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The structural variations of several alkali metal rare earth fluoride single crystals are summarized. Two different stoichiometric formulations are considered, namely those of ARE2F7 and ARE3F10 (A = K, Rb, Cs; RE = Y, La–Lu), over a wide range of ionic radii of both the alkali and rare earth (RE) ions. Previously reported and several new single-crystal structures are considered. The new single crystals are grown using hydrothermal methods and the structures are compared with literature reports of structures grown from both melts and hydrothermal fluids. The data reported here are combined with the literature data to gain a greater understanding of structural subtleties surrounding these systems. The work underscores the importance of the size of the cations to the observed structure type and also introduces synthetic technique as a contributor to the same. New insights based on single-crystal structure analysis in the work introduce a new disordered structure type in the case of ARE2F7, and examine the trends and boundaries of the ARE3F10 stoichiometry. Such fundamental structural information is useful in understanding the potential applications of these compounds as optical materials.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520615017916/bp5082sup1.cif
Contains datablocks CsY2F7, RbSm2F7, CsGd2F7, KY3F10, RbY3F10, RbSm3F10, RbGd3F10, KLu3F10

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520615017916/bp5082CsY2F7sup2.hkl
Contains datablock CsY2F7

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520615017916/bp5082RbSm2F7sup3.hkl
Contains datablock RbSm2F7

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520615017916/bp5082CsGd2F7sup4.hkl
Contains datablock CsGd2F7

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520615017916/bp5082KY3F10sup5.hkl
Contains datablock KY3F10

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520615017916/bp5082RbY3F10sup6.hkl
Contains datablock RbY3F10

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520615017916/bp5082RbSm3F10sup7.hkl
Contains datablock RbSm3F10

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520615017916/bp5082RbGd3F10sup8.hkl
Contains datablock RbGd3F10

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520615017916/bp5082KLu3F10sup9.hkl
Contains datablock KLu3F10

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S2052520615017916/bp5082sup10.pdf
Tables of selected interatomic distances, and Figs. S1 and S2

CCDC references: 1427210; 1427211; 1427212; 1427213; 1427214; 1427215; 1427216; 1427217

Computing details top

Data collection: CrystalClear (Rigaku/MSC, 2006) for CsY2F7, RbSm2F7, CsGd2F7, RbY3F10, RbSm3F10, RbGd3F10, KLu3F10. Cell refinement: CrystalClear (Rigaku/MSC, 2006) for CsY2F7, RbSm2F7, CsGd2F7, RbY3F10, RbSm3F10, RbGd3F10, KLu3F10. Data reduction: CrystalClear (Rigaku/MSC, 2006) for CsY2F7, RbSm2F7, CsGd2F7, RbY3F10, RbSm3F10, RbGd3F10, KLu3F10. For all structures, program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997). Molecular graphics: DIAMOND (Bradenburg, 1999) for CsY2F7, RbSm2F7, CsGd2F7, RbY3F10, RbSm3F10, RbGd3F10, KLu3F10. Software used to prepare material for publication: SHELXL97 (Sheldrick, 1997) for CsY2F7, RbSm2F7, CsGd2F7, RbY3F10, RbSm3F10, RbGd3F10, KLu3F10.

(CsY2F7) top
Crystal data top
CsF7Y2Dx = 4.490 Mg m3
Mr = 443.73Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, PnnaCell parameters from 4730 reflections
a = 13.6028 (14) Åθ = 3.0–26.7°
b = 12.3072 (13) ŵ = 23.12 mm1
c = 7.8426 (8) ÅT = 293 K
V = 1312.9 (2) Å3Prism, colorless
Z = 80.23 × 0.14 × 0.12 mm
F(000) = 1568
Data collection top
Rigaku AFC8S
diffractometer
1182 independent reflections
Radiation source: fine-focus sealed tube1009 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.071
Detector resolution: 14.6199 pixels mm-1θmax = 25.2°, θmin = 3.0°
ω scansh = 1516
Absorption correction: multi-scan
REQAB, CrystalClear
k = 1414
Tmin = 0.690, Tmax = 1.000l = 99
10355 measured reflections
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)] = 0.035 w = 1/[σ2(Fo2) + (0.032P)2 + 4.641P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.078(Δ/σ)max = 0.001
S = 1.14Δρmax = 1.03 e Å3
1182 reflectionsΔρmin = 1.40 e Å3
116 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
12 restraintsExtinction coefficient: 0.00085 (11)
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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)
Cs10.58120 (4)0.92160 (4)0.23015 (7)0.0262 (2)
Y10.43211 (7)1.25000.25000.0111 (3)
Y20.65951 (6)1.26353 (7)0.02423 (9)0.0189 (2)
Y30.25001.00000.24907 (14)0.0155 (3)
F10.8056 (4)1.3074 (5)0.0910 (7)0.0330 (13)
F20.1461 (8)1.0764 (9)0.4286 (15)0.021 (2)0.50
F2A0.1726 (9)1.0449 (8)0.4919 (14)0.021 (3)0.50
F30.6408 (8)1.3194 (7)0.2542 (12)0.023 (2)0.50
F40.5839 (3)1.3467 (3)0.2611 (6)0.0173 (10)
F50.7573 (5)1.25000.25000.0169 (13)
F60.4975 (3)1.2620 (4)0.0104 (6)0.0201 (10)
F70.3917 (4)1.0812 (4)0.1747 (6)0.0232 (11)
F80.3119 (9)0.8823 (9)0.0814 (16)0.032 (3)0.50
F8A0.2808 (7)0.9172 (7)0.0057 (13)0.016 (2)0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cs10.0364 (4)0.0129 (3)0.0293 (3)0.0004 (2)0.0008 (3)0.0009 (2)
Y10.0087 (5)0.0139 (5)0.0108 (5)0.0000.0000.0010 (4)
Y20.0103 (4)0.0375 (5)0.0090 (4)0.0023 (3)0.0004 (3)0.0019 (3)
Y30.0112 (5)0.0250 (6)0.0101 (5)0.0018 (4)0.0000.000
F10.019 (3)0.055 (3)0.025 (3)0.001 (2)0.009 (2)0.005 (2)
F20.020 (5)0.021 (5)0.021 (5)0.001 (4)0.004 (4)0.007 (4)
F2A0.030 (6)0.020 (5)0.014 (5)0.005 (4)0.005 (4)0.002 (4)
F30.029 (6)0.023 (5)0.017 (5)0.008 (4)0.006 (5)0.002 (4)
F40.016 (2)0.009 (2)0.027 (3)0.0007 (17)0.005 (2)0.0008 (18)
F50.013 (3)0.028 (3)0.010 (3)0.0000.0000.002 (3)
F60.009 (2)0.037 (3)0.014 (2)0.0014 (19)0.0009 (18)0.005 (2)
F70.025 (3)0.017 (2)0.028 (3)0.005 (2)0.000 (2)0.005 (2)
F80.043 (8)0.029 (6)0.025 (6)0.005 (5)0.006 (6)0.002 (5)
F8A0.023 (6)0.013 (4)0.013 (5)0.008 (4)0.000 (4)0.008 (4)
Geometric parameters (Å, º) top
Cs1—F4i2.853 (4)Y3—F22.205 (10)
Cs1—F2Aii2.933 (11)Y3—F2Avii2.245 (10)
Cs1—F6iii3.024 (4)Y3—F2A2.245 (10)
Cs1—F6iv3.037 (5)Y3—F7vii2.248 (5)
Cs1—F5v3.051 (5)Y3—F72.248 (5)
Cs1—F7iv3.197 (5)Y3—F8A2.281 (9)
Cs1—F8Avi3.236 (11)Y3—F8Avii2.281 (9)
Cs1—F8Aiv3.250 (10)Y3—F3viii2.674 (10)
Cs1—F73.270 (5)Y3—F3iii2.674 (10)
Cs1—F3iii3.273 (10)F1—Y1vi2.239 (5)
Cs1—F2ii3.402 (12)F1—Y3xi2.787 (6)
Cs1—F2vii3.461 (12)F1—Cs1xiii3.515 (5)
Y1—F72.229 (4)F2—F2A0.726 (11)
Y1—F7i2.229 (4)F2—Y2viii2.116 (10)
Y1—F6i2.232 (4)F2—Cs1xiv3.402 (12)
Y1—F62.232 (4)F2—Cs1vii3.461 (12)
Y1—F1viii2.239 (5)F2A—Y2viii2.377 (10)
Y1—F1ix2.239 (5)F2A—Cs1xiv2.933 (11)
Y1—F42.385 (4)F3—F8xv1.635 (16)
Y1—F4i2.385 (4)F3—F3xii1.710 (18)
Y1—Y2i3.5682 (12)F3—Y2xii2.365 (9)
Y1—Y23.5682 (12)F3—Y3xi2.674 (10)
Y1—Y33.9501 (7)F3—Cs1xv3.273 (10)
Y1—Y3x3.9501 (7)F4—Y2i2.394 (4)
Y2—F8iv2.014 (10)F4—Cs1i2.853 (4)
Y2—F2xi2.116 (10)F5—Y2i2.221 (4)
Y2—F62.221 (5)F5—Cs1xiii3.051 (5)
Y2—F52.221 (4)F5—Cs1v3.051 (5)
Y2—F12.249 (5)F6—Cs1xv3.024 (4)
Y2—F32.304 (10)F6—Cs1iv3.037 (5)
Y2—F42.357 (4)F7—Cs1iv3.197 (5)
Y2—F3xii2.365 (9)F8—F8A0.912 (12)
Y2—F8Aiv2.373 (9)F8—F3iii1.635 (16)
Y2—F2Axi2.377 (10)F8—Y2iv2.014 (10)
Y2—F4i2.394 (4)F8—Cs1iv3.729 (12)
Y2—Y2i3.5569 (15)F8A—Y2iv2.373 (9)
Y3—F82.130 (10)F8A—Cs1ix3.236 (11)
Y3—F8vii2.130 (10)F8A—Cs1iv3.250 (10)
Y3—F2vii2.205 (10)
F4i—Cs1—F2Aii57.3 (2)F3—Y2—F2Axi67.1 (4)
F4i—Cs1—F6iii129.62 (13)F4—Y2—F2Axi71.7 (3)
F2Aii—Cs1—F6iii89.2 (2)F3xii—Y2—F2Axi109.9 (3)
F4i—Cs1—F6iv139.64 (12)F8Aiv—Y2—F2Axi153.8 (4)
F2Aii—Cs1—F6iv163.0 (2)F8iv—Y2—F4i82.4 (3)
F6iii—Cs1—F6iv76.93 (14)F2xi—Y2—F4i137.7 (3)
F4i—Cs1—F5v132.95 (12)F6—Y2—F4i69.82 (16)
F2Aii—Cs1—F5v90.9 (2)F5—Y2—F4i69.77 (15)
F6iii—Cs1—F5v76.76 (10)F1—Y2—F4i142.95 (19)
F6iv—Cs1—F5v76.56 (10)F3—Y2—F4i142.0 (3)
F4i—Cs1—F7iv91.89 (12)F4—Y2—F4i60.28 (18)
F2Aii—Cs1—F7iv134.0 (2)F3xii—Y2—F4i109.8 (2)
F6iii—Cs1—F7iv134.61 (12)F8Aiv—Y2—F4i70.1 (3)
F6iv—Cs1—F7iv57.93 (11)F2Axi—Y2—F4i132.0 (3)
F5v—Cs1—F7iv87.72 (9)F8iv—Y2—Y2i109.0 (4)
F4i—Cs1—F8Avi91.07 (18)F2xi—Y2—Y2i116.1 (3)
F2Aii—Cs1—F8Avi93.3 (3)F6—Y2—Y2i96.94 (12)
F6iii—Cs1—F8Avi130.71 (17)F5—Y2—Y2i36.80 (14)
F6iv—Cs1—F8Avi88.5 (2)F1—Y2—Y2i115.00 (14)
F5v—Cs1—F8Avi54.01 (15)F3—Y2—Y2i166.3 (2)
F7iv—Cs1—F8Avi50.41 (19)F4—Y2—Y2i41.91 (11)
F4i—Cs1—F8Aiv52.79 (17)F3xii—Y2—Y2i148.3 (2)
F2Aii—Cs1—F8Aiv80.9 (3)F8Aiv—Y2—Y2i88.5 (2)
F6iii—Cs1—F8Aiv164.9 (2)F2Axi—Y2—Y2i101.5 (3)
F6iv—Cs1—F8Aiv110.51 (18)F4i—Y2—Y2i41.13 (11)
F5v—Cs1—F8Aiv91.96 (18)F8—Y3—F8vii103.8 (7)
F7iv—Cs1—F8Aiv53.26 (18)F8—Y3—F2vii81.4 (5)
F8Avi—Cs1—F8Aiv39.7 (3)F8vii—Y3—F2vii159.6 (4)
F4i—Cs1—F754.06 (12)F8—Y3—F2159.6 (4)
F2Aii—Cs1—F797.0 (2)F8vii—Y3—F281.4 (5)
F6iii—Cs1—F7101.56 (13)F2vii—Y3—F2100.7 (7)
F6iv—Cs1—F795.37 (12)F8—Y3—F2Avii99.8 (5)
F5v—Cs1—F7171.93 (10)F8vii—Y3—F2Avii151.2 (4)
F7iv—Cs1—F788.01 (12)F2vii—Y3—F2Avii18.7 (3)
F8Avi—Cs1—F7126.80 (17)F2—Y3—F2Avii82.2 (6)
F8Aiv—Cs1—F791.0 (2)F8—Y3—F2A151.2 (4)
F4i—Cs1—F3iii113.28 (19)F8vii—Y3—F2A99.8 (5)
F2Aii—Cs1—F3iii124.2 (3)F2vii—Y3—F2A82.2 (6)
F6iii—Cs1—F3iii53.03 (19)F2—Y3—F2A18.7 (3)
F6iv—Cs1—F3iii53.86 (19)F2Avii—Y3—F2A63.9 (6)
F5v—Cs1—F3iii113.34 (19)F8—Y3—F7vii82.9 (4)
F7iv—Cs1—F3iii98.02 (19)F8vii—Y3—F7vii78.6 (3)
F8Avi—Cs1—F3iii142.0 (2)F2vii—Y3—F7vii121.7 (3)
F8Aiv—Cs1—F3iii142.0 (3)F2—Y3—F7vii78.8 (3)
F7—Cs1—F3iii60.56 (19)F2Avii—Y3—F7vii120.8 (3)
F4i—Cs1—F2ii54.41 (19)F2A—Y3—F7vii85.8 (3)
F2Aii—Cs1—F2ii10.1 (3)F8—Y3—F778.6 (3)
F6iii—Cs1—F2ii85.8 (2)F8vii—Y3—F782.9 (4)
F6iv—Cs1—F2ii162.7 (2)F2vii—Y3—F778.8 (3)
F5v—Cs1—F2ii99.25 (19)F2—Y3—F7121.7 (3)
F7iv—Cs1—F2ii139.3 (2)F2Avii—Y3—F785.8 (3)
F8Avi—Cs1—F2ii102.7 (3)F2A—Y3—F7120.8 (3)
F8Aiv—Cs1—F2ii86.2 (2)F7vii—Y3—F7149.9 (3)
F7—Cs1—F2ii88.4 (2)F8—Y3—F8A23.5 (3)
F3iii—Cs1—F2ii115.2 (3)F8vii—Y3—F8A80.5 (5)
F4i—Cs1—F2vii89.6 (2)F2vii—Y3—F8A104.5 (4)
F2Aii—Cs1—F2vii92.4 (2)F2—Y3—F8A150.1 (4)
F6iii—Cs1—F2vii52.11 (19)F2Avii—Y3—F8A123.2 (4)
F6iv—Cs1—F2vii86.9 (2)F2A—Y3—F8A159.9 (4)
F5v—Cs1—F2vii128.69 (18)F7vii—Y3—F8A74.4 (3)
F7iv—Cs1—F2vii123.3 (2)F7—Y3—F8A79.3 (3)
F8Avi—Cs1—F2vii173.7 (3)F8—Y3—F8Avii80.5 (5)
F8Aiv—Cs1—F2vii139.1 (2)F8vii—Y3—F8Avii23.5 (3)
F7—Cs1—F2vii49.55 (18)F2vii—Y3—F8Avii150.1 (4)
F3iii—Cs1—F2vii33.1 (3)F2—Y3—F8Avii104.5 (4)
F2ii—Cs1—F2vii82.8 (3)F2Avii—Y3—F8Avii159.9 (4)
F7—Y1—F7i151.4 (3)F2A—Y3—F8Avii123.2 (4)
F7—Y1—F6i106.19 (17)F7vii—Y3—F8Avii79.3 (3)
F7i—Y1—F6i85.28 (18)F7—Y3—F8Avii74.4 (3)
F7—Y1—F685.28 (18)F8A—Y3—F8Avii57.7 (5)
F7i—Y1—F6106.19 (17)F8—Y3—F3viii141.2 (4)
F6i—Y1—F6133.0 (2)F8vii—Y3—F3viii37.7 (4)
F7—Y1—F1viii70.4 (2)F2vii—Y3—F3viii135.8 (4)
F7i—Y1—F1viii87.5 (2)F2—Y3—F3viii45.2 (4)
F6i—Y1—F1viii77.06 (18)F2Avii—Y3—F3viii118.3 (4)
F6—Y1—F1viii146.77 (19)F2A—Y3—F3viii62.8 (4)
F7—Y1—F1ix87.5 (2)F7vii—Y3—F3viii83.7 (2)
F7i—Y1—F1ix70.4 (2)F7—Y3—F3viii96.0 (2)
F6i—Y1—F1ix146.77 (19)F8A—Y3—F3viii117.7 (3)
F6—Y1—F1ix77.06 (18)F8Avii—Y3—F3viii61.2 (3)
F1viii—Y1—F1ix79.6 (3)F8—Y3—F3iii37.7 (4)
F7—Y1—F4133.49 (17)F8vii—Y3—F3iii141.2 (4)
F7i—Y1—F474.87 (16)F2vii—Y3—F3iii45.2 (4)
F6i—Y1—F469.79 (16)F2—Y3—F3iii135.8 (4)
F6—Y1—F469.84 (16)F2Avii—Y3—F3iii62.8 (4)
F1viii—Y1—F4143.36 (17)F2A—Y3—F3iii118.3 (4)
