Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520615017916/bp5082sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520615017916/bp5082CsY2F7sup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520615017916/bp5082RbSm2F7sup3.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520615017916/bp5082CsGd2F7sup4.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520615017916/bp5082KY3F10sup5.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520615017916/bp5082RbY3F10sup6.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520615017916/bp5082RbSm3F10sup7.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520615017916/bp5082RbGd3F10sup8.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2052520615017916/bp5082KLu3F10sup9.hkl | |
Portable Document Format (PDF) file https://doi.org/10.1107/S2052520615017916/bp5082sup10.pdf |
CCDC references: 1427210; 1427211; 1427212; 1427213; 1427214; 1427215; 1427216; 1427217
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.
CsF7Y2 | Dx = 4.490 Mg m−3 |
Mr = 443.73 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, Pnna | Cell parameters from 4730 reflections |
a = 13.6028 (14) Å | θ = 3.0–26.7° |
b = 12.3072 (13) Å | µ = 23.12 mm−1 |
c = 7.8426 (8) Å | T = 293 K |
V = 1312.9 (2) Å3 | Prism, colorless |
Z = 8 | 0.23 × 0.14 × 0.12 mm |
F(000) = 1568 |
Rigaku AFC8S diffractometer | 1182 independent reflections |
Radiation source: fine-focus sealed tube | 1009 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.071 |
Detector resolution: 14.6199 pixels mm-1 | θmax = 25.2°, θmin = 3.0° |
ω scans | h = −15→16 |
Absorption correction: multi-scan REQAB, CrystalClear | k = −14→14 |
Tmin = 0.690, Tmax = 1.000 | l = −9→9 |
10355 measured reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary 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 = 1.14 | Δρmax = 1.03 e Å−3 |
1182 reflections | Δρmin = −1.40 e Å−3 |
116 parameters | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
12 restraints | Extinction coefficient: 0.00085 (11) |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Cs1 | 0.58120 (4) | 0.92160 (4) | 0.23015 (7) | 0.0262 (2) | |
Y1 | 0.43211 (7) | 1.2500 | 0.2500 | 0.0111 (3) | |
Y2 | 0.65951 (6) | 1.26353 (7) | 0.02423 (9) | 0.0189 (2) | |
Y3 | 0.2500 | 1.0000 | 0.24907 (14) | 0.0155 (3) | |
F1 | 0.8056 (4) | 1.3074 (5) | −0.0910 (7) | 0.0330 (13) | |
F2 | 0.1461 (8) | 1.0764 (9) | 0.4286 (15) | 0.021 (2) | 0.50 |
F2A | 0.1726 (9) | 1.0449 (8) | 0.4919 (14) | 0.021 (3) | 0.50 |
F3 | 0.6408 (8) | 1.3194 (7) | −0.2542 (12) | 0.023 (2) | 0.50 |
F4 | 0.5839 (3) | 1.3467 (3) | 0.2611 (6) | 0.0173 (10) | |
F5 | 0.7573 (5) | 1.2500 | 0.2500 | 0.0169 (13) | |
F6 | 0.4975 (3) | 1.2620 (4) | −0.0104 (6) | 0.0201 (10) | |
F7 | 0.3917 (4) | 1.0812 (4) | 0.1747 (6) | 0.0232 (11) | |
F8 | 0.3119 (9) | 0.8823 (9) | 0.0814 (16) | 0.032 (3) | 0.50 |
F8A | 0.2808 (7) | 0.9172 (7) | −0.0057 (13) | 0.016 (2) | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cs1 | 0.0364 (4) | 0.0129 (3) | 0.0293 (3) | 0.0004 (2) | 0.0008 (3) | 0.0009 (2) |
Y1 | 0.0087 (5) | 0.0139 (5) | 0.0108 (5) | 0.000 | 0.000 | 0.0010 (4) |
Y2 | 0.0103 (4) | 0.0375 (5) | 0.0090 (4) | −0.0023 (3) | 0.0004 (3) | 0.0019 (3) |
Y3 | 0.0112 (5) | 0.0250 (6) | 0.0101 (5) | 0.0018 (4) | 0.000 | 0.000 |
F1 | 0.019 (3) | 0.055 (3) | 0.025 (3) | 0.001 (2) | 0.009 (2) | −0.005 (2) |
F2 | 0.020 (5) | 0.021 (5) | 0.021 (5) | 0.001 (4) | 0.004 (4) | −0.007 (4) |
F2A | 0.030 (6) | 0.020 (5) | 0.014 (5) | 0.005 (4) | 0.005 (4) | −0.002 (4) |
F3 | 0.029 (6) | 0.023 (5) | 0.017 (5) | 0.008 (4) | −0.006 (5) | −0.002 (4) |
F4 | 0.016 (2) | 0.009 (2) | 0.027 (3) | 0.0007 (17) | 0.005 (2) | 0.0008 (18) |
F5 | 0.013 (3) | 0.028 (3) | 0.010 (3) | 0.000 | 0.000 | −0.002 (3) |
F6 | 0.009 (2) | 0.037 (3) | 0.014 (2) | 0.0014 (19) | 0.0009 (18) | 0.005 (2) |
F7 | 0.025 (3) | 0.017 (2) | 0.028 (3) | −0.005 (2) | 0.000 (2) | −0.005 (2) |
F8 | 0.043 (8) | 0.029 (6) | 0.025 (6) | 0.005 (5) | 0.006 (6) | −0.002 (5) |
F8A | 0.023 (6) | 0.013 (4) | 0.013 (5) | 0.008 (4) | 0.000 (4) | −0.008 (4) |
Cs1—F4i | 2.853 (4) | Y3—F2 | 2.205 (10) |
Cs1—F2Aii | 2.933 (11) | Y3—F2Avii | 2.245 (10) |
Cs1—F6iii | 3.024 (4) | Y3—F2A | 2.245 (10) |
Cs1—F6iv | 3.037 (5) | Y3—F7vii | 2.248 (5) |
Cs1—F5v | 3.051 (5) | Y3—F7 | 2.248 (5) |
Cs1—F7iv | 3.197 (5) | Y3—F8A | 2.281 (9) |
Cs1—F8Avi | 3.236 (11) | Y3—F8Avii | 2.281 (9) |
Cs1—F8Aiv | 3.250 (10) | Y3—F3viii | 2.674 (10) |
Cs1—F7 | 3.270 (5) | Y3—F3iii | 2.674 (10) |
Cs1—F3iii | 3.273 (10) | F1—Y1vi | 2.239 (5) |
Cs1—F2ii | 3.402 (12) | F1—Y3xi | 2.787 (6) |
Cs1—F2vii | 3.461 (12) | F1—Cs1xiii | 3.515 (5) |
Y1—F7 | 2.229 (4) | F2—F2A | 0.726 (11) |
Y1—F7i | 2.229 (4) | F2—Y2viii | 2.116 (10) |
Y1—F6i | 2.232 (4) | F2—Cs1xiv | 3.402 (12) |
Y1—F6 | 2.232 (4) | F2—Cs1vii | 3.461 (12) |
Y1—F1viii | 2.239 (5) | F2A—Y2viii | 2.377 (10) |
Y1—F1ix | 2.239 (5) | F2A—Cs1xiv | 2.933 (11) |
Y1—F4 | 2.385 (4) | F3—F8xv | 1.635 (16) |
Y1—F4i | 2.385 (4) | F3—F3xii | 1.710 (18) |
Y1—Y2i | 3.5682 (12) | F3—Y2xii | 2.365 (9) |
Y1—Y2 | 3.5682 (12) | F3—Y3xi | 2.674 (10) |
Y1—Y3 | 3.9501 (7) | F3—Cs1xv | 3.273 (10) |
Y1—Y3x | 3.9501 (7) | F4—Y2i | 2.394 (4) |
Y2—F8iv | 2.014 (10) | F4—Cs1i | 2.853 (4) |
Y2—F2xi | 2.116 (10) | F5—Y2i | 2.221 (4) |
Y2—F6 | 2.221 (5) | F5—Cs1xiii | 3.051 (5) |
Y2—F5 | 2.221 (4) | F5—Cs1v | 3.051 (5) |
Y2—F1 | 2.249 (5) | F6—Cs1xv | 3.024 (4) |
Y2—F3 | 2.304 (10) | F6—Cs1iv | 3.037 (5) |
Y2—F4 | 2.357 (4) | F7—Cs1iv | 3.197 (5) |
Y2—F3xii | 2.365 (9) | F8—F8A | 0.912 (12) |
Y2—F8Aiv | 2.373 (9) | F8—F3iii | 1.635 (16) |
Y2—F2Axi | 2.377 (10) | F8—Y2iv | 2.014 (10) |
Y2—F4i | 2.394 (4) | F8—Cs1iv | 3.729 (12) |
Y2—Y2i | 3.5569 (15) | F8A—Y2iv | 2.373 (9) |
Y3—F8 | 2.130 (10) | F8A—Cs1ix | 3.236 (11) |
Y3—F8vii | 2.130 (10) | F8A—Cs1iv | 3.250 (10) |
Y3—F2vii | 2.205 (10) | ||
