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Structure analysis using single-crystal diffraction was carried out as a contribution to the dispute about the nature of the water channel structure of bassanite (CaSO4·0.5H2O). A recent result of Weiss & Bräu (2009) for the crystal structure of bassanite (monoclinic, space group C2) at ambient conditions of air humidity was confirmed. In the presence of high relative air humidity the crystal structure of bassanite transformed due to the incorporation of additional water of hydration. The crystal structure of CaSO4·0.625H2O was solved by single-crystal diffraction at 298 K and 75% relative air humidity. The experimental results provided an insight into both crystal structures. A model explaining the phase transition from CaSO4·0.625H2O to CaSO4·0.5H2O was derived. The monoclinic cell setting of CaSO4·0.5H2O and the trigonal cell setting of CaSO4·0.625H2O were confirmed by powder diffraction.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768111041759/sn5106sup1.cif
Contains datablocks caso40625, caso4_05, New_Global_Publ_Block

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768111041759/sn5106caso40625sup2.hkl
Contains datablock hs_hh_nacl_301010_0m

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768111041759/sn5106caso4_05sup3.hkl
Contains datablock tu_hklf5

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768111041759/sn5106Isup4.hkl
Contains datablock I

Comment top

The stucture of the title compound, (I), is shown below. Dimensions are available in the archived CIF.

For related literature, see [type here to add references to related literature].

Experimental top

(type here to add preparation details)

Refinement top

(type here to add refinement details)

Computing details top

For both compounds, data collection: Apex2; cell refinement: Apex2; data reduction: Apex2; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: Diamond 3.