F1ix—Y1—F4121.91 (18)F7vii—Y3—F3iii96.0 (2)
F7—Y1—F4i74.87 (16)F7—Y3—F3iii83.7 (2)
F7i—Y1—F4i133.49 (17)F8A—Y3—F3iii61.2 (3)
F6i—Y1—F4i69.84 (16)F8Avii—Y3—F3iii117.7 (3)
F6—Y1—F4i69.79 (16)F3viii—Y3—F3iii178.9 (4)
F1viii—Y1—F4i121.91 (18)Y1vi—F1—Y2145.8 (3)
F1ix—Y1—F4i143.36 (17)Y1vi—F1—Y3xi103.1 (2)
F4—Y1—F4i60.0 (2)Y2—F1—Y3xi98.34 (19)
F7—Y1—Y2i107.56 (13)Y1vi—F1—Cs1xiii103.76 (19)
F7i—Y1—Y2i97.23 (13)Y2—F1—Cs1xiii99.17 (17)
F6i—Y1—Y2i36.63 (12)Y3xi—F1—Cs1xiii98.10 (16)
F6—Y1—Y2i96.41 (12)F2A—F2—Y2viii102.2 (14)
F1viii—Y1—Y2i112.04 (14)F2A—F2—Y383.7 (13)
F1ix—Y1—Y2i163.19 (15)Y2viii—F2—Y3124.6 (5)
F4—Y1—Y2i41.79 (11)F2A—F2—Cs1xiv44.9 (13)
F4i—Y1—Y2i40.90 (11)Y2viii—F2—Cs1xiv105.4 (4)
F7—Y1—Y297.23 (13)Y3—F2—Cs1xiv115.5 (4)
F7i—Y1—Y2107.56 (13)F2A—F2—Cs1vii139.1 (16)
F6i—Y1—Y296.41 (12)Y2viii—F2—Cs1vii103.3 (4)
F6—Y1—Y236.63 (12)Y3—F2—Cs1vii106.8 (4)
F1viii—Y1—Y2163.19 (15)Cs1xiv—F2—Cs1vii97.2 (3)
F1ix—Y1—Y2112.04 (14)F2—F2A—Y377.5 (13)
F4—Y1—Y240.90 (11)F2—F2A—Y2viii60.5 (12)
F4i—Y1—Y241.79 (11)Y3—F2A—Y2viii111.7 (4)
Y2i—Y1—Y259.79 (3)F2—F2A—Cs1xiv125.0 (16)
F7—Y1—Y328.20 (13)Y3—F2A—Cs1xiv134.6 (4)
F7i—Y1—Y3124.89 (13)Y2viii—F2A—Cs1xiv113.7 (4)
F6i—Y1—Y3101.53 (12)F8xv—F3—F3xii120.2 (9)
F6—Y1—Y3107.45 (12)F8xv—F3—Y2147.7 (7)
F1viii—Y1—Y343.41 (15)F3xii—F3—Y270.4 (6)
F1ix—Y1—Y376.27 (15)F8xv—F3—Y2xii57.0 (5)
F4—Y1—Y3158.69 (10)F3xii—F3—Y2xii66.6 (6)
F4i—Y1—Y398.89 (10)Y2—F3—Y2xii135.1 (4)
Y2i—Y1—Y3120.547 (18)F8xv—F3—Y3xi52.8 (5)
Y2—Y1—Y3125.387 (18)F3xii—F3—Y3xi146.1 (2)
F7—Y1—Y3x124.89 (13)Y2—F3—Y3xi100.2 (3)
F7i—Y1—Y3x28.20 (13)Y2xii—F3—Y3xi107.9 (4)
F6i—Y1—Y3x107.45 (12)F8xv—F3—Cs1xv98.7 (6)
F6—Y1—Y3x101.53 (12)F3xii—F3—Cs1xv112.67 (17)
F1viii—Y1—Y3x76.27 (15)Y2—F3—Cs1xv104.6 (3)
F1ix—Y1—Y3x43.41 (15)Y2xii—F3—Cs1xv103.4 (3)
F4—Y1—Y3x98.89 (10)Y3xi—F3—Cs1xv101.2 (3)
F4i—Y1—Y3x158.69 (10)Y2—F4—Y197.61 (16)
Y2i—Y1—Y3x125.387 (18)Y2—F4—Y2i96.96 (16)
Y2—Y1—Y3x120.547 (18)Y1—F4—Y2i96.61 (15)
Y3—Y1—Y3x102.32 (2)Y2—F4—Cs1i117.29 (16)
F8iv—Y2—F2xi134.4 (5)Y1—F4—Cs1i119.22 (17)
F8iv—Y2—F697.7 (4)Y2i—F4—Cs1i123.72 (18)
F2xi—Y2—F683.0 (3)Y2i—F5—Y2106.4 (3)
F8iv—Y2—F598.4 (4)Y2i—F5—Cs1xiii116.26 (5)
F2xi—Y2—F5113.8 (3)Y2—F5—Cs1xiii114.84 (5)
F6—Y2—F5133.74 (18)Y2i—F5—Cs1v114.84 (5)
F8iv—Y2—F183.0 (4)Y2—F5—Cs1v116.26 (5)
F2xi—Y2—F173.2 (3)Cs1xiii—F5—Cs1v87.91 (17)
F6—Y2—F1146.09 (19)Y2—F6—Y1106.51 (19)
F5—Y2—F179.0 (2)Y2—F6—Cs1xv115.35 (17)
F8iv—Y2—F384.1 (4)Y1—F6—Cs1xv121.17 (18)
F2xi—Y2—F351.4 (4)Y2—F6—Cs1iv115.18 (18)
F6—Y2—F377.1 (3)Y1—F6—Cs1iv109.23 (17)
F5—Y2—F3147.6 (3)Cs1xv—F6—Cs1iv88.66 (12)
F1—Y2—F369.2 (3)Y1—F7—Y3123.9 (2)
F8iv—Y2—F4142.7 (3)Y1—F7—Cs1iv104.16 (16)
F2xi—Y2—F480.7 (3)Y3—F7—Cs1iv110.60 (17)
F6—Y2—F470.55 (16)Y1—F7—Cs1109.28 (18)
F5—Y2—F470.45 (16)Y3—F7—Cs1112.00 (16)
F1—Y2—F4126.74 (18)Cs1iv—F7—Cs191.99 (12)
F3—Y2—F4124.7 (3)F8A—F8—F3iii175.3 (14)
F8iv—Y2—F3xii42.9 (4)F8A—F8—Y2iv101.7 (10)
F2xi—Y2—F3xii94.3 (4)F3iii—F8—Y2iv80.0 (6)
F6—Y2—F3xii77.3 (3)F8A—F8—Y387.5 (9)
F5—Y2—F3xii138.3 (3)F3iii—F8—Y389.5 (6)
F1—Y2—F3xii80.7 (3)Y2iv—F8—Y3159.4 (6)
F3—Y2—F3xii43.0 (4)F8A—F8—Cs1iv52.1 (9)
F4—Y2—F3xii147.8 (3)F3iii—F8—Cs1iv132.0 (7)
F8iv—Y2—F8Aiv22.1 (4)Y2iv—F8—Cs1iv103.4 (4)
F2xi—Y2—F8Aiv151.7 (4)Y3—F8—Cs1iv96.8 (4)
F6—Y2—F8Aiv108.9 (3)F8—F8A—Y368.9 (9)
F5—Y2—F8Aiv76.9 (3)F8—F8A—Y2iv56.2 (8)
F1—Y2—F8Aiv84.1 (3)Y3—F8A—Y2iv122.4 (5)
F3—Y2—F8Aiv105.1 (3)F8—F8A—Cs1ix143.7 (11)
F4—Y2—F8Aiv127.2 (3)Y3—F8A—Cs1ix108.4 (3)
F3xii—Y2—F8Aiv65.0 (3)Y2iv—F8A—Cs1ix105.6 (3)
F8iv—Y2—F2Axi145.6 (4)F8—F8A—Cs1iv115.1 (11)
F2xi—Y2—F2Axi17.4 (3)Y3—F8A—Cs1iv107.9 (3)
F6—Y2—F2Axi94.0 (3)Y2iv—F8A—Cs1iv109.9 (3)
F5—Y2—F2Axi96.6 (3)Cs1ix—F8A—Cs1iv100.4 (3)
F1—Y2—F2Axi69.7 (3)
Symmetry codes: (i) x, y+5/2, z+1/2; (ii) x+1/2, y, z+1; (iii) x+1, y1/2, z+1/2; (iv) x+1, y+2, z; (v) x+3/2, y+2, z; (vi) x+1/2, y, z; (vii) x+1/2, y+2, z; (viii) x1/2, y+5/2, z+1/2; (ix) x1/2, y, z; (x) x+1/2, y+1/2, z+1/2; (xi) x+1/2, y+5/2, z1/2; (xii) x, y+5/2, z1/2; (xiii) x+3/2, y+1/2, z+1/2; (xiv) x1/2, y, z+1; (xv) x+1, y+1/2, z1/2.
(RbSm2F7) top
Crystal data top
F7RbSm2Dx = 5.096 Mg m3
Mr = 519.17Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, PnnaCell parameters from 4163 reflections
a = 13.9359 (16) Åθ = 2.9–28.3°
b = 12.2412 (13) ŵ = 24.39 mm1
c = 7.9329 (8) ÅT = 293 K
V = 1353.3 (3) Å3Prism, yellow
Z = 80.22 × 0.18 × 0.12 mm
F(000) = 1792
Data collection top
Rigaku AFC8S
diffractometer
1188 independent reflections
Radiation source: fine-focus sealed tube1035 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.039
Detector resolution: 14.6199 pixels mm-1θmax = 25.1°, θmin = 2.9°
ω scansh = 1616
Absorption correction: multi-scan
REQAB, CrystalClear
k = 1414
Tmin = 0.601, Tmax = 1.000l = 99
6252 measured reflections
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)] = 0.043 w = 1/[σ2(Fo2) + (0.0422P)2 + 55.8111P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.103(Δ/σ)max < 0.001
S = 1.12Δρmax = 1.90 e Å3
1188 reflectionsΔρmin = 2.91 e Å3
116 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
12 restraintsExtinction coefficient: 0.00061 (10)
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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)
Rb10.58337 (14)0.92108 (12)0.2243 (2)0.0434 (5)
Sm10.42886 (6)1.25000.25000.0141 (3)
Sm20.65539 (5)1.26764 (8)0.02417 (9)0.0326 (3)
Sm30.25001.00000.25078 (11)0.0126 (3)
F10.7992 (6)1.3218 (8)0.1021 (12)0.036 (2)
F20.1364 (12)1.0714 (12)0.434 (2)0.022 (3)0.50
F2A0.1647 (10)1.0311 (11)0.5020 (18)0.015 (3)0.50
F40.5794 (5)1.3492 (5)0.2658 (10)0.0206 (17)
F50.7578 (8)1.25000.25000.026 (3)
F60.4913 (6)1.2668 (8)0.0159 (10)0.031 (2)
F70.3929 (6)1.0795 (7)0.1559 (11)0.0281 (19)
F80.3206 (16)0.8724 (17)0.090 (3)0.048 (5)0.50
F8A0.2746 (12)0.9183 (12)0.014 (2)0.025 (4)0.50
F30.6360 (12)1.3325 (14)0.2564 (18)0.025 (3)0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Rb10.0614 (11)0.0223 (8)0.0465 (10)0.0032 (7)0.0027 (9)0.0020 (7)
Sm10.0109 (5)0.0178 (5)0.0137 (5)0.0000.0000.0005 (3)
Sm20.0136 (4)0.0744 (6)0.0099 (4)0.0075 (4)0.0006 (3)0.0086 (4)
Sm30.0129 (5)0.0141 (5)0.0108 (5)0.0003 (3)0.0000.000
F10.024 (5)0.041 (5)0.042 (6)0.009 (4)0.016 (4)0.011 (4)
F20.021 (4)0.022 (4)0.021 (4)0.000 (2)0.001 (2)0.001 (2)
F2A0.016 (3)0.015 (3)0.015 (3)0.001 (2)0.002 (2)0.001 (2)
F40.021 (4)0.012 (3)0.030 (5)0.004 (3)0.004 (3)0.001 (3)
F50.012 (5)0.053 (8)0.014 (5)0.0000.0000.002 (5)
F60.017 (4)0.060 (6)0.017 (4)0.002 (4)0.000 (3)0.006 (4)
F70.025 (5)0.030 (4)0.029 (5)0.009 (3)0.011 (4)0.005 (4)
F80.048 (13)0.052 (12)0.045 (13)0.002 (10)0.020 (11)0.001 (10)
F8A0.029 (9)0.018 (7)0.029 (9)0.011 (6)0.001 (7)0.013 (7)
F30.029 (9)0.037 (9)0.007 (7)0.003 (7)0.002 (7)0.003 (6)
Geometric parameters (Å, º) top
Rb1—F2Ai2.795 (14)Sm3—F8vii2.24 (2)
Rb1—F4ii2.814 (7)Sm3—F2vii2.318 (16)
Rb1—F6iii2.983 (9)Sm3—F22.318 (16)
Rb1—F6iv3.018 (9)Sm3—F7vii2.342 (8)
Rb1—F7iv3.034 (9)Sm3—F72.342 (8)
Rb1—F5v3.054 (8)Sm3—F8A2.348 (15)
Rb1—F8Avi3.147 (17)Sm3—F8Avii2.348 (15)
Rb1—F3iii3.247 (16)Sm3—F2Avii2.352 (14)
Rb1—F8Aiv3.252 (17)Sm3—F2A2.352 (14)
Rb1—F73.332 (9)Sm3—F1viii2.568 (9)
Rb1—F2i3.360 (17)Sm3—F1iii2.568 (9)
Rb1—F2vii3.485 (17)F1—Sm1vi2.326 (8)
Sm1—F72.272 (8)F1—Sm3xi2.568 (9)
Sm1—F7ii2.272 (8)F2—F2A0.832 (17)
Sm1—F6ii2.291 (8)F2—Sm2viii2.114 (15)
Sm1—F62.291 (8)F2—Rb1xiii3.360 (17)
Sm1—F1viii2.326 (8)F2—Rb1vii3.485 (17)
Sm1—F1ix2.326 (8)F2A—Sm2viii2.474 (13)
Sm1—F42.427 (8)F2A—Rb1xiii2.795 (14)
Sm1—F4ii2.427 (8)F4—Sm2ii2.438 (7)
Sm1—Sm2ii3.6362 (11)F4—Rb1ii2.814 (7)
Sm1—Sm23.6362 (11)F5—Sm2ii2.301 (7)
Sm1—Sm33.9469 (6)F5—Rb1xiv3.054 (8)
Sm1—Sm3x3.9469 (6)F5—Rb1v3.054 (8)
Sm2—F8iv1.97 (2)F6—Rb1xv2.983 (9)
Sm2—F2xi2.114 (15)F6—Rb1iv3.018 (9)
Sm2—F52.301 (7)F7—Rb1iv3.034 (9)
Sm2—F62.308 (8)F8—F8A1.19 (3)
Sm2—F12.337 (8)F8—F3iii1.44 (3)
Sm2—F32.379 (15)F8—Sm2iv1.97 (2)
Sm2—F42.407 (8)F8A—Sm2iv2.478 (14)
Sm2—F4ii2.438 (7)F8A—Rb1ix3.147 (17)
Sm2—F3xii2.467 (15)F8A—Rb1iv3.252 (17)
Sm2—F2Axi2.474 (13)F3—F8xv1.44 (3)
Sm2—F8Aiv2.478 (14)F3—Sm2xii2.467 (15)
Sm2—Sm2ii3.6089 (15)F3—Sm3xi2.594 (17)
Sm3—F82.24 (2)F3—Rb1xv3.247 (16)
F2Ai—Rb1—F4ii60.3 (3)F4ii—Sm2—F3xii104.4 (4)
F2Ai—Rb1—F6iii84.8 (3)F8iv—Sm2—F2Axi145.7 (7)
F4ii—Rb1—F6iii127.3 (2)F2xi—Sm2—F2Axi18.9 (5)
F2Ai—Rb1—F6iv158.8 (3)F5—Sm2—F2Axi96.7 (4)
F4ii—Rb1—F6iv140.4 (2)F6—Sm2—F2Axi92.7 (4)
F6iii—Rb1—F6iv77.0 (3)F1—Sm2—F2Axi69.0 (4)
F2Ai—Rb1—F7iv136.8 (3)F3—Sm2—F2Axi66.8 (5)
F4ii—Rb1—F7iv91.9 (2)F4—Sm2—F2Axi70.5 (4)
F6iii—Rb1—F7iv136.3 (2)F4ii—Sm2—F2Axi131.0 (4)
F6iv—Rb1—F7iv59.4 (2)F3xii—Sm2—F2Axi116.1 (5)
F2Ai—Rb1—F5v89.1 (3)F8iv—Sm2—F8Aiv28.1 (7)
F4ii—Rb1—F5v134.3 (2)F2xi—Sm2—F8Aiv153.4 (6)
F6iii—Rb1—F5v76.86 (19)F5—Sm2—F8Aiv72.3 (4)
F6iv—Rb1—F5v76.3 (2)F6—Sm2—F8Aiv112.4 (5)
F7iv—Rb1—F5v89.19 (18)F1—Sm2—F8Aiv84.7 (5)
F2Ai—Rb1—F8Avi94.3 (4)F3—Sm2—F8Aiv108.6 (5)
F4ii—Rb1—F8Avi92.4 (3)F4—Sm2—F8Aiv125.5 (4)
F6iii—Rb1—F8Avi131.0 (3)F4ii—Sm2—F8Aiv69.8 (4)
F6iv—Rb1—F8Avi89.6 (3)F3xii—Sm2—F8Aiv63.7 (5)
F7iv—Rb1—F8Avi51.7 (3)F2Axi—Sm2—F8Aiv153.1 (5)
F5v—Rb1—F8Avi54.1 (3)F8iv—Sm2—Sm2ii110.7 (7)
F2Ai—Rb1—F3iii120.4 (4)F2xi—Sm2—Sm2ii116.7 (5)
F4ii—Rb1—F3iii108.3 (4)F5—Sm2—Sm2ii38.4 (2)
F6iii—Rb1—F3iii55.1 (3)F6—Sm2—Sm2ii97.8 (2)
F6iv—Rb1—F3iii56.4 (3)F1—Sm2—Sm2ii117.4 (2)
F7iv—Rb1—F3iii98.5 (3)F3—Sm2—Sm2ii165.7 (4)
F5v—Rb1—F3iii116.8 (3)F4—Sm2—Sm2ii42.17 (17)
F8Avi—Rb1—F3iii145.0 (4)F4ii—Sm2—Sm2ii41.52 (18)
F2Ai—Rb1—F8Aiv82.0 (4)F3xii—Sm2—Sm2ii142.7 (4)
F4ii—Rb1—F8Aiv54.7 (3)F2Axi—Sm2—Sm2ii100.9 (3)
F6iii—Rb1—F8Aiv161.9 (3)F8Aiv—Sm2—Sm2ii85.6 (4)
F6iv—Rb1—F8Aiv112.9 (3)F8—Sm3—F8vii110.8 (12)
F7iv—Rb1—F8Aiv54.8 (3)F8—Sm3—F2vii78.1 (8)
F5v—Rb1—F8Aiv90.5 (3)F8vii—Sm3—F2vii156.5 (6)
F8Avi—Rb1—F8Aiv38.5 (5)F8—Sm3—F2156.5 (6)
F3iii—Rb1—F8Aiv143.0 (4)F8vii—Sm3—F278.1 (8)
F2Ai—Rb1—F799.7 (3)F2vii—Sm3—F2102.5 (9)
F4ii—Rb1—F753.6 (2)F8—Sm3—F7vii84.3 (6)
F6iii—Rb1—F7101.7 (2)F8vii—Sm3—F7vii74.6 (6)
F6iv—Rb1—F794.6 (2)F2vii—Sm3—F7vii128.7 (4)
F7iv—Rb1—F785.8 (2)F2—Sm3—F7vii77.1 (5)
F5v—Rb1—F7170.91 (18)F8—Sm3—F774.6 (6)
F8Avi—Rb1—F7126.5 (3)F8vii—Sm3—F784.3 (6)
F3iii—Rb1—F756.8 (3)F2vii—Sm3—F777.1 (5)
F8Aiv—Rb1—F792.8 (3)F2—Sm3—F7128.7 (4)
F2Ai—Rb1—F2i11.4 (4)F7vii—Sm3—F7142.5 (4)
F4ii—Rb1—F2i55.6 (3)F8—Sm3—F8A29.8 (7)
F6iii—Rb1—F2i82.3 (3)F8vii—Sm3—F8A81.6 (8)
F6iv—Rb1—F2i159.3 (3)F2vii—Sm3—F8A107.4 (6)
F7iv—Rb1—F2i141.3 (3)F2—Sm3—F8A145.0 (6)
F5v—Rb1—F2i99.3 (3)F7vii—Sm3—F8A70.1 (5)
F8Avi—Rb1—F2i104.4 (4)F7—Sm3—F8A76.4 (5)
F3iii—Rb1—F2i110.6 (4)F8—Sm3—F8Avii81.6 (8)
F8Aiv—Rb1—F2i87.2 (4)F8vii—Sm3—F8Avii29.8 (7)
F7—Rb1—F2i89.3 (3)F2vii—Sm3—F8Avii145.0 (6)
F2Ai—Rb1—F2vii88.5 (4)F2—Sm3—F8Avii107.4 (6)
F4ii—Rb1—F2vii86.7 (3)F7vii—Sm3—F8Avii76.4 (5)
F6iii—Rb1—F2vii51.7 (3)F7—Sm3—F8Avii70.1 (5)
F6iv—Rb1—F2vii88.7 (3)F8A—Sm3—F8Avii53.5 (8)
F7iv—Rb1—F2vii124.7 (3)F8—Sm3—F2Avii98.4 (7)
F5v—Rb1—F2vii128.6 (3)F8vii—Sm3—F2Avii144.6 (6)
F8Avi—Rb1—F2vii176.3 (4)F2vii—Sm3—F2Avii20.5 (4)
F3iii—Rb1—F2vii32.8 (4)F2—Sm3—F2Avii82.9 (7)
F8Aiv—Rb1—F2vii139.8 (4)F7vii—Sm3—F2Avii129.4 (4)
F7—Rb1—F2vii50.4 (3)F7—Sm3—F2Avii84.8 (4)
F2i—Rb1—F2vii78.1 (4)F8A—Sm3—F2Avii127.9 (5)
F7—Sm1—F7ii154.5 (4)F8Avii—Sm3—F2Avii154.1 (5)
F7—Sm1—F6ii107.7 (3)F8—Sm3—F2A144.6 (6)
F7ii—Sm1—F6ii82.2 (3)F8vii—Sm3—F2A98.4 (7)
F7—Sm1—F682.2 (3)F2vii—Sm3—F2A82.9 (7)