F4i—Cs1—F2Aii | 57.3 (2) | F3—Y2—F2Axi | 67.1 (4) |
F4i—Cs1—F6iii | 129.62 (13) | F4—Y2—F2Axi | 71.7 (3) |
F2Aii—Cs1—F6iii | 89.2 (2) | F3xii—Y2—F2Axi | 109.9 (3) |
F4i—Cs1—F6iv | 139.64 (12) | F8Aiv—Y2—F2Axi | 153.8 (4) |
F2Aii—Cs1—F6iv | 163.0 (2) | F8iv—Y2—F4i | 82.4 (3) |
F6iii—Cs1—F6iv | 76.93 (14) | F2xi—Y2—F4i | 137.7 (3) |
F4i—Cs1—F5v | 132.95 (12) | F6—Y2—F4i | 69.82 (16) |
F2Aii—Cs1—F5v | 90.9 (2) | F5—Y2—F4i | 69.77 (15) |
F6iii—Cs1—F5v | 76.76 (10) | F1—Y2—F4i | 142.95 (19) |
F6iv—Cs1—F5v | 76.56 (10) | F3—Y2—F4i | 142.0 (3) |
F4i—Cs1—F7iv | 91.89 (12) | F4—Y2—F4i | 60.28 (18) |
F2Aii—Cs1—F7iv | 134.0 (2) | F3xii—Y2—F4i | 109.8 (2) |
F6iii—Cs1—F7iv | 134.61 (12) | F8Aiv—Y2—F4i | 70.1 (3) |
F6iv—Cs1—F7iv | 57.93 (11) | F2Axi—Y2—F4i | 132.0 (3) |
F5v—Cs1—F7iv | 87.72 (9) | F8iv—Y2—Y2i | 109.0 (4) |
F4i—Cs1—F8Avi | 91.07 (18) | F2xi—Y2—Y2i | 116.1 (3) |
F2Aii—Cs1—F8Avi | 93.3 (3) | F6—Y2—Y2i | 96.94 (12) |
F6iii—Cs1—F8Avi | 130.71 (17) | F5—Y2—Y2i | 36.80 (14) |
F6iv—Cs1—F8Avi | 88.5 (2) | F1—Y2—Y2i | 115.00 (14) |
F5v—Cs1—F8Avi | 54.01 (15) | F3—Y2—Y2i | 166.3 (2) |
F7iv—Cs1—F8Avi | 50.41 (19) | F4—Y2—Y2i | 41.91 (11) |
F4i—Cs1—F8Aiv | 52.79 (17) | F3xii—Y2—Y2i | 148.3 (2) |
F2Aii—Cs1—F8Aiv | 80.9 (3) | F8Aiv—Y2—Y2i | 88.5 (2) |
F6iii—Cs1—F8Aiv | 164.9 (2) | F2Axi—Y2—Y2i | 101.5 (3) |
F6iv—Cs1—F8Aiv | 110.51 (18) | F4i—Y2—Y2i | 41.13 (11) |
F5v—Cs1—F8Aiv | 91.96 (18) | F8—Y3—F8vii | 103.8 (7) |
F7iv—Cs1—F8Aiv | 53.26 (18) | F8—Y3—F2vii | 81.4 (5) |
F8Avi—Cs1—F8Aiv | 39.7 (3) | F8vii—Y3—F2vii | 159.6 (4) |
F4i—Cs1—F7 | 54.06 (12) | F8—Y3—F2 | 159.6 (4) |
F2Aii—Cs1—F7 | 97.0 (2) | F8vii—Y3—F2 | 81.4 (5) |
F6iii—Cs1—F7 | 101.56 (13) | F2vii—Y3—F2 | 100.7 (7) |
F6iv—Cs1—F7 | 95.37 (12) | F8—Y3—F2Avii | 99.8 (5) |
F5v—Cs1—F7 | 171.93 (10) | F8vii—Y3—F2Avii | 151.2 (4) |
F7iv—Cs1—F7 | 88.01 (12) | F2vii—Y3—F2Avii | 18.7 (3) |
F8Avi—Cs1—F7 | 126.80 (17) | F2—Y3—F2Avii | 82.2 (6) |
F8Aiv—Cs1—F7 | 91.0 (2) | F8—Y3—F2A | 151.2 (4) |
F4i—Cs1—F3iii | 113.28 (19) | F8vii—Y3—F2A | 99.8 (5) |
F2Aii—Cs1—F3iii | 124.2 (3) | F2vii—Y3—F2A | 82.2 (6) |
F6iii—Cs1—F3iii | 53.03 (19) | F2—Y3—F2A | 18.7 (3) |
F6iv—Cs1—F3iii | 53.86 (19) | F2Avii—Y3—F2A | 63.9 (6) |
F5v—Cs1—F3iii | 113.34 (19) | F8—Y3—F7vii | 82.9 (4) |
F7iv—Cs1—F3iii | 98.02 (19) | F8vii—Y3—F7vii | 78.6 (3) |
F8Avi—Cs1—F3iii | 142.0 (2) | F2vii—Y3—F7vii | 121.7 (3) |
F8Aiv—Cs1—F3iii | 142.0 (3) | F2—Y3—F7vii | 78.8 (3) |
F7—Cs1—F3iii | 60.56 (19) | F2Avii—Y3—F7vii | 120.8 (3) |
F4i—Cs1—F2ii | 54.41 (19) | F2A—Y3—F7vii | 85.8 (3) |
F2Aii—Cs1—F2ii | 10.1 (3) | F8—Y3—F7 | 78.6 (3) |
F6iii—Cs1—F2ii | 85.8 (2) | F8vii—Y3—F7 | 82.9 (4) |
F6iv—Cs1—F2ii | 162.7 (2) | F2vii—Y3—F7 | 78.8 (3) |
F5v—Cs1—F2ii | 99.25 (19) | F2—Y3—F7 | 121.7 (3) |
F7iv—Cs1—F2ii | 139.3 (2) | F2Avii—Y3—F7 | 85.8 (3) |
F8Avi—Cs1—F2ii | 102.7 (3) | F2A—Y3—F7 | 120.8 (3) |
F8Aiv—Cs1—F2ii | 86.2 (2) | F7vii—Y3—F7 | 149.9 (3) |
F7—Cs1—F2ii | 88.4 (2) | F8—Y3—F8A | 23.5 (3) |
F3iii—Cs1—F2ii | 115.2 (3) | F8vii—Y3—F8A | 80.5 (5) |
F4i—Cs1—F2vii | 89.6 (2) | F2vii—Y3—F8A | 104.5 (4) |
F2Aii—Cs1—F2vii | 92.4 (2) | F2—Y3—F8A | 150.1 (4) |
F6iii—Cs1—F2vii | 52.11 (19) | F2Avii—Y3—F8A | 123.2 (4) |
F6iv—Cs1—F2vii | 86.9 (2) | F2A—Y3—F8A | 159.9 (4) |
F5v—Cs1—F2vii | 128.69 (18) | F7vii—Y3—F8A | 74.4 (3) |
F7iv—Cs1—F2vii | 123.3 (2) | F7—Y3—F8A | 79.3 (3) |
F8Avi—Cs1—F2vii | 173.7 (3) | F8—Y3—F8Avii | 80.5 (5) |
F8Aiv—Cs1—F2vii | 139.1 (2) | F8vii—Y3—F8Avii | 23.5 (3) |
F7—Cs1—F2vii | 49.55 (18) | F2vii—Y3—F8Avii | 150.1 (4) |
F3iii—Cs1—F2vii | 33.1 (3) | F2—Y3—F8Avii | 104.5 (4) |
F2ii—Cs1—F2vii | 82.8 (3) | F2Avii—Y3—F8Avii | 159.9 (4) |
F7—Y1—F7i | 151.4 (3) | F2A—Y3—F8Avii | 123.2 (4) |
F7—Y1—F6i | 106.19 (17) | F7vii—Y3—F8Avii | 79.3 (3) |
F7i—Y1—F6i | 85.28 (18) | F7—Y3—F8Avii | 74.4 (3) |
F7—Y1—F6 | 85.28 (18) | F8A—Y3—F8Avii | 57.7 (5) |
F7i—Y1—F6 | 106.19 (17) | F8—Y3—F3viii | 141.2 (4) |
F6i—Y1—F6 | 133.0 (2) | F8vii—Y3—F3viii | 37.7 (4) |
F7—Y1—F1viii | 70.4 (2) | F2vii—Y3—F3viii | 135.8 (4) |
F7i—Y1—F1viii | 87.5 (2) | F2—Y3—F3viii | 45.2 (4) |
F6i—Y1—F1viii | 77.06 (18) | F2Avii—Y3—F3viii | 118.3 (4) |
F6—Y1—F1viii | 146.77 (19) | F2A—Y3—F3viii | 62.8 (4) |
F7—Y1—F1ix | 87.5 (2) | F7vii—Y3—F3viii | 83.7 (2) |
F7i—Y1—F1ix | 70.4 (2) | F7—Y3—F3viii | 96.0 (2) |
F6i—Y1—F1ix | 146.77 (19) | F8A—Y3—F3viii | 117.7 (3) |
F6—Y1—F1ix | 77.06 (18) | F8Avii—Y3—F3viii | 61.2 (3) |
F1viii—Y1—F1ix | 79.6 (3) | F8—Y3—F3iii | 37.7 (4) |
F7—Y1—F4 | 133.49 (17) | F8vii—Y3—F3iii | 141.2 (4) |
F7i—Y1—F4 | 74.87 (16) | F2vii—Y3—F3iii | 45.2 (4) |
F6i—Y1—F4 | 69.79 (16) | F2—Y3—F3iii | 135.8 (4) |
F6—Y1—F4 | 69.84 (16) | F2Avii—Y3—F3iii | 62.8 (4) |
F1viii—Y1—F4 | 143.36 (17) | F2A—Y3—F3iii | 118.3 (4) |
F1ix—Y1—F4 | 121.91 (18) | F7vii—Y3—F3iii | 96.0 (2) |
F7—Y1—F4i | 74.87 (16) | F7—Y3—F3iii | 83.7 (2) |
F7i—Y1—F4i | 133.49 (17) | F8A—Y3—F3iii | 61.2 (3) |
F6i—Y1—F4i | 69.84 (16) | F8Avii—Y3—F3iii | 117.7 (3) |
F6—Y1—F4i | 69.79 (16) | F3viii—Y3—F3iii | 178.9 (4) |
F1viii—Y1—F4i | 121.91 (18) | Y1vi—F1—Y2 | 145.8 (3) |
F1ix—Y1—F4i | 143.36 (17) | Y1vi—F1—Y3xi | 103.1 (2) |
F4—Y1—F4i | 60.0 (2) | Y2—F1—Y3xi | 98.34 (19) |
F7—Y1—Y2i | 107.56 (13) | Y1vi—F1—Cs1xiii | 103.76 (19) |
F7i—Y1—Y2i | 97.23 (13) | Y2—F1—Cs1xiii | 99.17 (17) |
F6i—Y1—Y2i | 36.63 (12) | Y3xi—F1—Cs1xiii | 98.10 (16) |
F6—Y1—Y2i | 96.41 (12) | F2A—F2—Y2viii | 102.2 (14) |
F1viii—Y1—Y2i | 112.04 (14) | F2A—F2—Y3 | 83.7 (13) |
F1ix—Y1—Y2i | 163.19 (15) | Y2viii—F2—Y3 | 124.6 (5) |
F4—Y1—Y2i | 41.79 (11) | F2A—F2—Cs1xiv | 44.9 (13) |
F4i—Y1—Y2i | 40.90 (11) | Y2viii—F2—Cs1xiv | 105.4 (4) |
F7—Y1—Y2 | 97.23 (13) | Y3—F2—Cs1xiv | 115.5 (4) |
F7i—Y1—Y2 | 107.56 (13) | F2A—F2—Cs1vii | 139.1 (16) |
F6i—Y1—Y2 | 96.41 (12) | Y2viii—F2—Cs1vii | 103.3 (4) |
F6—Y1—Y2 | 36.63 (12) | Y3—F2—Cs1vii | 106.8 (4) |
F1viii—Y1—Y2 | 163.19 (15) | Cs1xiv—F2—Cs1vii | 97.2 (3) |
