4)0.1339 (2)0.0204 (7)
O140.6113 (4)0.6966 (5)0.1119 (3)0.0176 (10)0.710 (3)
O150.5330 (4)0.4502 (6)0.1224 (4)0.0293 (12)0.710 (3)
O160.5969 (4)0.6002 (6)0.2891 (4)0.0221 (11)0.710 (3)
O14B0.5796 (8)0.6183 (11)0.0716 (7)0.010 (2)0.290 (3)
O15B0.5199 (8)0.4406 (10)0.1898 (7)0.009 (2)0.290 (3)
O16B0.5983 (8)0.6880 (12)0.2618 (8)0.015 (2)0.290 (3)
O6C0.597 (4)0.487 (6)0.518 (4)0.0309 (12)0.078 (8)
O5C0.6427 (11)0.2910 (15)0.6450 (11)0.009 (3)0.290 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0183 (10)0.0101 (6)0.0196 (5)0.0010 (7)0.0024 (7)0.0067 (4)
Ca1B0.0183 (10)0.0101 (6)0.0196 (5)0.0010 (7)0.0024 (7)0.0067 (4)
Ca20.0336 (6)0.0267 (6)0.0162 (4)0.0068 (5)0.0113 (4)0.0058 (4)
Ca30.0115 (5)0.0236 (5)0.0189 (4)0.0070 (4)0.0004 (3)0.0097 (4)
Ca50.0073 (6)0.0165 (16)0.0295 (16)0.0039 (10)0.0014 (11)0.0117 (9)
Ca5B0.0073 (6)0.0165 (16)0.0295 (16)0.0039 (10)0.0014 (11)0.0117 (9)
Ca60.0104 (4)0.0130 (5)0.0171 (4)0.0026 (4)0.0004 (3)0.0071 (3)
Ca40.0344 (6)0.0113 (5)0.0167 (4)0.0015 (4)0.0128 (4)0.0027 (3)
P10.0073 (5)0.0119 (6)0.0105 (5)0.0011 (5)0.0012 (4)0.0024 (4)
O10.0193 (10)0.0196 (11)0.0189 (10)0.0001 (8)0.0072 (8)0.0035 (8)
O20.0100 (16)0.0099 (16)0.0102 (15)0.0002 (10)0.0023 (10)0.0005 (9)
O30.0158 (15)0.0166 (15)0.0166 (14)0.0014 (9)0.0051 (10)0.0008 (9)
O40.0183 (16)0.0181 (16)0.0182 (15)0.0005 (10)0.0043 (10)0.0011 (9)
O2B0.020 (4)0.019 (4)0.020 (4)0.0002 (10)0.0058 (15)0.0003 (10)
O3B0.006 (3)0.006 (3)0.007 (3)0.0005 (10)0.0016 (12)0.0006 (10)
O4B0.012 (3)0.012 (3)0.012 (3)0.0004 (10)0.0038 (13)0.0003 (10)
P20.0101 (6)0.0098 (6)0.0303 (6)0.0009 (5)0.0023 (5)0.0011 (5)
O50.0176 (18)0.0178 (18)0.0187 (18)0.0006 (9)0.0055 (10)0.0001 (10)
O60.0306 (13)0.0299 (13)0.0312 (13)0.0005 (6)0.0079 (7)0.0004 (6)
O70.0252 (16)0.0278 (16)0.0256 (16)0.0025 (10)0.0085 (10)0.0010 (10)
O80.028 (2)0.027 (2)0.027 (2)0.0030 (10)0.0074 (11)0.0003 (10)
O6B0.0306 (13)0.0299 (13)0.0312 (13)0.0005 (6)0.0079 (7)0.0004 (6)
O7B0.012 (3)0.012 (3)0.013 (3)0.0002 (10)0.0039 (12)0.0013 (10)
P30.0102 (5)0.0086 (5)0.0155 (5)0.0011 (5)0.0038 (4)0.0017 (4)
O90.0144 (17)0.0131 (17)0.0141 (17)0.0008 (10)0.0029 (10)0.0011 (10)
O100.0231 (14)0.0217 (14)0.0210 (13)0.0022 (9)0.0058 (9)0.0024 (9)
O110.0147 (12)0.0149 (12)0.0143 (12)0.0020 (9)0.0042 (9)0.0004 (9)
O120.0144 (13)0.0136 (13)0.0134 (12)0.0001 (9)0.0039 (9)0.0012 (9)
O9B0.013 (4)0.012 (4)0.012 (4)0.0003 (10)0.0031 (15)0.0002 (10)
O10B0.013 (2)0.014 (2)0.013 (2)0.0005 (10)0.0046 (12)0.0006 (10)
O11B0.020 (3)0.020 (3)0.020 (3)0.0003 (10)0.0056 (12)0.0005 (10)
O12B0.009 (2)0.008 (2)0.009 (2)0.0001 (10)0.0024 (12)0.0007 (10)
P40.0192 (6)0.0094 (5)0.0084 (5)0.0026 (5)0.0056 (4)0.0003 (4)
O130.0209 (11)0.0208 (11)0.0210 (10)0.0026 (9)0.0088 (8)0.0012 (8)
O140.0162 (13)0.0184 (13)0.0179 (12)0.0007 (9)0.0048 (9)0.0022 (9)
O150.0283 (15)0.0280 (15)0.0313 (14)0.0004 (10)0.0086 (10)0.0030 (9)
O160.0221 (13)0.0234 (14)0.0205 (13)0.0027 (9)0.0058 (9)0.0003 (9)
O14B0.011 (2)0.011 (2)0.010 (2)0.0008 (10)0.0040 (11)0.0002 (10)
O15B0.009 (2)0.008 (2)0.009 (2)0.0001 (10)0.0016 (11)0.0005 (10)
O16B0.015 (2)0.015 (2)0.015 (2)0.0011 (10)0.0046 (12)0.0008 (10)
O6C0.0306 (13)0.0299 (13)0.0312 (13)0.0005 (6)0.0079 (7)0.0004 (6)
O5C0.009 (3)0.009 (3)0.008 (3)0.0000 (10)0.0025 (14)0.0002 (10)
Geometric parameters (Å, º) top
Ca1—O12.347 (3)Ca4—O52.511 (6)
Ca1—O14i2.354 (5)Ca4—O9Bvi2.570 (14)
Ca1—O82.385 (7)Ca4—O2vii2.607 (6)
Ca1—O9i2.395 (6)P1—O2B1.503 (16)
Ca1—O3ii2.633 (6)P1—O31.517 (5)
Ca1—O4ii2.680 (6)P1—O41.522 (5)
Ca1—O11i2.925 (5)P1—O3B1.531 (11)
Ca1—P1ii3.2078 (18)P1—O11.537 (3)
Ca1—P3i3.2565 (19)P1—O21.559 (6)
Ca1—P23.502 (2)P1—O4B1.563 (12)
Ca1—P4i3.517 (2)P1—Ca4vi3.0718 (14)
Ca1—Ca23.5570 (17)P1—Ca3xii3.1360 (14)
Ca1B—O8B2.216 (15)P1—Ca1i3.2078 (18)
Ca1B—O82.229 (8)P1—Ca2iv3.4184 (14)
Ca1B—O9Bi2.383 (15)O1—Ca3xii2.481 (3)
Ca1B—O12.415 (5)O2—Ca3vi2.429 (5)
Ca1B—O16Bi2.442 (11)O2—Ca4vi2.607 (6)
Ca1B—O14Bi2.592 (11)O3—Ca6i2.389 (5)
Ca1B—O6B2.61 (2)O3—Ca4vi2.428 (5)
Ca1B—O4Bii2.828 (13)O3—Ca1i2.633 (6)
Ca1B—P4i2.980 (5)O4—Ca2iv2.256 (5)
Ca1B—P23.242 (4)O4—Ca3xii2.583 (6)
Ca1B—Ca63.540 (4)O4—Ca1i2.680 (6)
Ca1B—Ca4iii3.677 (4)O2B—Ca4vi2.918 (15)
Ca2—O4iv2.256 (5)O3B—Ca4vi2.320 (11)
Ca2—O82.229 (7)O3B—Ca6i2.411 (11)
Ca2—O11v2.472 (4)O4B—Ca1Bi2.828 (13)
Ca2—O22.478 (5)P2—O8B1.448 (14)
Ca2—O12.526 (3)P2—O51.489 (6)
Ca2—O12vi2.607 (5)P2—O6C1.49 (5)
Ca2—O10vi2.608 (5)P2—O81.541 (7)
Ca2—O10v2.974 (6)P2—O61.531 (5)
Ca2—P13.0733 (14)P2—O71.555 (6)
Ca2—P3vi3.1928 (15)P2—O7B1.587 (12)
Ca2—P3v3.2210 (15)P2—O6B1.598 (18)
Ca2—P1iv3.4184 (14)P2—O5C1.652 (14)
Ca3—O122.278 (4)O5—Ca6x2.320 (6)
Ca3—O10vi2.287 (5)O5—Ca5vi2.841 (7)
Ca3—O11v2.338 (4)O6—O6C0.74 (5)
Ca3—O72.378 (6)O7—O7B0.503 (11)
Ca3—O2vii2.429 (5)O8—O8B0.359 (15)