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
[Figure 7]
[Figure 8]
[Figure 9]
[Figure 10]
[Figure 11]
[Figure 12]
[Figure 13]
[Figure 14]
(caso40625) top
Crystal data top
CaH1.25O4.625SDx = 2.773 Mg m3
Mr = 147.40Mo Kα radiation, λ = 0.71073 Å
Trigonal, P3221Cell parameters from 943 reflections
Hall symbol: P 32 2"θ = 1–27.5°
a = 13.8690 (4) ŵ = 2.24 mm1
c = 12.7189 (1) ÅT = 296 K
V = 2118.70 (9) Å3Needle, colourless
Z = 240.4 × 0.08 × 0.07 mm
F(000) = 1782
Data collection top
Bruker X8 Kappa. Apex2
diffractometer
3252 independent reflections
Radiation source: fine-focus sealed tube2578 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.043
ω and phi scansθmax = 27.5°, θmin = 1.6°
Absorption correction: numerical
?
h = 1717
Tmin = 0.641, Tmax = 0.896k = 1717
38925 measured reflectionsl = 1616
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.039H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.108 w = 1/[σ2(Fo2) + (0.0478P)2 + 2.072P]
where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max = 0.027
3252 reflectionsΔρmax = 0.53 e Å3
260 parametersΔρmin = 0.45 e Å3
5 restraintsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
0 constraintsAbsolute structure parameter: 0.00
Primary atom site location: structure-invariant direct methods
Crystal data top
CaH1.25O4.625SZ = 24
Mr = 147.40Mo Kα radiation
Trigonal, P3221µ = 2.24 mm1
a = 13.8690 (4) ÅT = 296 K
c = 12.7189 (1) Å0.4 × 0.08 × 0.07 mm
V = 2118.70 (9) Å3
Data collection top
Bruker X8 Kappa. Apex2
diffractometer
3252 independent reflections
Absorption correction: numerical
?
2578 reflections with I > 2σ(I)
Tmin = 0.641, Tmax = 0.896Rint = 0.043
38925 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.039H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.108Δρmax = 0.53 e Å3
S = 1.03Δρmin = 0.45 e Å3
3252 reflectionsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
260 parametersAbsolute structure parameter: 0.00
5 restraints
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'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 > σ(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*/Ueq
S10.50186 (8)0.77388 (9)0.08244 (7)0.0099 (3)
S20.77410 (9)0.99600 (8)0.41478 (8)0.0103 (2)
S30.72701 (9)0.72106 (9)0.24660 (7)0.0096 (2)
S40.21741 (9)0.72177 (9)0.24212 (7)0.0100 (2)
Ca10.76903 (10)1.00000.16670.0126 (4)
Ca20.49029 (7)0.77610 (8)0.33088 (6)0.0142 (2)
Ca30.74268 (9)0.74268 (9)0.00000.0122 (3)
Ca40.71424 (9)0.71424 (9)0.50000.0148 (3)
Ca50.50256 (6)0.77197 (8)0.16455 (6)0.0135 (2)
Ca60.78358 (10)1.00000.66670.0123 (3)
O10.6334 (2)0.6938 (2)0.1736 (2)0.0160 (6)
O20.1951 (2)0.6233 (2)0.1778 (2)0.0166 (6)
O30.4352 (3)0.7974 (2)0.0072 (2)0.0169 (6)
O40.7339 (3)0.7999 (2)0.3272 (2)0.0169 (7)
O50.5663 (2)0.7355 (3)0.0209 (2)0.0206 (7)
O60.8680 (3)1.0603 (2)0.3412 (2)0.0164 (6)
O70.8289 (2)0.7705 (3)0.1815 (2)0.0175 (7)
O80.7927 (2)0.9169 (2)0.4753 (2)0.0180 (7)
O90.4298 (2)0.6907 (2)0.1594 (2)0.0151 (7)
O100.2966 (2)0.7407 (3)0.3266 (2)0.0167 (7)
O110.7664 (3)1.0720 (2)0.4902 (2)0.0163 (7)
O120.6738 (2)0.9397 (3)0.3496 (2)0.0178 (7)
O130.5778 (3)0.8753 (2)0.1423 (2)0.0187 (7)
O140.1128 (3)0.7027 (3)0.2901 (2)0.0200 (7)
O150.2623 (3)0.8162 (2)0.1692 (2)0.0171 (7)
O160.5018 (3)0.9431 (3)0.1888 (3)0.0336 (9)
O170.9508 (4)1.00000.66670.0560 (18)
O180.7094 (3)0.6206 (2)0.3009 (2)0.0199 (7)
O190.4803 (4)0.9522 (4)0.2989 (5)0.0663 (15)
H10.453 (7)0.985 (7)0.258 (5)0.099*
H20.545 (3)0.982 (6)0.277 (6)0.099*
H30.564 (3)0.993 (5)0.205 (6)0.099*
H40.457 (6)0.966 (7)0.181 (6)0.099*
H51.005 (4)1.060 (3)0.678 (7)0.099*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
S10.0110 (6)0.0113 (5)0.0065 (5)0.0050 (4)0.0002 (4)0.0002 (4)
S20.0128 (5)0.0122 (6)0.0063 (5)0.0066 (5)0.0001 (4)0.0002 (4)
S30.0118 (5)0.0128 (5)0.0061 (5)0.0074 (5)0.0005 (3)0.0007 (3)
S40.0119 (5)0.0120 (5)0.0067 (5)0.0066 (4)0.0004 (4)0.0006 (4)
Ca10.0162 (7)0.0130 (7)0.0076 (6)0.0065 (4)0.0002 (2)0.0004 (5)
Ca20.0138 (5)0.0189 (6)0.0082 (4)0.0071 (5)0.0005 (4)0.0012 (3)
Ca30.0154 (4)0.0154 (4)0.0074 (5)0.0088 (5)0.0001 (2)0.0001 (2)
Ca40.0187 (5)0.0187 (5)0.0115 (6)0.0129 (6)0.0008 (2)0.0008 (2)
Ca50.0134 (5)0.0148 (7)0.0102 (4)0.0054 (5)0.0003 (3)0.0013 (3)
Ca60.0139 (5)0.0130 (8)0.0097 (6)0.0065 (4)0.0001 (2)0.0003 (5)
O10.0150 (14)0.0203 (16)0.0126 (15)0.0087 (13)0.0053 (12)0.0009 (13)
O20.0187 (16)0.0169 (15)0.0154 (14)0.0097 (13)0.0007 (13)0.0063 (13)
O30.0199 (17)0.0231 (16)0.0073 (13)0.0104 (14)0.0038 (12)0.0006 (12)
O40.0250 (18)0.0208 (17)0.0063 (14)0.0125 (15)0.0013 (12)0.0032 (12)
O50.0184 (17)0.035 (2)0.0128 (15)0.0163 (16)0.0010 (13)0.0057 (13)
O60.0167 (16)0.0199 (16)0.0113 (14)0.0083 (13)0.0039 (12)0.0015 (12)
O70.0160 (15)0.0281 (18)0.0111 (14)0.0130 (14)0.0037 (11)0.0029 (13)
O80.0185 (16)0.0187 (16)0.0192 (15)0.0112 (14)0.0018 (13)0.0058 (13)
O90.0158 (16)0.0171 (16)0.0052 (13)0.0028 (13)0.0040 (12)0.0046 (11)
O100.0214 (16)0.0265 (19)0.0056 (14)0.0145 (15)0.0035 (11)0.0002 (13)
O110.0229 (18)0.0194 (17)0.0103 (14)0.0133 (15)0.0005 (12)0.0021 (12)
O120.0155 (15)0.0173 (17)0.0165 (15)0.0051 (14)0.0072 (12)0.0016 (13)
O130.0207 (17)0.0133 (16)0.0174 (16)0.0050 (15)0.0063 (12)0.0069 (13)
O140.0131 (16)0.0230 (18)0.0239 (17)0.0091 (14)0.0101 (13)0.0043 (14)
O150.0277 (18)0.0183 (16)0.0108 (15)0.0156 (15)0.0035 (12)0.0054 (12)
O160.022 (2)0.026 (2)0.051 (2)0.0103 (18)0.0043 (18)0.0107 (17)
O170.023 (2)0.022 (3)0.123 (6)0.0108 (16)0.005 (2)0.011 (4)