F1ix—Y1—Y2 | 112.04 (14) | F2—F2A—Y3 | 77.5 (13) |
F4—Y1—Y2 | 40.90 (11) | F2—F2A—Y2viii | 60.5 (12) |
F4i—Y1—Y2 | 41.79 (11) | Y3—F2A—Y2viii | 111.7 (4) |
Y2i—Y1—Y2 | 59.79 (3) | F2—F2A—Cs1xiv | 125.0 (16) |
F7—Y1—Y3 | 28.20 (13) | Y3—F2A—Cs1xiv | 134.6 (4) |
F7i—Y1—Y3 | 124.89 (13) | Y2viii—F2A—Cs1xiv | 113.7 (4) |
F6i—Y1—Y3 | 101.53 (12) | F8xv—F3—F3xii | 120.2 (9) |
F6—Y1—Y3 | 107.45 (12) | F8xv—F3—Y2 | 147.7 (7) |
F1viii—Y1—Y3 | 43.41 (15) | F3xii—F3—Y2 | 70.4 (6) |
F1ix—Y1—Y3 | 76.27 (15) | F8xv—F3—Y2xii | 57.0 (5) |
F4—Y1—Y3 | 158.69 (10) | F3xii—F3—Y2xii | 66.6 (6) |
F4i—Y1—Y3 | 98.89 (10) | Y2—F3—Y2xii | 135.1 (4) |
Y2i—Y1—Y3 | 120.547 (18) | F8xv—F3—Y3xi | 52.8 (5) |
Y2—Y1—Y3 | 125.387 (18) | F3xii—F3—Y3xi | 146.1 (2) |
F7—Y1—Y3x | 124.89 (13) | Y2—F3—Y3xi | 100.2 (3) |
F7i—Y1—Y3x | 28.20 (13) | Y2xii—F3—Y3xi | 107.9 (4) |
F6i—Y1—Y3x | 107.45 (12) | F8xv—F3—Cs1xv | 98.7 (6) |
F6—Y1—Y3x | 101.53 (12) | F3xii—F3—Cs1xv | 112.67 (17) |
F1viii—Y1—Y3x | 76.27 (15) | Y2—F3—Cs1xv | 104.6 (3) |
F1ix—Y1—Y3x | 43.41 (15) | Y2xii—F3—Cs1xv | 103.4 (3) |
F4—Y1—Y3x | 98.89 (10) | Y3xi—F3—Cs1xv | 101.2 (3) |
F4i—Y1—Y3x | 158.69 (10) | Y2—F4—Y1 | 97.61 (16) |
Y2i—Y1—Y3x | 125.387 (18) | Y2—F4—Y2i | 96.96 (16) |
Y2—Y1—Y3x | 120.547 (18) | Y1—F4—Y2i | 96.61 (15) |
Y3—Y1—Y3x | 102.32 (2) | Y2—F4—Cs1i | 117.29 (16) |
F8iv—Y2—F2xi | 134.4 (5) | Y1—F4—Cs1i | 119.22 (17) |
F8iv—Y2—F6 | 97.7 (4) | Y2i—F4—Cs1i | 123.72 (18) |
F2xi—Y2—F6 | 83.0 (3) | Y2i—F5—Y2 | 106.4 (3) |
F8iv—Y2—F5 | 98.4 (4) | Y2i—F5—Cs1xiii | 116.26 (5) |
F2xi—Y2—F5 | 113.8 (3) | Y2—F5—Cs1xiii | 114.84 (5) |
F6—Y2—F5 | 133.74 (18) | Y2i—F5—Cs1v | 114.84 (5) |
F8iv—Y2—F1 | 83.0 (4) | Y2—F5—Cs1v | 116.26 (5) |
F2xi—Y2—F1 | 73.2 (3) | Cs1xiii—F5—Cs1v | 87.91 (17) |
F6—Y2—F1 | 146.09 (19) | Y2—F6—Y1 | 106.51 (19) |
F5—Y2—F1 | 79.0 (2) | Y2—F6—Cs1xv | 115.35 (17) |
F8iv—Y2—F3 | 84.1 (4) | Y1—F6—Cs1xv | 121.17 (18) |
F2xi—Y2—F3 | 51.4 (4) | Y2—F6—Cs1iv | 115.18 (18) |
F6—Y2—F3 | 77.1 (3) | Y1—F6—Cs1iv | 109.23 (17) |
F5—Y2—F3 | 147.6 (3) | Cs1xv—F6—Cs1iv | 88.66 (12) |
F1—Y2—F3 | 69.2 (3) | Y1—F7—Y3 | 123.9 (2) |
F8iv—Y2—F4 | 142.7 (3) | Y1—F7—Cs1iv | 104.16 (16) |
F2xi—Y2—F4 | 80.7 (3) | Y3—F7—Cs1iv | 110.60 (17) |
F6—Y2—F4 | 70.55 (16) | Y1—F7—Cs1 | 109.28 (18) |
F5—Y2—F4 | 70.45 (16) | Y3—F7—Cs1 | 112.00 (16) |
F1—Y2—F4 | 126.74 (18) | Cs1iv—F7—Cs1 | 91.99 (12) |
F3—Y2—F4 | 124.7 (3) | F8A—F8—F3iii | 175.3 (14) |
F8iv—Y2—F3xii | 42.9 (4) | F8A—F8—Y2iv | 101.7 (10) |
F2xi—Y2—F3xii | 94.3 (4) | F3iii—F8—Y2iv | 80.0 (6) |
F6—Y2—F3xii | 77.3 (3) | F8A—F8—Y3 | 87.5 (9) |
F5—Y2—F3xii | 138.3 (3) | F3iii—F8—Y3 | 89.5 (6) |
F1—Y2—F3xii | 80.7 (3) | Y2iv—F8—Y3 | 159.4 (6) |
F3—Y2—F3xii | 43.0 (4) | F8A—F8—Cs1iv | 52.1 (9) |
F4—Y2—F3xii | 147.8 (3) | F3iii—F8—Cs1iv | 132.0 (7) |
F8iv—Y2—F8Aiv | 22.1 (4) | Y2iv—F8—Cs1iv | 103.4 (4) |
F2xi—Y2—F8Aiv | 151.7 (4) | Y3—F8—Cs1iv | 96.8 (4) |
F6—Y2—F8Aiv | 108.9 (3) | F8—F8A—Y3 | 68.9 (9) |
F5—Y2—F8Aiv | 76.9 (3) | F8—F8A—Y2iv | 56.2 (8) |
F1—Y2—F8Aiv | 84.1 (3) | Y3—F8A—Y2iv | 122.4 (5) |
F3—Y2—F8Aiv | 105.1 (3) | F8—F8A—Cs1ix | 143.7 (11) |
F4—Y2—F8Aiv | 127.2 (3) | Y3—F8A—Cs1ix | 108.4 (3) |
F3xii—Y2—F8Aiv | 65.0 (3) | Y2iv—F8A—Cs1ix | 105.6 (3) |
F8iv—Y2—F2Axi | 145.6 (4) | F8—F8A—Cs1iv | 115.1 (11) |
F2xi—Y2—F2Axi | 17.4 (3) | Y3—F8A—Cs1iv | 107.9 (3) |
F6—Y2—F2Axi | 94.0 (3) | Y2iv—F8A—Cs1iv | 109.9 (3) |
F5—Y2—F2Axi | 96.6 (3) | Cs1ix—F8A—Cs1iv | 100.4 (3) |
F1—Y2—F2Axi | 69.7 (3) |
Symmetry codes: (i) x, −y+5/2, −z+1/2; (ii) x+1/2, y, −z+1; (iii) −x+1, y−1/2, 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) x−1/2, −y+5/2, z+1/2; (ix) x−1/2, y, −z; (x) −x+1/2, y+1/2, −z+1/2; (xi) x+1/2, −y+5/2, z−1/2; (xii) x, −y+5/2, −z−1/2; (xiii) −x+3/2, y+1/2, −z+1/2; (xiv) x−1/2, y, −z+1; (xv) −x+1, y+1/2, z−1/2. |
F7RbSm2 | Dx = 5.096 Mg m−3 |
Mr = 519.17 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, Pnna | Cell parameters from 4163 reflections |
a = 13.9359 (16) Å | θ = 2.9–28.3° |
b = 12.2412 (13) Å | µ = 24.39 mm−1 |
c = 7.9329 (8) Å | T = 293 K |
V = 1353.3 (3) Å3 | Prism, yellow |
Z = 8 | 0.22 × 0.18 × 0.12 mm |
F(000) = 1792 |
Rigaku AFC8S diffractometer | 1188 independent reflections |
Radiation source: fine-focus sealed tube | 1035 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.039 |
Detector resolution: 14.6199 pixels mm-1 | θmax = 25.1°, θmin = 2.9° |
ω scans | h = −16→16 |
Absorption correction: multi-scan REQAB, CrystalClear | k = −14→14 |
Tmin = 0.601, Tmax = 1.000 | l = −9→9 |
6252 measured reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary 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 = 1.12 | Δρmax = 1.90 e Å−3 |
1188 reflections | Δρmin = −2.91 e Å−3 |
116 parameters | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
12 restraints | Extinction coefficient: 0.00061 (10) |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Rb1 | 0.58337 (14) | 0.92108 (12) | 0.2243 (2) | 0.0434 (5) | |
Sm1 | 0.42886 (6) | 1.2500 | 0.2500 | 0.0141 (3) | |
Sm2 | 0.65539 (5) | 1.26764 (8) | 0.02417 (9) | 0.0326 (3) | |
Sm3 | 0.2500 | 1.0000 | 0.25078 (11) | 0.0126 (3) | |
F1 | 0.7992 (6) | 1.3218 (8) | −0.1021 (12) | 0.036 (2) | |
F2 | 0.1364 (12) | 1.0714 (12) | 0.434 (2) | 0.022 (3) | 0.50 |
F2A | 0.1647 (10) | 1.0311 (11) | 0.5020 (18) | 0.015 (3) | 0.50 |
F4 | 0.5794 (5) | 1.3492 (5) | 0.2658 (10) | 0.0206 (17) | |
F5 | 0.7578 (8) | 1.2500 | 0.2500 | 0.026 (3) | |
F6 | 0.4913 (6) | 1.2668 (8) | −0.0159 (10) | 0.031 (2) | |
F7 | 0.3929 (6) | 1.0795 (7) | 0.1559 (11) | 0.0281 (19) | |
F8 | 0.3206 (16) | 0.8724 (17) | 0.090 (3) | 0.048 (5) | 0.50 |
F8A | 0.2746 (12) | 0.9183 (12) | −0.014 (2) | 0.025 (4) | 0.50 |
F3 | 0.6360 (12) | 1.3325 (14) | −0.2564 (18) | 0.025 (3) | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Rb1 | 0.0614 (11) | 0.0223 (8) | 0.0465 (10) | −0.0032 (7) | −0.0027 (9) | 0.0020 (7) |