Ca3—O1viii2.481 (3)O6B—O6C0.79 (5)
Ca3—O4viii2.583 (6)P3—O10B1.488 (10)
Ca3—P1viii3.1360 (14)P3—O111.493 (4)
Ca3—Ca2vii3.4816 (13)P3—O121.513 (4)
Ca3—P33.5229 (14)P3—O9B1.515 (14)
Ca3—P23.5682 (15)P3—O12B1.551 (10)
Ca5—O13ix2.237 (5)P3—O101.553 (5)
Ca5—O122.397 (6)P3—O91.569 (6)
Ca5—O162.420 (6)P3—O11B1.681 (11)
Ca5—O72.441 (7)P3—Ca2vii3.1928 (15)
Ca5—O5Cvii2.511 (14)P3—Ca2v3.2210 (15)
Ca5—O92.594 (7)O9—Ca4vii2.248 (6)
Ca5—O62.697 (6)O9—Ca1ii2.395 (6)
Ca5—O152.748 (6)O10—Ca3vii2.287 (5)
Ca5—O5vii2.841 (7)O10—Ca2vii2.608 (5)
Ca5—P33.106 (4)O10—Ca2v2.974 (6)
Ca5—P43.183 (4)O11—Ca3v2.338 (4)
Ca5—P23.375 (3)O11—Ca2v2.472 (4)
Ca5B—O72.202 (12)O11—Ca1ii2.925 (5)
Ca5B—O13ix2.374 (11)O12—Ca2vii2.607 (5)
Ca5B—O15B2.405 (14)O9B—Ca1Bii2.383 (15)
Ca5B—O12B2.534 (15)O9B—Ca4vii2.570 (14)
Ca5B—O9B2.672 (18)P4—O16B1.452 (10)
Ca5B—O7B2.695 (16)P4—O14B1.472 (9)
Ca5B—O6C2.90 (5)P4—O131.522 (3)
Ca5B—O5Cvii2.914 (16)P4—O151.530 (5)
Ca5B—O16B3.012 (15)P4—O161.547 (5)
Ca5B—P23.043 (9)P4—O141.565 (4)
Ca5B—P33.156 (11)P4—O15B1.578 (9)
Ca5B—P43.174 (11)P4—Ca1Bii2.980 (5)
Ca6—O6B2.142 (18)P4—Ca4xi3.1906 (15)
Ca6—O162.261 (5)P4—Ca4vii3.3208 (14)
Ca6—O62.272 (5)O13—Ca5xi2.237 (5)
Ca6—O14Bi2.304 (9)O13—Ca4xi2.336 (3)
Ca6—O5x2.320 (6)O13—Ca5Bxi2.374 (11)
Ca6—O16B2.332 (10)O14—Ca1ii2.354 (5)
Ca6—O15xi2.358 (5)O14—Ca6ii2.387 (4)
Ca6—O14i2.387 (4)O14—Ca4vii2.955 (5)
Ca6—O3ii2.389 (5)O15—Ca6ix2.358 (5)
Ca6—O3Bii2.411 (11)O15—Ca4vii2.479 (5)
Ca6—O6C2.45 (5)O15—Ca4xi3.129 (5)
Ca6—O5Cx2.482 (14)O14B—Ca6ii2.304 (9)
Ca4—O9vi2.248 (6)O14B—Ca4vii2.368 (10)
Ca4—O7B2.320 (12)O14B—Ca1Bii2.592 (11)
Ca4—O3Bvii2.320 (11)O15B—Ca6ix2.489 (9)
Ca4—O13ix2.336 (3)O16B—Ca1Bii2.442 (11)
Ca4—O14Bvi2.368 (10)O6C—Ca6x3.02 (6)
Ca4—O3vii2.428 (5)O5C—Ca6x2.482 (14)
Ca4—O72.469 (6)O5C—Ca5vi2.511 (14)
Ca4—O15vi2.479 (5)O5C—Ca5Bvi2.914 (15)
Ca4—O5C2.478 (14)
O1—Ca1—O14i120.39 (15)O3Bvii—Ca4—O13ix89.5 (3)
O1—Ca1—O873.96 (19)O9vi—Ca4—O14Bvi79.4 (3)
O14i—Ca1—O893.3 (2)O7B—Ca4—O14Bvi164.1 (4)
O1—Ca1—O9i104.78 (17)O3Bvii—Ca4—O14Bvi70.2 (4)
O14i—Ca1—O9i76.37 (19)O13ix—Ca4—O14Bvi105.2 (2)
O8—Ca1—O9i167.3 (2)O9vi—Ca4—O3vii84.5 (2)
O1—Ca1—O3ii176.39 (16)O7B—Ca4—O3vii126.6 (3)
O14i—Ca1—O3ii62.81 (15)O3Bvii—Ca4—O3vii11.1 (3)
O8—Ca1—O3ii104.7 (2)O13ix—Ca4—O3vii100.13 (15)
O9i—Ca1—O3ii77.32 (18)O14Bvi—Ca4—O3vii64.6 (3)
O1—Ca1—O4ii121.43 (15)O9vi—Ca4—O7101.6 (2)
O14i—Ca1—O4ii118.14 (16)O7B—Ca4—O711.5 (3)
O8—Ca1—O4ii104.9 (2)O3Bvii—Ca4—O7121.7 (3)
O9i—Ca1—O4ii86.59 (19)O13ix—Ca4—O773.24 (16)
O3ii—Ca1—O4ii55.47 (16)O14Bvi—Ca4—O7167.7 (3)
O1—Ca1—O11i68.86 (12)O3vii—Ca4—O7127.64 (18)
O14i—Ca1—O11i129.50 (15)O9vi—Ca4—O15vi81.4 (2)
O8—Ca1—O11i133.44 (19)O7B—Ca4—O15vi122.7 (3)
O9i—Ca1—O11i54.43 (17)O3Bvii—Ca4—O15vi114.1 (3)
O3ii—Ca1—O11i110.69 (15)O13ix—Ca4—O15vi99.75 (14)
O4ii—Ca1—O11i73.39 (14)O14Bvi—Ca4—O15vi44.3 (3)
O1—Ca1—P1ii149.23 (11)O3vii—Ca4—O15vi108.92 (17)
O14i—Ca1—P1ii90.06 (11)O7—Ca4—O15vi123.43 (18)
O8—Ca1—P1ii111.32 (17)O9vi—Ca4—O5C79.4 (4)
O9i—Ca1—P1ii76.43 (15)O7B—Ca4—O5C60.1 (4)
O3ii—Ca1—P1ii27.96 (11)O3Bvii—Ca4—O5C173.7 (4)
O4ii—Ca1—P1ii28.19 (11)O13ix—Ca4—O5C96.3 (3)
O11i—Ca1—P1ii88.95 (9)O14Bvi—Ca4—O5C105.8 (4)
O1—Ca1—P3i87.08 (9)O3vii—Ca4—O5C162.7 (3)
O14i—Ca1—P3i103.07 (12)O7—Ca4—O5C62.6 (3)
O8—Ca1—P3i159.56 (17)O15vi—Ca4—O5C62.6 (3)
O9i—Ca1—P3i27.16 (15)O9vi—Ca4—O587.4 (2)
O3ii—Ca1—P3i93.82 (12)O7B—Ca4—O558.5 (3)
O4ii—Ca1—P3i78.25 (13)O3Bvii—Ca4—O5177.2 (3)
O11i—Ca1—P3i27.28 (9)O13ix—Ca4—O588.28 (17)
P1ii—Ca1—P3i81.24 (5)O14Bvi—Ca4—O5108.7 (3)
O1—Ca1—P294.15 (9)O3vii—Ca4—O5170.3 (2)
O14i—Ca1—P277.47 (12)O7—Ca4—O559.25 (19)
O8—Ca1—P221.14 (17)O15vi—Ca4—O564.56 (19)
O9i—Ca1—P2152.99 (16)O5C—Ca4—O58.1 (3)
O3ii—Ca1—P284.88 (12)O9vi—Ca4—O9Bvi4.1 (4)
O4ii—Ca1—P299.96 (13)O7B—Ca4—O9Bvi94.0 (4)
O11i—Ca1—P2152.54 (10)O3Bvii—Ca4—O9Bvi91.7 (4)
P1ii—Ca1—P297.05 (5)O13ix—Ca4—O9Bvi178.6 (3)
P3i—Ca1—P2178.19 (6)O14Bvi—Ca4—O9Bvi75.9 (4)
O1—Ca1—P4i105.36 (10)O3vii—Ca4—O9Bvi81.1 (3)
O14i—Ca1—P4i20.98 (10)O7—Ca4—O9Bvi105.5 (4)
O8—Ca1—P4i103.76 (18)O15vi—Ca4—O9Bvi80.4 (4)
O9i—Ca1—P4i64.12 (15)O5C—Ca4—O9Bvi82.5 (5)
O3ii—Ca1—P4i78.17 (12)O5—Ca4—O9Bvi90.6 (4)
O4ii—Ca1—P4i130.05 (12)O9vi—Ca4—O2vii87.6 (2)
O11i—Ca1—P4i112.25 (9)O7B—Ca4—O2vii67.6 (3)
P1ii—Ca1—P4i102.65 (4)O3Bvii—Ca4—O2vii56.1 (3)
P3i—Ca1—P4i88.35 (4)O13ix—Ca4—O2vii92.20 (14)
P2—Ca1—P4i92.61 (5)O14Bvi—Ca4—O2vii123.2 (3)
O1—Ca1—Ca245.13 (8)O3vii—Ca4—O2vii59.13 (17)
O14i—Ca1—Ca2127.06 (13)O7—Ca4—O2vii69.13 (18)
O8—Ca1—Ca237.99 (17)O15vi—Ca4—O2vii164.71 (17)
O9i—Ca1—Ca2146.88 (15)O5C—Ca4—O2vii125.8 (3)
O3ii—Ca1—Ca2132.00 (12)O5—Ca4—O2vii125.78 (19)
O4ii—Ca1—Ca298.43 (13)O9Bvi—Ca4—O2vii87.9 (4)
O11i—Ca1—Ca295.49 (9)O2B—P1—O3120.9 (6)
P1ii—Ca1—Ca2121.00 (6)O2B—P1—O498.1 (6)
P3i—Ca1—Ca2121.89 (5)O3—P1—O4108.9 (3)
P2—Ca1—Ca258.51 (3)O2B—P1—O3B112.2 (7)