O180.0257 (18)0.0156 (16)0.0200 (16)0.0116 (14)0.0021 (14)0.0047 (12)
O190.039 (3)0.047 (3)0.093 (4)0.006 (2)0.017 (3)0.015 (3)
Geometric parameters (Å, º) top
S1—O91.461 (3)Ca3—O12.570 (3)
S1—O51.473 (3)Ca3—O1v2.570 (3)
S1—O31.476 (3)Ca3—S3v3.1479 (9)
S1—O131.478 (3)Ca3—Ca1vii4.0074 (7)
S1—Ca53.1416 (11)Ca4—O15viii2.403 (3)
S1—Ca23.1649 (12)Ca4—O15ix2.403 (3)
S2—O81.465 (3)Ca4—O42.448 (3)
S2—O121.465 (3)Ca4—O4x2.448 (3)
S2—O111.467 (3)Ca4—O8xi2.475 (3)
S2—O61.484 (3)Ca4—O8v2.475 (3)
S2—Ca13.1576 (10)Ca4—O18x2.831 (3)
S2—Ca63.2058 (10)Ca4—O182.831 (3)
S3—O181.461 (3)Ca4—S3x3.2267 (9)
S3—O41.467 (3)Ca4—Ca6xi4.1610 (8)
S3—O71.478 (3)Ca4—Ca6xii4.1611 (8)
S3—O11.483 (3)Ca5—O162.398 (4)
S3—Ca33.1479 (9)Ca5—O10viii2.403 (3)
S3—Ca43.2267 (9)Ca5—O2i2.433 (3)
S4—O101.463 (3)Ca5—O11iii2.453 (3)
S4—O151.466 (3)Ca5—O32.469 (3)
S4—O141.471 (3)Ca5—O9i2.486 (3)
S4—O21.487 (3)Ca5—O12.539 (3)
S4—Ca2i3.1154 (12)Ca5—O52.654 (3)
S4—Ca5ii3.3097 (12)Ca5—O14viii3.059 (3)
Ca1—O13iii2.353 (3)Ca5—S4viii3.3097 (12)
Ca1—O132.353 (3)Ca5—Ca2viii4.0094 (12)
Ca1—O7iv2.390 (3)Ca6—O172.319 (6)
Ca1—O7v2.390 (3)Ca6—O14vi2.400 (3)
Ca1—O62.523 (3)Ca6—O14xiii2.400 (3)
Ca1—O6iii2.523 (3)Ca6—O4iii2.504 (3)
Ca1—O122.598 (3)Ca6—O4xiv2.504 (3)
Ca1—O12iii2.598 (3)Ca6—O11xv2.516 (3)
Ca1—S2iii3.1576 (10)Ca6—O112.516 (3)
Ca1—Ca3iv4.0074 (7)Ca6—O8xv2.723 (3)
Ca1—Ca34.0074 (7)Ca6—O82.723 (3)
Ca2—O92.423 (3)Ca6—S2xv3.2058 (10)
Ca2—O122.431 (3)Ca6—Ca4xvi4.1611 (8)
Ca2—O18v2.438 (3)O2—Ca5vi2.433 (3)
Ca2—O102.479 (3)O2—Ca2i2.549 (3)
Ca2—O15vi2.510 (3)O3—Ca2i2.560 (3)
Ca2—O192.548 (6)O4—Ca6xi2.504 (3)
Ca2—O2vi2.549 (3)O6—Ca3iv2.414 (3)
Ca2—O3vi2.560 (3)O7—Ca1vii2.390 (3)
Ca2—O132.730 (3)O8—Ca4xiv2.475 (3)
Ca2—S4vi3.1154 (12)O9—Ca5vi2.486 (3)
Ca2—Ca5ii4.0094 (12)O10—Ca5ii2.403 (3)
Ca3—O52.413 (3)O11—Ca5iii2.453 (3)
Ca3—O5v2.413 (3)O14—Ca6i2.400 (3)
Ca3—O6iii2.414 (3)O14—Ca5ii3.059 (3)
Ca3—O6vii2.414 (3)O15—Ca4ii2.403 (3)
Ca3—O7v2.539 (3)O15—Ca2i2.510 (3)
Ca3—O72.539 (3)O18—Ca2v2.438 (3)
O9—S1—O5111.69 (19)O7—Ca3—Ca1121.30 (7)
O9—S1—O3110.64 (18)O1—Ca3—Ca1117.93 (7)
O5—S1—O3107.13 (17)O1v—Ca3—Ca187.16 (6)
O9—S1—O13106.69 (18)S3—Ca3—Ca1125.67 (3)
O5—S1—O13110.20 (18)S3v—Ca3—Ca159.839 (19)
O3—S1—O13110.53 (19)Ca1vii—Ca3—Ca1121.20 (5)
O9—S1—Ca5131.83 (12)O15viii—Ca4—O15ix133.50 (16)
O5—S1—Ca557.34 (12)O15viii—Ca4—O478.96 (10)
O3—S1—Ca550.06 (12)O15ix—Ca4—O4115.28 (9)
O13—S1—Ca5121.27 (13)O15viii—Ca4—O4x115.28 (9)
O9—S1—Ca247.23 (11)O15ix—Ca4—O4x78.96 (10)
O5—S1—Ca2125.26 (13)O4—Ca4—O4x145.27 (15)
O3—S1—Ca2127.24 (13)O15viii—Ca4—O8xi76.05 (10)
O13—S1—Ca259.48 (13)O15ix—Ca4—O8xi149.65 (11)
Ca5—S1—Ca2177.23 (4)O4—Ca4—O8xi71.57 (10)
O8—S2—O12111.95 (18)O4x—Ca4—O8xi81.13 (10)
O8—S2—O11107.33 (17)O15viii—Ca4—O8v149.65 (11)
O12—S2—O11111.24 (19)O15ix—Ca4—O8v76.05 (10)
O8—S2—O6110.52 (18)O4—Ca4—O8v81.13 (10)
O12—S2—O6106.10 (17)O4x—Ca4—O8v71.57 (10)
O11—S2—O6109.72 (17)O8xi—Ca4—O8v76.04 (14)
O8—S2—Ca1123.50 (13)O15viii—Ca4—O18x64.58 (9)
O12—S2—Ca154.55 (12)O15ix—Ca4—O18x103.82 (9)
O11—S2—Ca1129.07 (12)O4—Ca4—O18x138.87 (9)
O6—S2—Ca151.71 (12)O4x—Ca4—O18x52.46 (9)
O8—S2—Ca657.79 (12)O8xi—Ca4—O18x81.33 (9)
O12—S2—Ca6126.50 (13)O8v—Ca4—O18x122.04 (9)
O11—S2—Ca649.58 (12)O15viii—Ca4—O18103.82 (9)
O6—S2—Ca6127.10 (13)O15ix—Ca4—O1864.58 (9)
Ca1—S2—Ca6178.27 (3)O4—Ca4—O1852.46 (9)
O18—S3—O4107.32 (18)O4x—Ca4—O18138.87 (9)
O18—S3—O7111.83 (18)O8xi—Ca4—O18122.04 (9)
O4—S3—O7110.80 (19)O8v—Ca4—O1881.33 (9)
O18—S3—O1110.19 (19)O18x—Ca4—O18152.10 (13)
O4—S3—O1110.49 (18)O15viii—Ca4—S391.36 (7)
O7—S3—O1106.25 (16)O15ix—Ca4—S390.54 (7)
O18—S3—Ca3122.15 (13)O4—Ca4—S325.55 (7)
O4—S3—Ca3130.52 (12)O4x—Ca4—S3151.30 (7)
O7—S3—Ca352.62 (11)O8xi—Ca4—S396.15 (7)
O1—S3—Ca353.89 (12)O8v—Ca4—S380.01 (7)
O18—S3—Ca461.29 (13)O18x—Ca4—S3155.78 (6)
O4—S3—Ca446.04 (12)O18—Ca4—S326.92 (6)
O7—S3—Ca4126.81 (12)O15viii—Ca4—S3x90.54 (7)
O1—S3—Ca4126.11 (12)O15ix—Ca4—S3x91.36 (7)
Ca3—S3—Ca4176.55 (4)O4—Ca4—S3x151.30 (7)
O10—S4—O15111.06 (19)O4x—Ca4—S3x25.55 (7)
O10—S4—O14108.16 (18)O8xi—Ca4—S3x80.01 (7)
O15—S4—O14111.27 (18)O8v—Ca4—S3x96.15 (7)
O10—S4—O2111.22 (18)O18x—Ca4—S3x26.92 (6)
O15—S4—O2105.85 (17)O18—Ca4—S3x155.78 (6)
O14—S4—O2109.29 (19)S3—Ca4—S3x175.18 (6)
O10—S4—Ca2i135.05 (13)O15viii—Ca4—Ca6xi69.69 (7)
O15—S4—Ca2i52.53 (12)O15ix—Ca4—Ca6xi144.51 (7)
O14—S4—Ca2i116.80 (14)O4—Ca4—Ca6xi33.26 (7)
O2—S4—Ca2i54.22 (12)O4x—Ca4—Ca6xi118.88 (8)
O10—S4—Ca5ii40.89 (12)O8xi—Ca4—Ca6xi38.93 (7)
O15—S4—Ca5ii127.46 (12)O8v—Ca4—Ca6xi81.12 (8)
O14—S4—Ca5ii67.28 (13)O18x—Ca4—Ca6xi111.29 (6)
O2—S4—Ca5ii124.69 (12)O18—Ca4—Ca6xi85.54 (6)
Ca2i—S4—Ca5ii175.88 (4)S3—Ca4—Ca6xi58.67 (2)
O13iii—Ca1—O1381.10 (16)S3x—Ca4—Ca6xi118.04 (3)
O13iii—Ca1—O7iv81.17 (11)O15viii—Ca4—Ca6xii144.52 (7)
O13—Ca1—O7iv156.98 (11)O15ix—Ca4—Ca6xii69.69 (7)
O13iii—Ca1—O7v156.98 (12)O4—Ca4—Ca6xii118.88 (8)
O13—Ca1—O7v81.17 (11)O4x—Ca4—Ca6xii33.26 (7)
O7iv—Ca1—O7v119.39 (17)O8xi—Ca4—Ca6xii81.12 (8)
O13iii—Ca1—O689.35 (10)O8v—Ca4—Ca6xii38.93 (7)
O13—Ca1—O6125.89 (10)O18x—Ca4—Ca6xii85.54 (6)
O7iv—Ca1—O668.39 (9)O18—Ca4—Ca6xii111.29 (6)
O7v—Ca1—O689.23 (10)S3—Ca4—Ca6xii118.04 (3)
O13iii—Ca1—O6iii125.89 (10)S3x—Ca4—Ca6xii58.67 (2)
O13—Ca1—O6iii89.35 (10)Ca6xi—Ca4—Ca6xii107.43 (5)
O7iv—Ca1—O6iii89.23 (10)O16—Ca5—O10viii96.00 (13)
O7v—Ca1—O6iii68.39 (9)O16—Ca5—O2i141.21 (11)
O6—Ca1—O6iii135.55 (14)O10viii—Ca5—O2i71.62 (10)
O13iii—Ca1—O1278.20 (10)O16—Ca5—O11iii70.83 (11)
O13—Ca1—O1271.14 (10)O10viii—Ca5—O11iii112.87 (10)
O7iv—Ca1—O12119.04 (9)O2i—Ca5—O11iii147.97 (11)