F7ii—Sm1—F6107.7 (3)F2—Sm3—F2A20.5 (4)
F6ii—Sm1—F6135.3 (4)F7vii—Sm3—F2A84.8 (4)
F7—Sm1—F1viii69.4 (3)F7—Sm3—F2A129.4 (4)
F7ii—Sm1—F1viii90.6 (3)F8A—Sm3—F2A154.1 (5)
F6ii—Sm1—F1viii78.3 (3)F8Avii—Sm3—F2A127.9 (5)
F6—Sm1—F1viii142.5 (3)F2Avii—Sm3—F2A64.1 (7)
F7—Sm1—F1ix90.6 (3)F8—Sm3—F1viii137.1 (6)
F7ii—Sm1—F1ix69.4 (3)F8vii—Sm3—F1viii77.5 (6)
F6ii—Sm1—F1ix142.5 (3)F2vii—Sm3—F1viii81.6 (4)
F6—Sm1—F1ix78.3 (3)F2—Sm3—F1viii65.0 (4)
F1viii—Sm1—F1ix78.1 (5)F7vii—Sm3—F1viii136.6 (3)
F7—Sm1—F4131.8 (3)F7—Sm3—F1viii64.2 (3)
F7ii—Sm1—F473.4 (3)F8A—Sm3—F1viii136.8 (5)
F6ii—Sm1—F470.7 (3)F8Avii—Sm3—F1viii94.8 (4)
F6—Sm1—F471.0 (3)F2Avii—Sm3—F1viii67.5 (4)
F1viii—Sm1—F4146.5 (3)F2A—Sm3—F1viii67.2 (4)
F1ix—Sm1—F4120.6 (3)F8—Sm3—F1iii77.5 (6)
F7—Sm1—F4ii73.4 (3)F8vii—Sm3—F1iii137.1 (6)
F7ii—Sm1—F4ii131.8 (3)F2vii—Sm3—F1iii65.0 (4)
F6ii—Sm1—F4ii71.0 (3)F2—Sm3—F1iii81.6 (4)
F6—Sm1—F4ii70.7 (3)F7vii—Sm3—F1iii64.2 (3)
F1viii—Sm1—F4ii120.6 (3)F7—Sm3—F1iii136.6 (3)
F1ix—Sm1—F4ii146.5 (3)F8A—Sm3—F1iii94.8 (4)
F4—Sm1—F4ii60.4 (3)F8Avii—Sm3—F1iii136.8 (5)
F7—Sm1—Sm2ii107.4 (2)F2Avii—Sm3—F1iii67.2 (4)
F7ii—Sm1—Sm2ii94.8 (2)F2A—Sm3—F1iii67.5 (4)
F6ii—Sm1—Sm2ii37.9 (2)F1viii—Sm3—F1iii125.9 (4)
F6—Sm1—Sm2ii97.4 (2)Sm1vi—F1—Sm2140.8 (4)
F1viii—Sm1—Sm2ii113.8 (3)Sm1vi—F1—Sm3xi107.4 (3)
F1ix—Sm1—Sm2ii160.9 (2)Sm2—F1—Sm3xi101.9 (3)
F4—Sm1—Sm2ii41.74 (17)F2A—F2—Sm2viii105.8 (16)
F4ii—Sm1—Sm2ii41.01 (18)F2A—F2—Sm382.0 (15)
F7—Sm1—Sm294.8 (2)Sm2viii—F2—Sm3118.6 (7)
F7ii—Sm1—Sm2107.4 (2)F2A—F2—Rb1xiii41.7 (14)
F6ii—Sm1—Sm297.4 (2)Sm2viii—F2—Rb1xiii105.3 (6)
F6—Sm1—Sm237.9 (2)Sm3—F2—Rb1xiii116.7 (6)
F1viii—Sm1—Sm2160.9 (2)F2A—F2—Rb1vii138.0 (16)
F1ix—Sm1—Sm2113.8 (3)Sm2viii—F2—Rb1vii104.3 (6)
F4—Sm1—Sm241.01 (18)Sm3—F2—Rb1vii108.2 (6)
F4ii—Sm1—Sm241.74 (17)Rb1xiii—F2—Rb1vii101.9 (4)
Sm2ii—Sm1—Sm259.50 (3)F2—F2A—Sm377.5 (15)
F7—Sm1—Sm331.7 (2)F2—F2A—Sm2viii55.3 (13)
F7ii—Sm1—Sm3124.9 (2)Sm3—F2A—Sm2viii104.3 (5)
F6ii—Sm1—Sm399.7 (2)F2—F2A—Rb1xiii126.8 (16)
F6—Sm1—Sm3108.1 (2)Sm3—F2A—Rb1xiii141.8 (6)
F1viii—Sm1—Sm338.4 (2)Sm2viii—F2A—Rb1xiii113.8 (5)
F1ix—Sm1—Sm378.6 (2)Sm2—F4—Sm197.6 (3)
F4—Sm1—Sm3159.01 (16)Sm2—F4—Sm2ii96.3 (2)
F4ii—Sm1—Sm399.09 (16)Sm1—F4—Sm2ii96.7 (3)
Sm2ii—Sm1—Sm3120.096 (18)Sm2—F4—Rb1ii115.3 (3)
Sm2—Sm1—Sm3126.520 (19)Sm1—F4—Rb1ii121.2 (3)
F7—Sm1—Sm3x124.9 (2)Sm2ii—F4—Rb1ii124.0 (3)
F7ii—Sm1—Sm3x31.7 (2)Sm2—F5—Sm2ii103.3 (4)
F6ii—Sm1—Sm3x108.1 (2)Sm2—F5—Rb1xiv115.93 (8)
F6—Sm1—Sm3x99.7 (2)Sm2ii—F5—Rb1xiv117.52 (8)
F1viii—Sm1—Sm3x78.6 (2)Sm2—F5—Rb1v117.52 (8)
F1ix—Sm1—Sm3x38.4 (2)Sm2ii—F5—Rb1v115.93 (8)
F4—Sm1—Sm3x99.09 (16)Rb1xiv—F5—Rb1v87.1 (3)
F4ii—Sm1—Sm3x159.01 (16)Sm1—F6—Sm2104.5 (3)
Sm2ii—Sm1—Sm3x126.520 (18)Sm1—F6—Rb1xv124.1 (3)
Sm2—Sm1—Sm3x120.096 (18)Sm2—F6—Rb1xv116.0 (3)
Sm3—Sm1—Sm3x101.68 (2)Sm1—F6—Rb1iv107.7 (3)
F8iv—Sm2—F2xi132.6 (8)Sm2—F6—Rb1iv114.9 (3)
F8iv—Sm2—F599.9 (7)Rb1xv—F6—Rb1iv89.1 (2)
F2xi—Sm2—F5115.4 (5)Sm1—F7—Sm3117.6 (3)
F8iv—Sm2—F695.8 (7)Sm1—F7—Rb1iv107.8 (3)
F2xi—Sm2—F680.4 (5)Sm3—F7—Rb1iv114.3 (3)
F5—Sm2—F6136.2 (3)Sm1—F7—Rb1107.8 (3)
F8iv—Sm2—F184.4 (6)Sm3—F7—Rb1112.5 (3)
F2xi—Sm2—F172.4 (5)Rb1iv—F7—Rb194.2 (2)
F5—Sm2—F180.1 (3)F8A—F8—F3iii167 (2)
F6—Sm2—F1142.4 (3)F8A—F8—Sm2iv100.6 (15)
F8iv—Sm2—F383.0 (8)F3iii—F8—Sm2iv91.3 (13)
F2xi—Sm2—F350.0 (6)F8A—F8—Sm380.0 (13)
F5—Sm2—F3146.1 (4)F3iii—F8—Sm386.6 (12)
F6—Sm2—F376.1 (4)Sm2iv—F8—Sm3160.6 (11)
F1—Sm2—F366.5 (5)F8—F8A—Sm370.1 (12)
F8iv—Sm2—F4143.5 (6)F8—F8A—Sm2iv51.3 (11)
F2xi—Sm2—F480.1 (5)Sm3—F8A—Sm2iv118.6 (7)
F5—Sm2—F472.1 (3)F8—F8A—Rb1ix146.3 (15)
F6—Sm2—F471.1 (3)Sm3—F8A—Rb1ix110.2 (6)
F1—Sm2—F4127.0 (3)Sm2iv—F8A—Rb1ix109.0 (5)
F3—Sm2—F4123.8 (4)F8—F8A—Rb1iv108.4 (14)
F8iv—Sm2—F4ii83.0 (6)Sm3—F8A—Rb1iv106.9 (5)
F2xi—Sm2—F4ii136.4 (5)Sm2iv—F8A—Rb1iv107.4 (5)
F5—Sm2—F4ii71.5 (3)Rb1ix—F8A—Rb1iv103.6 (5)
F6—Sm2—F4ii70.2 (3)F8xv—F3—Sm2148.6 (13)
F1—Sm2—F4ii146.3 (3)F8xv—F3—Sm2xii52.9 (10)
F3—Sm2—F4ii141.8 (4)Sm2—F3—Sm2xii128.8 (7)
F4—Sm2—F4ii60.5 (3)F8xv—F3—Sm3xi59.6 (10)
F8iv—Sm2—F3xii35.8 (8)Sm2—F3—Sm3xi100.0 (6)
F2xi—Sm2—F3xii99.1 (6)Sm2xii—F3—Sm3xi110.2 (6)
F5—Sm2—F3xii133.7 (4)F8xv—F3—Rb1xv104.0 (11)
F6—Sm2—F3xii76.7 (4)Sm2—F3—Rb1xv105.2 (5)
F1—Sm2—F3xii82.3 (5)Sm2xii—F3—Rb1xv103.2 (5)
F3—Sm2—F3xii49.3 (7)Sm3xi—F3—Rb1xv108.3 (5)
F4—Sm2—F3xii147.5 (4)
Symmetry codes: (i) x+1/2, y, z+1; (ii) x, y+5/2, z+1/2; (iii) x+1, y1/2, z+1/2; (iv) x+1, y+2, z; (v) x+3/2, y+2, z; (vi) x+1/2, y, z; (vii) x+1/2, y+2, z; (viii) x1/2, y+5/2, z+1/2; (ix) x1/2, y, z; (x) x+1/2, y+1/2, z+1/2; (xi) x+1/2, y+5/2, z1/2; (xii) x, y+5/2, z1/2; (xiii) x1/2, y, z+1; (xiv) x+3/2, y+1/2, z+1/2; (xv) x+1, y+1/2, z1/2.
(CsGd2F7) top
Crystal data top
CsF7Gd2Dx = 5.637 Mg m3
Mr = 580.41Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, PnnaCell parameters from 7461 reflections
a = 13.828 (3) Åθ = 1.6–26.0°
b = 12.415 (3) ŵ = 24.53 mm1
c = 7.9681 (16) ÅT = 293 K
V = 1367.9 (5) Å3Prism, colorless
Z = 80.31 × 0.27 × 0.24 mm
F(000) = 1968
Data collection top
Rigaku AFC8S
diffractometer
1249 independent reflections
Radiation source: fine-focus sealed tube1227 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.102
Detector resolution: 14.6199 pixels mm-1θmax = 25.3°, θmin = 3.0°
ω scansh = 1616
Absorption correction: multi-scan
REQAB, CrystalClear
k = 1414
Tmin = 0.387, Tmax = 1.000l = 99
10980 measured reflections
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)] = 0.053 w = 1/[σ2(Fo2) + (0.0068P)2 + 200.3173P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.114(Δ/σ)max < 0.001
S = 1.10Δρmax = 1.96 e Å3
1249 reflectionsΔρmin = 2.93 e Å3
116 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
42 restraintsExtinction coefficient: 0.00099 (9)
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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)
Cs10.58148 (10)0.92205 (10)0.22867 (17)0.0270 (4)
Gd10.43090 (8)1.25000.25000.0104 (4)
Gd20.65812 (6)1.26449 (9)0.02418 (11)0.0170 (3)
Gd30.25001.00000.25128 (14)0.0090 (4)
F10.8022 (8)1.3178 (10)0.0933 (16)0.028 (3)
F20.1392 (16)1.079 (2)0.426 (3)0.021 (5)0.50
F2A0.1660 (15)1.0415 (16)0.494 (3)0.013 (4)0.50
F30.6428 (16)1.3217 (19)0.255 (3)0.019 (5)0.50
F40.5835 (8)1.3460 (9)0.2632 (14)0.017 (2)
F50.7561 (11)1.25000.25000.017 (3)
F60.4955 (7)1.2604 (9)0.0128 (14)0.017 (2)
F70.3924 (8)1.0813 (11)0.1681 (15)0.029 (3)
F80.314 (2)0.879 (2)0.083 (4)0.041 (7)0.50
F8A0.2787 (16)0.9179 (17)0.006 (3)0.017 (4)0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cs10.0408 (8)0.0103 (7)0.0298 (7)0.0005 (5)0.0017 (6)0.0011 (5)
Gd10.0066 (6)0.0179 (7)0.0068 (6)0.0000.0000.0015 (5)
Gd20.0076 (4)0.0387 (6)0.0046 (5)0.0043 (4)0.0005 (3)0.0046 (4)
Gd30.0074 (6)0.0148 (7)0.0048 (6)0.0003 (4)0.0000.000
F10.018 (6)0.034 (7)0.033 (7)0.004 (5)0.013 (5)0.009 (6)
F20.015 (8)0.032 (9)0.016 (8)0.002 (7)0.003 (7)0.003 (8)
F2A0.014 (6)0.009 (6)0.015 (6)0.000 (4)0.003 (4)0.002 (5)
F30.023 (8)0.024 (8)0.010 (8)0.003 (7)0.006 (7)0.002 (7)
F40.020 (5)0.010 (5)0.021 (5)0.006 (4)0.003 (4)0.000 (4)
F50.016 (5)0.024 (5)0.012 (5)0.0000.0000.001 (4)
F60.010 (3)0.027 (4)0.015 (4)0.008 (3)0.001 (3)0.001 (4)
F70.022 (6)0.043 (8)0.022 (6)0.005 (6)0.008 (5)0.002 (6)
F80.057 (19)0.041 (17)0.027 (14)0.011 (15)0.009 (14)0.011 (13)
F8A0.021 (8)0.016 (8)0.013 (8)0.009 (7)0.001 (7)0.002 (7)
Geometric parameters (Å, º) top
Cs1—F4i2.880 (11)Gd3—F22.29 (2)
Cs1—F2Aii2.91 (2)Gd3—F2vii2.29 (2)
Cs1—F6iii3.037 (11)Gd3—F7vii2.310 (12)
Cs1—F6iv3.067 (11)Gd3—F72.310 (12)
Cs1—F5v3.104 (11)Gd3—F2Avii2.31 (2)
Cs1—F7iii3.182 (12)Gd3—F2A2.31 (2)
Cs1—F8Avi3.25 (2)Gd3—F8A2.32 (2)
Cs1—F8Aiii3.29 (2)Gd3—F8Avii2.32 (2)
Cs1—F73.313 (13)Gd3—F3ix2.66 (2)
Cs1—F3iv3.34 (2)Gd3—F3iv2.66 (2)
Cs1—F2vii3.43 (2)F1—Gd1vi2.331 (11)
Cs1—F2ii3.46 (3)F1—Gd3xi2.678 (12)
Gd1—F72.257 (13)F1—Cs1xiii3.564 (14)
Gd1—F7i2.257 (13)F2—F2A0.81 (3)
Gd1—F6i2.280 (11)F2—Gd2ix2.12 (2)
Gd1—F62.280 (11)F2—Cs1vii3.43 (2)
Gd1—F1viii2.331 (11)F2—Cs1xiv3.46 (3)
Gd1—F1ix2.331 (11)F2A—Gd2ix2.42 (2)
Gd1—F42.426 (11)F2A—Cs1xiv2.91 (2)
Gd1—F4i2.426 (11)F3—F8xv1.59 (3)
Gd1—Gd23.6252 (14)F3—Gd2xii2.40 (2)
Gd1—Gd2i3.6252 (14)F3—Gd3xi2.66 (2)
Gd1—Gd33.9863 (9)F3—Cs1xv3.34 (2)
Gd1—Gd3x3.9863 (9)F4—Gd2i2.412 (11)
Gd2—F8iii2.02 (3)F4—Cs1i2.880 (11)
Gd2—F2xi2.12 (2)F5—Gd2i2.260 (9)
Gd2—F52.260 (9)F5—Cs1xiii3.104 (11)
Gd2—F62.268 (10)F5—Cs1v3.104 (11)
Gd2—F12.299 (11)F6—Cs1iii3.037 (11)
Gd2—F32.35 (2)F6—Cs1xv3.067 (11)
Gd2—F42.391 (10)F7—Cs1iii3.182 (12)
Gd2—F3xii2.40 (2)F8—F8A0.98 (3)
Gd2—F4i2.412 (11)F8—F3iv1.59 (3)
Gd2—F2Axi2.42 (2)F8—Gd2iii2.02 (3)
Gd2—F8Aiii2.43 (2)F8—Cs1iii3.79 (3)
Gd2—Gd2i3.6167 (19)F8A—Gd2iii2.43 (2)
Gd3—F82.19 (3)F8A—Cs1viii3.25 (2)
Gd3—F8vii2.19 (3)F8A—Cs1iii3.29 (2)
F4i—Cs1—F2Aii57.9 (4)F5—Gd2—F2Axi97.5 (6)
F4i—Cs1—F6iii139.6 (3)F6—Gd2—F2Axi93.1 (6)
F2Aii—Cs1—F6iii162.2 (4)F1—Gd2—F2Axi68.6 (6)
F4i—Cs1—F6iv130.0 (3)F3—Gd2—F2Axi67.0 (8)
F2Aii—Cs1—F6iv87.9 (5)F4—Gd2—F2Axi71.2 (6)
F6iii—Cs1—F6iv76.7 (3)F3xii—Gd2—F2Axi111.0 (8)
F4i—Cs1—F5v132.8 (3)F4i—Gd2—F2Axi130.9 (6)
F2Aii—Cs1—F5v91.1 (4)F8iii—Gd2—F8Aiii23.2 (9)
F6iii—Cs1—F5v76.8 (2)F2xi—Gd2—F8Aiii151.5 (8)
F6iv—Cs1—F5v76.4 (2)F5—Gd2—F8Aiii76.0 (5)
F4i—Cs1—F7iii92.0 (3)F6—Gd2—F8Aiii109.1 (6)
F2Aii—Cs1—F7iii135.7 (5)F1—Gd2—F8Aiii86.1 (6)
F6iii—Cs1—F7iii57.8 (3)F3—Gd2—F8Aiii104.9 (8)
F6iv—Cs1—F7iii134.3 (3)F4—Gd2—F8Aiii126.7 (6)
F5v—Cs1—F7iii87.9 (2)F3xii—Gd2—F8Aiii64.1 (7)
F4i—Cs1—F8Avi91.1 (4)F4i—Gd2—F8Aiii70.5 (6)
F2Aii—Cs1—F8Avi94.9 (6)F2Axi—Gd2—F8Aiii154.6 (7)
F6iii—Cs1—F8Avi88.4 (4)F8iii—Gd2—Gd2i109.5 (8)
F6iv—Cs1—F8Avi130.3 (4)F2xi—Gd2—Gd2i117.4 (7)
F5v—Cs1—F8Avi54.0 (4)F5—Gd2—Gd2i36.8 (3)
F7iii—Cs1—F8Avi50.4 (4)F6—Gd2—Gd2i97.3 (3)
F4i—Cs1—F8Aiii53.4 (4)F1—Gd2—Gd2i115.7 (3)
F2Aii—Cs1—F8Aiii82.3 (6)F3—Gd2—Gd2i167.0 (6)
F6iii—Cs1—F8Aiii110.5 (4)F4—Gd2—Gd2i41.4 (3)
F6iv—Cs1—F8Aiii164.0 (4)F3xii—Gd2—Gd2i147.4 (5)
F5v—Cs1—F8Aiii91.1 (4)F4i—Gd2—Gd2i40.9 (2)
F7iii—Cs1—F8Aiii53.5 (4)F2Axi—Gd2—Gd2i101.4 (5)
F8Avi—Cs1—F8Aiii39.0 (7)F8Aiii—Gd2—Gd2i88.1 (5)
F4i—Cs1—F754.2 (3)F8—Gd3—F8vii104.8 (15)
F2Aii—Cs1—F797.1 (5)F8—Gd3—F2158.6 (10)
F6iii—Cs1—F794.9 (3)F8vii—Gd3—F279.1 (11)
F6iv—Cs1—F7102.4 (3)F8—Gd3—F2vii79.1 (11)
F5v—Cs1—F7171.7 (3)F8vii—Gd3—F2vii158.6 (10)
F7iii—Cs1—F787.3 (3)F2—Gd3—F2vii105.2 (13)
F8Avi—Cs1—F7126.2 (4)F8—Gd3—F7vii82.4 (9)
F8Aiii—Cs1—F791.4 (4)F8vii—Gd3—F7vii77.4 (9)
F4i—Cs1—F3iv112.4 (5)F2—Gd3—F7vii77.9 (7)
F2Aii—Cs1—F3iv122.3 (6)F2vii—Gd3—F7vii124.0 (7)
F6iii—Cs1—F3iv54.4 (4)F8—Gd3—F777.4 (9)
F6iv—Cs1—F3iv53.8 (4)F8vii—Gd3—F782.4 (9)
F5v—Cs1—F3iv114.4 (4)F2—Gd3—F7124.0 (7)
F7iii—Cs1—F3iv97.9 (4)F2vii—Gd3—F777.9 (7)
F8Avi—Cs1—F3iv142.3 (5)F7vii—Gd3—F7146.6 (6)
F8Aiii—Cs1—F3iv142.2 (5)F8—Gd3—F2Avii99.1 (10)
F7—Cs1—F3iv59.7 (4)F8vii—Gd3—F2Avii149.7 (9)
F4i—Cs1—F2vii90.1 (5)F2—Gd3—F2Avii85.6 (10)
F2Aii—Cs1—F2vii90.7 (5)F2vii—Gd3—F2Avii20.1 (6)
F6iii—Cs1—F2vii86.9 (5)F7vii—Gd3—F2Avii124.8 (6)
F6iv—Cs1—F2vii51.8 (4)F7—Gd3—F2Avii84.8 (6)
F5v—Cs1—F2vii128.1 (4)F8—Gd3—F2A149.7 (9)
F7iii—Cs1—F2vii123.7 (4)F8vii—Gd3—F2A99.1 (10)
F8Avi—Cs1—F2vii174.1 (5)F2—Gd3—F2A20.1 (6)
F8Aiii—Cs1—F2vii140.4 (5)F2vii—Gd3—F2A85.6 (10)
F7—Cs1—F2vii50.7 (4)F7vii—Gd3—F2A84.8 (6)
F3iv—Cs1—F2vii32.6 (6)F7—Gd3—F2A124.8 (6)
F4i—Cs1—F2ii54.5 (4)F2Avii—Gd3—F2A66.6 (11)
F2Aii—Cs1—F2ii10.5 (5)F8—Gd3—F8A24.9 (8)