Sm1 | 0.0109 (5) | 0.0178 (5) | 0.0137 (5) | 0.000 | 0.000 | 0.0005 (3) |
Sm2 | 0.0136 (4) | 0.0744 (6) | 0.0099 (4) | −0.0075 (4) | 0.0006 (3) | 0.0086 (4) |
Sm3 | 0.0129 (5) | 0.0141 (5) | 0.0108 (5) | 0.0003 (3) | 0.000 | 0.000 |
F1 | 0.024 (5) | 0.041 (5) | 0.042 (6) | 0.009 (4) | 0.016 (4) | 0.011 (4) |
F2 | 0.021 (4) | 0.022 (4) | 0.021 (4) | 0.000 (2) | 0.001 (2) | −0.001 (2) |
F2A | 0.016 (3) | 0.015 (3) | 0.015 (3) | 0.001 (2) | 0.002 (2) | −0.001 (2) |
F4 | 0.021 (4) | 0.012 (3) | 0.030 (5) | 0.004 (3) | −0.004 (3) | 0.001 (3) |
F5 | 0.012 (5) | 0.053 (8) | 0.014 (5) | 0.000 | 0.000 | −0.002 (5) |
F6 | 0.017 (4) | 0.060 (6) | 0.017 (4) | −0.002 (4) | 0.000 (3) | 0.006 (4) |
F7 | 0.025 (5) | 0.030 (4) | 0.029 (5) | −0.009 (3) | 0.011 (4) | −0.005 (4) |
F8 | 0.048 (13) | 0.052 (12) | 0.045 (13) | 0.002 (10) | 0.020 (11) | −0.001 (10) |
F8A | 0.029 (9) | 0.018 (7) | 0.029 (9) | 0.011 (6) | −0.001 (7) | −0.013 (7) |
F3 | 0.029 (9) | 0.037 (9) | 0.007 (7) | 0.003 (7) | 0.002 (7) | −0.003 (6) |
Rb1—F2Ai | 2.795 (14) | Sm3—F8vii | 2.24 (2) |
Rb1—F4ii | 2.814 (7) | Sm3—F2vii | 2.318 (16) |
Rb1—F6iii | 2.983 (9) | Sm3—F2 | 2.318 (16) |
Rb1—F6iv | 3.018 (9) | Sm3—F7vii | 2.342 (8) |
Rb1—F7iv | 3.034 (9) | Sm3—F7 | 2.342 (8) |
Rb1—F5v | 3.054 (8) | Sm3—F8A | 2.348 (15) |
Rb1—F8Avi | 3.147 (17) | Sm3—F8Avii | 2.348 (15) |
Rb1—F3iii | 3.247 (16) | Sm3—F2Avii | 2.352 (14) |
Rb1—F8Aiv | 3.252 (17) | Sm3—F2A | 2.352 (14) |
Rb1—F7 | 3.332 (9) | Sm3—F1viii | 2.568 (9) |
Rb1—F2i | 3.360 (17) | Sm3—F1iii | 2.568 (9) |
Rb1—F2vii | 3.485 (17) | F1—Sm1vi | 2.326 (8) |
Sm1—F7 | 2.272 (8) | F1—Sm3xi | 2.568 (9) |
Sm1—F7ii | 2.272 (8) | F2—F2A | 0.832 (17) |
Sm1—F6ii | 2.291 (8) | F2—Sm2viii | 2.114 (15) |
Sm1—F6 | 2.291 (8) | F2—Rb1xiii | 3.360 (17) |
Sm1—F1viii | 2.326 (8) | F2—Rb1vii | 3.485 (17) |
Sm1—F1ix | 2.326 (8) | F2A—Sm2viii | 2.474 (13) |
Sm1—F4 | 2.427 (8) | F2A—Rb1xiii | 2.795 (14) |
Sm1—F4ii | 2.427 (8) | F4—Sm2ii | 2.438 (7) |
Sm1—Sm2ii | 3.6362 (11) | F4—Rb1ii | 2.814 (7) |
Sm1—Sm2 | 3.6362 (11) | F5—Sm2ii | 2.301 (7) |
Sm1—Sm3 | 3.9469 (6) | F5—Rb1xiv | 3.054 (8) |
Sm1—Sm3x | 3.9469 (6) | F5—Rb1v | 3.054 (8) |
Sm2—F8iv | 1.97 (2) | F6—Rb1xv | 2.983 (9) |
Sm2—F2xi | 2.114 (15) | F6—Rb1iv | 3.018 (9) |
Sm2—F5 | 2.301 (7) | F7—Rb1iv | 3.034 (9) |
Sm2—F6 | 2.308 (8) | F8—F8A | 1.19 (3) |
Sm2—F1 | 2.337 (8) | F8—F3iii | 1.44 (3) |
Sm2—F3 | 2.379 (15) | F8—Sm2iv | 1.97 (2) |
Sm2—F4 | 2.407 (8) | F8A—Sm2iv | 2.478 (14) |
Sm2—F4ii | 2.438 (7) | F8A—Rb1ix | 3.147 (17) |
Sm2—F3xii | 2.467 (15) | F8A—Rb1iv | 3.252 (17) |
Sm2—F2Axi | 2.474 (13) | F3—F8xv | 1.44 (3) |
Sm2—F8Aiv | 2.478 (14) | F3—Sm2xii | 2.467 (15) |
Sm2—Sm2ii | 3.6089 (15) | F3—Sm3xi | 2.594 (17) |
Sm3—F8 | 2.24 (2) | F3—Rb1xv | 3.247 (16) |
F2Ai—Rb1—F4ii | 60.3 (3) | F4ii—Sm2—F3xii | 104.4 (4) |
F2Ai—Rb1—F6iii | 84.8 (3) | F8iv—Sm2—F2Axi | 145.7 (7) |
F4ii—Rb1—F6iii | 127.3 (2) | F2xi—Sm2—F2Axi | 18.9 (5) |
F2Ai—Rb1—F6iv | 158.8 (3) | F5—Sm2—F2Axi | 96.7 (4) |
F4ii—Rb1—F6iv | 140.4 (2) | F6—Sm2—F2Axi | 92.7 (4) |
F6iii—Rb1—F6iv | 77.0 (3) | F1—Sm2—F2Axi | 69.0 (4) |
F2Ai—Rb1—F7iv | 136.8 (3) | F3—Sm2—F2Axi | 66.8 (5) |
F4ii—Rb1—F7iv | 91.9 (2) | F4—Sm2—F2Axi | 70.5 (4) |
F6iii—Rb1—F7iv | 136.3 (2) | F4ii—Sm2—F2Axi | 131.0 (4) |
F6iv—Rb1—F7iv | 59.4 (2) | F3xii—Sm2—F2Axi | 116.1 (5) |
F2Ai—Rb1—F5v | 89.1 (3) | F8iv—Sm2—F8Aiv | 28.1 (7) |
F4ii—Rb1—F5v | 134.3 (2) | F2xi—Sm2—F8Aiv | 153.4 (6) |
F6iii—Rb1—F5v | 76.86 (19) | F5—Sm2—F8Aiv | 72.3 (4) |
F6iv—Rb1—F5v | 76.3 (2) | F6—Sm2—F8Aiv | 112.4 (5) |
F7iv—Rb1—F5v | 89.19 (18) | F1—Sm2—F8Aiv | 84.7 (5) |
F2Ai—Rb1—F8Avi | 94.3 (4) | F3—Sm2—F8Aiv | 108.6 (5) |
F4ii—Rb1—F8Avi | 92.4 (3) | F4—Sm2—F8Aiv | 125.5 (4) |
F6iii—Rb1—F8Avi | 131.0 (3) | F4ii—Sm2—F8Aiv | 69.8 (4) |
F6iv—Rb1—F8Avi | 89.6 (3) | F3xii—Sm2—F8Aiv | 63.7 (5) |
F7iv—Rb1—F8Avi | 51.7 (3) | F2Axi—Sm2—F8Aiv | 153.1 (5) |
F5v—Rb1—F8Avi | 54.1 (3) | F8iv—Sm2—Sm2ii | 110.7 (7) |
F2Ai—Rb1—F3iii | 120.4 (4) | F2xi—Sm2—Sm2ii | 116.7 (5) |
F4ii—Rb1—F3iii | 108.3 (4) | F5—Sm2—Sm2ii | 38.4 (2) |
F6iii—Rb1—F3iii | 55.1 (3) | F6—Sm2—Sm2ii | 97.8 (2) |
F6iv—Rb1—F3iii | 56.4 (3) | F1—Sm2—Sm2ii | 117.4 (2) |
F7iv—Rb1—F3iii | 98.5 (3) | F3—Sm2—Sm2ii | 165.7 (4) |
F5v—Rb1—F3iii | 116.8 (3) | F4—Sm2—Sm2ii | 42.17 (17) |
F8Avi—Rb1—F3iii | 145.0 (4) | F4ii—Sm2—Sm2ii | 41.52 (18) |
F2Ai—Rb1—F8Aiv | 82.0 (4) | F3xii—Sm2—Sm2ii | 142.7 (4) |
F4ii—Rb1—F8Aiv | 54.7 (3) | F2Axi—Sm2—Sm2ii | 100.9 (3) |
F6iii—Rb1—F8Aiv | 161.9 (3) | F8Aiv—Sm2—Sm2ii | 85.6 (4) |
F6iv—Rb1—F8Aiv | 112.9 (3) | F8—Sm3—F8vii | 110.8 (12) |
F7iv—Rb1—F8Aiv | 54.8 (3) | F8—Sm3—F2vii | 78.1 (8) |
F5v—Rb1—F8Aiv | 90.5 (3) | F8vii—Sm3—F2vii | 156.5 (6) |
F8Avi—Rb1—F8Aiv | 38.5 (5) | F8—Sm3—F2 | 156.5 (6) |
F3iii—Rb1—F8Aiv | 143.0 (4) | F8vii—Sm3—F2 | 78.1 (8) |
F2Ai—Rb1—F7 | 99.7 (3) | F2vii—Sm3—F2 | 102.5 (9) |
F4ii—Rb1—F7 | 53.6 (2) | F8—Sm3—F7vii | 84.3 (6) |
F6iii—Rb1—F7 | 101.7 (2) | F8vii—Sm3—F7vii | 74.6 (6) |
F6iv—Rb1—F7 | 94.6 (2) | F2vii—Sm3—F7vii | 128.7 (4) |
F7iv—Rb1—F7 | 85.8 (2) | F2—Sm3—F7vii | 77.1 (5) |
F5v—Rb1—F7 | 170.91 (18) | F8—Sm3—F7 | 74.6 (6) |
F8Avi—Rb1—F7 | 126.5 (3) | F8vii—Sm3—F7 | 84.3 (6) |
F3iii—Rb1—F7 | 56.8 (3) | F2vii—Sm3—F7 | 77.1 (5) |
F8Aiv—Rb1—F7 | 92.8 (3) | F2—Sm3—F7 | 128.7 (4) |
F2Ai—Rb1—F2i | 11.4 (4) | F7vii—Sm3—F7 | 142.5 (4) |
F4ii—Rb1—F2i | 55.6 (3) | F8—Sm3—F8A | 29.8 (7) |
F6iii—Rb1—F2i | 82.3 (3) | F8vii—Sm3—F8A | 81.6 (8) |
F6iv—Rb1—F2i | 159.3 (3) | F2vii—Sm3—F8A | 107.4 (6) |
F7iv—Rb1—F2i | 141.3 (3) | F2—Sm3—F8A | 145.0 (6) |
F5v—Rb1—F2i | 99.3 (3) | F7vii—Sm3—F8A | 70.1 (5) |
F8Avi—Rb1—F2i | 104.4 (4) | F7—Sm3—F8A | 76.4 (5) |
F3iii—Rb1—F2i | 110.6 (4) | F8—Sm3—F8Avii | 81.6 (8) |
F8Aiv—Rb1—F2i | 87.2 (4) | F8vii—Sm3—F8Avii | 29.8 (7) |
F7—Rb1—F2i | 89.3 (3) | F2vii—Sm3—F8Avii | 145.0 (6) |
F2Ai—Rb1—F2vii | 88.5 (4) | F2—Sm3—F8Avii | 107.4 (6) |