O7v—Ca1—O1282.24 (10)O16—Ca5—O377.50 (12)
O6—Ca1—O1254.78 (9)O10viii—Ca5—O3143.29 (10)
O6iii—Ca1—O12147.07 (9)O2i—Ca5—O390.83 (10)
O13iii—Ca1—O12iii71.14 (10)O11iii—Ca5—O399.18 (10)
O13—Ca1—O12iii78.20 (10)O16—Ca5—O9i68.74 (11)
O7iv—Ca1—O12iii82.24 (10)O10viii—Ca5—O9i76.34 (10)
O7v—Ca1—O12iii119.04 (9)O2i—Ca5—O9i72.59 (11)
O6—Ca1—O12iii147.07 (9)O11iii—Ca5—O9i139.28 (12)
O6iii—Ca1—O12iii54.78 (9)O3—Ca5—O9i67.58 (9)
O12—Ca1—O12iii139.36 (14)O16—Ca5—O1140.73 (11)
O13iii—Ca1—S284.34 (8)O10viii—Ca5—O187.73 (11)
O13—Ca1—S298.38 (8)O2i—Ca5—O176.89 (10)
O7iv—Ca1—S294.36 (7)O11iii—Ca5—O171.76 (10)
O7v—Ca1—S283.83 (7)O3—Ca5—O1120.20 (9)
O6—Ca1—S227.50 (7)O9i—Ca5—O1148.70 (11)
O6iii—Ca1—S2149.71 (8)O16—Ca5—O5117.98 (13)
O12—Ca1—S227.34 (6)O10viii—Ca5—O5145.97 (12)
O12iii—Ca1—S2155.48 (7)O2i—Ca5—O581.86 (10)
O13iii—Ca1—S2iii98.38 (8)O11iii—Ca5—O579.32 (10)
O13—Ca1—S2iii84.34 (8)O3—Ca5—O555.02 (9)
O7iv—Ca1—S2iii83.83 (7)O9i—Ca5—O5116.02 (9)
O7v—Ca1—S2iii94.36 (7)O1—Ca5—O565.30 (9)
O6—Ca1—S2iii149.71 (8)O16—Ca5—O14viii64.30 (12)
O6iii—Ca1—S2iii27.50 (7)O10viii—Ca5—O14viii49.82 (9)
O12—Ca1—S2iii155.48 (7)O2i—Ca5—O14viii120.55 (9)
O12iii—Ca1—S2iii27.34 (6)O11iii—Ca5—O14viii66.59 (9)
S2—Ca1—S2iii176.44 (6)O3—Ca5—O14viii141.69 (10)
O13iii—Ca1—Ca3iv73.04 (8)O9i—Ca5—O14viii99.36 (9)
O13—Ca1—Ca3iv146.08 (8)O1—Ca5—O14viii90.11 (9)
O7iv—Ca1—Ca3iv36.86 (6)O5—Ca5—O14viii143.14 (9)
O7v—Ca1—Ca3iv116.28 (9)O16—Ca5—S196.82 (11)
O6—Ca1—Ca3iv34.84 (7)O10viii—Ca5—S1158.52 (8)
O6iii—Ca1—Ca3iv123.57 (7)O2i—Ca5—S187.66 (7)
O12—Ca1—Ca3iv82.21 (6)O11iii—Ca5—S187.65 (7)
O12iii—Ca1—Ca3iv112.43 (7)O3—Ca5—S127.28 (7)
S2—Ca1—Ca3iv58.134 (19)O9i—Ca5—S192.40 (7)
S2iii—Ca1—Ca3iv120.39 (2)O1—Ca5—S193.15 (7)
O13iii—Ca1—Ca3146.08 (8)O5—Ca5—S127.84 (6)
O13—Ca1—Ca373.04 (8)O14viii—Ca5—S1151.54 (7)
O7iv—Ca1—Ca3116.28 (9)O16—Ca5—S4viii80.28 (11)
O7v—Ca1—Ca336.86 (6)O10viii—Ca5—S4viii23.48 (7)
O6—Ca1—Ca3123.57 (7)O2i—Ca5—S4viii94.75 (7)
O6iii—Ca1—Ca334.84 (7)O11iii—Ca5—S4viii91.15 (7)
O12—Ca1—Ca3112.43 (7)O3—Ca5—S4viii150.76 (8)
O12iii—Ca1—Ca382.21 (6)O9i—Ca5—S4viii86.77 (7)
S2—Ca1—Ca3120.39 (2)O1—Ca5—S4viii88.99 (7)
S2iii—Ca1—Ca358.134 (19)O5—Ca5—S4viii154.22 (7)
Ca3iv—Ca1—Ca3138.53 (5)O14viii—Ca5—S4viii26.34 (5)
O9—Ca2—O12119.30 (10)S1—Ca5—S4viii177.09 (4)
O9—Ca2—O18v79.31 (11)O16—Ca5—Ca2viii117.10 (10)
O12—Ca2—O18v74.95 (11)O10viii—Ca5—Ca2viii35.41 (7)
O9—Ca2—O1078.91 (11)O2i—Ca5—Ca2viii37.42 (7)
O12—Ca2—O10135.44 (12)O11iii—Ca5—Ca2viii144.37 (7)
O18v—Ca2—O10149.05 (11)O3—Ca5—Ca2viii116.39 (7)
O9—Ca2—O15vi138.73 (12)O9i—Ca5—Ca2viii63.73 (8)
O12—Ca2—O15vi78.32 (10)O1—Ca5—Ca2viii87.69 (7)
O18v—Ca2—O15vi69.47 (10)O5—Ca5—Ca2viii118.68 (7)
O10—Ca2—O15vi116.02 (9)O14viii—Ca5—Ca2viii85.22 (6)
O9—Ca2—O1998.84 (16)S1—Ca5—Ca2viii123.14 (3)
O12—Ca2—O1969.78 (14)S4viii—Ca5—Ca2viii58.88 (2)
O18v—Ca2—O19138.16 (13)O17—Ca6—O14vi142.47 (8)
O10—Ca2—O1967.24 (13)O17—Ca6—O14xiii142.47 (8)
O15vi—Ca2—O19122.41 (15)O14vi—Ca6—O14xiii75.06 (15)
O9—Ca2—O2vi145.53 (10)O17—Ca6—O4iii73.79 (8)
O12—Ca2—O2vi92.53 (10)O14vi—Ca6—O4iii139.11 (11)
O18v—Ca2—O2vi124.96 (10)O14xiii—Ca6—O4iii71.75 (11)
O10—Ca2—O2vi68.46 (9)O17—Ca6—O4xiv73.79 (8)
O15vi—Ca2—O2vi55.50 (9)O14vi—Ca6—O4xiv71.75 (11)
O19—Ca2—O2vi78.99 (14)O14xiii—Ca6—O4xiv139.11 (12)
O9—Ca2—O3vi67.08 (9)O4iii—Ca6—O4xiv147.58 (16)
O12—Ca2—O3vi150.16 (11)O17—Ca6—O11xv107.03 (7)
O18v—Ca2—O3vi78.18 (10)O14vi—Ca6—O11xv77.19 (10)
O10—Ca2—O3vi73.21 (11)O14xiii—Ca6—O11xv75.95 (11)
O15vi—Ca2—O3vi80.34 (10)O4iii—Ca6—O11xv116.05 (9)
O19—Ca2—O3vi139.98 (13)O4xiv—Ca6—O11xv74.00 (10)
O2vi—Ca2—O3vi92.33 (10)O17—Ca6—O11107.03 (7)
O9—Ca2—O1354.08 (9)O14vi—Ca6—O1175.95 (11)
O12—Ca2—O1367.76 (9)O14xiii—Ca6—O1177.19 (10)
O18v—Ca2—O1380.02 (11)O4iii—Ca6—O1174.00 (10)
O10—Ca2—O13104.18 (10)O4xiv—Ca6—O11116.05 (9)
O15vi—Ca2—O13139.16 (9)O11xv—Ca6—O11145.94 (15)
O19—Ca2—O1366.41 (14)O17—Ca6—O8xv75.04 (7)
O2vi—Ca2—O13144.21 (11)O14vi—Ca6—O8xv128.05 (10)
O3vi—Ca2—O13119.88 (9)O14xiii—Ca6—O8xv78.06 (10)
O9—Ca2—S4vi156.10 (8)O4iii—Ca6—O8xv66.67 (9)
O12—Ca2—S4vi81.61 (8)O4xiv—Ca6—O8xv104.59 (9)
O18v—Ca2—S4vi96.87 (8)O11xv—Ca6—O8xv53.41 (9)
O10—Ca2—S4vi94.23 (7)O11—Ca6—O8xv138.36 (9)
O15vi—Ca2—S4vi27.62 (7)O17—Ca6—O875.04 (7)
O19—Ca2—S4vi99.48 (13)O14vi—Ca6—O878.06 (10)
O2vi—Ca2—S4vi28.24 (7)O14xiii—Ca6—O8128.05 (10)
O3vi—Ca2—S4vi89.02 (7)O4iii—Ca6—O8104.59 (9)
O13—Ca2—S4vi149.03 (7)O4xiv—Ca6—O866.67 (9)
O9—Ca2—S126.28 (7)O11xv—Ca6—O8138.36 (9)
O12—Ca2—S194.14 (7)O11—Ca6—O853.41 (9)
O18v—Ca2—S177.83 (8)O8xv—Ca6—O8150.08 (13)
O10—Ca2—S191.80 (7)O17—Ca6—S2xv91.85 (3)
O15vi—Ca2—S1147.29 (7)O14vi—Ca6—S2xv102.22 (8)
O19—Ca2—S182.94 (13)O14xiii—Ca6—S2xv74.75 (8)
O2vi—Ca2—S1157.21 (7)O4iii—Ca6—S2xv91.48 (7)
O3vi—Ca2—S192.64 (7)O4xiv—Ca6—S2xv89.56 (7)
O13—Ca2—S127.80 (6)O11xv—Ca6—S2xv26.35 (7)
S4vi—Ca2—S1173.97 (4)O11—Ca6—S2xv151.30 (7)
O9—Ca2—Ca5ii110.31 (8)O8xv—Ca6—S2xv27.07 (6)
O12—Ca2—Ca5ii122.55 (8)O8—Ca6—S2xv155.11 (7)
O18v—Ca2—Ca5ii144.27 (8)O17—Ca6—S291.85 (3)
O10—Ca2—Ca5ii34.17 (6)O14vi—Ca6—S274.75 (8)
O15vi—Ca2—Ca5ii83.22 (6)O14xiii—Ca6—S2102.22 (8)
O19—Ca2—Ca5ii75.99 (11)O4iii—Ca6—S289.56 (7)
O2vi—Ca2—Ca5ii35.43 (7)O4xiv—Ca6—S291.48 (7)
O3vi—Ca2—Ca5ii74.81 (7)O11xv—Ca6—S2151.30 (7)
O13—Ca2—Ca5ii134.14 (8)O11—Ca6—S226.35 (7)
S4vi—Ca2—Ca5ii60.06 (2)O8xv—Ca6—S2155.11 (7)
S1—Ca2—Ca5ii125.96 (3)O8—Ca6—S227.07 (6)
O5—Ca3—O5v116.35 (16)S2xv—Ca6—S2176.29 (6)
O5—Ca3—O6iii81.27 (10)O17—Ca6—Ca4xvi75.81 (2)
O5v—Ca3—O6iii161.06 (11)O14vi—Ca6—Ca4xvi140.96 (8)
O5—Ca3—O6vii161.06 (11)O14xiii—Ca6—Ca4xvi67.18 (8)