F6iii—Cs1—F2ii161.7 (4)F8vii—Gd3—F8A80.2 (10)
F6iv—Cs1—F2ii85.0 (4)F2—Gd3—F8A146.9 (8)
F5v—Cs1—F2ii100.1 (4)F2vii—Gd3—F8A103.5 (9)
F7iii—Cs1—F2ii140.4 (5)F7vii—Gd3—F8A72.6 (6)
F8Avi—Cs1—F2ii104.4 (6)F7—Gd3—F8A78.1 (6)
F8Aiii—Cs1—F2ii87.4 (5)F2Avii—Gd3—F8A123.7 (8)
F7—Cs1—F2ii87.9 (4)F2A—Gd3—F8A157.0 (7)
F3iv—Cs1—F2ii113.1 (5)F8—Gd3—F8Avii80.2 (10)
F2vii—Cs1—F2ii81.0 (6)F8vii—Gd3—F8Avii24.9 (8)
F7—Gd1—F7i152.7 (6)F2—Gd3—F8Avii103.5 (9)
F7—Gd1—F6i107.8 (4)F2vii—Gd3—F8Avii146.9 (8)
F7i—Gd1—F6i83.1 (4)F7vii—Gd3—F8Avii78.1 (6)
F7—Gd1—F683.1 (4)F7—Gd3—F8Avii72.6 (6)
F7i—Gd1—F6107.8 (4)F2Avii—Gd3—F8Avii157.0 (7)
F6i—Gd1—F6133.8 (5)F2A—Gd3—F8Avii123.7 (8)
F7—Gd1—F1viii90.0 (4)F8A—Gd3—F8Avii56.2 (11)
F7i—Gd1—F1viii68.9 (4)F8—Gd3—F3ix141.1 (9)
F6i—Gd1—F1viii144.2 (4)F8vii—Gd3—F3ix36.6 (9)
F6—Gd1—F1viii77.7 (4)F2—Gd3—F3ix44.4 (8)
F7—Gd1—F1ix68.9 (4)F2vii—Gd3—F3ix137.7 (8)
F7i—Gd1—F1ix90.0 (4)F7vii—Gd3—F3ix83.3 (6)
F6i—Gd1—F1ix77.7 (4)F7—Gd3—F3ix96.1 (6)
F6—Gd1—F1ix144.2 (4)F2Avii—Gd3—F3ix118.7 (7)
F1viii—Gd1—F1ix80.5 (7)F2A—Gd3—F3ix63.5 (7)
F7—Gd1—F4132.3 (4)F8A—Gd3—F3ix116.2 (7)
F7i—Gd1—F474.7 (4)F8Avii—Gd3—F3ix61.5 (7)
F6i—Gd1—F469.3 (4)F8—Gd3—F3iv36.6 (9)
F6—Gd1—F470.8 (4)F8vii—Gd3—F3iv141.1 (9)
F1viii—Gd1—F4120.6 (4)F2—Gd3—F3iv137.7 (8)
F1ix—Gd1—F4144.9 (4)F2vii—Gd3—F3iv44.4 (8)
F7—Gd1—F4i74.7 (4)F7vii—Gd3—F3iv96.1 (6)
F7i—Gd1—F4i132.3 (4)F7—Gd3—F3iv83.3 (6)
F6i—Gd1—F4i70.8 (4)F2Avii—Gd3—F3iv63.5 (7)
F6—Gd1—F4i69.3 (4)F2A—Gd3—F3iv118.7 (7)
F1viii—Gd1—F4i144.9 (4)F8A—Gd3—F3iv61.5 (7)
F1ix—Gd1—F4i120.6 (4)F8Avii—Gd3—F3iv116.2 (7)
F4—Gd1—F4i59.1 (5)F3ix—Gd3—F3iv177.7 (9)
F7—Gd1—Gd296.1 (3)Gd2—F1—Gd1vi140.9 (6)
F7i—Gd1—Gd2107.6 (3)Gd2—F1—Gd3xi101.4 (4)
F6i—Gd1—Gd296.8 (3)Gd1vi—F1—Gd3xi105.2 (4)
F6—Gd1—Gd237.0 (3)Gd2—F1—Cs1xiii99.4 (4)
F1viii—Gd1—Gd2112.2 (3)Gd1vi—F1—Cs1xiii102.9 (4)
F1ix—Gd1—Gd2161.0 (3)Gd3xi—F1—Cs1xiii101.1 (4)
F4—Gd1—Gd240.8 (2)F2A—F2—Gd2ix103 (2)
F4i—Gd1—Gd241.3 (3)F2A—F2—Gd382 (2)
F7—Gd1—Gd2i107.6 (3)Gd2ix—F2—Gd3122.4 (10)
F7i—Gd1—Gd2i96.1 (3)F2A—F2—Cs1vii136 (3)
F6i—Gd1—Gd2i37.0 (3)Gd2ix—F2—Cs1vii106.4 (9)
F6—Gd1—Gd2i96.8 (3)Gd3—F2—Cs1vii108.4 (8)
F1viii—Gd1—Gd2i161.0 (3)F2A—F2—Cs1xiv41 (2)
F1ix—Gd1—Gd2i112.2 (3)Gd2ix—F2—Cs1xiv104.5 (8)
F4—Gd1—Gd2i41.3 (3)Gd3—F2—Cs1xiv113.4 (9)
F4i—Gd1—Gd2i40.8 (2)Cs1vii—F2—Cs1xiv99.0 (6)
Gd2—Gd1—Gd2i59.84 (4)F2—F2A—Gd378 (2)
F7—Gd1—Gd329.6 (3)F2—F2A—Gd2ix58 (2)
F7i—Gd1—Gd3125.0 (3)Gd3—F2A—Gd2ix109.0 (8)
F6i—Gd1—Gd3101.5 (3)F2—F2A—Cs1xiv129 (2)
F6—Gd1—Gd3107.0 (3)Gd3—F2A—Cs1xiv136.4 (8)
F1viii—Gd1—Gd378.7 (3)Gd2ix—F2A—Cs1xiv114.5 (7)
F1ix—Gd1—Gd340.4 (3)F8xv—F3—Gd2150.4 (16)
F4—Gd1—Gd3158.2 (2)F8xv—F3—Gd2xii56.4 (12)
F4i—Gd1—Gd399.4 (2)Gd2—F3—Gd2xii134.7 (10)
Gd2—Gd1—Gd3125.72 (2)F8xv—F3—Gd3xi55.4 (12)
Gd2i—Gd1—Gd3120.26 (2)Gd2—F3—Gd3xi100.5 (8)
F7—Gd1—Gd3x125.0 (3)Gd2xii—F3—Gd3xi109.8 (8)
F7i—Gd1—Gd3x29.6 (3)F8xv—F3—Cs1xv98.8 (15)
F6i—Gd1—Gd3x107.0 (3)Gd2—F3—Cs1xv103.4 (7)
F6—Gd1—Gd3x101.5 (3)Gd2xii—F3—Cs1xv102.4 (7)
F1viii—Gd1—Gd3x40.4 (3)Gd3xi—F3—Cs1xv102.0 (7)
F1ix—Gd1—Gd3x78.7 (3)Gd2—F4—Gd2i97.7 (4)
F4—Gd1—Gd3x99.4 (2)Gd2—F4—Gd197.6 (4)
F4i—Gd1—Gd3x158.2 (2)Gd2i—F4—Gd197.1 (4)
Gd2—Gd1—Gd3x120.26 (2)Gd2—F4—Cs1i116.4 (4)
Gd2i—Gd1—Gd3x125.72 (2)Gd2i—F4—Cs1i123.9 (4)
Gd3—Gd1—Gd3x102.27 (3)Gd1—F4—Cs1i118.9 (4)
F8iii—Gd2—F2xi132.9 (11)Gd2i—F5—Gd2106.3 (6)
F8iii—Gd2—F598.7 (9)Gd2i—F5—Cs1xiii116.42 (11)
F2xi—Gd2—F5116.3 (7)Gd2—F5—Cs1xiii115.00 (11)
F8iii—Gd2—F696.7 (10)Gd2i—F5—Cs1v115.00 (11)
F2xi—Gd2—F681.4 (7)Gd2—F5—Cs1v116.42 (11)
F5—Gd2—F6134.1 (4)Cs1xiii—F5—Cs1v87.3 (4)
F8iii—Gd2—F185.1 (9)Gd2—F6—Gd1105.7 (4)
F2xi—Gd2—F172.0 (7)Gd2—F6—Cs1iii116.0 (4)
F5—Gd2—F180.1 (4)Gd1—F6—Cs1iii109.9 (4)
F6—Gd2—F1144.4 (4)Gd2—F6—Cs1xv114.6 (4)
F8iii—Gd2—F383.3 (10)Gd1—F6—Cs1xv121.2 (4)
F2xi—Gd2—F350.1 (9)Cs1iii—F6—Cs1xv89.2 (3)
F5—Gd2—F3146.5 (6)Gd1—F7—Gd3121.6 (5)
F6—Gd2—F378.1 (6)Gd1—F7—Cs1iii105.8 (4)
F1—Gd2—F366.7 (6)Gd3—F7—Cs1iii112.1 (4)
F8iii—Gd2—F4142.7 (8)Gd1—F7—Cs1109.0 (4)
F2xi—Gd2—F481.5 (7)Gd3—F7—Cs1111.7 (5)
F5—Gd2—F470.0 (4)Cs1iii—F7—Cs192.7 (3)
F6—Gd2—F471.6 (4)F8A—F8—F3iv172 (3)
F1—Gd2—F4125.2 (4)F8A—F8—Gd2iii103 (2)
F3—Gd2—F4126.1 (6)F3iv—F8—Gd2iii82.6 (15)
F8iii—Gd2—F3xii41.0 (10)F8A—F8—Gd385 (2)
F2xi—Gd2—F3xii93.9 (9)F3iv—F8—Gd388.0 (15)
F5—Gd2—F3xii136.6 (5)Gd2iii—F8—Gd3160.2 (15)
F6—Gd2—F3xii77.7 (6)F8A—F8—Cs1iii53 (2)
F1—Gd2—F3xii80.9 (6)F3iv—F8—Cs1iii132.7 (17)
F3—Gd2—F3xii44.0 (10)Gd2iii—F8—Cs1iii102.9 (10)
F4—Gd2—F3xii149.3 (6)Gd3—F8—Cs1iii96.3 (9)
F8iii—Gd2—F4i83.0 (8)F8—F8A—Gd370 (2)
F2xi—Gd2—F4i137.0 (7)F8—F8A—Gd2iii54 (2)
F5—Gd2—F4i69.6 (4)Gd3—F8A—Gd2iii121.5 (10)
F6—Gd2—F4i69.8 (4)F8—F8A—Cs1viii144 (2)
F1—Gd2—F4i145.2 (4)Gd3—F8A—Cs1viii109.3 (7)
F3—Gd2—F4i143.1 (6)Gd2iii—F8A—Cs1viii106.5 (7)
F4—Gd2—F4i59.8 (5)F8—F8A—Cs1iii113 (2)
F3xii—Gd2—F4i109.6 (6)Gd3—F8A—Cs1iii108.1 (7)
F8iii—Gd2—F2Axi146.0 (9)Gd2iii—F8A—Cs1iii108.6 (7)
F2xi—Gd2—F2Axi18.9 (7)Cs1viii—F8A—Cs1iii100.9 (6)
Symmetry codes: (i) x, y+5/2, z+1/2; (ii) x+1/2, y, z+1; (iii) x+1, y+2, z; (iv) x+1, y1/2, z+1/2; (v) x+3/2, y+2, z; (vi) x+1/2, y, z; (vii) x+1/2, y+2, z; (viii) x1/2, y, z; (ix) x1/2, y+5/2, z+1/2; (x) x+1/2, y+1/2, z+1/2; (xi) x+1/2, y+5/2, z1/2; (xii) x, y+5/2, z1/2; (xiii) x+3/2, y+1/2, z+1/2; (xiv) x1/2, y, z+1; (xv) x+1, y+1/2, z1/2.
(KY3F10) top
Crystal data top
F10KY3Mo Kα radiation, λ = 0.71073 Å
Mr = 495.83Cell parameters from 3620 reflections
Cubic, Fm3mθ = 2.6–26.6°
a = 11.5439 (13) ŵ = 23.12 mm1
V = 1538.4 (3) Å3T = 293 K
Z = 8Block, colorless
F(000) = 18080.15 × 0.15 × 0.12 mm
Dx = 4.282 Mg m3
Data collection top
Rigaku AFC8S
diffractometer
115 independent reflections
Radiation source: fine-focus sealed tube114 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.059
Detector resolution: 0 pixels mm-1θmax = 26.6°, θmin = 3.1°
ω scansh = 1414
Absorption correction: multi-scan
REQAB, CrystalClear
k = 1414
Tmin = 0.801, Tmax = 1.000l = 1414
3620 measured reflections
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)] = 0.025 w = 1/[σ2(Fo2) + (0.0187P)2 + 35.2674P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.055(Δ/σ)max < 0.001
S = 1.19Δρmax = 0.55 e Å3
115 reflectionsΔρmin = 0.53 e Å3
13 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.00104 (13)
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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
K10.25000.25000.25000.0196 (9)
Y10.24082 (8)0.00000.00000.0116 (4)
F10.1121 (3)0.1121 (3)0.1121 (3)0.0150 (11)
F20.50000.1659 (3)0.1659 (3)0.0206 (10)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
K10.0196 (9)0.0196 (9)0.0196 (9)0.0000.0000.000
Y10.0115 (6)0.0117 (5)0.0117 (5)0.0000.0000.000
F10.0150 (11)0.0150 (11)0.0150 (11)0.0013 (11)0.0013 (11)0.0013 (11)
F20.026 (2)0.0180 (14)0.0180 (14)0.0000.0000.0062 (18)
Geometric parameters (Å, º) top
K1—F12.757 (5)Y1—F2xiv2.1973 (12)
K1—F1i2.757 (5)Y1—F1xv2.3573 (15)
K1—F1ii2.757 (5)Y1—F12.3573 (15)
K1—F1iii2.757 (5)Y1—F1xvi2.3573 (15)
K1—F2iv3.1957 (18)Y1—F1xvii2.3573 (15)
K1—F2v3.1957 (18)Y1—Y1xviii3.9314 (14)
K1—F2vi3.1957 (18)Y1—Y1xix3.9314 (14)
K1—F2vii3.1957 (18)Y1—Y1xx3.9314 (14)
K1—F2viii3.1957 (18)Y1—Y1xxi3.9314 (14)
K1—F2ix3.1957 (18)F1—Y1xxi2.3573 (15)
K1—F2x3.1957 (18)F1—Y1xx2.3573 (15)
K1—F2xi3.1957 (18)F2—Y1xxii2.1973 (12)
Y1—F2xi2.1973 (12)F2—Y1xxiii2.1973 (12)
Y1—F2xii2.1973 (12)F2—K1xxiv3.1957 (18)
Y1—F2xiii2.1973 (12)F2—K1xxv3.1957 (18)
F1—K1—F1i109.5F2xi—Y1—F1xv141.94 (5)
F1—K1—F1ii109.5F2xii—Y1—F1xv141.94 (5)
F1i—K1—F1ii109.5F2xiii—Y1—F1xv80.23 (13)
F1—K1—F1iii109.5F2xiv—Y1—F1xv80.23 (13)
F1i—K1—F1iii109.5F2xi—Y1—F180.23 (13)
F1ii—K1—F1iii109.5F2xii—Y1—F180.23 (13)
F1—K1—F2iv150.70 (7)F2xiii—Y1—F1141.94 (5)
F1i—K1—F2iv99.83 (7)F2xiv—Y1—F1141.94 (5)
F1ii—K1—F2iv58.574 (19)F1xv—Y1—F1101.8 (2)
F1iii—K1—F2iv58.574 (19)F2xi—Y1—F1xvi141.94 (5)
F1—K1—F2v150.70 (7)F2xii—Y1—F1xvi80.23 (13)
F1i—K1—F2v58.574 (19)F2xiii—Y1—F1xvi80.23 (13)
F1ii—K1—F2v58.574 (19)F2xiv—Y1—F1xvi141.94 (5)
F1iii—K1—F2v99.83 (7)F1xv—Y1—F1xvi66.58 (13)
F2iv—K1—F2v50.16 (11)F1—Y1—F1xvi66.58 (13)
F1—K1—F2vi150.70 (7)F2xi—Y1—F1xvii80.23 (13)
F1i—K1—F2vi58.574 (19)F2xii—Y1—F1xvii141.94 (5)
F1ii—K1—F2vi99.83 (7)F2xiii—Y1—F1xvii141.94 (5)
F1iii—K1—F2vi58.574 (19)F2xiv—Y1—F1xvii80.23 (13)
F2iv—K1—F2vi50.16 (11)F1xv—Y1—F1xvii66.58 (13)
F2v—K1—F2vi50.16 (11)F1—Y1—F1xvii66.58 (13)
F1—K1—F2vii58.574 (19)F1xvi—Y1—F1xvii101.8 (2)
F1i—K1—F2vii58.574 (19)F2xi—Y1—Y1xviii164.33 (10)
F1ii—K1—F2vii150.70 (7)F2xii—Y1—Y1xviii110.27 (7)
F1iii—K1—F2vii99.83 (7)F2xiii—Y1—Y1xviii74.33 (10)
F2iv—K1—F2vii144.64 (9)F2xiv—Y1—Y1xviii110.27 (7)
F2v—K1—F2vii117.15 (4)F1xv—Y1—Y1xviii33.50 (5)
F2vi—K1—F2vii95.29 (3)F1—Y1—Y1xviii86.70 (10)
F1—K1—F2viii58.574 (19)F1xvi—Y1—Y1xviii33.50 (5)
F1i—K1—F2viii58.574 (19)F1xvii—Y1—Y1xviii86.70 (10)
F1ii—K1—F2viii99.83 (7)F2xi—Y1—Y1xix110.27 (7)
F1iii—K1—F2viii150.70 (7)F2xii—Y1—Y1xix164.33 (10)
F2iv—K1—F2viii144.64 (9)F2xiii—Y1—Y1xix110.27 (7)
F2v—K1—F2viii95.29 (3)F2xiv—Y1—Y1xix74.33 (10)
F2vi—K1—F2viii117.15 (4)F1xv—Y1—Y1xix33.50 (5)
F2vii—K1—F2viii50.86 (13)F1—Y1—Y1xix86.70 (10)
F1—K1—F2ix58.574 (19)F1xvi—Y1—Y1xix86.70 (10)
F1i—K1—F2ix99.83 (7)F1xvii—Y1—Y1xix33.50 (5)
F1ii—K1—F2ix150.70 (7)Y1xviii—Y1—Y1xix60.0
F1iii—K1—F2ix58.574 (19)F2xi—Y1—Y1xx74.33 (10)
F2iv—K1—F2ix117.15 (4)F2xii—Y1—Y1xx110.27 (7)
F2v—K1—F2ix144.64 (9)F2xiii—Y1—Y1xx164.33 (10)
F2vi—K1—F2ix95.29 (3)F2xiv—Y1—Y1xx110.27 (7)
F2vii—K1—F2ix50.16 (11)F1xv—Y1—Y1xx86.70 (10)
F2viii—K1—F2ix95.29 (3)F1—Y1—Y1xx33.50 (5)
F1—K1—F2x58.574 (19)F1xvi—Y1—Y1xx86.70 (10)
F1i—K1—F2x99.83 (7)F1xvii—Y1—Y1xx33.50 (5)
F1ii—K1—F2x58.574 (19)Y1xviii—Y1—Y1xx90.0
F1iii—K1—F2x150.70 (7)Y1xix—Y1—Y1xx60.0
F2iv—K1—F2x117.15 (4)F2xi—Y1—Y1xxi110.27 (7)
F2v—K1—F2x95.29 (3)F2xii—Y1—Y1xxi74.33 (10)
F2vi—K1—F2x144.64 (9)F2xiii—Y1—Y1xxi110.27 (7)
F2vii—K1—F2x95.29 (3)F2xiv—Y1—Y1xxi164.33 (10)
F2viii—K1—F2x50.16 (11)F1xv—Y1—Y1xxi86.70 (10)
F2ix—K1—F2x117.15 (4)F1—Y1—Y1xxi33.50 (5)
F1—K1—F2xi58.574 (19)F1xvi—Y1—Y1xxi33.50 (5)
F1i—K1—F2xi150.70 (7)F1xvii—Y1—Y1xxi86.70 (10)
F1ii—K1—F2xi99.83 (7)Y1xviii—Y1—Y1xxi60.0
F1iii—K1—F2xi58.574 (19)Y1xix—Y1—Y1xxi90.0
F2iv—K1—F2xi95.29 (3)Y1xx—Y1—Y1xxi60.0
F2v—K1—F2xi144.64 (9)Y1xxi—F1—Y1xx113.00 (10)
F2vi—K1—F2xi117.15 (4)Y1xxi—F1—Y1113.00 (10)
F2vii—K1—F2xi95.29 (3)Y1xx—F1—Y1113.00 (10)
F2viii—K1—F2xi117.15 (4)Y1xxi—F1—K1105.66 (12)
F2ix—K1—F2xi50.86 (13)Y1xx—F1—K1105.66 (12)
F2x—K1—F2xi95.29 (3)Y1—F1—K1105.66 (12)
F2xi—Y1—F2xii76.11 (9)Y1xxii—F2—Y1xxiii148.7 (2)
F2xi—Y1—F2xiii121.3 (2)Y1xxii—F2—K1xxiv96.66 (3)
F2xii—Y1—F2xiii76.11 (9)Y1xxiii—F2—K1xxiv96.66 (3)
F2xi—Y1—F2xiv76.11 (9)Y1xxii—F2—K1xxv96.66 (3)
F2xii—Y1—F2xiv121.3 (2)Y1xxiii—F2—K1xxv96.66 (3)
F2xiii—Y1—F2xiv76.11 (9)K1xxiv—F2—K1xxv129.14 (13)
Symmetry codes: (i) x, y1/2, z1/2; (ii) x1/2, y, z1/2; (iii) x1/2, y1/2, z; (iv) x1, y1/2, z1/2; (v) y1/2, z1/2, x1; (vi) z1/2, x1, y1/2; (vii) x1/2, y1/2, z; (viii) x+1/2, y, z1/2; (ix) y, z1/2, x+1/2; (x) z, x1/2, y1/2; (xi) y1/2, z, x1/2; (xii) z1/2, x+1/2, y; (xiii) y1/2, z, x1/2; (xiv) z1/2, x1/2, y; (xv) x, y, z; (xvi) x, y, z; (xvii) x, y, z; (xviii) z, x, y; (xix) y, z, x; (xx) z, x, y; (xxi) y, z, x; (xxii) y+1/2, z, x+1/2; (xxiii) z+1/2, x+1/2, y; (xxiv) x+1, y+1/2, z+1/2; (xxv) x, y, z.