P4i—Ca1—Ca2128.55 (6)O4—P1—O3B126.6 (5)
O8B—Ca1B—O89.3 (4)O2B—P1—O1105.0 (6)
O8B—Ca1B—O9Bi153.7 (6)O3—P1—O1116.4 (2)
O8—Ca1B—O9Bi156.9 (5)O4—P1—O1105.0 (2)
O8B—Ca1B—O181.9 (4)O3B—P1—O1107.8 (4)
O8—Ca1B—O175.5 (2)O3—P1—O2108.0 (3)
O9Bi—Ca1B—O190.3 (4)O4—P1—O2110.6 (3)
O8B—Ca1B—O16Bi124.0 (5)O3B—P1—O297.8 (5)
O8—Ca1B—O16Bi117.1 (4)O1—P1—O2107.8 (2)
O9Bi—Ca1B—O16Bi81.4 (5)O2B—P1—O4B106.0 (7)
O1—Ca1B—O16Bi93.9 (3)O3—P1—O4B91.5 (5)
O8B—Ca1B—O14Bi122.0 (5)O3B—P1—O4B109.1 (6)
O8—Ca1B—O14Bi125.5 (3)O1—P1—O4B116.8 (5)
O9Bi—Ca1B—O14Bi75.2 (4)O2—P1—O4B115.6 (5)
O1—Ca1B—O14Bi150.0 (3)O2B—P1—Ca4vi69.9 (6)
O16Bi—Ca1B—O14Bi58.5 (3)O3—P1—Ca4vi51.2 (2)
O8B—Ca1B—O6B50.6 (5)O4—P1—Ca4vi115.2 (2)
O8—Ca1B—O6B54.1 (4)O3B—P1—Ca4vi47.1 (4)
O9Bi—Ca1B—O6B142.8 (5)O1—P1—Ca4vi139.79 (13)
O1—Ca1B—O6B126.9 (4)O2—P1—Ca4vi58.1 (2)
O16Bi—Ca1B—O6B94.8 (5)O4B—P1—Ca4vi102.5 (5)
O14Bi—Ca1B—O6B71.6 (5)O2B—P1—Ca250.7 (6)
O8B—Ca1B—O4Bii83.4 (5)O3—P1—Ca2134.9 (2)
O8—Ca1B—O4Bii91.1 (4)O4—P1—Ca2116.1 (2)
O9Bi—Ca1B—O4Bii73.2 (5)O3B—P1—Ca2117.1 (4)
O1—Ca1B—O4Bii99.9 (3)O1—P1—Ca254.95 (12)
O16Bi—Ca1B—O4Bii151.0 (4)O2—P1—Ca253.23 (19)
O14Bi—Ca1B—O4Bii100.7 (3)O4B—P1—Ca2133.3 (5)
O6B—Ca1B—O4Bii97.0 (5)Ca4vi—P1—Ca2103.75 (4)
O8B—Ca1B—P4i130.4 (4)O2B—P1—Ca3xii100.2 (6)
O8—Ca1B—P4i128.1 (3)O3—P1—Ca3xii138.4 (2)
O9Bi—Ca1B—P4i74.9 (4)O4—P1—Ca3xii55.0 (2)
O1—Ca1B—P4i121.59 (18)O3B—P1—Ca3xii145.9 (4)
O16Bi—Ca1B—P4i29.0 (2)O1—P1—Ca3xii51.17 (12)
O14Bi—Ca1B—P4i29.6 (2)O2—P1—Ca3xii113.5 (2)
O6B—Ca1B—P4i84.1 (4)O4B—P1—Ca3xii69.9 (5)
O4Bii—Ca1B—P4i126.8 (3)Ca4vi—P1—Ca3xii165.88 (4)
O8B—Ca1B—P222.0 (4)Ca2—P1—Ca3xii75.45 (4)
O8—Ca1B—P224.95 (18)O2B—P1—Ca1i112.8 (6)
O9Bi—Ca1B—P2164.4 (4)O3—P1—Ca1i54.5 (2)
O1—Ca1B—P299.64 (15)O4—P1—Ca1i56.3 (2)
O16Bi—Ca1B—P2109.7 (3)O3B—P1—Ca1i71.5 (4)
O14Bi—Ca1B—P2100.8 (2)O1—P1—Ca1i139.42 (14)
O6B—Ca1B—P229.2 (4)O2—P1—Ca1i112.47 (19)
O4Bii—Ca1B—P293.1 (3)Ca4vi—P1—Ca1i70.36 (4)
P4i—Ca1B—P2109.27 (14)Ca2—P1—Ca1i162.69 (5)
O8B—Ca1B—Ca683.4 (4)Ca3xii—P1—Ca1i106.16 (5)
O8—Ca1B—Ca689.1 (2)O2B—P1—Ca2iv67.1 (6)
O9Bi—Ca1B—Ca6105.8 (4)O3—P1—Ca2iv124.5 (2)
O1—Ca1B—Ca6163.88 (18)O3B—P1—Ca2iv138.5 (4)
O16Bi—Ca1B—Ca688.9 (3)O1—P1—Ca2iv112.32 (13)
O14Bi—Ca1B—Ca640.6 (2)O2—P1—Ca2iv79.8 (2)
O6B—Ca1B—Ca637.0 (4)Ca4vi—P1—Ca2iv102.27 (4)
O4Bii—Ca1B—Ca684.8 (3)Ca2—P1—Ca2iv94.71 (4)
P4i—Ca1B—Ca664.71 (8)Ca3xii—P1—Ca2iv64.00 (3)
P2—Ca1B—Ca664.57 (8)Ca1i—P1—Ca2iv71.46 (4)
O8B—Ca1B—Ca4iii136.3 (4)P1—O1—Ca1147.79 (19)
O8—Ca1B—Ca4iii145.1 (2)P1—O1—Ca1B131.0 (2)
O9Bi—Ca1B—Ca4iii44.1 (3)P1—O1—Ca3xii99.97 (15)
O1—Ca1B—Ca4iii134.24 (17)Ca1—O1—Ca3xii109.17 (13)
O16Bi—Ca1B—Ca4iii83.4 (3)Ca1B—O1—Ca3xii124.99 (17)
O14Bi—Ca1B—Ca4iii39.9 (2)P1—O1—Ca295.19 (15)
O6B—Ca1B—Ca4iii98.8 (4)Ca1—O1—Ca293.69 (11)
O4Bii—Ca1B—Ca4iii68.7 (3)Ca1B—O1—Ca295.90 (15)
P4i—Ca1B—Ca4iii58.74 (7)Ca3xii—O1—Ca298.73 (11)
P2—Ca1B—Ca4iii124.38 (11)P1—O2—Ca3vi151.7 (3)
Ca6—Ca1B—Ca4iii61.85 (6)P1—O2—Ca296.5 (2)
O4iv—Ca2—O8169.5 (2)Ca3vi—O2—Ca290.39 (18)
O4iv—Ca2—O11v90.28 (18)P1—O2—Ca4vi91.5 (2)
O8—Ca2—O11v87.8 (2)Ca3vi—O2—Ca4vi99.09 (19)
O4iv—Ca2—O283.99 (19)Ca2—O2—Ca4vi143.8 (2)
O8—Ca2—O2100.2 (2)P1—O3—Ca6i152.9 (3)
O11v—Ca2—O2165.49 (17)P1—O3—Ca4vi99.7 (2)
O4iv—Ca2—O1116.97 (16)Ca6i—O3—Ca4vi100.76 (19)
O8—Ca2—O173.23 (19)P1—O3—Ca1i97.6 (2)
O11v—Ca2—O1111.81 (12)Ca6i—O3—Ca1i99.65 (19)
O2—Ca2—O159.99 (15)Ca4vi—O3—Ca1i91.20 (17)
O4iv—Ca2—O12vi69.84 (18)P1—O4—Ca2iv128.5 (3)
O8—Ca2—O12vi102.5 (2)P1—O4—Ca3xii96.2 (2)
O11v—Ca2—O12vi121.33 (14)Ca2iv—O4—Ca3xii91.8 (2)
O2—Ca2—O12vi69.04 (17)P1—O4—Ca1i95.5 (3)
O1—Ca2—O12vi126.57 (12)Ca2iv—O4—Ca1i103.0 (2)
O4iv—Ca2—O10vi77.40 (18)Ca3xii—O4—Ca1i149.0 (2)
O8—Ca2—O10vi92.4 (2)P1—O2B—Ca4vi81.2 (6)
O11v—Ca2—O10vi65.22 (14)P1—O3B—Ca4vi103.9 (5)
O2—Ca2—O10vi125.88 (17)P1—O3B—Ca6i148.6 (7)
O1—Ca2—O10vi165.62 (13)Ca4vi—O3B—Ca6i103.3 (4)
O12vi—Ca2—O10vi56.85 (14)P1—O4B—Ca1Bi108.6 (6)
O4iv—Ca2—O10v92.94 (17)O8B—P2—O5125.0 (6)
O8—Ca2—O10v94.2 (2)O8B—P2—O6C116 (2)
O11v—Ca2—O10v53.65 (13)O5—P2—O6C86 (2)
O2—Ca2—O10v113.19 (17)O5—P2—O8111.7 (4)
O1—Ca2—O10v63.11 (12)O6C—P2—O8119 (2)
O12vi—Ca2—O10v162.55 (14)O8B—P2—O6109.4 (6)
O10vi—Ca2—O10v118.06 (5)O5—P2—O6110.7 (3)
O4iv—Ca2—P199.94 (14)O8—P2—O6118.2 (3)
O8—Ca2—P188.13 (18)O8B—P2—O7106.9 (6)
O11v—Ca2—P1139.69 (11)O5—P2—O7108.0 (3)
O2—Ca2—P130.27 (13)O6C—P2—O7113 (2)
O1—Ca2—P129.86 (7)O8—P2—O7114.9 (3)
O12vi—Ca2—P198.68 (10)O6—P2—O791.6 (3)
O10vi—Ca2—P1155.05 (11)O8B—P2—O7B99.4 (7)
O10v—Ca2—P186.73 (9)O5—P2—O7B100.6 (5)
O4iv—Ca2—P3vi71.50 (14)O6C—P2—O7B131 (2)
O8—Ca2—P3vi98.31 (18)O8—P2—O7B104.0 (5)
O11v—Ca2—P3vi93.77 (10)O6—P2—O7B110.0 (5)
O2—Ca2—P3vi97.02 (14)O8B—P2—O6B86.7 (10)
O1—Ca2—P3vi152.30 (8)O5—P2—O6B106.1 (7)
O12vi—Ca2—P3vi27.98 (10)O8—P2—O6B90.4 (8)
O10vi—Ca2—P3vi28.87 (10)O7—P2—O6B124.7 (7)