O5v—Ca3—O6vii81.27 (10)O4iii—Ca6—Ca4xvi32.41 (6)
O6iii—Ca3—O6vii82.33 (14)O4xiv—Ca6—Ca4xvi135.02 (8)
O5—Ca3—O7v80.28 (10)O11xv—Ca6—Ca4xvi84.29 (7)
O5v—Ca3—O7v119.82 (9)O11—Ca6—Ca4xvi104.07 (7)
O6iii—Ca3—O7v67.78 (9)O8xv—Ca6—Ca4xvi34.81 (6)
O6vii—Ca3—O7v84.80 (10)O8—Ca6—Ca4xvi133.98 (7)
O5—Ca3—O7119.82 (9)S2xv—Ca6—Ca4xvi59.099 (19)
O5v—Ca3—O780.28 (10)S2—Ca6—Ca4xvi121.97 (2)
O6iii—Ca3—O784.80 (10)S3—O1—Ca5129.88 (17)
O6vii—Ca3—O767.78 (9)S3—O1—Ca398.32 (14)
O7v—Ca3—O7143.71 (14)Ca5—O1—Ca3107.55 (10)
O5—Ca3—O168.38 (9)S4—O2—Ca5vi135.82 (18)
O5v—Ca3—O185.32 (10)S4—O2—Ca2i97.54 (15)
O6iii—Ca3—O195.73 (9)Ca5vi—O2—Ca2i107.15 (10)
O6vii—Ca3—O1122.86 (9)S1—O3—Ca5102.66 (15)
O7v—Ca3—O1146.71 (9)S1—O3—Ca2i129.33 (17)
O7—Ca3—O155.24 (9)Ca5—O3—Ca2i108.84 (11)
O5—Ca3—O1v85.32 (10)S3—O4—Ca4108.42 (16)
O5v—Ca3—O1v68.38 (9)S3—O4—Ca6xi136.66 (17)
O6iii—Ca3—O1v122.86 (9)Ca4—O4—Ca6xi114.33 (11)
O6vii—Ca3—O1v95.73 (9)S1—O5—Ca3146.02 (19)
O7v—Ca3—O1v55.24 (9)S1—O5—Ca594.82 (14)
O7—Ca3—O1v146.71 (9)Ca3—O5—Ca5108.76 (11)
O1—Ca3—O1v129.48 (13)S2—O6—Ca3iv130.32 (16)
O5—Ca3—S394.90 (7)S2—O6—Ca1100.79 (15)
O5v—Ca3—S380.09 (7)Ca3iv—O6—Ca1108.51 (10)
O6iii—Ca3—S392.02 (7)S3—O7—Ca1vii139.76 (18)
O6vii—Ca3—S395.08 (7)S3—O7—Ca399.82 (14)
O7v—Ca3—S3159.67 (7)Ca1vii—O7—Ca3108.75 (10)
O7—Ca3—S327.56 (6)S2—O8—Ca4xiv140.84 (18)
O1—Ca3—S327.79 (6)S2—O8—Ca695.14 (15)
O1v—Ca3—S3144.55 (7)Ca4xiv—O8—Ca6106.26 (10)
O5—Ca3—S3v80.09 (7)S1—O9—Ca2106.49 (15)
O5v—Ca3—S3v94.90 (7)S1—O9—Ca5vi140.65 (17)
O6iii—Ca3—S3v95.08 (7)Ca2—O9—Ca5vi112.85 (11)
O6vii—Ca3—S3v92.02 (7)S4—O10—Ca5ii115.63 (17)
O7v—Ca3—S3v27.56 (6)S4—O10—Ca2133.90 (17)
O7—Ca3—S3v159.67 (7)Ca5ii—O10—Ca2110.43 (11)
O1—Ca3—S3v144.54 (7)S2—O11—Ca5iii141.19 (17)
O1v—Ca3—S3v27.79 (6)S2—O11—Ca6104.07 (15)
S3—Ca3—S3v170.57 (6)Ca5iii—O11—Ca6114.53 (11)
O5—Ca3—Ca1vii154.20 (7)S2—O12—Ca2145.59 (19)
O5v—Ca3—Ca1vii67.51 (7)S2—O12—Ca198.11 (15)
O6iii—Ca3—Ca1vii93.62 (8)Ca2—O12—Ca1109.84 (11)
O6vii—Ca3—Ca1vii36.66 (7)S1—O13—Ca1140.5 (2)
O7v—Ca3—Ca1vii121.30 (8)S1—O13—Ca292.71 (15)
O7—Ca3—Ca1vii34.39 (6)Ca1—O13—Ca2107.94 (11)
O1—Ca3—Ca1vii87.16 (6)S4—O14—Ca6i145.68 (19)
O1v—Ca3—Ca1vii117.93 (7)S4—O14—Ca5ii86.38 (14)
S3—Ca3—Ca1vii59.84 (2)Ca6i—O14—Ca5ii99.24 (10)
S3v—Ca3—Ca1vii125.67 (3)S4—O15—Ca4ii136.74 (17)
O5—Ca3—Ca167.51 (7)S4—O15—Ca2i99.85 (14)
O5v—Ca3—Ca1154.20 (7)Ca4ii—O15—Ca2i117.70 (11)
O6iii—Ca3—Ca136.66 (7)S3—O18—Ca2v146.74 (19)
O6vii—Ca3—Ca193.62 (8)S3—O18—Ca491.80 (14)
O7v—Ca3—Ca134.39 (6)Ca2v—O18—Ca4105.62 (11)
Symmetry codes: (i) y+1, xy+1, z1/3; (ii) y+1, xy+1, z+2/3; (iii) xy+1, y+2, z+1/3; (iv) x+y+1, x+2, z+1/3; (v) y, x, z; (vi) x+y, x+1, z+1/3; (vii) y+2, xy+1, z1/3; (viii) x+y, x+1, z2/3; (ix) x+1, x+y, z1/3; (x) y, x, z1; (xi) x, y, z1; (xii) y+2, xy+1, z4/3; (xiii) y, x+1, z+1; (xiv) x, y, z+1; (xv) xy+1, y+2, z+4/3; (xvi) x+y+1, x+2, z+4/3.
(caso4_05) top
Crystal data top
CaO4.5SHF(000) = 924
Mr = 145.16Dx = 2.887 Mg m3
Monoclinic, C2Mo Kα radiation, λ = 0.71073 Å
Hall symbol: C 2yCell parameters from 100 reflections
a = 17.5180 (8) Åθ = 1–27.5°
b = 6.9291 (1) ŵ = 2.25 mm1
c = 12.0344 (2) ÅT = 293 K
β = 133.655 (4)°Needle, colourless
V = 1056.88 (4) Å30.4 × 0.08 × 0.07 mm
Z = 12
Data collection top
Bruker X8 Kappa. Apex2
diffractometer
12774 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.000
Graphite monochromatorθmax = 27.5°, θmin = 2.3°
ω and phi scansh = 2222
15532 measured reflectionsk = 99
15543 independent reflectionsl = 1515
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: full w = 1/[σ2(Fo2) + (0.0301P)2]
where P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.042(Δ/σ)max = 0.006
wR(F2) = 0.096Δρmax = 0.58 e Å3
S = 0.97Δρmin = 0.49 e Å3
15543 reflectionsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
193 parametersExtinction coefficient: 0.00034 (10)
1 restraintAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.06 (3)
Crystal data top
CaO4.5SHV = 1056.88 (4) Å3
Mr = 145.16Z = 12
Monoclinic, C2Mo Kα radiation
a = 17.5180 (8) ŵ = 2.25 mm1
b = 6.9291 (1) ÅT = 293 K
c = 12.0344 (2) Å0.4 × 0.08 × 0.07 mm
β = 133.655 (4)°
Data collection top
Bruker X8 Kappa. Apex2
diffractometer
12774 reflections with I > 2σ(I)
15532 measured reflectionsRint = 0.000
15543 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0421 restraint
wR(F2) = 0.096Δρmax = 0.58 e Å3
S = 0.97Δρmin = 0.49 e Å3
15543 reflectionsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
193 parametersAbsolute structure parameter: 0.06 (3)
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'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 > σ(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*/Ueq
Ca10.33496 (10)0.29588 (13)0.57126 (16)0.0128 (2)
Ca20.16388 (10)0.34101 (14)0.05509 (15)0.01086 (19)
Ca30.00000.5050 (3)0.50000.0118 (3)
Ca40.00000.0014 (3)0.00000.0118 (3)
S10.08626 (12)0.3120 (2)0.31005 (19)0.0102 (3)
S20.24834 (5)0.0029 (3)0.24705 (7)0.0084 (3)
S30.57935 (13)0.3338 (2)0.80377 (19)0.0096 (2)
O10.0134 (3)0.3877 (4)0.3186 (4)0.0125 (7)
O20.0272 (2)0.2603 (5)0.1521 (4)0.0164 (8)
O30.1466 (2)0.1475 (4)0.4151 (4)0.0177 (7)
O40.1659 (2)0.4619 (4)0.3609 (3)0.0141 (6)
O50.1720 (3)0.1210 (5)0.1076 (4)0.0141 (8)
O60.1830 (2)0.3859 (6)0.7602 (4)0.0146 (8)
O70.3192 (3)0.1274 (5)0.3843 (4)0.0146 (8)
O80.6651 (2)0.1904 (4)0.9036 (4)0.0140 (7)
O90.6290 (2)0.5187 (4)0.8348 (3)0.0197 (7)
O100.5120 (3)0.3333 (4)0.8354 (4)0.0165 (8)
O110.5122 (2)0.2868 (5)0.6418 (4)0.0153 (8)