(RbY3F10) top
Crystal data top
F10RbY3Dx = 4.624 Mg m3
Mr = 542.20Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P63mcCell parameters from 3303 reflections
a = 8.1976 (12) Åθ = 2.9–26.7°
c = 13.384 (3) ŵ = 28.51 mm1
V = 778.9 (2) Å3T = 293 K
Z = 4Block, colorless
F(000) = 9760.22 × 0.12 × 0.10 mm
Data collection top
Rigaku AFC8S
diffractometer
557 independent reflections
Radiation source: fine-focus sealed tube522 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.057
Detector resolution: 14.6199 pixels mm-1θmax = 25.2°, θmin = 2.9°
ω scansh = 99
Absorption correction: multi-scan
REQAB, CrystalClear
k = 99
Tmin = 0.692, Tmax = 1.000l = 1416
6434 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: full w = 1/[σ2(Fo2) + (0.0412P)2 + 3.0565P]
where P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.030(Δ/σ)max < 0.001
wR(F2) = 0.086Δρmax = 1.17 e Å3
S = 1.16Δρmin = 0.86 e Å3
557 reflectionsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
60 parametersExtinction coefficient: 0.0057 (5)
1 restraintAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.21 (3)
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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
Rb10.33330.66670.95169 (17)0.0163 (6)
Rb20.00001.00000.70814 (19)0.0209 (9)
Y10.01072 (15)0.50536 (7)0.69776 (8)0.0085 (3)
Y20.34722 (14)0.17361 (7)0.95759 (8)0.0083 (4)
F10.33330.66670.7412 (12)0.017 (3)
F20.66670.33330.9128 (11)0.010 (3)
F30.0435 (9)0.5217 (5)0.5225 (6)0.0115 (15)
F40.3664 (10)0.1832 (5)1.1334 (7)0.0136 (17)
F50.3396 (7)0.0032 (9)0.8284 (9)0.0188 (8)
F60.2218 (5)0.2218 (5)0.6594 (7)0.0167 (15)
F70.1105 (5)0.1105 (5)0.9894 (7)0.0177 (16)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Rb10.0172 (7)0.0172 (7)0.0145 (15)0.0086 (4)0.0000.000
Rb20.0164 (6)0.0164 (6)0.030 (3)0.0082 (3)0.0000.000
Y10.0097 (6)0.0094 (4)0.0066 (7)0.0048 (3)0.0003 (7)0.0001 (3)
Y20.0085 (6)0.0085 (4)0.0079 (7)0.0042 (3)0.0017 (8)0.0009 (4)
F10.016 (5)0.016 (5)0.019 (7)0.008 (3)0.0000.000
F20.003 (4)0.003 (4)0.023 (8)0.001 (2)0.0000.000
F30.013 (4)0.014 (3)0.007 (4)0.0063 (19)0.001 (3)0.0007 (13)
F40.011 (4)0.013 (3)0.016 (4)0.0053 (18)0.000 (3)0.0002 (15)
F50.025 (3)0.017 (2)0.0113 (17)0.008 (3)0.0042 (17)0.0007 (16)
F60.016 (3)0.016 (3)0.015 (4)0.005 (3)0.0009 (15)0.0009 (15)
F70.015 (3)0.015 (3)0.016 (4)0.003 (3)0.0004 (16)0.0004 (16)
Geometric parameters (Å, º) top
Rb1—F12.817 (16)Y1—Y1xv3.9670 (19)
Rb1—F3i2.838 (7)Y1—Y1xviii3.9670 (19)
Rb1—F3ii2.838 (7)Y2—F72.203 (2)
Rb1—F3iii2.838 (7)Y2—F7v2.203 (2)
Rb1—F5iv3.192 (9)Y2—F52.204 (10)
Rb1—F5v3.192 (9)Y2—F5viii2.204 (10)
Rb1—F5vi3.192 (9)Y2—F3iii2.338 (4)
Rb1—F5vii3.192 (9)Y2—F3xix2.338 (4)
Rb1—F5viii3.192 (9)Y2—F22.346 (4)
Rb1—F5ix3.192 (9)Y2—F42.357 (9)
Rb1—F6ii3.199 (10)Y2—Y2ix3.9281 (19)
Rb1—F6i3.199 (10)Y2—Y2xx3.9280 (18)
Rb2—F4x2.787 (8)Y2—Y1iii3.9405 (15)
Rb2—F4xi2.787 (7)Y2—Y1xix3.9405 (15)
Rb2—F4xii2.787 (8)F1—Y1xv2.363 (4)
Rb2—F5xiii3.205 (8)F1—Y1xviii2.363 (4)
Rb2—F5xiv3.205 (8)F2—Y2xx2.346 (4)
Rb2—F5xv3.205 (8)F2—Y2ix2.346 (4)
Rb2—F5vi3.205 (8)F3—Y2xvii2.338 (4)
Rb2—F5xvi3.205 (8)F3—Y2xi2.338 (4)
Rb2—F5iv3.205 (8)F3—Rb1x2.838 (7)
Rb2—F6xiv3.216 (8)F4—Y1iii2.377 (4)
Rb2—F6xv3.216 (8)F4—Y1xix2.377 (4)
Rb2—F6vi3.216 (8)F4—Rb2ii2.787 (7)
Y1—F5iv2.198 (10)F5—Y1xxi2.198 (10)
Y1—F5v2.198 (10)F5—Rb1xxii3.192 (9)
Y1—F62.207 (3)F5—Rb2xxii3.205 (8)
Y1—F6xiv2.207 (3)F6—Y1xxiii2.207 (3)
Y1—F32.357 (8)F6—Rb1x3.199 (10)
Y1—F12.363 (4)F6—Rb2xxii3.216 (8)
Y1—F4xi2.377 (4)F7—Y2xxi2.203 (2)
Y1—F4xvii2.377 (4)F7—Rb1xxii3.204 (7)
Y1—Y2xvii3.9405 (15)F7—Rb2ii3.321 (10)
Y1—Y2xi3.9405 (15)
F1—Rb1—F3i109.51 (19)F1—Y1—F4xi65.8 (2)
F1—Rb1—F3ii109.51 (19)F5iv—Y1—F4xvii141.3 (3)
F3i—Rb1—F3ii109.43 (19)F5v—Y1—F4xvii80.9 (3)
F1—Rb1—F3iii109.51 (19)F6—Y1—F4xvii79.5 (2)
F3i—Rb1—F3iii109.43 (19)F6xiv—Y1—F4xvii141.6 (3)
F3ii—Rb1—F3iii109.43 (19)F3—Y1—F4xvii65.7 (2)
F1—Rb1—F5iv58.9 (2)F1—Y1—F4xvii65.8 (2)
F3i—Rb1—F5iv100.71 (13)F4xi—Y1—F4xvii101.9 (4)
F3ii—Rb1—F5iv57.8 (2)F5iv—Y1—Y2xvii164.43 (18)
F3iii—Rb1—F5iv149.85 (15)F5v—Y1—Y2xvii111.2 (2)
F1—Rb1—F5v58.9 (2)F6—Y1—Y2xvii73.7 (2)
F3i—Rb1—F5v149.85 (15)F6xiv—Y1—Y2xvii109.8 (2)
F3ii—Rb1—F5v57.8 (2)F3—Y1—Y2xvii32.78 (6)
F3iii—Rb1—F5v100.71 (13)F1—Y1—Y2xvii85.2 (3)
F5iv—Rb1—F5v49.1 (2)F4xi—Y1—Y2xvii86.6 (2)
F1—Rb1—F5vi58.9 (2)F4xvii—Y1—Y2xvii33.5 (2)
F3i—Rb1—F5vi57.8 (2)F5iv—Y1—Y2xi111.2 (2)
F3ii—Rb1—F5vi100.71 (13)F5v—Y1—Y2xi164.43 (18)
F3iii—Rb1—F5vi149.85 (15)F6—Y1—Y2xi109.8 (2)
F5iv—Rb1—F5vi52.2 (2)F6xiv—Y1—Y2xi73.7 (2)
F5v—Rb1—F5vi95.7 (3)F3—Y1—Y2xi32.78 (6)
F1—Rb1—F5vii58.9 (2)F1—Y1—Y2xi85.2 (3)
F3i—Rb1—F5vii57.8 (2)F4xi—Y1—Y2xi33.5 (2)
F3ii—Rb1—F5vii149.85 (15)F4xvii—Y1—Y2xi86.6 (2)
F3iii—Rb1—F5vii100.71 (13)Y2xvii—Y1—Y2xi59.79 (4)
F5iv—Rb1—F5vii95.7 (3)F5iv—Y1—Y1xv74.74 (18)
F5v—Rb1—F5vii117.7 (4)F5v—Y1—Y1xv109.9 (2)
F5vi—Rb1—F5vii49.1 (2)F6—Y1—Y1xv163.4 (2)
F1—Rb1—F5viii58.9 (2)F6xiv—Y1—Y1xv109.70 (19)
F3i—Rb1—F5viii149.85 (15)F3—Y1—Y1xv85.10 (14)
F3ii—Rb1—F5viii100.71 (13)F1—Y1—Y1xv32.93 (14)
F3iii—Rb1—F5viii57.8 (2)F4xi—Y1—Y1xv33.44 (15)
F5iv—Rb1—F5viii95.7 (3)F4xvii—Y1—Y1xv86.69 (15)
F5v—Rb1—F5viii52.2 (2)Y2xvii—Y1—Y1xv89.72 (2)
F5vi—Rb1—F5viii117.7 (4)Y2xi—Y1—Y1xv59.777 (17)
F5vii—Rb1—F5viii95.7 (3)F5iv—Y1—Y1xviii109.93 (19)
F1—Rb1—F5ix58.9 (2)F5v—Y1—Y1xviii74.74 (17)
F3i—Rb1—F5ix100.71 (13)F6—Y1—Y1xviii109.70 (19)
F3ii—Rb1—F5ix149.85 (15)F6xiv—Y1—Y1xviii163.4 (2)
F3iii—Rb1—F5ix57.8 (2)F3—Y1—Y1xviii85.10 (14)
F5iv—Rb1—F5ix117.7 (4)F1—Y1—Y1xviii32.93 (14)
F5v—Rb1—F5ix95.7 (3)F4xi—Y1—Y1xviii86.69 (15)
F5vi—Rb1—F5ix95.7 (3)F4xvii—Y1—Y1xviii33.44 (15)
F5vii—Rb1—F5ix52.2 (2)Y2xvii—Y1—Y1xviii59.777 (17)
F5viii—Rb1—F5ix49.1 (2)Y2xi—Y1—Y1xviii89.72 (2)
F1—Rb1—F6ii150.33 (15)Y1xv—Y1—Y1xviii60.0
F3i—Rb1—F6ii58.44 (15)F7—Y2—F7v76.2 (4)
F3ii—Rb1—F6ii58.44 (15)F7—Y2—F575.6 (3)
F3iii—Rb1—F6ii100.2 (3)F7v—Y2—F5121.0 (3)
F5iv—Rb1—F6ii94.9 (2)F7—Y2—F5viii121.0 (3)
F5v—Rb1—F6ii116.24 (18)F7v—Y2—F5viii75.6 (3)
F5vi—Rb1—F6ii94.9 (2)F5—Y2—F5viii76.6 (5)
F5vii—Rb1—F6ii116.24 (18)F7—Y2—F3iii143.4 (3)
F5viii—Rb1—F6ii145.0 (2)F7v—Y2—F3iii82.1 (3)
F5ix—Rb1—F6ii145.0 (2)F5—Y2—F3iii141.0 (3)
F1—Rb1—F6i150.33 (15)F5viii—Y2—F3iii80.3 (3)
F3i—Rb1—F6i58.44 (15)F7—Y2—F3xix82.1 (3)
F3ii—Rb1—F6i100.2 (3)F7v—Y2—F3xix143.4 (3)
F3iii—Rb1—F6i58.44 (15)F5—Y2—F3xix80.3 (3)
F5iv—Rb1—F6i145.0 (2)F5viii—Y2—F3xix141.0 (3)
F5v—Rb1—F6i145.0 (2)F3iii—Y2—F3xix99.3 (3)
F5vi—Rb1—F6i116.24 (18)F7—Y2—F2141.91 (19)
F5vii—Rb1—F6i94.9 (2)F7v—Y2—F2141.9 (2)
F5viii—Rb1—F6i116.24 (18)F5—Y2—F279.8 (3)
F5ix—Rb1—F6i94.9 (2)F5viii—Y2—F279.8 (3)
F6ii—Rb1—F6i50.8 (2)F3iii—Y2—F265.3 (2)
F4x—Rb2—F4xi107.9 (2)F3xix—Y2—F265.3 (2)
F4x—Rb2—F4xii107.9 (2)F7—Y2—F481.4 (3)
F4xi—Rb2—F4xii107.9 (2)F7v—Y2—F481.4 (3)
F4x—Rb2—F5xiii151.95 (15)F5—Y2—F4141.7 (2)
F4xi—Rb2—F5xiii100.01 (16)F5viii—Y2—F4141.7 (2)
F4xii—Rb2—F5xiii59.0 (2)F3iii—Y2—F466.3 (2)
F4x—Rb2—F5xiv100.01 (16)F3xix—Y2—F466.3 (2)
F4xi—Rb2—F5xiv151.95 (15)F2—Y2—F4101.5 (4)
F4xii—Rb2—F5xiv59.0 (2)F7—Y2—Y2ix165.7 (2)
F5xiii—Rb2—F5xiv52.0 (3)F7v—Y2—Y2ix110.63 (19)
F4x—Rb2—F5xv59.0 (2)F5—Y2—Y2ix109.33 (18)
F4xi—Rb2—F5xv100.01 (16)F5viii—Y2—Y2ix73.22 (15)
F4xii—Rb2—F5xv151.95 (15)F3iii—Y2—Y2ix32.85 (16)
F5xiii—Rb2—F5xv119.7 (4)F3xix—Y2—Y2ix85.53 (15)
F5xiv—Rb2—F5xv97.0 (3)F2—Y2—Y2ix33.15 (14)
F4x—Rb2—F5vi151.95 (15)F4—Y2—Y2ix87.13 (15)
F4xi—Rb2—F5vi59.0 (2)F7—Y2—Y2xx110.63 (18)
F4xii—Rb2—F5vi100.01 (16)F7v—Y2—Y2xx165.7 (2)
F5xiii—Rb2—F5vi50.5 (2)F5—Y2—Y2xx73.22 (15)
F5xiv—Rb2—F5vi97.0 (3)F5viii—Y2—Y2xx109.33 (18)
F5xv—Rb2—F5vi97.0 (3)F3iii—Y2—Y2xx85.53 (15)
F4x—Rb2—F5xvi59.0 (2)F3xix—Y2—Y2xx32.85 (16)
F4xi—Rb2—F5xvi151.95 (15)F2—Y2—Y2xx33.15 (14)
F4xii—Rb2—F5xvi100.01 (16)F4—Y2—Y2xx87.13 (15)
F5xiii—Rb2—F5xvi97.0 (3)Y2ix—Y2—Y2xx60.0
F5xiv—Rb2—F5xvi50.5 (2)F7—Y2—Y1iii111.7 (3)
F5xv—Rb2—F5xvi52.0 (3)F7v—Y2—Y1iii75.5 (2)
F5vi—Rb2—F5xvi119.7 (4)F5—Y2—Y1iii163.49 (15)
F4x—Rb2—F5iv100.01 (16)F5viii—Y2—Y1iii109.6 (2)
F4xi—Rb2—F5iv59.0 (2)F3iii—Y2—Y1iii33.09 (19)
F4xii—Rb2—F5iv151.95 (15)F3xix—Y2—Y1iii85.96 (19)
F5xiii—Rb2—F5iv97.0 (3)F2—Y2—Y1iii86.2 (3)
F5xiv—Rb2—F5iv119.7 (4)F4—Y2—Y1iii33.81 (7)
F5xv—Rb2—F5iv50.5 (2)Y2ix—Y2—Y1iii60.104 (18)
F5vi—Rb2—F5iv52.0 (3)Y2xx—Y2—Y1iii90.28 (2)
F5xvi—Rb2—F5iv97.0 (3)F7—Y2—Y1xix75.5 (2)
F4x—Rb2—F6xiv58.01 (6)F7v—Y2—Y1xix111.7 (3)
F4xi—Rb2—F6xiv58.01 (6)F5—Y2—Y1xix109.6 (2)
F4xii—Rb2—F6xiv147.3 (3)F5viii—Y2—Y1xix163.49 (15)
F5xiii—Rb2—F6xiv146.3 (2)F3iii—Y2—Y1xix85.96 (19)
F5xiv—Rb2—F6xiv146.3 (2)F3xix—Y2—Y1xix33.09 (19)
F5xv—Rb2—F6xiv50.60 (19)F2—Y2—Y1xix86.2 (3)
F5vi—Rb2—F6xiv96.25 (14)F4—Y2—Y1xix33.81 (7)
F5xvi—Rb2—F6xiv96.25 (15)Y2ix—Y2—Y1xix90.28 (2)
F5iv—Rb2—F6xiv50.60 (19)Y2xx—Y2—Y1xix60.104 (18)
F4x—Rb2—F6xv147.3 (3)Y1iii—Y2—Y1xix60.45 (3)
F4xi—Rb2—F6xv58.01 (6)Y1—F1—Y1xv114.1 (3)
F4xii—Rb2—F6xv58.01 (6)Y1—F1—Y1xviii114.1 (3)
F5xiii—Rb2—F6xv50.60 (19)Y1xv—F1—Y1xviii114.1 (3)
F5xiv—Rb2—F6xv96.25 (15)Y1—F1—Rb1104.3 (4)
F5xv—Rb2—F6xv146.3 (2)Y1xv—F1—Rb1104.3 (4)
F5vi—Rb2—F6xv50.60 (19)Y1xviii—F1—Rb1104.3 (4)
F5xvi—Rb2—F6xv146.3 (2)Y2xx—F2—Y2ix113.7 (3)
F5iv—Rb2—F6xv96.25 (14)Y2xx—F2—Y2113.7 (3)
F6xiv—Rb2—F6xv115.99 (12)Y2ix—F2—Y2113.7 (3)
F4x—Rb2—F6vi58.01 (6)Y2xvii—F3—Y2xi114.3 (3)
F4xi—Rb2—F6vi147.3 (3)Y2xvii—F3—Y1114.1 (2)
F4xii—Rb2—F6vi58.01 (6)Y2xi—F3—Y1114.1 (2)
F5xiii—Rb2—F6vi96.25 (14)Y2xvii—F3—Rb1x104.4 (2)
F5xiv—Rb2—F6vi50.60 (19)Y2xi—F3—Rb1x104.4 (2)
F5xv—Rb2—F6vi96.25 (14)Y1—F3—Rb1x103.8 (3)
F5vi—Rb2—F6vi146.3 (2)Y2—F4—Y1iii112.7 (2)
F5xvi—Rb2—F6vi50.60 (19)Y2—F4—Y1xix112.7 (2)
F5iv—Rb2—F6vi146.3 (2)Y1iii—F4—Y1xix113.1 (3)
F6xiv—Rb2—F6vi115.99 (13)Y2—F4—Rb2ii107.7 (3)
F6xv—Rb2—F6vi115.99 (13)Y1iii—F4—Rb2ii104.9 (2)
F5iv—Y1—F5v74.3 (4)Y1xix—F4—Rb2ii104.9 (2)
F5iv—Y1—F6121.8 (3)Y1xxi—F5—Y2145.4 (3)
F5v—Y1—F677.1 (3)Y1xxi—F5—Rb1xxii97.26 (19)
F5iv—Y1—F6xiv77.1 (3)Y2—F5—Rb1xxii97.2 (4)
F5v—Y1—F6xiv121.8 (3)Y1xxi—F5—Rb2xxii97.0 (4)
F6—Y1—F6xiv76.9 (4)Y2—F5—Rb2xxii98.52 (18)
F5iv—Y1—F3142.8 (2)Rb1xxii—F5—Rb2xxii127.9 (2)
F5v—Y1—F3142.8 (2)Y1—F6—Y1xxiii146.9 (4)
F6—Y1—F380.9 (3)Y1—F6—Rb1x96.9 (2)
F6xiv—Y1—F380.9 (3)Y1xxiii—F6—Rb1x96.9 (2)
F5iv—Y1—F181.2 (4)Y1—F6—Rb2xxii96.5 (2)
F5v—Y1—F181.2 (4)Y1xxiii—F6—Rb2xxii96.5 (2)
F6—Y1—F1141.5 (2)Rb1x—F6—Rb2xxii131.4 (3)
F6xiv—Y1—F1141.5 (2)Y2xxi—F7—Y2151.5 (4)
F3—Y1—F198.6 (4)Y2xxi—F7—Rb1xxii96.9 (2)
F5iv—Y1—F4xi80.9 (3)Y2—F7—Rb1xxii96.9 (2)
F5v—Y1—F4xi141.3 (3)Y2xxi—F7—Rb2ii95.6 (2)
F6—Y1—F4xi141.6 (3)Y2—F7—Rb2ii95.6 (2)
F6xiv—Y1—F4xi79.5 (2)Rb1xxii—F7—Rb2ii127.2 (3)
F3—Y1—F4xi65.7 (2)
Symmetry codes: (i) xy+1, x+1, z+1/2; (ii) x, y+1, z+1/2; (iii) y, x+y, z+1/2; (iv) y, x+1, z; (v) y, xy, z; (vi) x, y+1, z; (vii) x+y+1, y+1, z; (viii) x, xy, z; (ix) x+y+1, x+1, z; (x) x, y+1, z1/2; (xi) y, x+y+1, z1/2; (xii) xy, x+1, z1/2; (xiii) x, xy+1, z; (xiv) y, xy+1, z; (xv) x+y, x+1, z; (xvi) x+y, y+1, z; (xvii) xy, x, z1/2; (xviii) y+1, xy+1, z; (xix) xy+1, x, z+1/2; (xx) y+1, xy, z; (xxi) x+y, x, z; (xxii) x, y1, z; (xxiii) x+y1, x, z.