F4ii—Rb1—F2vii | 86.7 (3) | F7vii—Sm3—F8Avii | 76.4 (5) |
F6iii—Rb1—F2vii | 51.7 (3) | F7—Sm3—F8Avii | 70.1 (5) |
F6iv—Rb1—F2vii | 88.7 (3) | F8A—Sm3—F8Avii | 53.5 (8) |
F7iv—Rb1—F2vii | 124.7 (3) | F8—Sm3—F2Avii | 98.4 (7) |
F5v—Rb1—F2vii | 128.6 (3) | F8vii—Sm3—F2Avii | 144.6 (6) |
F8Avi—Rb1—F2vii | 176.3 (4) | F2vii—Sm3—F2Avii | 20.5 (4) |
F3iii—Rb1—F2vii | 32.8 (4) | F2—Sm3—F2Avii | 82.9 (7) |
F8Aiv—Rb1—F2vii | 139.8 (4) | F7vii—Sm3—F2Avii | 129.4 (4) |
F7—Rb1—F2vii | 50.4 (3) | F7—Sm3—F2Avii | 84.8 (4) |
F2i—Rb1—F2vii | 78.1 (4) | F8A—Sm3—F2Avii | 127.9 (5) |
F7—Sm1—F7ii | 154.5 (4) | F8Avii—Sm3—F2Avii | 154.1 (5) |
F7—Sm1—F6ii | 107.7 (3) | F8—Sm3—F2A | 144.6 (6) |
F7ii—Sm1—F6ii | 82.2 (3) | F8vii—Sm3—F2A | 98.4 (7) |
F7—Sm1—F6 | 82.2 (3) | F2vii—Sm3—F2A | 82.9 (7) |
F7ii—Sm1—F6 | 107.7 (3) | F2—Sm3—F2A | 20.5 (4) |
F6ii—Sm1—F6 | 135.3 (4) | F7vii—Sm3—F2A | 84.8 (4) |
F7—Sm1—F1viii | 69.4 (3) | F7—Sm3—F2A | 129.4 (4) |
F7ii—Sm1—F1viii | 90.6 (3) | F8A—Sm3—F2A | 154.1 (5) |
F6ii—Sm1—F1viii | 78.3 (3) | F8Avii—Sm3—F2A | 127.9 (5) |
F6—Sm1—F1viii | 142.5 (3) | F2Avii—Sm3—F2A | 64.1 (7) |
F7—Sm1—F1ix | 90.6 (3) | F8—Sm3—F1viii | 137.1 (6) |
F7ii—Sm1—F1ix | 69.4 (3) | F8vii—Sm3—F1viii | 77.5 (6) |
F6ii—Sm1—F1ix | 142.5 (3) | F2vii—Sm3—F1viii | 81.6 (4) |
F6—Sm1—F1ix | 78.3 (3) | F2—Sm3—F1viii | 65.0 (4) |
F1viii—Sm1—F1ix | 78.1 (5) | F7vii—Sm3—F1viii | 136.6 (3) |
F7—Sm1—F4 | 131.8 (3) | F7—Sm3—F1viii | 64.2 (3) |
F7ii—Sm1—F4 | 73.4 (3) | F8A—Sm3—F1viii | 136.8 (5) |
F6ii—Sm1—F4 | 70.7 (3) | F8Avii—Sm3—F1viii | 94.8 (4) |
F6—Sm1—F4 | 71.0 (3) | F2Avii—Sm3—F1viii | 67.5 (4) |
F1viii—Sm1—F4 | 146.5 (3) | F2A—Sm3—F1viii | 67.2 (4) |
F1ix—Sm1—F4 | 120.6 (3) | F8—Sm3—F1iii | 77.5 (6) |
F7—Sm1—F4ii | 73.4 (3) | F8vii—Sm3—F1iii | 137.1 (6) |
F7ii—Sm1—F4ii | 131.8 (3) | F2vii—Sm3—F1iii | 65.0 (4) |
F6ii—Sm1—F4ii | 71.0 (3) | F2—Sm3—F1iii | 81.6 (4) |
F6—Sm1—F4ii | 70.7 (3) | F7vii—Sm3—F1iii | 64.2 (3) |
F1viii—Sm1—F4ii | 120.6 (3) | F7—Sm3—F1iii | 136.6 (3) |
F1ix—Sm1—F4ii | 146.5 (3) | F8A—Sm3—F1iii | 94.8 (4) |
F4—Sm1—F4ii | 60.4 (3) | F8Avii—Sm3—F1iii | 136.8 (5) |
F7—Sm1—Sm2ii | 107.4 (2) | F2Avii—Sm3—F1iii | 67.2 (4) |
F7ii—Sm1—Sm2ii | 94.8 (2) | F2A—Sm3—F1iii | 67.5 (4) |
F6ii—Sm1—Sm2ii | 37.9 (2) | F1viii—Sm3—F1iii | 125.9 (4) |
F6—Sm1—Sm2ii | 97.4 (2) | Sm1vi—F1—Sm2 | 140.8 (4) |
F1viii—Sm1—Sm2ii | 113.8 (3) | Sm1vi—F1—Sm3xi | 107.4 (3) |
F1ix—Sm1—Sm2ii | 160.9 (2) | Sm2—F1—Sm3xi | 101.9 (3) |
F4—Sm1—Sm2ii | 41.74 (17) | F2A—F2—Sm2viii | 105.8 (16) |
F4ii—Sm1—Sm2ii | 41.01 (18) | F2A—F2—Sm3 | 82.0 (15) |
F7—Sm1—Sm2 | 94.8 (2) | Sm2viii—F2—Sm3 | 118.6 (7) |
F7ii—Sm1—Sm2 | 107.4 (2) | F2A—F2—Rb1xiii | 41.7 (14) |
F6ii—Sm1—Sm2 | 97.4 (2) | Sm2viii—F2—Rb1xiii | 105.3 (6) |
F6—Sm1—Sm2 | 37.9 (2) | Sm3—F2—Rb1xiii | 116.7 (6) |
F1viii—Sm1—Sm2 | 160.9 (2) | F2A—F2—Rb1vii | 138.0 (16) |
F1ix—Sm1—Sm2 | 113.8 (3) | Sm2viii—F2—Rb1vii | 104.3 (6) |
F4—Sm1—Sm2 | 41.01 (18) | Sm3—F2—Rb1vii | 108.2 (6) |
F4ii—Sm1—Sm2 | 41.74 (17) | Rb1xiii—F2—Rb1vii | 101.9 (4) |
Sm2ii—Sm1—Sm2 | 59.50 (3) | F2—F2A—Sm3 | 77.5 (15) |
F7—Sm1—Sm3 | 31.7 (2) | F2—F2A—Sm2viii | 55.3 (13) |
F7ii—Sm1—Sm3 | 124.9 (2) | Sm3—F2A—Sm2viii | 104.3 (5) |
F6ii—Sm1—Sm3 | 99.7 (2) | F2—F2A—Rb1xiii | 126.8 (16) |
F6—Sm1—Sm3 | 108.1 (2) | Sm3—F2A—Rb1xiii | 141.8 (6) |
F1viii—Sm1—Sm3 | 38.4 (2) | Sm2viii—F2A—Rb1xiii | 113.8 (5) |
F1ix—Sm1—Sm3 | 78.6 (2) | Sm2—F4—Sm1 | 97.6 (3) |
F4—Sm1—Sm3 | 159.01 (16) | Sm2—F4—Sm2ii | 96.3 (2) |
F4ii—Sm1—Sm3 | 99.09 (16) | Sm1—F4—Sm2ii | 96.7 (3) |
Sm2ii—Sm1—Sm3 | 120.096 (18) | Sm2—F4—Rb1ii | 115.3 (3) |
Sm2—Sm1—Sm3 | 126.520 (19) | Sm1—F4—Rb1ii | 121.2 (3) |
F7—Sm1—Sm3x | 124.9 (2) | Sm2ii—F4—Rb1ii | 124.0 (3) |
F7ii—Sm1—Sm3x | 31.7 (2) | Sm2—F5—Sm2ii | 103.3 (4) |
F6ii—Sm1—Sm3x | 108.1 (2) | Sm2—F5—Rb1xiv | 115.93 (8) |
F6—Sm1—Sm3x | 99.7 (2) | Sm2ii—F5—Rb1xiv | 117.52 (8) |
F1viii—Sm1—Sm3x | 78.6 (2) | Sm2—F5—Rb1v | 117.52 (8) |
F1ix—Sm1—Sm3x | 38.4 (2) | Sm2ii—F5—Rb1v | 115.93 (8) |
F4—Sm1—Sm3x | 99.09 (16) | Rb1xiv—F5—Rb1v | 87.1 (3) |
F4ii—Sm1—Sm3x | 159.01 (16) | Sm1—F6—Sm2 | 104.5 (3) |
Sm2ii—Sm1—Sm3x | 126.520 (18) | Sm1—F6—Rb1xv | 124.1 (3) |
Sm2—Sm1—Sm3x | 120.096 (18) | Sm2—F6—Rb1xv | 116.0 (3) |
Sm3—Sm1—Sm3x | 101.68 (2) | Sm1—F6—Rb1iv | 107.7 (3) |
F8iv—Sm2—F2xi | 132.6 (8) | Sm2—F6—Rb1iv | 114.9 (3) |
F8iv—Sm2—F5 | 99.9 (7) | Rb1xv—F6—Rb1iv | 89.1 (2) |
F2xi—Sm2—F5 | 115.4 (5) | Sm1—F7—Sm3 | 117.6 (3) |
F8iv—Sm2—F6 | 95.8 (7) | Sm1—F7—Rb1iv | 107.8 (3) |
F2xi—Sm2—F6 | 80.4 (5) | Sm3—F7—Rb1iv | 114.3 (3) |
F5—Sm2—F6 | 136.2 (3) | Sm1—F7—Rb1 | 107.8 (3) |
F8iv—Sm2—F1 | 84.4 (6) | Sm3—F7—Rb1 | 112.5 (3) |
F2xi—Sm2—F1 | 72.4 (5) | Rb1iv—F7—Rb1 | 94.2 (2) |
F5—Sm2—F1 | 80.1 (3) | F8A—F8—F3iii | 167 (2) |
F6—Sm2—F1 | 142.4 (3) | F8A—F8—Sm2iv | 100.6 (15) |
F8iv—Sm2—F3 | 83.0 (8) | F3iii—F8—Sm2iv | 91.3 (13) |
F2xi—Sm2—F3 | 50.0 (6) | F8A—F8—Sm3 | 80.0 (13) |
F5—Sm2—F3 | 146.1 (4) | F3iii—F8—Sm3 | 86.6 (12) |
F6—Sm2—F3 | 76.1 (4) | Sm2iv—F8—Sm3 | 160.6 (11) |
F1—Sm2—F3 | 66.5 (5) | F8—F8A—Sm3 | 70.1 (12) |
F8iv—Sm2—F4 | 143.5 (6) | F8—F8A—Sm2iv | 51.3 (11) |
F2xi—Sm2—F4 | 80.1 (5) | Sm3—F8A—Sm2iv | 118.6 (7) |
F5—Sm2—F4 | 72.1 (3) | F8—F8A—Rb1ix | 146.3 (15) |
F6—Sm2—F4 | 71.1 (3) | Sm3—F8A—Rb1ix | 110.2 (6) |
F1—Sm2—F4 | 127.0 (3) | Sm2iv—F8A—Rb1ix | 109.0 (5) |
F3—Sm2—F4 | 123.8 (4) | F8—F8A—Rb1iv | 108.4 (14) |
F8iv—Sm2—F4ii | 83.0 (6) | Sm3—F8A—Rb1iv | 106.9 (5) |
F2xi—Sm2—F4ii | 136.4 (5) | Sm2iv—F8A—Rb1iv | 107.4 (5) |
F5—Sm2—F4ii | 71.5 (3) | Rb1ix—F8A—Rb1iv | 103.6 (5) |
F6—Sm2—F4ii | 70.2 (3) | F8xv—F3—Sm2 | 148.6 (13) |
F1—Sm2—F4ii | 146.3 (3) | F8xv—F3—Sm2xii | 52.9 (10) |
F3—Sm2—F4ii | 141.8 (4) | Sm2—F3—Sm2xii | 128.8 (7) |
F4—Sm2—F4ii | 60.5 (3) | F8xv—F3—Sm3xi | 59.6 (10) |
F8iv—Sm2—F3xii | 35.8 (8) | Sm2—F3—Sm3xi | 100.0 (6) |
F2xi—Sm2—F3xii | 99.1 (6) | Sm2xii—F3—Sm3xi | 110.2 (6) |