O120.3171 (2)0.3751 (6)0.7433 (4)0.0144 (7)
O130.00000.1599 (6)0.50000.0355 (12)
O140.1689 (4)0.5093 (5)0.1181 (5)0.0667 (12)
H10.185 (5)0.603 (7)0.151 (7)0.100*
H20.198 (5)0.472 (8)0.199 (6)0.100*
H30.017 (5)0.100 (6)0.550 (5)0.100*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0062 (3)0.0164 (7)0.0127 (5)0.0001 (4)0.0053 (4)0.0024 (4)
Ca20.0080 (3)0.0111 (6)0.0109 (4)0.0007 (4)0.0056 (3)0.0005 (3)
Ca30.0070 (6)0.0190 (8)0.0077 (7)0.0000.0044 (6)0.000
Ca40.0060 (5)0.0197 (8)0.0076 (7)0.0000.0039 (6)0.000
S10.0064 (4)0.0134 (7)0.0092 (6)0.0003 (4)0.0048 (4)0.0005 (4)
S20.0032 (6)0.0177 (8)0.0050 (8)0.0009 (2)0.0031 (6)0.0011 (2)
S30.0063 (4)0.0130 (7)0.0084 (6)0.0013 (5)0.0045 (4)0.0028 (5)
O10.0132 (13)0.0142 (16)0.0117 (13)0.0004 (10)0.0092 (11)0.0024 (10)
O20.0094 (15)0.0205 (17)0.0148 (16)0.0002 (11)0.0066 (14)0.0023 (12)
O30.0103 (14)0.0188 (15)0.0150 (14)0.0090 (11)0.0053 (12)0.0083 (11)
O40.0116 (15)0.0064 (13)0.0208 (14)0.0030 (10)0.0099 (14)0.0024 (10)
O50.0088 (14)0.0163 (15)0.0125 (16)0.0044 (11)0.0055 (13)0.0063 (12)
O60.0078 (15)0.0190 (18)0.0183 (16)0.0057 (12)0.0095 (14)0.0018 (12)
O70.0130 (15)0.0145 (16)0.0137 (16)0.0025 (12)0.0083 (13)0.0062 (12)
O80.0011 (12)0.0146 (14)0.0145 (14)0.0028 (10)0.0010 (11)0.0029 (10)
O90.0172 (16)0.0176 (14)0.0212 (16)0.0073 (11)0.0120 (14)0.0043 (12)
O100.0122 (15)0.019 (2)0.0133 (13)0.0029 (10)0.0069 (12)0.0037 (10)
O110.0146 (16)0.0134 (16)0.0132 (15)0.0033 (12)0.0078 (14)0.0030 (12)
O120.0048 (14)0.0167 (16)0.0171 (15)0.0036 (12)0.0058 (13)0.0011 (13)
O130.058 (3)0.019 (3)0.033 (3)0.0000.033 (3)0.000
O140.161 (4)0.0177 (18)0.084 (3)0.017 (2)0.109 (3)0.0137 (16)
Geometric parameters (Å, º) top
Ca1—O122.362 (4)Ca4—O10ii2.429 (4)
Ca1—O72.375 (4)Ca4—O10ix2.429 (4)
Ca1—O3i2.449 (3)Ca4—O5v2.462 (3)
Ca1—O4ii2.458 (3)Ca4—O52.462 (3)
Ca1—O42.480 (3)Ca4—O12ix2.629 (3)
Ca1—O102.486 (4)Ca4—O12ii2.629 (3)
Ca1—O112.594 (3)Ca4—S2v3.1477 (7)
Ca1—O32.630 (3)Ca4—S23.1477 (7)
Ca1—S33.1125 (14)Ca4—Ca1ix4.0514 (19)
Ca1—S13.1571 (14)Ca4—Ca1ii4.0514 (19)
Ca1—Ca4iii4.0514 (19)S1—O11.447 (4)
Ca1—Ca3iv4.072 (2)S1—O21.448 (4)
Ca2—O142.336 (3)S1—O31.473 (3)
Ca2—O5v2.406 (4)S1—O41.491 (3)
Ca2—O8vi2.417 (3)S2—O51.475 (4)
Ca2—O9ii2.450 (3)S2—O71.477 (4)
Ca2—O8i2.475 (3)S2—O6ii1.502 (4)
Ca2—O6vii2.486 (4)S2—O12ii1.515 (4)
Ca2—O12.492 (4)S2—Ca3iv3.1897 (7)
Ca2—O22.736 (3)S3—O91.446 (4)
Ca2—O9vi2.903 (3)S3—O111.457 (4)
Ca2—S13.1770 (14)S3—O101.468 (4)
Ca2—S3vi3.2558 (15)S3—O81.482 (3)
Ca2—Ca44.104 (2)S3—Ca2x3.2558 (15)
Ca3—O132.392 (5)O3—Ca1ii2.449 (3)
Ca3—O1vii2.488 (3)O4—Ca1i2.458 (3)
Ca3—O12.488 (3)O5—Ca2v2.406 (4)
Ca3—O11viii2.503 (4)O6—S2i1.502 (4)
Ca3—O11i2.503 (4)O6—Ca2vii2.486 (4)
Ca3—O7viii2.570 (3)O7—Ca3iv2.570 (3)
Ca3—O7i2.570 (3)O8—Ca2x2.417 (3)
Ca3—O6vii2.628 (3)O8—Ca2ii2.475 (3)
Ca3—O62.628 (3)O9—Ca2i2.450 (3)
Ca3—S2viii3.1897 (7)O9—Ca2x2.903 (3)
Ca3—S2i3.1897 (7)O10—Ca4iii2.429 (4)
Ca3—Ca1i4.072 (2)O11—Ca3iv2.503 (4)
Ca4—O22.365 (4)O12—S2i1.515 (4)
Ca4—O2v2.365 (4)O12—Ca4iii2.629 (3)
O12—Ca1—O7160.93 (16)O7viii—Ca3—S2viii27.08 (9)
O12—Ca1—O3i78.52 (14)O7i—Ca3—S2viii153.30 (9)
O7—Ca1—O3i118.45 (11)O6vii—Ca3—S2viii27.84 (8)
O12—Ca1—O4ii83.83 (12)O6—Ca3—S2viii151.81 (8)
O7—Ca1—O4ii80.13 (12)O13—Ca3—S2i89.74 (4)
O3i—Ca1—O4ii161.00 (14)O1vii—Ca3—S2i93.82 (8)
O12—Ca1—O490.00 (11)O1—Ca3—S2i86.00 (8)
O7—Ca1—O489.11 (11)O11viii—Ca3—S2i86.66 (7)
O3i—Ca1—O467.43 (10)O11i—Ca3—S2i93.76 (8)
O4ii—Ca1—O4119.93 (8)O7viii—Ca3—S2i153.30 (9)
O12—Ca1—O1070.02 (11)O7i—Ca3—S2i27.08 (9)
O7—Ca1—O10119.28 (13)O6vii—Ca3—S2i151.81 (8)
O3i—Ca1—O1079.63 (10)O6—Ca3—S2i27.84 (8)
O4ii—Ca1—O1087.81 (10)S2viii—Ca3—S2i179.47 (7)
O4—Ca1—O10144.45 (11)O13—Ca3—Ca1i119.67 (2)
O12—Ca1—O11124.87 (13)O1vii—Ca3—Ca1i149.03 (8)
O7—Ca1—O1168.19 (12)O1—Ca3—Ca1i57.72 (8)
O3i—Ca1—O1185.95 (11)O11viii—Ca3—Ca1i91.06 (10)
O4ii—Ca1—O1198.59 (11)O11i—Ca3—Ca1i37.75 (8)
O4—Ca1—O11131.39 (10)O7viii—Ca3—Ca1i120.77 (10)
O10—Ca1—O1155.18 (12)O7i—Ca3—Ca1i33.05 (8)
O12—Ca1—O381.79 (12)O6vii—Ca3—Ca1i111.36 (9)
O7—Ca1—O382.11 (11)O6—Ca3—Ca1i86.95 (8)
O3i—Ca1—O3118.64 (9)S2viii—Ca3—Ca1i121.05 (3)
O4ii—Ca1—O364.96 (9)S2i—Ca3—Ca1i59.25 (3)
O4—Ca1—O355.03 (8)O2—Ca4—O2v81.3 (2)
O10—Ca1—O3142.86 (9)O2—Ca4—O10ii79.47 (11)
O11—Ca1—O3148.49 (12)O2v—Ca4—O10ii155.56 (14)
O12—Ca1—S397.16 (9)O2—Ca4—O10ix155.56 (14)
O7—Ca1—S394.68 (10)O2v—Ca4—O10ix79.47 (11)
O3i—Ca1—S379.62 (9)O10ii—Ca4—O10ix122.69 (16)
O4ii—Ca1—S395.80 (7)O2—Ca4—O5v70.80 (11)
O4—Ca1—S3144.15 (8)O2v—Ca4—O5v79.52 (13)
O10—Ca1—S327.61 (9)O10ii—Ca4—O5v80.00 (11)
O11—Ca1—S327.73 (9)O10ix—Ca4—O5v119.77 (12)
O3—Ca1—S3160.76 (7)O2—Ca4—O579.52 (13)
O12—Ca1—S186.44 (9)O2v—Ca4—O570.80 (11)
O7—Ca1—S184.02 (9)O10ii—Ca4—O5119.77 (12)
O3i—Ca1—S193.39 (8)O10ix—Ca4—O580.00 (11)
O4ii—Ca1—S192.47 (7)O5v—Ca4—O5140.65 (18)
O4—Ca1—S127.46 (7)O2—Ca4—O12ix126.39 (12)
O10—Ca1—S1156.30 (9)O2v—Ca4—O12ix84.95 (11)
O11—Ca1—S1147.58 (10)O10ii—Ca4—O12ix94.43 (12)
O3—Ca1—S127.61 (7)O10ix—Ca4—O12ix66.64 (11)
S3—Ca1—S1171.28 (5)O5v—Ca4—O12ix55.77 (12)
O12—Ca1—Ca4iii37.99 (8)O5—Ca4—O12ix141.87 (11)
O7—Ca1—Ca4iii153.28 (10)O2—Ca4—O12ii84.95 (11)
O3i—Ca1—Ca4iii67.64 (10)O2v—Ca4—O12ii126.39 (12)
O4ii—Ca1—Ca4iii94.04 (8)O10ii—Ca4—O12ii66.64 (11)
O4—Ca1—Ca4iii115.89 (9)O10ix—Ca4—O12ii94.43 (12)
O10—Ca1—Ca4iii34.04 (8)O5v—Ca4—O12ii141.87 (11)
O11—Ca1—Ca4iii87.20 (9)O5—Ca4—O12ii55.77 (12)
O3—Ca1—Ca4iii119.20 (8)O12ix—Ca4—O12ii141.1 (2)
S3—Ca1—Ca4iii59.73 (4)O2—Ca4—S2v97.89 (8)
S1—Ca1—Ca4iii122.46 (4)O2v—Ca4—S2v81.82 (8)