O10v—Ca2—P3vi144.58 (10)O7B—P2—O6B142.4 (8)
P1—Ca2—P3vi126.49 (4)O8B—P2—O5C116.2 (7)
O4iv—Ca2—P3v85.14 (15)O6C—P2—O5C97 (2)
O8—Ca2—P3v97.56 (18)O8—P2—O5C103.0 (5)
O11v—Ca2—P3v26.46 (10)O6—P2—O5C122.1 (5)
O2—Ca2—P3v139.24 (15)O7—P2—O5C106.6 (5)
O1—Ca2—P3v91.15 (8)O7B—P2—O5C96.0 (6)
O12vi—Ca2—P3v140.96 (10)O6B—P2—O5C114.6 (8)
O10vi—Ca2—P3v89.41 (11)O8B—P2—Ca5B121.7 (6)
O10v—Ca2—P3v28.68 (9)O5—P2—Ca5B112.9 (3)
P1—Ca2—P3v115.25 (4)O6C—P2—Ca5B70 (2)
P3vi—Ca2—P3v116.34 (4)O8—P2—Ca5B135.0 (3)
O4iv—Ca2—P1iv20.39 (14)O6—P2—Ca5B48.3 (3)
O8—Ca2—P1iv170.05 (18)O7B—P2—Ca5B62.1 (5)
O11v—Ca2—P1iv92.39 (10)O6B—P2—Ca5B83.0 (7)
O2—Ca2—P1iv77.66 (13)O5C—P2—Ca5B120.2 (5)
O1—Ca2—P1iv97.53 (8)O8B—P2—Ca4135.2 (6)
O12vi—Ca2—P1iv85.92 (10)O5—P2—Ca454.7 (2)
O10vi—Ca2—P1iv96.67 (11)O6C—P2—Ca4109 (2)
O10v—Ca2—P1iv77.97 (9)O8—P2—Ca4130.2 (3)
P1—Ca2—P1iv85.29 (4)O6—P2—Ca4110.7 (2)
P3vi—Ca2—P1iv91.61 (4)O7—P2—Ca453.4 (2)
P3v—Ca2—P1iv78.61 (4)O7B—P2—Ca448.0 (4)
O12—Ca3—O10vi151.43 (17)O6B—P2—Ca4138.1 (8)
O12—Ca3—O11v125.76 (17)O5C—P2—Ca454.0 (5)
O10vi—Ca3—O11v72.64 (16)Ca5B—P2—Ca474.54 (18)
O12—Ca3—O769.77 (18)O5—P2—Ca1B120.0 (3)
O10vi—Ca3—O785.58 (19)O6C—P2—Ca1B82 (2)
O11v—Ca3—O7102.92 (17)O6—P2—Ca1B82.3 (2)
O12—Ca3—O2vii75.47 (18)O7—P2—Ca1B130.7 (2)
O10vi—Ca3—O2vii84.07 (18)O7B—P2—Ca1B130.7 (4)
O11v—Ca3—O2vii156.69 (16)O6B—P2—Ca1B52.9 (8)
O7—Ca3—O2vii73.7 (2)O5C—P2—Ca1B118.0 (5)
O12—Ca3—O1viii126.94 (14)Ca5B—P2—Ca1B117.4 (2)
O10vi—Ca3—O1viii74.91 (15)Ca4—P2—Ca1B166.85 (8)
O11v—Ca3—O1viii77.51 (13)P2—O5—Ca6x133.9 (4)
O7—Ca3—O1viii159.50 (17)P2—O5—Ca496.4 (3)
O2vii—Ca3—O1viii97.68 (16)Ca6x—O5—Ca499.6 (2)
O12—Ca3—O4viii69.98 (16)P2—O5—Ca5vi129.7 (3)
O10vi—Ca3—O4viii125.46 (18)Ca6x—O5—Ca5vi94.3 (2)
O11v—Ca3—O4viii115.79 (16)Ca4—O5—Ca5vi86.9 (2)
O7—Ca3—O4viii135.42 (18)O6C—O6—P273 (4)
O2vii—Ca3—O4viii78.45 (18)O6C—O6—Ca695 (4)
O1viii—Ca3—O4viii57.24 (13)P2—O6—Ca6144.7 (3)
O12—Ca3—P1viii98.81 (12)O6C—O6—Ca5133 (5)
O10vi—Ca3—P1viii98.75 (14)P2—O6—Ca5102.4 (3)
O11v—Ca3—P1viii99.94 (11)Ca6—O6—Ca5109.8 (2)
O7—Ca3—P1viii156.98 (14)O7B—O7—P284.4 (17)
O2vii—Ca3—P1viii84.24 (14)O7B—O7—Ca5B166.9 (19)
O1viii—Ca3—P1viii28.85 (7)P2—O7—Ca5B106.9 (4)
O4viii—Ca3—P1viii28.86 (11)O7B—O7—Ca363.1 (17)
O12—Ca3—Ca2vii48.48 (13)P2—O7—Ca3129.0 (3)
O10vi—Ca3—Ca2vii124.70 (14)Ca5B—O7—Ca3111.8 (4)
O11v—Ca3—Ca2vii154.85 (11)O7B—O7—Ca5158.7 (18)
O7—Ca3—Ca2vii96.97 (14)P2—O7—Ca5113.4 (3)
O2vii—Ca3—Ca2vii45.37 (12)Ca3—O7—Ca5108.9 (2)
O1viii—Ca3—Ca2vii89.21 (7)O7B—O7—Ca467.1 (17)
O4viii—Ca3—Ca2vii40.37 (12)P2—O7—Ca496.3 (3)
P1viii—Ca3—Ca2vii61.94 (3)Ca5B—O7—Ca4104.4 (3)
O12—Ca3—P317.46 (11)Ca3—O7—Ca4104.5 (2)
O10vi—Ca3—P3168.22 (13)Ca5—O7—Ca498.2 (2)
O11v—Ca3—P3112.88 (11)O8B—O8—P269 (3)
O7—Ca3—P383.03 (15)O8B—O8—Ca1B83 (3)
O2vii—Ca3—P389.85 (12)P2—O8—Ca1B117.4 (4)
O1viii—Ca3—P3116.02 (8)O8B—O8—Ca2116 (3)
O4viii—Ca3—P362.62 (12)P2—O8—Ca2131.6 (4)
P1viii—Ca3—P390.64 (3)Ca1B—O8—Ca2110.8 (3)
Ca2vii—Ca3—P354.23 (3)O8B—O8—Ca175 (3)
O12—Ca3—P285.21 (12)P2—O8—Ca1124.9 (4)
O10vi—Ca3—P274.60 (14)Ca2—O8—Ca1100.8 (3)
O11v—Ca3—P283.85 (11)O6C—O6B—P268 (4)
O7—Ca3—P219.79 (14)O6C—O6B—Ca6103 (4)
O2vii—Ca3—P289.16 (14)P2—O6B—Ca6152.0 (11)
O1viii—Ca3—P2147.84 (8)O6C—O6B—Ca1B160 (4)
O4viii—Ca3—P2154.29 (12)P2—O6B—Ca1B97.9 (8)
P1viii—Ca3—P2171.13 (4)Ca6—O6B—Ca1B95.8 (8)
Ca2vii—Ca3—P2116.75 (4)O7—O7B—P277.2 (17)
P3—Ca3—P295.28 (3)O7—O7B—Ca4101.4 (18)
O12—Ca3—Ca2135.75 (13)P2—O7B—Ca4101.4 (5)
O10vi—Ca3—Ca242.87 (14)P2—O7B—Ca5B86.5 (6)
O11v—Ca3—Ca239.70 (10)Ca4—O7B—Ca5B94.6 (4)
O7—Ca3—Ca275.25 (14)O8—O8B—P298 (3)
O2vii—Ca3—Ca2119.48 (13)O8—O8B—Ca1B87 (3)
O1viii—Ca3—Ca293.99 (7)P2—O8B—Ca1B123.0 (8)
O4viii—Ca3—Ca2149.32 (12)O10B—P3—O1182.9 (5)
P1viii—Ca3—Ca2122.78 (4)O10B—P3—O12128.4 (5)
Ca2vii—Ca3—Ca2164.84 (4)O11—P3—O12116.8 (3)
P3—Ca3—Ca2135.40 (4)O10B—P3—O9B119.9 (7)
P2—Ca3—Ca256.03 (3)O11—P3—O9B96.7 (6)
O13ix—Ca5—O12117.7 (2)O12—P3—O9B105.3 (6)
O13ix—Ca5—O16119.9 (2)O10B—P3—O12B113.3 (6)
O12—Ca5—O16117.6 (2)O11—P3—O12B137.3 (4)
O13ix—Ca5—O775.50 (19)O9B—P3—O12B106.6 (7)
O12—Ca5—O766.83 (19)O11—P3—O10110.2 (3)
O16—Ca5—O7106.94 (19)O12—P3—O10108.1 (3)
O13ix—Ca5—O5Cvii84.6 (3)O9B—P3—O10119.9 (6)
O12—Ca5—O5Cvii92.9 (4)O12B—P3—O1088.6 (5)
O16—Ca5—O5Cvii113.9 (3)O10B—P3—O9113.0 (4)
O7—Ca5—O5Cvii139.2 (4)O11—P3—O9108.0 (3)
O13ix—Ca5—O9156.34 (19)O12—P3—O9105.3 (3)
O12—Ca5—O958.65 (19)O12B—P3—O9101.3 (4)
O16—Ca5—O976.6 (2)O10—P3—O9108.1 (3)
O7—Ca5—O9118.0 (2)O10B—P3—O11B108.3 (6)
O5Cvii—Ca5—O972.6 (4)O12—P3—O11B76.4 (4)
O13ix—Ca5—O684.33 (18)O9B—P3—O11B108.7 (7)
O12—Ca5—O6105.32 (19)O12B—P3—O11B97.5 (6)
O16—Ca5—O660.14 (17)O10—P3—O11B126.8 (4)
O7—Ca5—O650.71 (18)O9—P3—O11B122.0 (4)
O5Cvii—Ca5—O6161.5 (4)O10B—P3—Ca5147.4 (5)
O9—Ca5—O6119.3 (2)O11—P3—Ca5129.11 (17)
O13ix—Ca5—O15103.29 (18)O12—P3—Ca548.82 (18)