(RbSm3F10) top
Crystal data top
F10RbSm3Mo Kα radiation, λ = 0.71073 Å
Mr = 726.52Cell parameters from 3876 reflections
Cubic, Fm3mθ = 3.0–26.7°
a = 11.8576 (14) ŵ = 26.78 mm1
V = 1667.2 (3) Å3T = 293 K
Z = 8Block, yellow
F(000) = 25040.18 × 0.15 × 0.15 mm
Dx = 5.789 Mg m3
Data collection top
Rigaku AFC8S
diffractometer
103 independent reflections
Radiation source: fine-focus sealed tube103 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.060
Detector resolution: 14.6199 pixels mm-1θmax = 25.1°, θmin = 3.0°
ω scansh = 1414
Absorption correction: multi-scan
REQAB, CrystalClear
k = 1412
Tmin = 0.681, Tmax = 1.000l = 1414
3438 measured reflections
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)] = 0.030 w = 1/[σ2(Fo2) + (0.0407P)2 + 344.4752P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.105(Δ/σ)max < 0.001
S = 1.18Δρmax = 1.77 e Å3
103 reflectionsΔρmin = 1.06 e Å3
13 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraints
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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
Rb10.25000.25000.25000.0157 (12)
Sm10.24234 (12)0.00000.00000.0084 (9)
F10.1107 (6)0.1107 (6)0.1107 (6)0.016 (3)
F20.50000.1686 (9)0.1686 (9)0.042 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Rb10.0157 (12)0.0157 (12)0.0157 (12)0.0000.0000.000
Sm10.0105 (10)0.0074 (9)0.0074 (9)0.0000.0000.000
F10.016 (3)0.016 (3)0.016 (3)0.001 (3)0.001 (3)0.001 (3)
F20.043 (8)0.042 (5)0.042 (5)0.0000.0000.012 (7)
Geometric parameters (Å, º) top
Rb1—F12.861 (13)Sm1—F2xiii2.261 (4)
Rb1—F1i2.861 (13)Sm1—F1xiv2.425 (4)
Rb1—F1ii2.861 (13)Sm1—F12.425 (4)
Rb1—F1iii2.861 (13)Sm1—F1xv2.425 (4)
Rb1—F2iv3.264 (6)Sm1—F1xvi2.425 (4)
Rb1—F2v3.264 (6)Sm1—Sm1xvii4.064 (2)
Rb1—F2vi3.264 (6)Sm1—Sm1xviii4.064 (2)
Rb1—F2vii3.264 (6)Sm1—Sm1xix4.064 (2)
Rb1—F2viii3.264 (6)Sm1—Sm1xx4.064 (2)
Rb1—F2ix3.264 (6)F1—Sm1xx2.425 (4)
Rb1—F2x3.264 (6)F1—Sm1xix2.425 (4)
Rb1—F2xi3.264 (6)F2—Sm1xxi2.261 (4)
Sm1—F2ix2.261 (4)F2—Sm1xxii2.261 (4)
Sm1—F2x2.261 (4)F2—Rb1xxiii3.264 (6)
Sm1—F2xii2.261 (4)F2—Rb1xxiv3.264 (6)
F1—Rb1—F1i109.5F2ix—Sm1—F1xiv141.19 (18)
F1—Rb1—F1ii109.5F2x—Sm1—F1xiv141.19 (18)
F1i—Rb1—F1ii109.471 (1)F2xii—Sm1—F1xiv79.8 (4)
F1—Rb1—F1iii109.5F2xiii—Sm1—F1xiv79.8 (4)
F1i—Rb1—F1iii109.5F2ix—Sm1—F179.8 (4)
F1ii—Rb1—F1iii109.5F2x—Sm1—F179.8 (4)
F1—Rb1—F2iv150.0 (2)F2xii—Sm1—F1141.19 (18)
F1i—Rb1—F2iv58.37 (7)F2xiii—Sm1—F1141.19 (18)
F1ii—Rb1—F2iv100.5 (2)F1xiv—Sm1—F199.9 (6)
F1iii—Rb1—F2iv58.37 (7)F2ix—Sm1—F1xv141.19 (18)
F1—Rb1—F2v150.0 (2)F2x—Sm1—F1xv79.8 (4)
F1i—Rb1—F2v100.5 (2)F2xii—Sm1—F1xv79.8 (4)
F1ii—Rb1—F2v58.37 (7)F2xiii—Sm1—F1xv141.19 (18)
F1iii—Rb1—F2v58.37 (7)F1xiv—Sm1—F1xv65.5 (3)
F2iv—Rb1—F2v51.3 (4)F1—Sm1—F1xv65.5 (3)
F1—Rb1—F2vi150.0 (2)F2ix—Sm1—F1xvi79.8 (4)
F1i—Rb1—F2vi58.37 (7)F2x—Sm1—F1xvi141.19 (18)
F1ii—Rb1—F2vi58.37 (7)F2xii—Sm1—F1xvi141.19 (18)
F1iii—Rb1—F2vi100.5 (2)F2xiii—Sm1—F1xvi79.8 (4)
F2iv—Rb1—F2vi51.3 (4)F1xiv—Sm1—F1xvi65.5 (3)
F2v—Rb1—F2vi51.3 (4)F1—Sm1—F1xvi65.5 (3)
F1—Rb1—F2vii58.37 (7)F1xv—Sm1—F1xvi99.9 (6)
F1i—Rb1—F2vii150.0 (2)F2ix—Sm1—Sm1xvii162.9 (4)
F1ii—Rb1—F2vii58.37 (7)F2x—Sm1—Sm1xvii109.3 (2)
F1iii—Rb1—F2vii100.5 (2)F2xii—Sm1—Sm1xvii72.9 (4)
F2iv—Rb1—F2vii145.6 (3)F2xiii—Sm1—Sm1xvii109.3 (2)
F2v—Rb1—F2vii95.02 (9)F1xiv—Sm1—Sm1xvii33.10 (12)
F2vi—Rb1—F2vii116.74 (14)F1—Sm1—Sm1xvii85.9 (3)
F1—Rb1—F2viii58.37 (7)F1xv—Sm1—Sm1xvii33.10 (12)
F1i—Rb1—F2viii58.37 (7)F1xvi—Sm1—Sm1xvii85.9 (3)
F1ii—Rb1—F2viii150.0 (2)F2ix—Sm1—Sm1xviii109.3 (2)
F1iii—Rb1—F2viii100.5 (2)F2x—Sm1—Sm1xviii162.9 (4)
F2iv—Rb1—F2viii95.02 (9)F2xii—Sm1—Sm1xviii109.3 (2)
F2v—Rb1—F2viii145.6 (3)F2xiii—Sm1—Sm1xviii72.9 (4)
F2vi—Rb1—F2viii116.74 (14)F1xiv—Sm1—Sm1xviii33.10 (12)
F2vii—Rb1—F2viii116.74 (14)F1—Sm1—Sm1xviii85.9 (3)
F1—Rb1—F2ix58.37 (7)F1xv—Sm1—Sm1xviii85.9 (3)
F1i—Rb1—F2ix100.5 (2)F1xvi—Sm1—Sm1xviii33.10 (12)
F1ii—Rb1—F2ix58.37 (7)Sm1xvii—Sm1—Sm1xviii60.0
F1iii—Rb1—F2ix150.0 (2)F2ix—Sm1—Sm1xix72.9 (4)
F2iv—Rb1—F2ix145.6 (3)F2x—Sm1—Sm1xix109.3 (2)
F2v—Rb1—F2ix116.74 (14)F2xii—Sm1—Sm1xix162.9 (4)
F2vi—Rb1—F2ix95.02 (9)F2xiii—Sm1—Sm1xix109.3 (2)
F2vii—Rb1—F2ix49.5 (5)F1xiv—Sm1—Sm1xix85.9 (3)
F2viii—Rb1—F2ix95.02 (9)F1—Sm1—Sm1xix33.10 (12)
F1—Rb1—F2x58.37 (7)F1xv—Sm1—Sm1xix85.9 (3)
F1i—Rb1—F2x58.37 (7)F1xvi—Sm1—Sm1xix33.10 (12)
F1ii—Rb1—F2x100.5 (2)Sm1xvii—Sm1—Sm1xix90.0
F1iii—Rb1—F2x150.0 (2)Sm1xviii—Sm1—Sm1xix60.0
F2iv—Rb1—F2x116.74 (14)F2ix—Sm1—Sm1xx109.3 (2)
F2v—Rb1—F2x145.6 (3)F2x—Sm1—Sm1xx72.9 (4)
F2vi—Rb1—F2x95.02 (9)F2xii—Sm1—Sm1xx109.3 (2)
F2vii—Rb1—F2x95.02 (9)F2xiii—Sm1—Sm1xx162.9 (4)
F2viii—Rb1—F2x49.5 (5)F1xiv—Sm1—Sm1xx85.9 (3)
F2ix—Rb1—F2x51.3 (4)F1—Sm1—Sm1xx33.10 (12)
F1—Rb1—F2xi58.37 (7)F1xv—Sm1—Sm1xx33.10 (12)
F1i—Rb1—F2xi150.0 (2)F1xvi—Sm1—Sm1xx85.9 (3)
F1ii—Rb1—F2xi100.5 (2)Sm1xvii—Sm1—Sm1xx60.0
F1iii—Rb1—F2xi58.37 (7)Sm1xviii—Sm1—Sm1xx90.0
F2iv—Rb1—F2xi116.74 (14)Sm1xix—Sm1—Sm1xx60.0
F2v—Rb1—F2xi95.02 (9)Sm1xx—F1—Sm1xix113.8 (2)
F2vi—Rb1—F2xi145.6 (3)Sm1xx—F1—Sm1113.8 (2)
F2vii—Rb1—F2xi51.3 (4)Sm1xix—F1—Sm1113.8 (2)
F2viii—Rb1—F2xi95.02 (9)Sm1xx—F1—Rb1104.7 (3)
F2ix—Rb1—F2xi95.02 (9)Sm1xix—F1—Rb1104.7 (3)
F2x—Rb1—F2xi116.74 (14)Sm1—F1—Rb1104.7 (3)
F2ix—Sm1—F2x77.4 (3)Sm1xxi—F2—Sm1xxii145.7 (7)
F2ix—Sm1—F2xii124.3 (7)Sm1xxi—F2—Rb1xxiii97.08 (8)
F2x—Sm1—F2xii77.4 (3)Sm1xxii—F2—Rb1xxiii97.08 (8)
F2ix—Sm1—F2xiii77.4 (3)Sm1xxi—F2—Rb1xxiv97.08 (8)
F2x—Sm1—F2xiii124.3 (7)Sm1xxii—F2—Rb1xxiv97.08 (8)
F2xii—Sm1—F2xiii77.4 (3)Rb1xxiii—F2—Rb1xxiv130.5 (5)
Symmetry codes: (i) x1/2, y, z1/2; (ii) x1/2, y1/2, z; (iii) x, y1/2, z1/2; (iv) y1/2, z1/2, x1; (v) z1/2, x1, y1/2; (vi) x1, y1/2, z1/2; (vii) y, z1/2, x+1/2; (viii) z, x1/2, y1/2; (ix) y1/2, z, x1/2; (x) z1/2, x+1/2, y; (xi) x1/2, y1/2, z; (xii) y1/2, z, x1/2; (xiii) z1/2, x1/2, y; (xiv) x, y, z; (xv) x, y, z; (xvi) x, y, z; (xvii) z, x, y; (xviii) y, z, x; (xix) z, x, y; (xx) y, z, x; (xxi) y+1/2, z, x+1/2; (xxii) z+1/2, x+1/2, y; (xxiii) x+1, y+1/2, z+1/2; (xxiv) x, y, z.
(RbGd3F10) top
Crystal data top
F10Gd3RbDx = 6.017 Mg m3
Mr = 747.22Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P63mcCell parameters from 5211 reflections
a = 8.3540 (12) Åθ = 2.8–25.4°
c = 13.649 (3) ŵ = 29.83 mm1
V = 824.9 (2) Å3T = 293 K
Z = 4Block, colorless
F(000) = 12760.25 × 0.23 × 0.20 mm
Data collection top
Rigaku AFC8S
diffractometer
613 independent reflections
Radiation source: fine-focus sealed tube611 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.075
Detector resolution: 14.6199 pixels mm-1θmax = 25.4°, θmin = 2.8°
ω scansh = 1010
Absorption correction: multi-scan
REQAB,RIGAKU/MSC,The Woodlands,TX,USA,1999.