F5—Sm2—F3xii | 133.7 (4) | F8xv—F3—Rb1xv | 104.0 (11) |
F6—Sm2—F3xii | 76.7 (4) | Sm2—F3—Rb1xv | 105.2 (5) |
F1—Sm2—F3xii | 82.3 (5) | Sm2xii—F3—Rb1xv | 103.2 (5) |
F3—Sm2—F3xii | 49.3 (7) | Sm3xi—F3—Rb1xv | 108.3 (5) |
F4—Sm2—F3xii | 147.5 (4) |
Symmetry codes: (i) x+1/2, y, −z+1; (ii) x, −y+5/2, −z+1/2; (iii) −x+1, y−1/2, 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) x−1/2, −y+5/2, z+1/2; (ix) x−1/2, y, −z; (x) −x+1/2, y+1/2, −z+1/2; (xi) x+1/2, −y+5/2, z−1/2; (xii) x, −y+5/2, −z−1/2; (xiii) x−1/2, y, −z+1; (xiv) −x+3/2, y+1/2, −z+1/2; (xv) −x+1, y+1/2, z−1/2. |
CsF7Gd2 | Dx = 5.637 Mg m−3 |
Mr = 580.41 | Mo Kα radiation, λ = 0.71073 Å |
Orthorhombic, Pnna | Cell parameters from 7461 reflections |
a = 13.828 (3) Å | θ = 1.6–26.0° |
b = 12.415 (3) Å | µ = 24.53 mm−1 |
c = 7.9681 (16) Å | T = 293 K |
V = 1367.9 (5) Å3 | Prism, colorless |
Z = 8 | 0.31 × 0.27 × 0.24 mm |
F(000) = 1968 |
Rigaku AFC8S diffractometer | 1249 independent reflections |
Radiation source: fine-focus sealed tube | 1227 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.102 |
Detector resolution: 14.6199 pixels mm-1 | θmax = 25.3°, θmin = 3.0° |
ω scans | h = −16→16 |
Absorption correction: multi-scan REQAB, CrystalClear | k = −14→14 |
Tmin = 0.387, Tmax = 1.000 | l = −9→9 |
10980 measured reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary 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 = 1.10 | Δρmax = 1.96 e Å−3 |
1249 reflections | Δρmin = −2.93 e Å−3 |
116 parameters | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
42 restraints | Extinction coefficient: 0.00099 (9) |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Cs1 | 0.58148 (10) | 0.92205 (10) | 0.22867 (17) | 0.0270 (4) | |
Gd1 | 0.43090 (8) | 1.2500 | 0.2500 | 0.0104 (4) | |
Gd2 | 0.65812 (6) | 1.26449 (9) | 0.02418 (11) | 0.0170 (3) | |
Gd3 | 0.2500 | 1.0000 | 0.25128 (14) | 0.0090 (4) | |
F1 | 0.8022 (8) | 1.3178 (10) | −0.0933 (16) | 0.028 (3) | |
F2 | 0.1392 (16) | 1.079 (2) | 0.426 (3) | 0.021 (5) | 0.50 |
F2A | 0.1660 (15) | 1.0415 (16) | 0.494 (3) | 0.013 (4) | 0.50 |
F3 | 0.6428 (16) | 1.3217 (19) | −0.255 (3) | 0.019 (5) | 0.50 |
F4 | 0.5835 (8) | 1.3460 (9) | 0.2632 (14) | 0.017 (2) | |
F5 | 0.7561 (11) | 1.2500 | 0.2500 | 0.017 (3) | |
F6 | 0.4955 (7) | 1.2604 (9) | −0.0128 (14) | 0.017 (2) | |
F7 | 0.3924 (8) | 1.0813 (11) | 0.1681 (15) | 0.029 (3) | |
F8 | 0.314 (2) | 0.879 (2) | 0.083 (4) | 0.041 (7) | 0.50 |
F8A | 0.2787 (16) | 0.9179 (17) | −0.006 (3) | 0.017 (4) | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cs1 | 0.0408 (8) | 0.0103 (7) | 0.0298 (7) | 0.0005 (5) | 0.0017 (6) | 0.0011 (5) |
Gd1 | 0.0066 (6) | 0.0179 (7) | 0.0068 (6) | 0.000 | 0.000 | 0.0015 (5) |
Gd2 | 0.0076 (4) | 0.0387 (6) | 0.0046 (5) | −0.0043 (4) | 0.0005 (3) | 0.0046 (4) |
Gd3 | 0.0074 (6) | 0.0148 (7) | 0.0048 (6) | 0.0003 (4) | 0.000 | 0.000 |
F1 | 0.018 (6) | 0.034 (7) | 0.033 (7) | 0.004 (5) | 0.013 (5) | 0.009 (6) |
F2 | 0.015 (8) | 0.032 (9) | 0.016 (8) | 0.002 (7) | 0.003 (7) | −0.003 (8) |
F2A | 0.014 (6) | 0.009 (6) | 0.015 (6) | 0.000 (4) | 0.003 (4) | 0.002 (5) |
F3 | 0.023 (8) | 0.024 (8) | 0.010 (8) | −0.003 (7) | 0.006 (7) | 0.002 (7) |
F4 | 0.020 (5) | 0.010 (5) | 0.021 (5) | 0.006 (4) | 0.003 (4) | 0.000 (4) |
F5 | 0.016 (5) | 0.024 (5) | 0.012 (5) | 0.000 | 0.000 | 0.001 (4) |
F6 | 0.010 (3) | 0.027 (4) | 0.015 (4) | −0.008 (3) | 0.001 (3) | 0.001 (4) |
F7 | 0.022 (6) | 0.043 (8) | 0.022 (6) | −0.005 (6) | 0.008 (5) | 0.002 (6) |
F8 | 0.057 (19) | 0.041 (17) | 0.027 (14) | 0.011 (15) | 0.009 (14) | 0.011 (13) |
F8A | 0.021 (8) | 0.016 (8) | 0.013 (8) | 0.009 (7) | 0.001 (7) | −0.002 (7) |
Cs1—F4i | 2.880 (11) | Gd3—F2 | 2.29 (2) |
Cs1—F2Aii | 2.91 (2) | Gd3—F2vii | 2.29 (2) |
Cs1—F6iii | 3.037 (11) | Gd3—F7vii | 2.310 (12) |
Cs1—F6iv | 3.067 (11) | Gd3—F7 | 2.310 (12) |
Cs1—F5v | 3.104 (11) | Gd3—F2Avii | 2.31 (2) |
Cs1—F7iii | 3.182 (12) | Gd3—F2A | 2.31 (2) |
Cs1—F8Avi | 3.25 (2) | Gd3—F8A | 2.32 (2) |
Cs1—F8Aiii | 3.29 (2) | Gd3—F8Avii | 2.32 (2) |
Cs1—F7 | 3.313 (13) | Gd3—F3ix | 2.66 (2) |
Cs1—F3iv | 3.34 (2) | Gd3—F3iv | 2.66 (2) |
Cs1—F2vii | 3.43 (2) | F1—Gd1vi | 2.331 (11) |
Cs1—F2ii | 3.46 (3) | F1—Gd3xi | 2.678 (12) |
Gd1—F7 | 2.257 (13) | F1—Cs1xiii | 3.564 (14) |
Gd1—F7i | 2.257 (13) | F2—F2A | 0.81 (3) |
Gd1—F6i | 2.280 (11) | F2—Gd2ix | 2.12 (2) |
Gd1—F6 | 2.280 (11) | F2—Cs1vii | 3.43 (2) |
Gd1—F1viii | 2.331 (11) | F2—Cs1xiv | 3.46 (3) |
Gd1—F1ix | 2.331 (11) | F2A—Gd2ix | 2.42 (2) |
Gd1—F4 | 2.426 (11) | F2A—Cs1xiv | 2.91 (2) |
Gd1—F4i | 2.426 (11) | F3—F8xv | 1.59 (3) |
Gd1—Gd2 | 3.6252 (14) | F3—Gd2xii | 2.40 (2) |
Gd1—Gd2i | 3.6252 (14) | F3—Gd3xi | 2.66 (2) |
Gd1—Gd3 | 3.9863 (9) | F3—Cs1xv | 3.34 (2) |
Gd1—Gd3x | 3.9863 (9) | F4—Gd2i | 2.412 (11) |
Gd2—F8iii | 2.02 (3) | F4—Cs1i | 2.880 (11) |
Gd2—F2xi | 2.12 (2) | F5—Gd2i | 2.260 (9) |
Gd2—F5 | 2.260 (9) | F5—Cs1xiii | 3.104 (11) |
Gd2—F6 | 2.268 (10) | F5—Cs1v | 3.104 (11) |
Gd2—F1 | 2.299 (11) | F6—Cs1iii | 3.037 (11) |
Gd2—F3 | 2.35 (2) | F6—Cs1xv | 3.067 (11) |
Gd2—F4 | 2.391 (10) | F7—Cs1iii | 3.182 (12) |
Gd2—F3xii | 2.40 (2) | F8—F8A | 0.98 (3) |
Gd2—F4i | 2.412 (11) | F8—F3iv | 1.59 (3) |
Gd2—F2Axi | 2.42 (2) | F8—Gd2iii | 2.02 (3) |
Gd2—F8Aiii | 2.43 (2) | F8—Cs1iii | 3.79 (3) |
Gd2—Gd2i | 3.6167 (19) | F8A—Gd2iii | 2.43 (2) |
Gd3—F8 | 2.19 (3) | F8A—Cs1viii | 3.25 (2) |
Gd3—F8vii | 2.19 (3) | F8A—Cs1iii | 3.29 (2) |
F4i—Cs1—F2Aii | 57.9 (4) | F5—Gd2—F2Axi | 97.5 (6) |
F4i—Cs1—F6iii | 139.6 (3) | F6—Gd2—F2Axi | 93.1 (6) |
F2Aii—Cs1—F6iii | 162.2 (4) | F1—Gd2—F2Axi | 68.6 (6) |
F4i—Cs1—F6iv | 130.0 (3) | F3—Gd2—F2Axi | 67.0 (8) |
F2Aii—Cs1—F6iv | 87.9 (5) | F4—Gd2—F2Axi | 71.2 (6) |
F6iii—Cs1—F6iv | 76.7 (3) | F3xii—Gd2—F2Axi | 111.0 (8) |
F4i—Cs1—F5v | 132.8 (3) | F4i—Gd2—F2Axi | 130.9 (6) |
F2Aii—Cs1—F5v | 91.1 (4) | F8iii—Gd2—F8Aiii | 23.2 (9) |
F6iii—Cs1—F5v | 76.8 (2) | F2xi—Gd2—F8Aiii | 151.5 (8) |