O12—Ca5—O15127.6 (2)O9B—P3—Ca557.9 (6)
O16—Ca5—O1556.46 (17)O12B—P3—Ca549.9 (4)
O7—Ca5—O15160.7 (2)O10—P3—Ca5120.7 (2)
O5Cvii—Ca5—O1558.5 (3)O9—P3—Ca556.5 (2)
O9—Ca5—O1570.57 (19)O11B—P3—Ca5102.1 (4)
O6—Ca5—O15110.1 (2)O10B—P3—Ca5B154.8 (5)
O13ix—Ca5—O5vii83.07 (17)O11—P3—Ca5B121.9 (2)
O12—Ca5—O5vii95.6 (2)O12—P3—Ca5B47.8 (3)
O16—Ca5—O5vii112.8 (2)O9B—P3—Ca5B57.7 (6)
O7—Ca5—O5vii140.2 (2)O12B—P3—Ca5B52.6 (4)
O5Cvii—Ca5—O5vii2.7 (4)O10—P3—Ca5B127.9 (3)
O9—Ca5—O5vii74.5 (2)O9—P3—Ca5B58.3 (3)
O6—Ca5—O5vii158.8 (2)O11B—P3—Ca5B95.1 (4)
O15—Ca5—O5vii56.94 (17)O10B—P3—Ca2vii77.3 (4)
O13ix—Ca5—P3141.61 (17)O11—P3—Ca2vii133.23 (17)
O12—Ca5—P328.36 (11)O12—P3—Ca2vii53.94 (19)
O16—Ca5—P398.35 (16)O9B—P3—Ca2vii129.9 (6)
O7—Ca5—P391.63 (17)O10—P3—Ca2vii54.2 (2)
O5Cvii—Ca5—P382.2 (3)O9—P3—Ca2vii118.7 (2)
O9—Ca5—P330.29 (14)O11B—P3—Ca2vii108.5 (4)
O6—Ca5—P3115.37 (16)Ca5—P3—Ca2vii82.28 (7)
O15—Ca5—P3100.10 (15)Ca5B—P3—Ca2vii86.73 (18)
O5vii—Ca5—P384.75 (16)O11—P3—Ca2v47.54 (15)
O13ix—Ca5—P4117.49 (17)O12—P3—Ca2v150.24 (18)
O12—Ca5—P4124.42 (18)O9B—P3—Ca2v102.0 (6)
O16—Ca5—P428.05 (11)O12B—P3—Ca2v149.1 (4)
O7—Ca5—P4134.89 (17)O10—P3—Ca2v66.8 (2)
O5Cvii—Ca5—P485.9 (3)O9—P3—Ca2v104.0 (2)
O9—Ca5—P468.29 (16)O11B—P3—Ca2v83.9 (4)
O6—Ca5—P486.08 (15)Ca5—P3—Ca2v159.96 (8)
O15—Ca5—P428.73 (11)Ca5B—P3—Ca2v158.3 (2)
O5vii—Ca5—P484.74 (15)Ca2vii—P3—Ca2v114.22 (4)
P3—Ca5—P497.36 (11)P3—O9—Ca4vii131.9 (3)
O13ix—Ca5—P274.80 (12)P3—O9—Ca1ii108.7 (3)
O12—Ca5—P287.96 (14)Ca4vii—O9—Ca1ii102.4 (2)
O16—Ca5—P285.55 (13)P3—O9—Ca593.2 (3)
O7—Ca5—P225.01 (14)Ca4vii—O9—Ca598.9 (2)
O5Cvii—Ca5—P2157.1 (3)Ca1ii—O9—Ca5124.0 (3)
O9—Ca5—P2126.02 (16)P3—O10—Ca3vii151.6 (3)
O6—Ca5—P226.29 (12)P3—O10—Ca2vii97.0 (2)
O15—Ca5—P2135.74 (16)Ca3vii—O10—Ca2vii100.5 (2)
O5vii—Ca5—P2156.53 (18)P3—O10—Ca2v84.5 (2)
P3—Ca5—P2107.82 (9)Ca3vii—O10—Ca2v91.51 (16)
P4—Ca5—P2112.27 (9)Ca2vii—O10—Ca2v149.48 (19)
O7—Ca5B—O13ix77.5 (4)P3—O11—Ca3v150.3 (2)
O7—Ca5B—O15B153.5 (6)P3—O11—Ca2v106.0 (2)
O13ix—Ca5B—O15B85.8 (4)Ca3v—O11—Ca2v103.13 (16)
O7—Ca5B—O12B78.6 (4)P3—O11—Ca1ii88.83 (18)
O13ix—Ca5B—O12B104.1 (4)Ca3v—O11—Ca1ii96.14 (14)
O15B—Ca5B—O12B126.0 (5)Ca2v—O11—Ca1ii91.33 (13)
O7—Ca5B—O9B119.1 (5)P3—O12—Ca3135.7 (3)
O13ix—Ca5B—O9B145.8 (5)P3—O12—Ca5102.8 (2)
O15B—Ca5B—O9B86.0 (5)Ca3—O12—Ca5114.0 (2)
O12B—Ca5B—O9B56.3 (5)P3—O12—Ca2vii98.1 (2)
O7—Ca5B—O7B2.4 (3)Ca3—O12—Ca2vii90.65 (15)
O13ix—Ca5B—O7B76.2 (4)Ca5—O12—Ca2vii111.7 (2)
O15B—Ca5B—O7B154.2 (6)P3—O9B—Ca1Bii137.4 (9)
O12B—Ca5B—O7B77.0 (4)P3—O9B—Ca4vii115.3 (7)
O9B—Ca5B—O7B119.2 (5)Ca1Bii—O9B—Ca4vii95.8 (5)
O7—Ca5B—O6C57.9 (10)P3—O9B—Ca5B93.7 (7)
O13ix—Ca5B—O6C80.3 (13)Ca1Bii—O9B—Ca5B110.9 (6)
O15B—Ca5B—O6C99.3 (11)Ca4vii—O9B—Ca5B97.8 (5)
O12B—Ca5B—O6C134.6 (11)P3—O12B—Ca5B98.3 (5)
O9B—Ca5B—O6C133.8 (13)O16B—P4—O14B114.7 (6)
O7B—Ca5B—O6C59.9 (10)O16B—P4—O13105.5 (4)
O7—Ca5B—O5Cvii129.7 (5)O14B—P4—O13109.1 (4)
O13ix—Ca5B—O5Cvii73.8 (3)O16B—P4—O15136.6 (5)
O15B—Ca5B—O5Cvii62.5 (4)O14B—P4—O1575.1 (4)
O12B—Ca5B—O5Cvii69.7 (4)O13—P4—O15110.6 (2)
O9B—Ca5B—O5Cvii73.0 (5)O14B—P4—O16130.1 (4)
O7B—Ca5B—O5Cvii127.3 (5)O13—P4—O16116.0 (2)
O6C—Ca5B—O5Cvii148.9 (13)O15—P4—O16106.2 (3)
O7—Ca5B—O16B125.1 (4)O16B—P4—O1482.0 (4)
O13ix—Ca5B—O16B130.5 (5)O13—P4—O14110.6 (2)
O15B—Ca5B—O16B54.2 (4)O15—P4—O14106.2 (3)
O12B—Ca5B—O16B122.2 (5)O16—P4—O14106.6 (2)
O9B—Ca5B—O16B67.0 (4)O16B—P4—O15B112.7 (5)
O7B—Ca5B—O16B127.5 (4)O14B—P4—O15B109.3 (5)
O6C—Ca5B—O16B79.3 (11)O13—P4—O15B104.8 (4)
O5Cvii—Ca5B—O16B104.9 (4)O16—P4—O15B79.0 (4)
O7—Ca5B—P229.27 (19)O14—P4—O15B136.1 (4)
O13ix—Ca5B—P280.2 (3)O16B—P4—Ca1Bii54.5 (4)
O15B—Ca5B—P2127.8 (5)O14B—P4—Ca1Bii60.5 (4)
O12B—Ca5B—P2106.2 (4)O13—P4—Ca1Bii128.20 (16)
O9B—Ca5B—P2129.6 (4)O15—P4—Ca1Bii113.9 (2)
O7B—Ca5B—P231.4 (3)O16—P4—Ca1Bii75.1 (2)
O6C—Ca5B—P228.9 (10)O15B—P4—Ca1Bii126.9 (4)
O5Cvii—Ca5B—P2151.4 (5)O16B—P4—Ca5B70.3 (5)
O16B—Ca5B—P2101.0 (3)O14B—P4—Ca5B110.7 (4)
O7—Ca5B—P395.1 (4)O13—P4—Ca5B137.5 (2)
O13ix—Ca5B—P3131.6 (4)O15—P4—Ca5B66.9 (2)
O15B—Ca5B—P3111.4 (4)O14—P4—Ca5B110.5 (3)
O12B—Ca5B—P329.1 (3)O15B—P4—Ca5B47.4 (4)
O9B—Ca5B—P328.6 (3)Ca1Bii—P4—Ca5B85.2 (2)
O7B—Ca5B—P394.4 (4)O16B—P4—Ca577.3 (4)
O6C—Ca5B—P3135.6 (12)O14B—P4—Ca5106.2 (4)
O5Cvii—Ca5B—P375.5 (4)O13—P4—Ca5138.93 (15)
O16B—Ca5B—P393.1 (4)O15—P4—Ca559.64 (19)
P2—Ca5B—P3115.4 (3)O16—P4—Ca547.37 (19)
O7—Ca5B—P4150.3 (4)O14—P4—Ca5110.31 (18)
O13ix—Ca5B—P4113.5 (4)Ca1Bii—P4—Ca587.58 (11)
O15B—Ca5B—P428.9 (3)O16B—P4—Ca4xi148.1 (4)
O12B—Ca5B—P4121.8 (4)O14B—P4—Ca4xi78.0 (4)
O9B—Ca5B—P468.0 (4)O15—P4—Ca4xi73.77 (19)
O7B—Ca5B—P4152.7 (4)O16—P4—Ca4xi151.55 (19)
O6C—Ca5B—P495.5 (10)O14—P4—Ca4xi100.44 (16)
O5Cvii—Ca5B—P479.8 (3)O15B—P4—Ca4xi87.7 (3)
O16B—Ca5B—P427.0 (2)Ca1Bii—P4—Ca4xi131.80 (8)
P2—Ca5B—P4122.4 (3)Ca5B—P4—Ca4xi135.06 (16)