k = 99
Tmin = 0.456, Tmax = 1.000l = 1616
6420 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: full w = 1/[σ2(Fo2) + (0.0224P)2 + 44.1111P]
where P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.035(Δ/σ)max < 0.001
wR(F2) = 0.083Δρmax = 2.30 e Å3
S = 1.18Δρmin = 1.44 e Å3
613 reflectionsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
59 parametersExtinction coefficient: 0.0112 (5)
25 restraintsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.11 (9)
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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
Gd10.50576 (7)0.50576 (7)0.01044 (7)0.0052 (3)
Gd20.17390 (7)0.17390 (7)0.24930 (7)0.0051 (4)
Rb20.00000.00000.0069 (10)0.0198 (10)
Rb10.33330.33330.7436 (8)0.0161 (12)
F50.3339 (14)0.3357 (14)0.1141 (15)0.0166 (19)
F60.2209 (11)0.2209 (11)0.9523 (11)0.016 (3)
F40.1836 (10)0.1836 (10)0.4266 (11)0.013 (3)
F70.1090 (10)0.1090 (10)0.7827 (11)0.015 (3)
F20.33330.33330.2082 (17)0.0044 (13)
F10.33330.33330.540 (2)0.021 (6)
F30.4794 (9)0.4794 (9)0.3168 (10)0.006 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Gd10.0060 (4)0.0060 (4)0.0044 (5)0.0035 (4)0.0008 (4)0.0008 (4)
Gd20.0056 (4)0.0056 (4)0.0044 (6)0.0030 (4)0.0007 (5)0.0007 (5)
Rb20.0168 (11)0.0168 (11)0.026 (3)0.0084 (5)0.0000.000
Rb10.0162 (12)0.0162 (12)0.016 (3)0.0081 (6)0.0000.000
F50.027 (5)0.022 (5)0.007 (4)0.017 (4)0.008 (4)0.007 (4)
F60.009 (4)0.009 (4)0.022 (6)0.003 (5)0.002 (3)0.002 (3)
F40.011 (4)0.011 (4)0.018 (5)0.006 (4)0.004 (2)0.004 (2)
F70.011 (3)0.011 (3)0.023 (5)0.007 (4)0.000 (2)0.000 (2)
F20.0043 (12)0.0043 (12)0.0047 (17)0.0021 (6)0.0000.000
F10.015 (8)0.015 (8)0.032 (14)0.007 (4)0.0000.000
F30.004 (4)0.004 (4)0.003 (5)0.002 (5)0.001 (3)0.001 (3)
Geometric parameters (Å, º) top
Gd1—F5i2.192 (17)Rb2—F5xii3.248 (19)
Gd1—F5ii2.192 (17)Rb1—F12.77 (3)
Gd1—F6iii2.252 (4)Rb1—F3xvi2.888 (15)
Gd1—F6iv2.252 (4)Rb1—F3xvii2.888 (15)
Gd1—F3v2.368 (13)Rb1—F3xxv2.888 (15)
Gd1—F4vi2.410 (8)Rb1—F63.28 (2)
Gd1—F4vii2.410 (8)Rb1—F6xv3.28 (2)
Gd1—F1v2.430 (8)Rb1—F6xiv3.28 (2)
Gd1—Gd2vi4.0155 (13)Rb1—F73.289 (14)
Gd1—Gd2vii4.0155 (13)Rb1—F7xv3.289 (14)
Gd1—Gd1viii4.0327 (18)Rb1—F7xiv3.289 (14)
Gd1—Gd1ix4.0327 (18)Rb1—F5xxvi3.302 (18)
Gd2—F7x2.249 (4)Rb1—F5xxvii3.302 (19)
Gd2—F7xi2.249 (4)F5—Gd1xxviii2.192 (17)
Gd2—F5xii2.310 (18)F5—Gd2xxiv2.310 (18)
Gd2—F5xiii2.310 (18)F5—Rb1xxix3.302 (18)
Gd2—F22.374 (5)F6—Gd1xxx2.252 (4)
Gd2—F3xiv2.400 (7)F6—Gd1xxxi2.252 (4)
Gd2—F3xv2.400 (7)F6—Rb2xxxii3.244 (16)
Gd2—F42.424 (16)F4—Gd1xvi2.410 (8)
Gd2—Gd2xv3.9957 (18)F4—Gd1xvii2.410 (8)
Gd2—Gd2xiv3.9957 (18)F4—Rb2xxxiii2.807 (16)
Gd2—Gd1xvi4.0155 (13)F7—Gd2xxxiv2.249 (4)
Gd2—Gd1xvii4.0155 (13)F7—Gd2xxxv2.249 (4)
Rb2—F4xi2.807 (16)F7—Rb2xxxii3.28 (2)
Rb2—F4x2.807 (16)F2—Gd2xv2.374 (5)
Rb2—F4xviii2.807 (16)F2—Gd2xiv2.374 (5)
Rb2—F6xix3.244 (16)F1—Gd1xvii2.430 (8)
Rb2—F6xx3.244 (16)F1—Gd1xvi2.430 (8)
Rb2—F6xxi3.244 (16)F1—Gd1xxv2.430 (8)
Rb2—F53.248 (19)F3—Gd1xxv2.368 (13)
Rb2—F5xxii3.248 (19)F3—Gd2xiv2.400 (7)
Rb2—F5xiii3.248 (19)F3—Gd2xv2.400 (7)
Rb2—F5xxiii3.248 (19)F3—Rb1v2.888 (15)
Rb2—F5xxiv3.248 (19)
F5i—Gd1—F5ii78.0 (8)F6xxi—Rb2—F595.2 (3)
F5i—Gd1—F6iii122.4 (5)F4xi—Rb2—F5xxii150.7 (4)
F5ii—Gd1—F6iii75.4 (5)F4x—Rb2—F5xxii99.2 (3)
F5i—Gd1—F6iv75.4 (5)F4xviii—Rb2—F5xxii57.4 (4)
F5ii—Gd1—F6iv122.4 (5)F6xix—Rb2—F5xxii95.2 (3)
F6iii—Gd1—F6iv77.5 (8)F6xx—Rb2—F5xxii49.5 (3)
F5i—Gd1—F3v140.9 (4)F6xxi—Rb2—F5xxii145.1 (5)
F5ii—Gd1—F3v140.9 (4)F5—Rb2—F5xxii50.6 (4)
F6iii—Gd1—F3v81.0 (5)F4xi—Rb2—F5xiii99.2 (3)
F6iv—Gd1—F3v81.0 (5)F4x—Rb2—F5xiii57.4 (4)
F5i—Gd1—F4vi142.1 (5)F4xviii—Rb2—F5xiii150.7 (4)
F5ii—Gd1—F4vi79.0 (5)F6xix—Rb2—F5xiii145.1 (5)
F6iii—Gd1—F4vi79.5 (5)F6xx—Rb2—F5xiii95.2 (3)
F6iv—Gd1—F4vi142.4 (5)F6xxi—Rb2—F5xiii49.5 (3)
F3v—Gd1—F4vi66.3 (4)F5—Rb2—F5xiii51.4 (5)
F5i—Gd1—F4vii79.0 (5)F5xxii—Rb2—F5xiii96.4 (6)
F5ii—Gd1—F4vii142.1 (5)F4xi—Rb2—F5xxiii57.4 (4)
F6iii—Gd1—F4vii142.4 (5)F4x—Rb2—F5xxiii150.7 (4)
F6iv—Gd1—F4vii79.5 (5)F4xviii—Rb2—F5xxiii99.2 (3)
F3v—Gd1—F4vii66.3 (4)F6xix—Rb2—F5xxiii49.5 (3)
F4vi—Gd1—F4vii102.3 (7)F6xx—Rb2—F5xxiii145.1 (5)
F5i—Gd1—F1v79.7 (6)F6xxi—Rb2—F5xxiii95.2 (3)
F5ii—Gd1—F1v79.7 (6)F5—Rb2—F5xxiii118.9 (9)
F6iii—Gd1—F1v141.3 (4)F5xxii—Rb2—F5xxiii96.4 (6)
F6iv—Gd1—F1v141.3 (4)F5xiii—Rb2—F5xxiii96.4 (6)
F3v—Gd1—F1v101.4 (7)F4xi—Rb2—F5xxiv99.2 (3)
F4vi—Gd1—F1v66.9 (4)F4x—Rb2—F5xxiv150.7 (4)
F4vii—Gd1—F1v66.9 (4)F4xviii—Rb2—F5xxiv57.4 (4)
F5i—Gd1—Gd2vi163.6 (3)F6xix—Rb2—F5xxiv49.5 (3)
F5ii—Gd1—Gd2vi109.4 (4)F6xx—Rb2—F5xxiv95.2 (3)
F6iii—Gd1—Gd2vi73.9 (4)F6xxi—Rb2—F5xxiv145.1 (5)
F6iv—Gd1—Gd2vi110.2 (4)F5—Rb2—F5xxiv96.4 (6)
F3v—Gd1—Gd2vi32.89 (13)F5xxii—Rb2—F5xxiv51.4 (5)
F4vi—Gd1—Gd2vi34.0 (4)F5xiii—Rb2—F5xxiv118.9 (9)
F4vii—Gd1—Gd2vi86.9 (4)F5xxiii—Rb2—F5xxiv50.6 (4)
F1v—Gd1—Gd2vi87.3 (6)F4xi—Rb2—F5xii57.4 (4)
F5i—Gd1—Gd2vii109.4 (4)F4x—Rb2—F5xii99.2 (3)
F5ii—Gd1—Gd2vii163.6 (3)F4xviii—Rb2—F5xii150.7 (4)
F6iii—Gd1—Gd2vii110.2 (4)F6xix—Rb2—F5xii95.2 (3)
F6iv—Gd1—Gd2vii73.9 (4)F6xx—Rb2—F5xii145.1 (5)
F3v—Gd1—Gd2vii32.89 (13)F6xxi—Rb2—F5xii49.5 (3)
F4vi—Gd1—Gd2vii86.9 (4)F5—Rb2—F5xii96.4 (6)
F4vii—Gd1—Gd2vii34.0 (4)F5xxii—Rb2—F5xii118.9 (9)
F1v—Gd1—Gd2vii87.3 (6)F5xiii—Rb2—F5xii50.6 (4)
Gd2vi—Gd1—Gd2vii59.67 (3)F5xxiii—Rb2—F5xii51.4 (5)
F5i—Gd1—Gd1viii73.9 (3)F5xxiv—Rb2—F5xii96.4 (6)
F5ii—Gd1—Gd1viii110.7 (3)F1—Rb1—F3xvi110.2 (4)
F6iii—Gd1—Gd1viii163.6 (4)F1—Rb1—F3xvii110.2 (4)
F6iv—Gd1—Gd1viii109.5 (4)F3xvi—Rb1—F3xvii108.7 (4)
F3v—Gd1—Gd1viii85.5 (3)F1—Rb1—F3xxv110.2 (4)
F4vi—Gd1—Gd1viii86.7 (3)F3xvi—Rb1—F3xxv108.7 (4)
F4vii—Gd1—Gd1viii33.2 (3)F3xvii—Rb1—F3xxv108.7 (4)
F1v—Gd1—Gd1viii33.9 (3)F1—Rb1—F6150.3 (3)
Gd2vi—Gd1—Gd1viii89.736 (18)F3xvi—Rb1—F657.8 (3)
Gd2vii—Gd1—Gd1viii59.858 (16)F3xvii—Rb1—F657.8 (3)
F5i—Gd1—Gd1ix110.7 (3)F3xxv—Rb1—F699.5 (6)
F5ii—Gd1—Gd1ix73.9 (3)F1—Rb1—F6xv150.3 (3)
F6iii—Gd1—Gd1ix109.5 (4)F3xvi—Rb1—F6xv57.8 (3)
F6iv—Gd1—Gd1ix163.6 (4)F3xvii—Rb1—F6xv99.5 (6)
F3v—Gd1—Gd1ix85.5 (3)F3xxv—Rb1—F6xv57.8 (3)
F4vi—Gd1—Gd1ix33.2 (3)F6—Rb1—F6xv50.9 (5)
F4vii—Gd1—Gd1ix86.7 (3)F1—Rb1—F6xiv150.3 (3)
F1v—Gd1—Gd1ix33.9 (3)F3xvi—Rb1—F6xiv99.5 (6)
Gd2vi—Gd1—Gd1ix59.858 (16)F3xvii—Rb1—F6xiv57.8 (3)
Gd2vii—Gd1—Gd1ix89.736 (18)F3xxv—Rb1—F6xiv57.8 (3)
Gd1viii—Gd1—Gd1ix60.0F6—Rb1—F6xiv50.9 (5)
F7x—Gd2—F7xi74.8 (7)F6xv—Rb1—F6xiv50.9 (5)
F7x—Gd2—F5xii119.8 (5)F1—Rb1—F799.3 (4)
F7xi—Gd2—F5xii76.6 (5)F3xvi—Rb1—F758.73 (12)
F7x—Gd2—F5xiii76.6 (5)F3xvii—Rb1—F758.73 (12)
F7xi—Gd2—F5xiii119.8 (5)F3xxv—Rb1—F7150.4 (7)
F5xii—Gd2—F5xiii73.8 (8)F6—Rb1—F750.9 (4)
F7x—Gd2—F2142.6 (4)F6xv—Rb1—F796.0 (5)
F7xi—Gd2—F2142.6 (3)F6xiv—Rb1—F796.0 (5)
F5xii—Gd2—F281.3 (5)F1—Rb1—F7xv99.3 (4)
F5xiii—Gd2—F281.3 (5)F3xvi—Rb1—F7xv58.73 (12)
F7x—Gd2—F3xiv81.9 (4)F3xvii—Rb1—F7xv150.4 (7)
F7xi—Gd2—F3xiv141.8 (5)F3xxv—Rb1—F7xv58.73 (12)
F5xii—Gd2—F3xiv141.6 (4)F6—Rb1—F7xv96.0 (5)
F5xiii—Gd2—F3xiv82.4 (5)F6xv—Rb1—F7xv50.9 (4)
F2—Gd2—F3xiv65.5 (4)F6xiv—Rb1—F7xv96.0 (5)
F7x—Gd2—F3xv141.8 (5)F7—Rb1—F7xv117.4 (2)
F7xi—Gd2—F3xv81.9 (4)F1—Rb1—F7xiv99.3 (4)
F5xii—Gd2—F3xv82.4 (5)F3xvi—Rb1—F7xiv150.4 (7)
F5xiii—Gd2—F3xv141.6 (4)F3xvii—Rb1—F7xiv58.73 (12)
F2—Gd2—F3xv65.5 (4)F3xxv—Rb1—F7xiv58.73 (12)
F3xiv—Gd2—F3xv99.4 (6)F6—Rb1—F7xiv96.0 (5)
F7x—Gd2—F480.9 (5)F6xv—Rb1—F7xiv96.0 (5)
F7xi—Gd2—F480.9 (5)F6xiv—Rb1—F7xiv50.9 (4)
F5xii—Gd2—F4143.1 (4)F7—Rb1—F7xiv117.4 (2)
F5xiii—Gd2—F4143.1 (4)F7xv—Rb1—F7xiv117.4 (2)
F2—Gd2—F4100.4 (6)F1—Rb1—F5xxvi57.6 (4)
F3xiv—Gd2—F465.6 (3)F3xvi—Rb1—F5xxvi100.9 (2)
F3xv—Gd2—F465.6 (3)F3xvii—Rb1—F5xxvi59.7 (4)
F7x—Gd2—Gd2xv111.2 (3)F3xxv—Rb1—F5xxvi150.4 (3)
F7xi—Gd2—Gd2xv165.7 (3)F6—Rb1—F5xxvi95.9 (4)
F5xii—Gd2—Gd2xv109.5 (3)F6xv—Rb1—F5xxvi146.0 (5)
F5xiii—Gd2—Gd2xv74.5 (3)F6xiv—Rb1—F5xxvi117.5 (4)
F2—Gd2—Gd2xv32.7 (2)F7—Rb1—F5xxvi50.8 (3)
F3xiv—Gd2—Gd2xv33.7 (3)F7xv—Rb1—F5xxvi144.2 (5)
F3xv—Gd2—Gd2xv86.0 (3)F7xiv—Rb1—F5xxvi94.7 (2)
F4—Gd2—Gd2xv87.1 (3)F1—Rb1—F5xxvii57.6 (4)
F7x—Gd2—Gd2xiv165.7 (3)F3xvi—Rb1—F5xxvii150.4 (3)
F7xi—Gd2—Gd2xiv111.2 (3)F3xvii—Rb1—F5xxvii59.7 (4)
F5xii—Gd2—Gd2xiv74.5 (3)F3xxv—Rb1—F5xxvii100.9 (2)
F5xiii—Gd2—Gd2xiv109.5 (3)F6—Rb1—F5xxvii117.5 (4)
F2—Gd2—Gd2xiv32.7 (2)F6xv—Rb1—F5xxvii146.0 (5)
F3xiv—Gd2—Gd2xiv86.0 (3)F6xiv—Rb1—F5xxvii95.9 (4)
F3xv—Gd2—Gd2xiv33.7 (3)F7—Rb1—F5xxvii94.7 (2)
F4—Gd2—Gd2xiv87.1 (3)F7xv—Rb1—F5xxvii144.2 (5)
Gd2xv—Gd2—Gd2xiv60.0F7xiv—Rb1—F5xxvii50.8 (3)
F7x—Gd2—Gd1xvi75.4 (3)F5xxvi—Rb1—F5xxvii49.4 (4)
F7xi—Gd2—Gd1xvi111.0 (4)Gd1xxviii—F5—Gd2xxiv144.2 (5)
F5xii—Gd2—Gd1xvi164.7 (3)Gd1xxviii—F5—Rb298.5 (8)
F5xiii—Gd2—Gd1xvi111.2 (4)Gd2xxiv—F5—Rb2100.3 (4)
F2—Gd2—Gd1xvi85.2 (5)Gd1xxviii—F5—Rb1xxix96.9 (4)
F3xiv—Gd2—Gd1xvi32.4 (3)Gd2xxiv—F5—Rb1xxix94.6 (7)
F3xv—Gd2—Gd1xvi85.5 (3)Rb2—F5—Rb1xxix129.0 (3)
F4—Gd2—Gd1xvi33.73 (14)Gd1xxx—F6—Gd1xxxi147.3 (7)
Gd2xv—Gd2—Gd1xvi60.163 (15)Gd1xxx—F6—Rb2xxxii97.3 (4)
Gd2xiv—Gd2—Gd1xvi90.264 (18)Gd1xxxi—F6—Rb2xxxii97.3 (4)
F7x—Gd2—Gd1xvii111.0 (4)Gd1xxx—F6—Rb196.5 (4)
F7xi—Gd2—Gd1xvii75.4 (4)Gd1xxxi—F6—Rb196.5 (4)
F5xii—Gd2—Gd1xvii111.2 (4)Rb2xxxii—F6—Rb1129.6 (7)
F5xiii—Gd2—Gd1xvii164.7 (3)Gd1xvi—F4—Gd1xvii113.6 (6)
F2—Gd2—Gd1xvii85.2 (5)Gd1xvi—F4—Gd2112.3 (4)
F3xiv—Gd2—Gd1xvii85.5 (3)Gd1xvii—F4—Gd2112.3 (4)
F3xv—Gd2—Gd1xvii32.4 (3)Gd1xvi—F4—Rb2xxxiii106.2 (4)
F4—Gd2—Gd1xvii33.73 (14)Gd1xvii—F4—Rb2xxxiii106.2 (4)
Gd2xv—Gd2—Gd1xvii90.264 (18)Gd2—F4—Rb2xxxiii105.6 (6)
Gd2xiv—Gd2—Gd1xvii60.163 (15)Gd2xxxiv—F7—Gd2xxxv151.3 (7)
Gd1xvi—Gd2—Gd1xvii60.28 (3)Gd2xxxiv—F7—Rb2xxxii96.3 (4)
F4xi—Rb2—F4x110.1 (4)Gd2xxxv—F7—Rb2xxxii96.3 (4)
F4xi—Rb2—F4xviii110.1 (4)Gd2xxxiv—F7—Rb196.2 (4)
F4x—Rb2—F4xviii110.1 (4)Gd2xxxv—F7—Rb196.2 (4)
F4xi—Rb2—F6xix58.56 (12)Rb2xxxii—F7—Rb1128.1 (6)
F4x—Rb2—F6xix151.3 (8)Gd2—F2—Gd2xv114.6 (4)
F4xviii—Rb2—F6xix58.56 (12)Gd2—F2—Gd2xiv114.6 (4)
F4xi—Rb2—F6xx151.3 (8)Gd2xv—F2—Gd2xiv114.6 (4)
F4x—Rb2—F6xx58.56 (12)Gd1xvii—F1—Gd1xvi112.2 (6)
F4xviii—Rb2—F6xx58.56 (12)Gd1xvii—F1—Gd1xxv112.2 (6)
F6xix—Rb2—F6xx117.1 (3)Gd1xvi—F1—Gd1xxv112.2 (6)
F4xi—Rb2—F6xxi58.56 (12)Gd1xvii—F1—Rb1106.6 (6)
F4x—Rb2—F6xxi58.56 (12)Gd1xvi—F1—Rb1106.6 (6)
F4xviii—Rb2—F6xxi151.3 (8)Gd1xxv—F1—Rb1106.6 (6)
F6xix—Rb2—F6xxi117.1 (3)Gd1xxv—F3—Gd2xiv114.7 (3)
F6xx—Rb2—F6xxi117.1 (3)Gd1xxv—F3—Gd2xv114.7 (3)
F4xi—Rb2—F5150.7 (4)Gd2xiv—F3—Gd2xv112.7 (5)
F4x—Rb2—F557.4 (4)Gd1xxv—F3—Rb1v105.0 (5)
F4xviii—Rb2—F599.2 (3)Gd2xiv—F3—Rb1v104.0 (4)
F6xix—Rb2—F5145.1 (5)Gd2xv—F3—Rb1v104.0 (4)
F6xx—Rb2—F549.5 (3)
Symmetry codes: (i) y+1, x, z; (ii) x, y1, z; (iii) y, xy1, z1; (iv) x+y+1, x, z1; (v) x+1, y1, z1/2; (vi) xy, x1, z1/2; (vii) y+1, x+y, z1/2; (viii) x+y+2, x, z; (ix) y, xy2, z; (x) xy, x, z1/2; (xi) y, x+y, z1/2; (xii) x+y, x, z; (xiii) x, xy, z; (xiv) y, xy1, z; (xv) x+y+1, x, z; (xvi) y+1, x+y+1, z+1/2; (xvii) xy1, x1, z+1/2; (xviii) x, y, z1/2; (xix) x+y, x, z1; (xx) y, xy, z1; (xxi) x, y, z1; (xxii) x+y, y, z; (xxiii) y, x, z; (xxiv) y, xy, z; (xxv) x+1, y1, z+1/2; (xxvi) xy, y, z+1/2; (xxvii) xy, x1, z+1/2; (xxviii) x, y+1, z; (xxix) x+1, y, z1/2; (xxx) y, xy1, z+1; (xxxi) x+y+1, x, z+1; (xxxii) x, y, z+1; (xxxiii) x, y, z+1/2; (xxxiv) y, x+y, z+1/2; (xxxv) xy, x, z+1/2.