O12—Ca1—Ca3iv147.41 (10)O10ii—Ca4—S2v86.01 (8)
O7—Ca1—Ca3iv36.16 (8)O10ix—Ca4—S2v94.17 (8)
O3i—Ca1—Ca3iv115.26 (8)O5v—Ca4—S2v27.14 (9)
O4ii—Ca1—Ca3iv76.84 (8)O5—Ca4—S2v152.59 (9)
O4—Ca1—Ca3iv122.37 (8)O12ix—Ca4—S2v28.65 (8)
O10—Ca1—Ca3iv83.12 (8)O12ii—Ca4—S2v151.61 (9)
O11—Ca1—Ca3iv36.22 (8)O2—Ca4—S281.82 (8)
O3—Ca1—Ca3iv112.28 (9)O2v—Ca4—S297.89 (8)
S3—Ca1—Ca3iv59.68 (4)O10ii—Ca4—S294.17 (8)
S1—Ca1—Ca3iv120.02 (4)O10ix—Ca4—S286.01 (8)
Ca4iii—Ca1—Ca3iv117.13 (3)O5v—Ca4—S2152.59 (9)
O14—Ca2—O5v69.27 (14)O5—Ca4—S227.14 (9)
O14—Ca2—O8vi106.17 (16)O12ix—Ca4—S2151.61 (9)
O5v—Ca2—O8vi76.47 (11)O12ii—Ca4—S228.65 (8)
O14—Ca2—O9ii141.24 (14)S2v—Ca4—S2179.62 (7)
O5v—Ca2—O9ii73.46 (12)O2—Ca4—Ca1ix146.92 (10)
O8vi—Ca2—O9ii74.38 (10)O2v—Ca4—Ca1ix72.27 (10)
O14—Ca2—O8i71.99 (12)O10ii—Ca4—Ca1ix118.85 (9)
O5v—Ca2—O8i141.22 (10)O10ix—Ca4—Ca1ix34.95 (8)
O8vi—Ca2—O8i113.30 (9)O5v—Ca4—Ca1ix84.86 (8)
O9ii—Ca2—O8i144.75 (13)O5—Ca4—Ca1ix109.05 (9)
O14—Ca2—O6vii142.18 (14)O12ix—Ca4—Ca1ix33.58 (8)
O5v—Ca2—O6vii146.91 (17)O12ii—Ca4—Ca1ix126.80 (11)
O8vi—Ca2—O6vii82.34 (12)S2v—Ca4—Ca1ix59.49 (3)
O9ii—Ca2—O6vii76.54 (12)S2—Ca4—Ca1ix120.66 (3)
O8i—Ca2—O6vii70.88 (13)O2—Ca4—Ca1ii72.27 (10)
O14—Ca2—O1108.46 (16)O2v—Ca4—Ca1ii146.92 (10)
O5v—Ca2—O1116.07 (13)O10ii—Ca4—Ca1ii34.95 (8)
O8vi—Ca2—O1145.37 (9)O10ix—Ca4—Ca1ii118.85 (9)
O9ii—Ca2—O178.68 (10)O5v—Ca4—Ca1ii109.05 (9)
O8i—Ca2—O178.07 (11)O5—Ca4—Ca1ii84.86 (8)
O6vii—Ca2—O170.42 (10)O12ix—Ca4—Ca1ii126.80 (11)
O14—Ca2—O276.36 (15)O12ii—Ca4—Ca1ii33.58 (8)
O5v—Ca2—O265.53 (11)S2v—Ca4—Ca1ii120.66 (3)
O8vi—Ca2—O2138.38 (12)S2—Ca4—Ca1ii59.49 (3)
O9ii—Ca2—O278.95 (11)Ca1ix—Ca4—Ca1ii138.84 (5)
O8i—Ca2—O2106.99 (11)O1—S1—O2108.49 (19)
O6vii—Ca2—O2121.64 (13)O1—S1—O3111.41 (18)
O1—Ca2—O253.16 (11)O2—S1—O3112.0 (3)
O14—Ca2—O9vi73.72 (14)O1—S1—O4109.9 (2)
O5v—Ca2—O9vi100.99 (11)O2—S1—O4109.19 (19)
O8vi—Ca2—O9vi51.51 (8)O3—S1—O4105.84 (16)
O9ii—Ca2—O9vi124.64 (9)O1—S1—Ca1128.33 (17)
O8i—Ca2—O9vi65.78 (10)O2—S1—Ca1122.85 (16)
O6vii—Ca2—O9vi84.76 (10)O3—S1—Ca155.84 (12)
O1—Ca2—O9vi141.37 (12)O4—S1—Ca150.09 (10)
O2—Ca2—O9vi149.98 (9)O1—S1—Ca249.46 (15)
O14—Ca2—S194.05 (13)O2—S1—Ca259.25 (14)
O5v—Ca2—S190.77 (10)O3—S1—Ca2124.90 (14)
O8vi—Ca2—S1149.98 (8)O4—S1—Ca2128.96 (13)
O9ii—Ca2—S175.96 (8)Ca1—S1—Ca2177.68 (7)
O8i—Ca2—S193.76 (9)O5—S2—O7110.5 (3)
O6vii—Ca2—S195.27 (8)O5—S2—O6ii111.48 (18)
O1—Ca2—S126.19 (9)O7—S2—O6ii106.99 (17)
O2—Ca2—S127.05 (9)O5—S2—O12ii105.81 (18)
O9vi—Ca2—S1158.41 (7)O7—S2—O12ii110.57 (18)
O14—Ca2—S3vi90.11 (13)O6ii—S2—O12ii111.6 (4)
O5v—Ca2—S3vi88.08 (10)O5—S2—Ca449.56 (14)
O8vi—Ca2—S3vi25.16 (8)O7—S2—Ca4127.19 (15)
O9ii—Ca2—S3vi99.03 (8)O6ii—S2—Ca4125.67 (13)
O8i—Ca2—S3vi90.20 (8)O12ii—S2—Ca456.29 (13)
O6vii—Ca2—S3vi83.10 (8)O5—S2—Ca3iv130.77 (16)
O1—Ca2—S3vi153.28 (9)O7—S2—Ca3iv52.38 (14)
O2—Ca2—S3vi153.13 (9)O6ii—S2—Ca3iv54.79 (13)
O9vi—Ca2—S3vi26.36 (7)O12ii—S2—Ca3iv123.37 (13)
S1—Ca2—S3vi174.98 (6)Ca4—S2—Ca3iv179.43 (2)
O14—Ca2—Ca475.04 (10)O9—S3—O11109.22 (18)
O5v—Ca2—Ca432.94 (9)O9—S3—O10112.6 (2)
O8vi—Ca2—Ca4105.74 (9)O11—S3—O10107.2 (2)
O9ii—Ca2—Ca467.91 (8)O9—S3—O8107.0 (2)
O8i—Ca2—Ca4134.23 (7)O11—S3—O8111.4 (3)
O6vii—Ca2—Ca4139.23 (10)O10—S3—O8109.57 (15)
O1—Ca2—Ca483.32 (8)O9—S3—Ca1121.09 (14)
O2—Ca2—Ca433.45 (8)O11—S3—Ca155.91 (14)
O9vi—Ca2—Ca4131.92 (7)O10—S3—Ca151.71 (14)
S1—Ca2—Ca457.83 (4)O8—S3—Ca1131.92 (16)
S3vi—Ca2—Ca4120.86 (4)O9—S3—Ca2x63.06 (13)
O13—Ca3—O1vii70.93 (8)O11—S3—Ca2x124.60 (16)
O13—Ca3—O170.93 (8)O10—S3—Ca2x126.94 (16)
O1vii—Ca3—O1141.86 (16)O8—S3—Ca2x43.90 (13)
O13—Ca3—O11viii141.26 (10)Ca1—S3—Ca2x175.77 (6)
O1vii—Ca3—O11viii70.86 (11)S1—O1—Ca3143.4 (2)
O1—Ca3—O11viii146.89 (14)S1—O1—Ca2104.4 (2)
O13—Ca3—O11i141.26 (10)Ca3—O1—Ca2111.67 (13)
O1vii—Ca3—O11i146.89 (14)S1—O2—Ca4141.6 (2)
O1—Ca3—O11i70.86 (11)S1—O2—Ca293.69 (18)
O11viii—Ca3—O11i77.5 (2)Ca4—O2—Ca2106.93 (12)
O13—Ca3—O7viii109.26 (9)S1—O3—Ca1ii144.2 (2)
O1vii—Ca3—O7viii75.83 (11)S1—O3—Ca196.55 (15)
O1—Ca3—O7viii117.41 (12)Ca1ii—O3—Ca1107.37 (11)
O11viii—Ca3—O7viii66.75 (10)S1—O4—Ca1i124.97 (16)
O11i—Ca3—O7viii83.12 (13)S1—O4—Ca1102.46 (14)
O13—Ca3—O7i109.26 (9)Ca1i—O4—Ca1111.99 (11)
O1vii—Ca3—O7i117.41 (12)S2—O5—Ca2v140.9 (2)
O1—Ca3—O7i75.83 (11)S2—O5—Ca4103.31 (19)
O11viii—Ca3—O7i83.12 (13)Ca2v—O5—Ca4114.95 (14)
O11i—Ca3—O7i66.75 (10)S2i—O6—Ca2vii136.6 (2)
O7viii—Ca3—O7i141.48 (19)S2i—O6—Ca397.37 (17)
O13—Ca3—O6vii71.69 (11)Ca2vii—O6—Ca3107.34 (12)
O1vii—Ca3—O6vii99.57 (12)S2—O7—Ca1143.6 (2)
O1—Ca3—O6vii68.19 (11)S2—O7—Ca3iv100.54 (18)
O11viii—Ca3—O6vii121.14 (12)Ca1—O7—Ca3iv110.79 (14)
O11i—Ca3—O6vii88.45 (11)S3—O8—Ca2x110.94 (17)
O7viii—Ca3—O6vii54.85 (11)S3—O8—Ca2ii132.37 (18)
O7i—Ca3—O6vii141.53 (10)Ca2x—O8—Ca2ii116.67 (12)
O13—Ca3—O671.69 (10)S3—O9—Ca2i145.9 (2)
O1vii—Ca3—O668.19 (11)S3—O9—Ca2x90.58 (15)
O1—Ca3—O699.57 (12)Ca2i—O9—Ca2x101.83 (10)
O11viii—Ca3—O688.45 (11)S3—O10—Ca4iii138.4 (2)
O11i—Ca3—O6121.14 (12)S3—O10—Ca1100.67 (19)
O7viii—Ca3—O6141.53 (10)Ca4iii—O10—Ca1111.01 (13)
O7i—Ca3—O654.85 (11)S3—O11—Ca3iv134.1 (2)
O6vii—Ca3—O6143.4 (2)S3—O11—Ca196.36 (19)
O13—Ca3—S2viii89.74 (4)Ca3iv—O11—Ca1106.03 (12)
O1vii—Ca3—S2viii86.00 (8)S2i—O12—Ca1140.2 (2)
O1—Ca3—S2viii93.82 (8)S2i—O12—Ca4iii95.06 (17)
O11viii—Ca3—S2viii93.76 (8)Ca1—O12—Ca4iii108.43 (13)
O11i—Ca3—S2viii86.66 (7)
Symmetry codes: (i) x+1/2, y+1/2, z+1; (ii) x+1/2, y1/2, z+1; (iii) x+1/2, y+1/2, z+1; (iv) x+1/2, y1/2, z; (v) x, y, z; (vi) x1, y, z1; (vii) x, y, z+1; (viii) x1/2, y+1/2, z; (ix) x1/2, y1/2, z1; (x) x+1, y, z+1.