P3—Ca5B—P496.5 (3)Ca5—P4—Ca4xi129.28 (6)
O6B—Ca6—O1693.5 (5)O16B—P4—Ca4vii116.3 (4)
O6B—Ca6—O624.6 (5)O13—P4—Ca4vii135.28 (13)
O16—Ca6—O669.23 (19)O16—P4—Ca4vii107.69 (18)
O6B—Ca6—O14Bi86.3 (6)O14—P4—Ca4vii62.85 (17)
O16—Ca6—O14Bi160.4 (3)O15B—P4—Ca4vii73.8 (3)
O6—Ca6—O14Bi110.5 (3)Ca1Bii—P4—Ca4vii71.17 (9)
O6B—Ca6—O5x105.6 (6)Ca5B—P4—Ca4vii74.86 (17)
O16—Ca6—O5x100.1 (2)Ca5—P4—Ca4vii69.03 (6)
O6—Ca6—O5x105.3 (2)Ca4xi—P4—Ca4vii92.31 (4)
O14Bi—Ca6—O5x98.7 (3)P4—O13—Ca5xi140.6 (2)
O6B—Ca6—O16B112.8 (6)P4—O13—Ca4xi109.79 (16)
O16—Ca6—O16B21.9 (3)Ca5xi—O13—Ca4xi108.54 (16)
O6—Ca6—O16B89.5 (3)P4—O13—Ca5Bxi142.5 (3)
O14Bi—Ca6—O16B145.0 (4)Ca4xi—O13—Ca5Bxi103.4 (3)
O5x—Ca6—O16B103.4 (3)P4—O14—Ca1ii126.5 (2)
O6B—Ca6—O15xi150.4 (5)P4—O14—Ca6ii124.6 (2)
O16—Ca6—O15xi115.98 (18)Ca1ii—O14—Ca6ii108.21 (17)
O6—Ca6—O15xi172.8 (2)P4—O14—Ca4vii89.0 (2)
O14Bi—Ca6—O15xi66.4 (3)Ca1ii—O14—Ca4vii85.17 (14)
O5x—Ca6—O15xi69.5 (2)Ca6ii—O14—Ca4vii87.31 (13)
O16B—Ca6—O15xi96.5 (3)P4—O15—Ca6ix150.0 (3)
O6B—Ca6—O14i64.3 (6)P4—O15—Ca4vii109.6 (3)
O16—Ca6—O14i150.04 (16)Ca6ix—O15—Ca4vii99.51 (18)
O6—Ca6—O14i88.44 (18)P4—O15—Ca591.6 (2)
O14Bi—Ca6—O14i22.1 (2)Ca6ix—O15—Ca595.86 (18)
O5x—Ca6—O14i105.00 (19)Ca4vii—O15—Ca589.57 (18)
O16B—Ca6—O14i151.1 (3)P4—O15—Ca4xi78.2 (2)
O15xi—Ca6—O14i88.29 (17)Ca6ix—O15—Ca4xi83.84 (15)
O6B—Ca6—O3ii87.2 (6)Ca4vii—O15—Ca4xi113.24 (18)
O16—Ca6—O3ii94.23 (17)Ca5—O15—Ca4xi157.0 (2)
O6—Ca6—O3ii92.7 (2)P4—O16—Ca6128.1 (3)
O14Bi—Ca6—O3ii66.2 (3)P4—O16—Ca5104.6 (2)
O5x—Ca6—O3ii160.0 (2)Ca6—O16—Ca5120.8 (2)
O16B—Ca6—O3ii85.0 (3)P4—O14B—Ca6ii136.5 (6)
O15xi—Ca6—O3ii91.80 (18)P4—O14B—Ca4vii117.8 (5)
O14i—Ca6—O3ii66.25 (16)Ca6ii—O14B—Ca4vii105.2 (4)
O6B—Ca6—O3Bii98.1 (6)P4—O14B—Ca1Bii89.9 (5)
O16—Ca6—O3Bii91.0 (3)Ca6ii—O14B—Ca1Bii92.4 (4)
O6—Ca6—O3Bii101.7 (3)Ca4vii—O14B—Ca1Bii95.6 (3)
O14Bi—Ca6—O3Bii69.7 (4)P4—O15B—Ca5B103.7 (5)
O5x—Ca6—O3Bii153.0 (3)P4—O15B—Ca6ix134.1 (5)
O16B—Ca6—O3Bii78.5 (4)Ca5B—O15B—Ca6ix114.3 (4)
O15xi—Ca6—O3Bii83.5 (3)P4—O16B—Ca6129.1 (6)
O14i—Ca6—O3Bii73.7 (3)P4—O16B—Ca1Bii96.5 (5)
O3ii—Ca6—O3Bii11.2 (3)Ca6—O16B—Ca1Bii134.4 (5)
O6B—Ca6—O6C18.4 (12)P4—O16B—Ca5B82.7 (5)
O16—Ca6—O6C82.9 (13)Ca6—O16B—Ca5B87.8 (4)
O6—Ca6—O6C17.4 (12)Ca1Bii—O16B—Ca5B99.1 (4)
O14Bi—Ca6—O6C101.4 (13)O6—O6C—O6B77 (6)
O5x—Ca6—O6C92.6 (14)O6—O6C—P279 (4)
O16B—Ca6—O6C104.3 (13)O6B—O6C—P283 (4)
O15xi—Ca6—O6C155.4 (13)O6—O6C—Ca668 (4)
O14i—Ca6—O6C80.0 (13)O6B—O6C—Ca658 (4)
O3ii—Ca6—O6C102.9 (14)P2—O6C—Ca6133 (4)
O3Bii—Ca6—O6C113.2 (14)O6B—O6C—Ca5B110 (5)
O6B—Ca6—O5Cx112.8 (6)P2—O6C—Ca5B81 (2)
O16—Ca6—O5Cx97.4 (3)Ca6—O6C—Ca5B88.3 (16)
O6—Ca6—O5Cx110.9 (4)O6—O6C—Ca6x147 (6)
O14Bi—Ca6—O5Cx100.7 (4)O6B—O6C—Ca6x136 (5)
O5x—Ca6—O5Cx7.5 (4)P2—O6C—Ca6x97 (3)
O16B—Ca6—O5Cx98.2 (4)Ca6—O6C—Ca6x129 (2)
O15xi—Ca6—O5Cx64.3 (4)Ca5B—O6C—Ca6x113 (2)
O14i—Ca6—O5Cx109.5 (3)P2—O5C—Ca493.4 (6)
O3ii—Ca6—O5Cx156.0 (4)P2—O5C—Ca6x115.3 (7)
O3Bii—Ca6—O5Cx147.2 (4)Ca4—O5C—Ca6x96.2 (5)
O6C—Ca6—O5Cx99.3 (14)P2—O5C—Ca5vi143.3 (7)
O9vi—Ca4—O7B90.1 (3)Ca4—O5C—Ca5vi95.3 (5)
O9vi—Ca4—O3Bvii94.9 (3)Ca6x—O5C—Ca5vi99.1 (5)
O7B—Ca4—O3Bvii123.0 (4)P2—O5C—Ca5Bvi143.9 (7)
O9vi—Ca4—O13ix174.51 (17)Ca4—O5C—Ca5Bvi93.8 (5)
O7B—Ca4—O13ix84.8 (3)Ca6x—O5C—Ca5Bvi99.0 (5)
Symmetry codes: (i) x, y+3/2, z+1/2; (ii) x, y+3/2, z1/2; (iii) x, y+1, z; (iv) x+2, y+1, z+2; (v) x+2, y+1, z+1; (vi) x, y+1/2, z+1/2; (vii) x, y+1/2, z1/2; (viii) x+2, y1/2, z+3/2; (ix) x+1, y1/2, z+1/2; (x) x+1, y+1, z+1; (xi) x+1, y+1/2, z+1/2; (xii) x+2, y+1/2, z+3/2.

Experimental details

(h_room_needle)(e_room_prism)(c_room_prism)(v_room)
Crystal data
Chemical formula3(O4P)·Cl·5(Ca)3(O4P)·Cl·5(Ca)3(O4P)·Cl·5(Ca)3(O4P)·Cl·5(C)a
Mr520.76520.76520.76520.76
Crystal system, space groupTrigonal, P63/mTrigonal, P63/mTrigonal, P63/mTrigonal, P63/m
Temperature (K)293293293293
a, b, c (Å)9.6452 (2), 9.6452 (2), 6.7636 (2)9.6434 (2), 9.6434 (2), 6.7643 (2)9.6430 (2), 9.6430 (2), 6.7620 (1)9.6414 (2), 9.6414 (2), 6.7631 (2)
α, β, γ (°)90, 90, 12090, 90, 12090, 90, 12090, 90, 120
V3)544.92 (2)544.77 (2)544.54 (2)544.45 (2)
Z2222
Radiation typeMo KαMo KαMo KαMo Kα
µ (mm1)3.213.213.213.21
Crystal size (mm)0.30 × 0.03 × 0.020.29 × 0.12 × 0.10.25 × 0.12 × 0.050.45 × 0.19 × 0.16
Data collection
DiffractometerBRUKER APPEX-II CCD
diffractometer
BRUKER APPEX-II CCD
diffractometer
BRUKER APPEX-II CCD
diffractometer
BRUKER APPEX-II CCD
diffractometer
Absorption correctionMulti-scan
BRUKER SADABS
Multi-scan
BRUKER SADABS
Multi-scan
BRUKER SADABS
Multi-scan
BRUKER SADABS
Tmin, Tmax0.802, 10.654, 10.852, 10.746, 1
No. of measured, independent and
observed [I > 2σ(I)] reflections
12306, 403, 345 11773, 399, 386 6423, 403, 398 2637, 405, 392
Rint0.0610.0270.0150.016
(sin θ/λ)max1)0.6250.6230.6250.625