F6iv—Cs1—F5v | 76.4 (2) | F5—Gd2—F8Aiii | 76.0 (5) |
F4i—Cs1—F7iii | 92.0 (3) | F6—Gd2—F8Aiii | 109.1 (6) |
F2Aii—Cs1—F7iii | 135.7 (5) | F1—Gd2—F8Aiii | 86.1 (6) |
F6iii—Cs1—F7iii | 57.8 (3) | F3—Gd2—F8Aiii | 104.9 (8) |
F6iv—Cs1—F7iii | 134.3 (3) | F4—Gd2—F8Aiii | 126.7 (6) |
F5v—Cs1—F7iii | 87.9 (2) | F3xii—Gd2—F8Aiii | 64.1 (7) |
F4i—Cs1—F8Avi | 91.1 (4) | F4i—Gd2—F8Aiii | 70.5 (6) |
F2Aii—Cs1—F8Avi | 94.9 (6) | F2Axi—Gd2—F8Aiii | 154.6 (7) |
F6iii—Cs1—F8Avi | 88.4 (4) | F8iii—Gd2—Gd2i | 109.5 (8) |
F6iv—Cs1—F8Avi | 130.3 (4) | F2xi—Gd2—Gd2i | 117.4 (7) |
F5v—Cs1—F8Avi | 54.0 (4) | F5—Gd2—Gd2i | 36.8 (3) |
F7iii—Cs1—F8Avi | 50.4 (4) | F6—Gd2—Gd2i | 97.3 (3) |
F4i—Cs1—F8Aiii | 53.4 (4) | F1—Gd2—Gd2i | 115.7 (3) |
F2Aii—Cs1—F8Aiii | 82.3 (6) | F3—Gd2—Gd2i | 167.0 (6) |
F6iii—Cs1—F8Aiii | 110.5 (4) | F4—Gd2—Gd2i | 41.4 (3) |
F6iv—Cs1—F8Aiii | 164.0 (4) | F3xii—Gd2—Gd2i | 147.4 (5) |
F5v—Cs1—F8Aiii | 91.1 (4) | F4i—Gd2—Gd2i | 40.9 (2) |
F7iii—Cs1—F8Aiii | 53.5 (4) | F2Axi—Gd2—Gd2i | 101.4 (5) |
F8Avi—Cs1—F8Aiii | 39.0 (7) | F8Aiii—Gd2—Gd2i | 88.1 (5) |
F4i—Cs1—F7 | 54.2 (3) | F8—Gd3—F8vii | 104.8 (15) |
F2Aii—Cs1—F7 | 97.1 (5) | F8—Gd3—F2 | 158.6 (10) |
F6iii—Cs1—F7 | 94.9 (3) | F8vii—Gd3—F2 | 79.1 (11) |
F6iv—Cs1—F7 | 102.4 (3) | F8—Gd3—F2vii | 79.1 (11) |
F5v—Cs1—F7 | 171.7 (3) | F8vii—Gd3—F2vii | 158.6 (10) |
F7iii—Cs1—F7 | 87.3 (3) | F2—Gd3—F2vii | 105.2 (13) |
F8Avi—Cs1—F7 | 126.2 (4) | F8—Gd3—F7vii | 82.4 (9) |
F8Aiii—Cs1—F7 | 91.4 (4) | F8vii—Gd3—F7vii | 77.4 (9) |
F4i—Cs1—F3iv | 112.4 (5) | F2—Gd3—F7vii | 77.9 (7) |
F2Aii—Cs1—F3iv | 122.3 (6) | F2vii—Gd3—F7vii | 124.0 (7) |
F6iii—Cs1—F3iv | 54.4 (4) | F8—Gd3—F7 | 77.4 (9) |
F6iv—Cs1—F3iv | 53.8 (4) | F8vii—Gd3—F7 | 82.4 (9) |
F5v—Cs1—F3iv | 114.4 (4) | F2—Gd3—F7 | 124.0 (7) |
F7iii—Cs1—F3iv | 97.9 (4) | F2vii—Gd3—F7 | 77.9 (7) |
F8Avi—Cs1—F3iv | 142.3 (5) | F7vii—Gd3—F7 | 146.6 (6) |
F8Aiii—Cs1—F3iv | 142.2 (5) | F8—Gd3—F2Avii | 99.1 (10) |
F7—Cs1—F3iv | 59.7 (4) | F8vii—Gd3—F2Avii | 149.7 (9) |
F4i—Cs1—F2vii | 90.1 (5) | F2—Gd3—F2Avii | 85.6 (10) |
F2Aii—Cs1—F2vii | 90.7 (5) | F2vii—Gd3—F2Avii | 20.1 (6) |
F6iii—Cs1—F2vii | 86.9 (5) | F7vii—Gd3—F2Avii | 124.8 (6) |
F6iv—Cs1—F2vii | 51.8 (4) | F7—Gd3—F2Avii | 84.8 (6) |
F5v—Cs1—F2vii | 128.1 (4) | F8—Gd3—F2A | 149.7 (9) |
F7iii—Cs1—F2vii | 123.7 (4) | F8vii—Gd3—F2A | 99.1 (10) |
F8Avi—Cs1—F2vii | 174.1 (5) | F2—Gd3—F2A | 20.1 (6) |
F8Aiii—Cs1—F2vii | 140.4 (5) | F2vii—Gd3—F2A | 85.6 (10) |
F7—Cs1—F2vii | 50.7 (4) | F7vii—Gd3—F2A | 84.8 (6) |
F3iv—Cs1—F2vii | 32.6 (6) | F7—Gd3—F2A | 124.8 (6) |
F4i—Cs1—F2ii | 54.5 (4) | F2Avii—Gd3—F2A | 66.6 (11) |
F2Aii—Cs1—F2ii | 10.5 (5) | F8—Gd3—F8A | 24.9 (8) |
F6iii—Cs1—F2ii | 161.7 (4) | F8vii—Gd3—F8A | 80.2 (10) |
F6iv—Cs1—F2ii | 85.0 (4) | F2—Gd3—F8A | 146.9 (8) |
F5v—Cs1—F2ii | 100.1 (4) | F2vii—Gd3—F8A | 103.5 (9) |
F7iii—Cs1—F2ii | 140.4 (5) | F7vii—Gd3—F8A | 72.6 (6) |
F8Avi—Cs1—F2ii | 104.4 (6) | F7—Gd3—F8A | 78.1 (6) |
F8Aiii—Cs1—F2ii | 87.4 (5) | F2Avii—Gd3—F8A | 123.7 (8) |
F7—Cs1—F2ii | 87.9 (4) | F2A—Gd3—F8A | 157.0 (7) |
F3iv—Cs1—F2ii | 113.1 (5) | F8—Gd3—F8Avii | 80.2 (10) |
F2vii—Cs1—F2ii | 81.0 (6) | F8vii—Gd3—F8Avii | 24.9 (8) |
F7—Gd1—F7i | 152.7 (6) | F2—Gd3—F8Avii | 103.5 (9) |
F7—Gd1—F6i | 107.8 (4) | F2vii—Gd3—F8Avii | 146.9 (8) |
F7i—Gd1—F6i | 83.1 (4) | F7vii—Gd3—F8Avii | 78.1 (6) |
F7—Gd1—F6 | 83.1 (4) | F7—Gd3—F8Avii | 72.6 (6) |
F7i—Gd1—F6 | 107.8 (4) | F2Avii—Gd3—F8Avii | 157.0 (7) |
F6i—Gd1—F6 | 133.8 (5) | F2A—Gd3—F8Avii | 123.7 (8) |
F7—Gd1—F1viii | 90.0 (4) | F8A—Gd3—F8Avii | 56.2 (11) |
F7i—Gd1—F1viii | 68.9 (4) | F8—Gd3—F3ix | 141.1 (9) |
F6i—Gd1—F1viii | 144.2 (4) | F8vii—Gd3—F3ix | 36.6 (9) |
F6—Gd1—F1viii | 77.7 (4) | F2—Gd3—F3ix | 44.4 (8) |
F7—Gd1—F1ix | 68.9 (4) | F2vii—Gd3—F3ix | 137.7 (8) |
F7i—Gd1—F1ix | 90.0 (4) | F7vii—Gd3—F3ix | 83.3 (6) |
F6i—Gd1—F1ix | 77.7 (4) | F7—Gd3—F3ix | 96.1 (6) |
F6—Gd1—F1ix | 144.2 (4) | F2Avii—Gd3—F3ix | 118.7 (7) |
F1viii—Gd1—F1ix | 80.5 (7) | F2A—Gd3—F3ix | 63.5 (7) |
F7—Gd1—F4 | 132.3 (4) | F8A—Gd3—F3ix | 116.2 (7) |
F7i—Gd1—F4 | 74.7 (4) | F8Avii—Gd3—F3ix | 61.5 (7) |
F6i—Gd1—F4 | 69.3 (4) | F8—Gd3—F3iv | 36.6 (9) |
F6—Gd1—F4 | 70.8 (4) | F8vii—Gd3—F3iv | 141.1 (9) |
F1viii—Gd1—F4 | 120.6 (4) | F2—Gd3—F3iv | 137.7 (8) |
F1ix—Gd1—F4 | 144.9 (4) | F2vii—Gd3—F3iv | 44.4 (8) |
F7—Gd1—F4i | 74.7 (4) | F7vii—Gd3—F3iv | 96.1 (6) |
F7i—Gd1—F4i | 132.3 (4) | F7—Gd3—F3iv | 83.3 (6) |
F6i—Gd1—F4i | 70.8 (4) | F2Avii—Gd3—F3iv | 63.5 (7) |
F6—Gd1—F4i | 69.3 (4) | F2A—Gd3—F3iv | 118.7 (7) |
F1viii—Gd1—F4i | 144.9 (4) | F8A—Gd3—F3iv | 61.5 (7) |
F1ix—Gd1—F4i | 120.6 (4) | F8Avii—Gd3—F3iv | 116.2 (7) |
F4—Gd1—F4i | 59.1 (5) | F3ix—Gd3—F3iv | 177.7 (9) |
F7—Gd1—Gd2 | 96.1 (3) | Gd2—F1—Gd1vi | 140.9 (6) |
F7i—Gd1—Gd2 | 107.6 (3) | Gd2—F1—Gd3xi | 101.4 (4) |
F6i—Gd1—Gd2 | 96.8 (3) | Gd1vi—F1—Gd3xi | 105.2 (4) |
F6—Gd1—Gd2 | 37.0 (3) | Gd2—F1—Cs1xiii | 99.4 (4) |
F1viii—Gd1—Gd2 | 112.2 (3) | Gd1vi—F1—Cs1xiii | 102.9 (4) |
F1ix—Gd1—Gd2 | 161.0 (3) | Gd3xi—F1—Cs1xiii | 101.1 (4) |
F4—Gd1—Gd2 | 40.8 (2) | F2A—F2—Gd2ix | 103 (2) |
F4i—Gd1—Gd2 | 41.3 (3) | F2A—F2—Gd3 | 82 (2) |
F7—Gd1—Gd2i | 107.6 (3) | Gd2ix—F2—Gd3 | 122.4 (10) |
F7i—Gd1—Gd2i | 96.1 (3) | F2A—F2—Cs1vii | 136 (3) |
F6i—Gd1—Gd2i | 37.0 (3) | Gd2ix—F2—Cs1vii | 106.4 (9) |
F6—Gd1—Gd2i | 96.8 (3) | Gd3—F2—Cs1vii | 108.4 (8) |
F1viii—Gd1—Gd2i | 161.0 (3) | F2A—F2—Cs1xiv | 41 (2) |
F1ix—Gd1—Gd2i | 112.2 (3) | Gd2ix—F2—Cs1xiv | 104.5 (8) |
F4—Gd1—Gd2i | 41.3 (3) | Gd3—F2—Cs1xiv | 113.4 (9) |
F4i—Gd1—Gd2i | 40.8 (2) | Cs1vii—F2—Cs1xiv | 99.0 (6) |
Gd2—Gd1—Gd2i | 59.84 (4) | F2—F2A—Gd3 | 78 (2) |
F7—Gd1—Gd3 | 29.6 (3) | F2—F2A—Gd2ix | 58 (2) |
F7i—Gd1—Gd3 | 125.0 (3) | Gd3—F2A—Gd2ix | 109.0 (8) |
F6i—Gd1—Gd3 | 101.5 (3) | F2—F2A—Cs1xiv | 129 (2) |
F6—Gd1—Gd3 | 107.0 (3) | Gd3—F2A—Cs1xiv | 136.4 (8) |
F1viii—Gd1—Gd3 | 78.7 (3) | Gd2ix—F2A—Cs1xiv | 114.5 (7) |