(KLu3F10) top
Crystal data top
F10KLu3Dx = 6.798 Mg m3
Mr = 754.01Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P63mcCell parameters from 3712 reflections
a = 8.0420 (11) Åθ = 2.9–25.9°
c = 13.154 (3) ŵ = 40.59 mm1
V = 736.8 (2) Å3T = 293 K
Z = 4Block, colorless
F(000) = 12880.26 × 0.21 × 0.20 mm
Data collection top
Rigaku AFC8S
diffractometer
547 independent reflections
Radiation source: fine-focus sealed tube542 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.086
Detector resolution: 14.6199 pixels mm-1θmax = 25.2°, θmin = 2.9°
ω scansh = 99
Absorption correction: multi-scan
REQAB,RIGAKU/MSC,The Woodlands,TX,USA,1999.
k = 98
Tmin = 0.308, Tmax = 1.000l = 1515
5397 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: full w = 1/[σ2(Fo2) + (0.0418P)2 + 5.7237P]
where P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.029(Δ/σ)max < 0.001
wR(F2) = 0.076Δρmax = 2.74 e Å3
S = 1.19Δρmin = 1.92 e Å3
547 reflectionsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
59 parametersExtinction coefficient: 0.0025 (2)
25 restraintsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.02 (6)
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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
K10.66670.33330.0482 (16)0.0097 (18)
K21.00000.00000.3016 (18)0.0132 (15)
Lu10.98918 (12)0.49459 (6)0.30267 (5)0.0067 (3)
Lu20.65254 (9)0.82627 (5)0.04309 (7)0.0059 (3)
F10.66670.33330.2564 (15)0.011 (3)
F20.33330.66670.0886 (13)0.002 (3)
F30.9664 (15)0.4832 (7)0.4769 (10)0.007 (3)
F40.6323 (15)0.8161 (8)0.1329 (10)0.012 (3)
F50.6626 (11)0.9970 (11)0.1693 (16)0.0178 (14)
F61.2229 (8)0.7771 (8)0.3416 (8)0.014 (2)
F70.8881 (9)1.1119 (9)0.0106 (8)0.016 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
K10.013 (2)0.013 (2)0.004 (4)0.0063 (11)0.0000.000
K20.014 (2)0.014 (2)0.011 (4)0.0070 (10)0.0000.000
Lu10.0087 (4)0.0085 (4)0.0030 (5)0.0043 (2)0.0005 (5)0.0002 (2)
Lu20.0075 (4)0.0071 (4)0.0034 (4)0.0037 (2)0.0004 (6)0.0002 (3)
F10.013 (4)0.013 (4)0.009 (5)0.0065 (19)0.0000.000
F20.003 (3)0.003 (3)0.002 (5)0.0013 (17)0.0000.000
F30.009 (5)0.005 (4)0.009 (6)0.004 (3)0.006 (4)0.003 (2)
F40.011 (5)0.017 (5)0.006 (6)0.005 (2)0.002 (4)0.0008 (19)
F50.021 (3)0.019 (3)0.007 (3)0.004 (3)0.004 (2)0.002 (3)
F60.016 (4)0.016 (4)0.008 (5)0.007 (5)0.000 (2)0.000 (2)
F70.016 (4)0.016 (4)0.011 (5)0.004 (5)0.002 (2)0.002 (2)
Geometric parameters (Å, º) top
K1—F3i2.722 (14)Lu1—Lu1xii3.8905 (16)
K1—F3ii2.722 (14)Lu1—Lu1xv3.8905 (16)
K1—F3iii2.722 (14)Lu2—F52.130 (17)
K1—F12.74 (3)Lu2—F5xvi2.130 (17)
K1—F6ii3.12 (2)Lu2—F7vi2.167 (3)
K1—F6i3.12 (2)Lu2—F72.167 (3)
K1—F6iii3.12 (2)Lu2—F22.302 (4)
K1—F7iv3.124 (13)Lu2—F42.320 (13)
K1—F7v3.124 (13)Lu2—F3xvii2.327 (6)
K1—F7vi3.124 (13)Lu2—F3iii2.327 (6)
K1—F5vii3.125 (18)Lu2—Lu2v3.8505 (12)
K1—F5vi3.125 (18)Lu2—Lu2xviii3.8505 (12)
K2—F4viii2.702 (14)Lu2—Lu1xvii3.8725 (12)
K2—F4ix2.702 (14)Lu2—Lu1iii3.8725 (12)
K2—F4x2.702 (14)F1—Lu1xii2.327 (5)
K2—F6xi3.148 (12)F1—Lu1xv2.327 (5)
K2—F6xii3.148 (12)F2—Lu2xviii2.302 (4)
K2—F6iv3.148 (12)F2—Lu2v2.302 (4)
K2—F7x3.16 (3)F3—Lu2x2.327 (6)
K2—F7viii3.16 (3)F3—Lu2xiv2.327 (6)
K2—F7ix3.16 (3)F3—K1viii2.722 (14)
K2—F5xiii3.21 (2)F4—Lu1xvii2.328 (6)
K2—F5iv3.21 (2)F4—Lu1iii2.328 (6)
K2—F5xi3.21 (2)F4—K2ii2.702 (14)
Lu1—F6xi2.165 (3)F5—Lu1xix2.197 (17)
Lu1—F62.165 (3)F5—K1xx3.125 (18)
Lu1—F5vii2.197 (17)F5—K2xx3.21 (2)
Lu1—F5vi2.197 (17)F6—Lu1xxi2.165 (3)
Lu1—F32.298 (13)F6—K1viii3.12 (2)
Lu1—F12.327 (5)F6—K2xx3.148 (12)
Lu1—F4x2.328 (6)F7—Lu2xix2.167 (3)
Lu1—F4xiv2.328 (6)F7—K1xx3.124 (13)
Lu1—Lu2x3.8725 (12)F7—K2ii3.16 (3)
Lu1—Lu2xiv3.8725 (12)
F3i—K1—F3ii108.8 (5)F1—Lu1—F4x66.2 (3)
F3i—K1—F3iii108.8 (5)F6xi—Lu1—F4xiv141.2 (4)
F3ii—K1—F3iii108.8 (5)F6—Lu1—F4xiv80.0 (4)
F3i—K1—F1110.1 (5)F5vii—Lu1—F4xiv141.1 (4)
F3ii—K1—F1110.1 (5)F5vi—Lu1—F4xiv81.3 (4)
F3iii—K1—F1110.1 (5)F3—Lu1—F4xiv66.5 (3)
F3i—K1—F6ii57.9 (4)F1—Lu1—F4xiv66.2 (3)
F3ii—K1—F6ii57.9 (4)F4x—Lu1—F4xiv101.5 (6)
F3iii—K1—F6ii99.4 (8)F6xi—Lu1—Lu2x73.8 (3)
F1—K1—F6ii150.5 (3)F6—Lu1—Lu2x109.5 (3)
F3i—K1—F6i57.9 (4)F5vii—Lu1—Lu2x111.5 (4)
F3ii—K1—F6i99.4 (8)F5vi—Lu1—Lu2x164.5 (2)
F3iii—K1—F6i57.9 (4)F3—Lu1—Lu2x33.39 (11)
F1—K1—F6i150.5 (3)F1—Lu1—Lu2x86.0 (4)
F6ii—K1—F6i50.5 (5)F4x—Lu1—Lu2x33.5 (3)
F3i—K1—F6iii99.4 (8)F4xiv—Lu1—Lu2x86.3 (3)
F3ii—K1—F6iii57.9 (4)F6xi—Lu1—Lu2xiv109.5 (3)
F3iii—K1—F6iii57.9 (4)F6—Lu1—Lu2xiv73.8 (3)
F1—K1—F6iii150.5 (3)F5vii—Lu1—Lu2xiv164.5 (2)
F6ii—K1—F6iii50.5 (5)F5vi—Lu1—Lu2xiv111.5 (4)
F6i—K1—F6iii50.5 (5)F3—Lu1—Lu2xiv33.39 (11)
F3i—K1—F7iv58.81 (15)F1—Lu1—Lu2xiv86.0 (4)
F3ii—K1—F7iv58.81 (15)F4x—Lu1—Lu2xiv86.3 (3)
F3iii—K1—F7iv150.8 (10)F4xiv—Lu1—Lu2xiv33.5 (3)
F1—K1—F7iv99.1 (5)Lu2x—Lu1—Lu2xiv59.63 (3)
F6ii—K1—F7iv51.4 (3)F6xi—Lu1—Lu1xii110.1 (3)
F6i—K1—F7iv96.1 (6)F6—Lu1—Lu1xii163.5 (3)
F6iii—K1—F7iv96.1 (6)F5vii—Lu1—Lu1xii74.8 (2)
F3i—K1—F7v58.81 (15)F5vi—Lu1—Lu1xii109.8 (3)
F3ii—K1—F7v150.8 (10)F3—Lu1—Lu1xii86.6 (2)
F3iii—K1—F7v58.81 (15)F1—Lu1—Lu1xii33.30 (19)
F1—K1—F7v99.1 (5)F4x—Lu1—Lu1xii33.3 (2)
F6ii—K1—F7v96.1 (6)F4xiv—Lu1—Lu1xii86.5 (2)
F6i—K1—F7v51.4 (3)Lu2x—Lu1—Lu1xii59.846 (14)
F6iii—K1—F7v96.1 (6)Lu2xiv—Lu1—Lu1xii89.705 (14)
F7iv—K1—F7v117.6 (3)F6xi—Lu1—Lu1xv163.5 (3)
F3i—K1—F7vi150.8 (10)F6—Lu1—Lu1xv110.1 (3)
F3ii—K1—F7vi58.81 (15)F5vii—Lu1—Lu1xv109.8 (3)
F3iii—K1—F7vi58.81 (15)F5vi—Lu1—Lu1xv74.8 (2)
F1—K1—F7vi99.1 (5)F3—Lu1—Lu1xv86.6 (2)
F6ii—K1—F7vi96.1 (6)F1—Lu1—Lu1xv33.30 (19)
F6i—K1—F7vi96.1 (6)F4x—Lu1—Lu1xv86.5 (2)
F6iii—K1—F7vi51.4 (3)F4xiv—Lu1—Lu1xv33.3 (2)
F7iv—K1—F7vi117.6 (3)Lu2x—Lu1—Lu1xv89.705 (14)
F7v—K1—F7vi117.6 (3)Lu2xiv—Lu1—Lu1xv59.846 (14)
F3i—K1—F5vii100.6 (2)Lu1xii—Lu1—Lu1xv60.0
F3ii—K1—F5vii58.1 (4)F5—Lu2—F5xvi77.4 (8)
F3iii—K1—F5vii150.5 (4)F5—Lu2—F7vi121.2 (4)
F1—K1—F5vii59.3 (5)F5xvi—Lu2—F7vi74.9 (4)
F6ii—K1—F5vii94.5 (4)F5—Lu2—F774.9 (4)
F6i—K1—F5vii144.4 (6)F5xvi—Lu2—F7121.2 (4)
F6iii—K1—F5vii116.1 (4)F7vi—Lu2—F777.1 (6)
F7iv—K1—F5vii49.4 (3)F5—Lu2—F280.2 (4)
F7v—K1—F5vii145.1 (6)F5xvi—Lu2—F280.2 (4)
F7vi—K1—F5vii94.1 (2)F7vi—Lu2—F2141.5 (3)
F3i—K1—F5vi150.5 (4)F7—Lu2—F2141.5 (3)
F3ii—K1—F5vi58.1 (4)F5—Lu2—F4141.3 (4)
F3iii—K1—F5vi100.6 (2)F5xvi—Lu2—F4141.3 (4)
F1—K1—F5vi59.3 (5)F7vi—Lu2—F481.3 (4)
F6ii—K1—F5vi116.1 (4)F7—Lu2—F481.3 (4)
F6i—K1—F5vi144.4 (6)F2—Lu2—F4101.6 (5)
F6iii—K1—F5vi94.5 (4)F5—Lu2—F3xvii79.8 (5)
F7iv—K1—F5vi94.1 (2)F5xvi—Lu2—F3xvii142.6 (4)
F7v—K1—F5vi145.1 (6)F7vi—Lu2—F3xvii142.5 (4)
F7vi—K1—F5vi49.4 (3)F7—Lu2—F3xvii80.0 (4)
F5vii—K1—F5vi50.0 (4)F2—Lu2—F3xvii66.9 (3)
F4viii—K2—F4ix110.3 (6)F4—Lu2—F3xvii66.2 (3)
F4viii—K2—F4x110.3 (6)F5—Lu2—F3iii142.6 (4)
F4ix—K2—F4x110.3 (6)F5xvi—Lu2—F3iii79.8 (5)
F4viii—K2—F6xi58.64 (15)F7vi—Lu2—F3iii80.0 (4)
F4ix—K2—F6xi151.8 (11)F7—Lu2—F3iii142.5 (4)
F4x—K2—F6xi58.64 (15)F2—Lu2—F3iii66.9 (3)
F4viii—K2—F6xii151.8 (11)F4—Lu2—F3iii66.2 (3)
F4ix—K2—F6xii58.64 (15)F3xvii—Lu2—F3iii101.9 (6)
F4x—K2—F6xii58.64 (15)F5—Lu2—Lu2v110.0 (3)
F6xi—K2—F6xii117.3 (3)F5xvi—Lu2—Lu2v73.5 (2)
F4viii—K2—F6iv58.64 (15)F7vi—Lu2—Lu2v110.1 (3)
F4ix—K2—F6iv58.64 (15)F7—Lu2—Lu2v165.3 (3)
F4x—K2—F6iv151.8 (11)F2—Lu2—Lu2v33.26 (17)
F6xi—K2—F6iv117.3 (3)F4—Lu2—Lu2v87.0 (2)
F6xii—K2—F6iv117.3 (3)F3xvii—Lu2—Lu2v87.1 (2)
F4viii—K2—F7x59.3 (4)F3iii—Lu2—Lu2v34.2 (2)
F4ix—K2—F7x101.0 (8)F5—Lu2—Lu2xviii73.5 (2)
F4x—K2—F7x59.3 (4)F5xvi—Lu2—Lu2xviii110.0 (3)
F6xi—K2—F7x50.8 (4)F7vi—Lu2—Lu2xviii165.3 (3)
F6xii—K2—F7x95.6 (6)F7—Lu2—Lu2xviii110.1 (3)
F6iv—K2—F7x95.6 (6)F2—Lu2—Lu2xviii33.26 (17)
F4viii—K2—F7viii59.3 (4)F4—Lu2—Lu2xviii87.0 (2)
F4ix—K2—F7viii59.3 (4)F3xvii—Lu2—Lu2xviii34.2 (2)
F4x—K2—F7viii101.0 (8)F3iii—Lu2—Lu2xviii87.1 (2)
F6xi—K2—F7viii95.6 (6)Lu2v—Lu2—Lu2xviii60.0
F6xii—K2—F7viii95.6 (6)F5—Lu2—Lu1xvii109.4 (4)
F6iv—K2—F7viii50.8 (4)F5xvi—Lu2—Lu1xvii163.8 (3)
F7x—K2—F7viii50.6 (5)F7vi—Lu2—Lu1xvii111.5 (3)
F4viii—K2—F7ix101.0 (8)F7—Lu2—Lu1xvii75.0 (3)
F4ix—K2—F7ix59.3 (4)F2—Lu2—Lu1xvii86.5 (3)
F4x—K2—F7ix59.3 (4)F4—Lu2—Lu1xvii33.65 (11)
F6xi—K2—F7ix95.6 (6)F3xvii—Lu2—Lu1xvii32.9 (3)
F6xii—K2—F7ix50.8 (4)F3iii—Lu2—Lu1xvii86.6 (3)
F6iv—K2—F7ix95.6 (6)Lu2v—Lu2—Lu1xvii90.295 (15)
F7x—K2—F7ix50.6 (5)Lu2xviii—Lu2—Lu1xvii60.187 (13)
F7viii—K2—F7ix50.6 (5)F5—Lu2—Lu1iii163.8 (3)
F4viii—K2—F5xiii150.0 (5)F5xvi—Lu2—Lu1iii109.4 (4)
F4ix—K2—F5xiii59.0 (4)F7vi—Lu2—Lu1iii75.0 (3)
F4x—K2—F5xiii99.6 (3)F7—Lu2—Lu1iii111.5 (3)
F6xi—K2—F5xiii143.6 (6)F2—Lu2—Lu1iii86.5 (3)
F6xii—K2—F5xiii50.9 (3)F4—Lu2—Lu1iii33.65 (11)
F6iv—K2—F5xiii95.5 (3)F3xvii—Lu2—Lu1iii86.6 (3)
F7x—K2—F5xiii146.0 (6)F3iii—Lu2—Lu1iii32.9 (3)
F7viii—K2—F5xiii118.3 (4)Lu2v—Lu2—Lu1iii60.187 (13)
F7ix—K2—F5xiii96.3 (4)Lu2xviii—Lu2—Lu1iii90.295 (14)
F4viii—K2—F5iv150.0 (5)Lu1xvii—Lu2—Lu1iii60.31 (3)
F4ix—K2—F5iv99.6 (3)Lu1—F1—Lu1xii113.4 (4)
F4x—K2—F5iv59.0 (4)Lu1—F1—Lu1xv113.4 (4)
F6xi—K2—F5iv95.5 (3)Lu1xii—F1—Lu1xv113.4 (4)
F6xii—K2—F5iv50.9 (3)Lu1—F1—K1105.2 (5)
F6iv—K2—F5iv143.6 (6)Lu1xii—F1—K1105.2 (5)
F7x—K2—F5iv118.3 (4)Lu1xv—F1—K1105.2 (5)
F7viii—K2—F5iv146.0 (6)Lu2xviii—F2—Lu2v113.5 (3)
F7ix—K2—F5iv96.3 (4)Lu2xviii—F2—Lu2113.5 (3)
F5xiii—K2—F5iv49.0 (4)Lu2v—F2—Lu2113.5 (3)
F4viii—K2—F5xi99.6 (3)Lu1—F3—Lu2x113.7 (3)
F4ix—K2—F5xi59.0 (4)Lu1—F3—Lu2xiv113.7 (3)
F4x—K2—F5xi150.0 (5)Lu2x—F3—Lu2xiv111.6 (5)
F6xi—K2—F5xi143.6 (6)Lu1—F3—K1viii106.2 (6)
F6xii—K2—F5xi95.5 (3)Lu2x—F3—K1viii105.4 (4)
F6iv—K2—F5xi50.9 (3)Lu2xiv—F3—K1viii105.4 (4)
F7x—K2—F5xi146.0 (6)Lu2—F4—Lu1xvii112.8 (4)
F7viii—K2—F5xi96.3 (4)Lu2—F4—Lu1iii112.8 (4)
F7ix—K2—F5xi118.3 (4)Lu1xvii—F4—Lu1iii113.3 (5)
F5xiii—K2—F5xi50.4 (4)Lu2—F4—K2ii105.1 (6)
F5iv—K2—F5xi93.4 (7)Lu1xvii—F4—K2ii105.9 (5)
F6xi—Lu1—F676.0 (6)Lu1iii—F4—K2ii105.9 (5)
F6xi—Lu1—F5vii77.6 (4)Lu2—F5—Lu1xix144.8 (4)
F6—Lu1—F5vii121.7 (4)Lu2—F5—K1xx98.1 (8)
F6xi—Lu1—F5vi121.7 (4)Lu1xix—F5—K1xx96.9 (4)
F6—Lu1—F5vi77.6 (4)Lu2—F5—K2xx100.8 (4)
F5vii—Lu1—F5vi73.8 (7)Lu1xix—F5—K2xx94.1 (8)
F6xi—Lu1—F379.4 (3)K1xx—F5—K2xx128.8 (3)
F6—Lu1—F379.4 (4)Lu1xxi—F6—Lu1147.0 (6)
F5vii—Lu1—F3143.1 (4)Lu1xxi—F6—K1viii97.4 (3)
F5vi—Lu1—F3143.1 (4)Lu1—F6—K1viii97.4 (3)
F6xi—Lu1—F1141.9 (3)Lu1xxi—F6—K2xx96.6 (3)
F6—Lu1—F1141.9 (3)Lu1—F6—K2xx96.6 (3)
F5vii—Lu1—F180.4 (4)K1viii—F6—K2xx129.1 (8)
F5vi—Lu1—F180.4 (4)Lu2xix—F7—Lu2150.5 (6)
F3—Lu1—F1101.2 (5)Lu2xix—F7—K1xx97.3 (3)
F6xi—Lu1—F4x80.0 (4)Lu2—F7—K1xx97.3 (3)
F6—Lu1—F4x141.2 (4)Lu2xix—F7—K2ii95.3 (3)
F5vii—Lu1—F4x81.3 (5)Lu2—F7—K2ii95.3 (3)
F5vi—Lu1—F4x141.1 (4)K1xx—F7—K2ii128.6 (8)
F3—Lu1—F4x66.5 (3)
Symmetry codes: (i) xy, x1, z1/2; (ii) x+2, y+1, z1/2; (iii) y, x+y+1, z1/2; (iv) x, y1, z; (v) x+y, x+1, z; (vi) y+2, xy+1, z; (vii) y+2, x+1, z; (viii) x+2, y+1, z+1/2; (ix) xy+1, x1, z+1/2; (x) y, x+y, z+1/2; (xi) y+2, xy, z; (xii) x+y+1, x+1, z; (xiii) x, xy, z; (xiv) xy+1, x, z+1/2; (xv) y+1, xy, z; (xvi) x, xy+1, z; (xvii) xy, x, z1/2; (xviii) y+1, xy+1, z; (xix) x+y+1, x+2, z; (xx) x, y+1, z; (xxi) x+y+2, x+2, z.
 

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