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.022, 0.056, 1.08 0.017, 0.046, 1.11 0.017, 0.045, 1.18 0.017, 0.052, 1.12
No. of reflections403399403405
No. of parameters40414141
No. of restraints0000
H-atom treatment
Δρmax, Δρmin (e Å3)0.56, 0.520.28, 0.420.34, 0.350.37, 0.36


(1_low_needle)(2_low_prism)(3_low_prism)(4_low_needle)
Crystal data
Chemical formula3(O4P)·Cl·5(Ca)3(O4P)·Cl·5(Ca)3(O4P)·Cl·5(Ca)3(O4P)·Cl·5(Ca)
Mr520.76520.76520.76520.76
Crystal system, space groupTrigonal, P63/mTrigonal, P63/mTrigonal, P63/mTrigonal, P63/m
Temperature (K)100100100100
a, b, c (Å)9.6368 (2), 9.6368 (2), 6.7482 (2)9.6341 (1), 9.6341 (1), 6.7445 (2)9.6340 (2), 9.6340 (2), 6.7440 (3)9.6343 (1), 9.6343 (1), 6.7430 (1)
α, β, γ (°)90, 90, 12090, 90, 12090, 90, 12090, 90, 120
V3)542.73 (2)542.13 (2)542.08 (3)542.03 (1)
Z2222
Radiation typeMo KαMo KαMo KαMo Kα
µ (mm1)3.233.233.233.23
Crystal size (mm)0.34 × 0.02 × 0.020.17 × 0.07 × 0.050.25 × 0.12 × 0.050.17 × 0.07 × 0.05
Data collection
DiffractometerBRUKER APPEX-II CCD
diffractometer
BRUKER APPEX-II CCD
diffractometer
BRUKER APPEX-II CCD
diffractometer
BRUKER APPEX-II CCD
diffractometer
Absorption correctionMulti-scan
BRUKER SADABS
Multi-scan
BRUKER SADABS
Multi-scan
BRUKER SADABS
Multi-scan
BRUKER SADABS
Tmin, Tmax0.829, 10.666, 10.666, 10.685, 1
No. of measured, independent and
observed [I > 2σ(I)] reflections
7462, 400, 354 6361, 403, 401 5403, 403, 400 15064, 435, 414
Rint0.0370.0330.0370.044
(sin θ/λ)max1)0.6240.6240.6240.641
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.016, 0.038, 1.10 0.023, 0.060, 1.30 0.029, 0.081, 1.37 0.015, 0.037, 1.05
No. of reflections400403403435
No. of parameters41414041
No. of restraints0000
H-atom treatment
Δρmax, Δρmin (e Å3)0.37, 0.360.40, 0.520.45, 1.230.32, 0.29


(C_mono)(E_mono)(H_mono)(G_mono)
Crystal data
Chemical formulaCa5ClO12P3Ca5ClO12P3Ca5ClO12P3Ca5ClO12P3
Mr520.76520.76520.76520.76
Crystal system, space groupMOnoclinic, P21/cMonoclinic, P21/cMonoclinic, P21/cMonoclinic, P21/c
Temperature (K)293293293293
a, b, c (Å)9.6410 (2), 6.7620 (3), 19.2850 (6)9.6430 (3), 6.7641 (2), 19.2882 (6)9.6434 (3), 6.7635 (2), 19.2846 (6)9.6397 (4), 6.7657 (3), 19.2731 (9)
α, β, γ (°)90, 119.984 (1), 9090, 120.003 (1), 9090, 119.965 (2), 9090, 119.984 (3), 90
V3)1088.97 (6)1089.51 (6)1089.67 (6)1088.75 (8)
Z4444
Radiation typeMo KαMo KαMo KαMo Kα
µ (mm1)3.213.213.213.21
Crystal size (mm)0.25 × 0.12 × 0.050.29 × 0.12 × 0.100.34 × 0.02 × 0.020.20 × 0.17 × 0.02
Data collection
DiffractometerBRUKER APPEX-II CCD
diffractometer
BRUKER APPEX-II CCD
diffractometer
BRUKER APPEX-II CCD
diffractometer
BRUKER APPEX-II CCD
diffractometer
Absorption correctionMulti-scan
BRUKER SADABS
Multi-scan
BRUKER SADABS
Multi-scan
BRUKER SADABS
Multi-scan
BRUKER SADABS
Tmin, Tmax0.836, 10.682, 10.815, 10.859, 1
No. of measured, independent and
observed [I > 2σ(I)] reflections
2218, 2218, 1276 11773, 2208, 1255 12810, 2208, 981 15519, 2209, 1142
Rint0.0240.0270.0540.042
(sin θ/λ)max1)0.6250.6250.6250.625
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.023, 0.073, 1.10 0.023, 0.076, 1.06 0.039, 0.109, 1.02 0.022, 0.076, 0.90
No. of reflections2218220822082209
No. of parameters201201129201
No. of restraints0000
H-atom treatment
Δρmax, Δρmin (e Å3)0.45, 0.430.44, 0.521.12, 0.760.49, 0.39


(B_mono)(D_mono)(F_mono)(A_mono)
Crystal data
Chemical formulaCa5ClO12P3Ca5ClO12P3Ca5ClO12P3Ca5ClO12P3
Mr520.76520.76520.76520.76
Crystal system, space groupMonoclinic, P21/cMonoclinic, P21/cMonoclinic, P21/cMonoclinic, P21/c
Temperature (K)100100100100
a, b, c (Å)9.6370 (3), 6.7479 (2), 19.2702 (7)9.6307 (4), 6.7425 (3), 19.2602 (7)9.6344 (3), 6.7442 (2), 19.2656 (5)9.6307 (4), 6.7425 (3), 19.2602 (7)
α, β, γ (°)90, 120.002 (1), 9090, 119.969 (1), 9090, 119.994 (1), 9090, 119.969 (1), 90
V3)1085.22 (6)1083.44 (8)1084.16 (5)1083.44 (8)
Z4444
Radiation typeMo KαMo KαMo KαMo Kα
µ (mm1)3.223.233.233.23
Crystal size (mm)0.34 × 0.02 × 0.020.25 × 0.12 × 0.050.29 × 0.12 × 0.100.17 × 0.07 × 0.05
Data collection
DiffractometerBRUKER APPEX-II CCD
diffractometer
BRUKER APPEX-II CCD
diffractometer
BRUKER APPEX-II CCD
diffractometer
BRUKER APPEX-II CCD
diffractometer
Absorption correctionMulti-scan
BRUKER SADABS
Multi-scan
BRUKER SADABS
Multi-scan
BRUKER SADABS
Multi-scan
BRUKER SADABS
Tmin, Tmax0.875, 10.806, 10.482, 10.870, 1
No. of measured, independent and
observed [I > 2σ(I)] reflections
16759, 2153, 998 14216, 2216, 1444 12807, 2213, 1431 17423, 2212, 1285
Rint0.0450.0270.0300.037
(sin θ/λ)max1)0.6250.6260.6250.625
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.029, 0.085, 0.94 0.039, 0.095, 1.15 0.038, 0.103, 1.15 0.036, 0.093, 1.16
No. of reflections2153221622132212
No. of parameters147130130129
No. of restraints0000