Experimental details

(caso40625)(caso4_05)
Crystal data
Chemical formulaCaH1.25O4.625SCaO4.5SH
Mr147.40145.16
Crystal system, space groupTrigonal, P3221Monoclinic, C2
Temperature (K)296293
a, b, c (Å)13.8690 (4), 13.8690 (4), 12.7189 (1)17.5180 (8), 6.9291 (1), 12.0344 (2)
α, β, γ (°)90, 90, 12090, 133.655 (4), 90
V3)2118.70 (9)1056.88 (4)
Z2412
Radiation typeMo KαMo Kα
µ (mm1)2.242.25
Crystal size (mm)0.4 × 0.08 × 0.070.4 × 0.08 × 0.07
Data collection
DiffractometerBruker X8 Kappa. Apex2
diffractometer
Bruker X8 Kappa. Apex2
diffractometer
Absorption correctionNumerical
Tmin, Tmax0.641, 0.896
No. of measured, independent and
observed [I > 2σ(I)] reflections
38925, 3252, 2578 15532, 15543, 12774
Rint0.0430.000
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.039, 0.108, 1.03 0.042, 0.096, 0.97
No. of reflections325215543
No. of parameters260193
No. of restraints51
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.53, 0.450.58, 0.49
Absolute structureFlack H D (1983), Acta Cryst. A39, 876-881Flack H D (1983), Acta Cryst. A39, 876-881
Absolute structure parameter0.000.06 (3)

Computer programs: Apex2, SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), Diamond 3.

 

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