H-atom treatment
Δρmax, Δρmin (e Å3)1.02, 0.581.03, 0.661.01, 0.61.12, 0.59


(1400l)(1400r)(1450l)(1450r)
Crystal data
Chemical formula3(O4P)·0.54(Cl)·0.46(OH)·5(Ca)3(O4P)·0.54(Cl)·0.46(OH)·5(Ca)3(O4P)·0.44(Cl)·0.56(OH)·5(Ca)3(O4P)·0.44(Cl)·0.56(OH)·5(Ca)
Mr512.32512.32510.42510.42
Crystal system, space groupTrigonal, P63/mTrigonal, P63/mTrigonal, P63/mTrigonal, P63/m
Temperature (K)100293100293
a, b, c (Å)9.5377 (3), 9.5377 (3), 6.7999 (5)9.5439 (2), 9.5439 (2), 6.8174 (3)9.4815 (2), 9.4815 (2), 6.8200 (3)9.4894 (4), 9.4894 (4), 6.8612 (7)
α, β, γ (°)90, 90, 12090, 90, 12090, 90, 12090, 90, 120
V3)535.70 (5)537.78 (3)530.97 (3)535.07 (6)
Z2222
Radiation typeMo KαMo KαMo KαMo Kα
µ (mm1)3.163.143.163.14
Crystal size (mm)0.48 × 0.11 × 0.060.23 × 0.09 × 0.070.11 × 0.08 × 0.040.25 × 0.12 × 0.05
Data collection
DiffractometerBRUKER APPEX-II CCD
diffractometer
BRUKER APPEX-II CCD
diffractometer
BRUKER APPEX-II CCD
diffractometer
BRUKER APPEX-II CCD
diffractometer
Absorption correctionMulti-scan
BRUKER SADABS
Multi-scan
BRUKER SADABS
Multi-scan
BRUKER SADABS
Multi-scan
BRUKER SADABS
Tmin, Tmax0.685, 10.343, 0.4300.815, 10.598, 0.748
No. of measured, independent and
observed [I > 2σ(I)] reflections
2425, 485, 456 2996, 402, 367 2999, 588, 552 5663, 397, 376
Rint0.0440.0310.0240.030
(sin θ/λ)max1)0.6670.6260.7150.623
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.027, 0.064, 1.18 0.028, 0.069, 1.20 0.034, 0.075, 1.13 0.032, 0.076, 0.96
No. of reflections485402588397
No. of parameters47464744
No. of restraints15141514
H-atom treatmentH atoms treated by a mixture of independent and constrained refinementH atoms treated by a mixture of independent and constrained refinementH atoms treated by a mixture of independent and constrained refinementH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.87, 0.860.74, 0.541.45, 0.920.89, 1.03


(1475l)(1475r)(1480l)(1480r)
Crystal data
Chemical formula3(O4P)·0.29(Cl)·0.71(OH)·5(Ca)3(O4P)·0.28(Cl)·0.72(OH)·5(Ca)3(O4P)·0.18(Cl)·0.82(OH)·5(Ca)3(O4P)·0.18(Cl)·0.82(OH)·5(Ca)
Mr507.86507.8505.67505.80
Crystal system, space groupTrigonal, P63/mTrigonal, P63/mTrigonal, P63/mTrigonal, P63/m
Temperature (K)100293100293
a, b, c (Å)9.431 (5), 9.431 (5), 6.860 (5)9.4284 (8), 9.4284 (8), 6.8756 (7)9.4139 (2), 9.4139 (2), 6.8679 (2)9.4230 (2), 9.4230 (2), 6.8794 (3)
α, β, γ (°)90.000 (5), 90.000 (5), 120.000 (5)90, 90, 12090, 90, 12090, 90, 120
V3)528.4 (6)529.32 (12)527.10 (2)529.00 (3)
Z2222
Radiation typeMo KαMo KαMo KαMo Kα
µ (mm1)3.143.133.083.11
Crystal size (mm)0.11 × 0.08 × 0.040.29 × 0.09 × 0.030.20 × 0.17 × 0.020.23 × 0.08 × 0.07
Data collection
DiffractometerBRUKER APPEX-II CCD
diffractometer
BRUKER APPEX-II CCD
diffractometer
BRUKER APPEX-II CCD
diffractometer
BRUKER APPEX-II CCD
diffractometer
Absorption correctionMulti-scan
BRUKER SADABS
Multi-scan
BRUKER SADABS
Multi-scan
BRUKER SADABS
Multi-scan
BRUKER SADABS
Tmin, Tmax0.672, 10.772, 10.745, 10.744, 1
No. of measured, independent and
observed [I > 2σ(I)] reflections
10188, 588, 542 2393, 393, 351 2668, 586, 545 5438, 389, 371
Rint0.0190.0380.0190.033
(sin θ/λ)max1)0.7150.6240.7130.626
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.037, 0.085, 1.22 0.033, 0.081, 1.07 0.039, 0.086, 1.13 0.029, 0.068, 1.15
No. of reflections588393586389
No. of parameters48474847
No. of restraints15321532
H-atom treatmentH atoms treated by a mixture of independent and constrained refinementH atoms treated by a mixture of independent and constrained refinementH atoms treated by a mixture of independent and constrained refinementH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)1.67, 1.180.84, 0.601.57, 1.290.77, 0.57


(1500l)
Crystal data
Chemical formulaCa64(PO4)
Mr620.36
Crystal system, space groupMonoclinic, P21/c
Temperature (K)100
a, b, c (Å)12.8348 (6), 9.0961 (4), 12.8365 (5)
α, β, γ (°)90, 107.434 (2), 90
V3)1429.78 (11)
Z4
Radiation typeMo Kα
µ (mm1)2.77
Crystal size (mm)0.23 × 0.07 × 0.06
Data collection
DiffractometerBRUKER APPEX-II CCD
diffractometer
Absorption correctionMulti-scan
BRUKER SADABS
Tmin, Tmax0.611, 0.746
No. of measured, independent and
observed [I > 2σ(I)] reflections
11763, 2916, 2303
Rint0.032
(sin θ/λ)max1)0.626
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.042, 0.101, 1.06
No. of reflections2916
No. of parameters362
No. of restraints205
H-atom treatment
Δρmax, Δρmin (e Å3)0.93, 0.85

Computer programs: APPEX2 (BRUKER AXS, 2005), SIR2004 (Giacovazzo et al., 2004), SIR97 (Giacovazzo et al.l, 1999), SHELXL97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 2008), ORTEP-3 for Windows (Farrugia, 1997), WinGX publication routines (Farrugia, 1999).

 

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