F1ix—Gd1—Gd3 | 40.4 (3) | F8xv—F3—Gd2 | 150.4 (16) |
F4—Gd1—Gd3 | 158.2 (2) | F8xv—F3—Gd2xii | 56.4 (12) |
F4i—Gd1—Gd3 | 99.4 (2) | Gd2—F3—Gd2xii | 134.7 (10) |
Gd2—Gd1—Gd3 | 125.72 (2) | F8xv—F3—Gd3xi | 55.4 (12) |
Gd2i—Gd1—Gd3 | 120.26 (2) | Gd2—F3—Gd3xi | 100.5 (8) |
F7—Gd1—Gd3x | 125.0 (3) | Gd2xii—F3—Gd3xi | 109.8 (8) |
F7i—Gd1—Gd3x | 29.6 (3) | F8xv—F3—Cs1xv | 98.8 (15) |
F6i—Gd1—Gd3x | 107.0 (3) | Gd2—F3—Cs1xv | 103.4 (7) |
F6—Gd1—Gd3x | 101.5 (3) | Gd2xii—F3—Cs1xv | 102.4 (7) |
F1viii—Gd1—Gd3x | 40.4 (3) | Gd3xi—F3—Cs1xv | 102.0 (7) |
F1ix—Gd1—Gd3x | 78.7 (3) | Gd2—F4—Gd2i | 97.7 (4) |
F4—Gd1—Gd3x | 99.4 (2) | Gd2—F4—Gd1 | 97.6 (4) |
F4i—Gd1—Gd3x | 158.2 (2) | Gd2i—F4—Gd1 | 97.1 (4) |
Gd2—Gd1—Gd3x | 120.26 (2) | Gd2—F4—Cs1i | 116.4 (4) |
Gd2i—Gd1—Gd3x | 125.72 (2) | Gd2i—F4—Cs1i | 123.9 (4) |
Gd3—Gd1—Gd3x | 102.27 (3) | Gd1—F4—Cs1i | 118.9 (4) |
F8iii—Gd2—F2xi | 132.9 (11) | Gd2i—F5—Gd2 | 106.3 (6) |
F8iii—Gd2—F5 | 98.7 (9) | Gd2i—F5—Cs1xiii | 116.42 (11) |
F2xi—Gd2—F5 | 116.3 (7) | Gd2—F5—Cs1xiii | 115.00 (11) |
F8iii—Gd2—F6 | 96.7 (10) | Gd2i—F5—Cs1v | 115.00 (11) |
F2xi—Gd2—F6 | 81.4 (7) | Gd2—F5—Cs1v | 116.42 (11) |
F5—Gd2—F6 | 134.1 (4) | Cs1xiii—F5—Cs1v | 87.3 (4) |
F8iii—Gd2—F1 | 85.1 (9) | Gd2—F6—Gd1 | 105.7 (4) |
F2xi—Gd2—F1 | 72.0 (7) | Gd2—F6—Cs1iii | 116.0 (4) |
F5—Gd2—F1 | 80.1 (4) | Gd1—F6—Cs1iii | 109.9 (4) |
F6—Gd2—F1 | 144.4 (4) | Gd2—F6—Cs1xv | 114.6 (4) |
F8iii—Gd2—F3 | 83.3 (10) | Gd1—F6—Cs1xv | 121.2 (4) |
F2xi—Gd2—F3 | 50.1 (9) | Cs1iii—F6—Cs1xv | 89.2 (3) |
F5—Gd2—F3 | 146.5 (6) | Gd1—F7—Gd3 | 121.6 (5) |
F6—Gd2—F3 | 78.1 (6) | Gd1—F7—Cs1iii | 105.8 (4) |
F1—Gd2—F3 | 66.7 (6) | Gd3—F7—Cs1iii | 112.1 (4) |
F8iii—Gd2—F4 | 142.7 (8) | Gd1—F7—Cs1 | 109.0 (4) |
F2xi—Gd2—F4 | 81.5 (7) | Gd3—F7—Cs1 | 111.7 (5) |
F5—Gd2—F4 | 70.0 (4) | Cs1iii—F7—Cs1 | 92.7 (3) |
F6—Gd2—F4 | 71.6 (4) | F8A—F8—F3iv | 172 (3) |
F1—Gd2—F4 | 125.2 (4) | F8A—F8—Gd2iii | 103 (2) |
F3—Gd2—F4 | 126.1 (6) | F3iv—F8—Gd2iii | 82.6 (15) |
F8iii—Gd2—F3xii | 41.0 (10) | F8A—F8—Gd3 | 85 (2) |
F2xi—Gd2—F3xii | 93.9 (9) | F3iv—F8—Gd3 | 88.0 (15) |
F5—Gd2—F3xii | 136.6 (5) | Gd2iii—F8—Gd3 | 160.2 (15) |
F6—Gd2—F3xii | 77.7 (6) | F8A—F8—Cs1iii | 53 (2) |
F1—Gd2—F3xii | 80.9 (6) | F3iv—F8—Cs1iii | 132.7 (17) |
F3—Gd2—F3xii | 44.0 (10) | Gd2iii—F8—Cs1iii | 102.9 (10) |
F4—Gd2—F3xii | 149.3 (6) | Gd3—F8—Cs1iii | 96.3 (9) |
F8iii—Gd2—F4i | 83.0 (8) | F8—F8A—Gd3 | 70 (2) |
F2xi—Gd2—F4i | 137.0 (7) | F8—F8A—Gd2iii | 54 (2) |
F5—Gd2—F4i | 69.6 (4) | Gd3—F8A—Gd2iii | 121.5 (10) |
F6—Gd2—F4i | 69.8 (4) | F8—F8A—Cs1viii | 144 (2) |
F1—Gd2—F4i | 145.2 (4) | Gd3—F8A—Cs1viii | 109.3 (7) |
F3—Gd2—F4i | 143.1 (6) | Gd2iii—F8A—Cs1viii | 106.5 (7) |
F4—Gd2—F4i | 59.8 (5) | F8—F8A—Cs1iii | 113 (2) |
F3xii—Gd2—F4i | 109.6 (6) | Gd3—F8A—Cs1iii | 108.1 (7) |
F8iii—Gd2—F2Axi | 146.0 (9) | Gd2iii—F8A—Cs1iii | 108.6 (7) |
F2xi—Gd2—F2Axi | 18.9 (7) | Cs1viii—F8A—Cs1iii | 100.9 (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, y−1/2, z+1/2; (v) −x+3/2, −y+2, z; (vi) x+1/2, y, −z; (vii) −x+1/2, −y+2, z; (viii) x−1/2, y, −z; (ix) x−1/2, −y+5/2, z+1/2; (x) −x+1/2, y+1/2, −z+1/2; (xi) x+1/2, −y+5/2, z−1/2; (xii) x, −y+5/2, −z−1/2; (xiii) −x+3/2, y+1/2, −z+1/2; (xiv) x−1/2, y, −z+1; (xv) −x+1, y+1/2, z−1/2. |
F10KY3 | Mo Kα radiation, λ = 0.71073 Å |
Mr = 495.83 | Cell parameters from 3620 reflections |
Cubic, Fm3m | θ = 2.6–26.6° |
a = 11.5439 (13) Å | µ = 23.12 mm−1 |
V = 1538.4 (3) Å3 | T = 293 K |
Z = 8 | Block, colorless |
F(000) = 1808 | 0.15 × 0.15 × 0.12 mm |
Dx = 4.282 Mg m−3 |
Rigaku AFC8S diffractometer | 115 independent reflections |
Radiation source: fine-focus sealed tube | 114 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.059 |
Detector resolution: 0 pixels mm-1 | θmax = 26.6°, θmin = 3.1° |
ω scans | h = −14→14 |
Absorption correction: multi-scan REQAB, CrystalClear | k = −14→14 |
Tmin = 0.801, Tmax = 1.000 | l = −14→14 |
3620 measured reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary 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 = 1.19 | Δρmax = 0.55 e Å−3 |
115 reflections | Δρmin = −0.53 e Å−3 |
13 parameters | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.00104 (13) |
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. |
x | y | z | Uiso*/Ueq | ||
K1 | −0.2500 | −0.2500 | −0.2500 | 0.0196 (9) | |
Y1 | −0.24082 (8) | 0.0000 | 0.0000 | 0.0116 (4) | |
F1 | −0.1121 (3) | −0.1121 (3) | −0.1121 (3) | 0.0150 (11) | |
F2 | 0.5000 | 0.1659 (3) | 0.1659 (3) | 0.0206 (10) |
U11 | U22 | U33 | U12 | U13 | U23 | |
K1 | 0.0196 (9) | 0.0196 (9) | 0.0196 (9) | 0.000 | 0.000 | 0.000 |
Y1 | 0.0115 (6) | 0.0117 (5) | 0.0117 (5) | 0.000 | 0.000 | 0.000 |
F1 | 0.0150 (11) | 0.0150 (11) | 0.0150 (11) | 0.0013 (11) | 0.0013 (11) | 0.0013 (11) |
F2 | 0.026 (2) | 0.0180 (14) | 0.0180 (14) | 0.000 | 0.000 | 0.0062 (18) |
K1—F1 | 2.757 (5) | Y1—F2xiv | 2.1973 (12) |
K1—F1i | 2.757 (5) | Y1—F1xv | 2.3573 (15) |
K1—F1ii | 2.757 (5) | Y1—F1 | 2.3573 (15) |
K1—F1iii | 2.757 (5) | Y1—F1xvi | 2.3573 (15) |
K1—F2iv | 3.1957 (18) | Y1—F1xvii | 2.3573 (15) |
K1—F2v | 3.1957 (18) | Y1—Y1xviii | 3.9314 (14) |
K1—F2vi | 3.1957 (18) | Y1—Y1xix | 3.9314 (14) |
K1—F2vii | 3.1957 (18) | Y1—Y1xx | 3.9314 (14) |
K1—F2viii | 3.1957 (18) | Y1—Y1xxi | 3.9314 (14) |
K1—F2ix | 3.1957 (18) | F1—Y1xxi | 2.3573 (15) |
K1—F2x | 3.1957 (18) | F1—Y1xx | 2.3573 (15) |
K1—F2xi | 3.1957 (18) | F2—Y1xxii | 2.1973 (12) |
Y1—F2xi | 2.1973 (12) | F2—Y1xxiii | 2.1973 (12) |
Y1—F2xii | 2.1973 (12) | F2—K1xxiv | 3.1957 (18) |
Y1—F2xiii | 2.1973 (12) | F2—K1xxv | 3.1957 (18) |
F1—K1—F1i | 109.5 | F2xi—Y1—F1xv | 141.94 (5) |
F1—K1—F1ii | 109.5 | F2xii—Y1—F1xv | 141.94 (5) |
F1i—K1—F1ii | 109.5 | F2xiii—Y1—F1xv | 80.23 (13) |
F1—K1—F1iii | 109.5 | F2xiv—Y1—F1xv | 80.23 (13) |
F1i—K1—F1iii | 109.5 | F2xi—Y1—F1 | 80.23 (13) |
F1ii—K1—F1iii | 109.5 | F2xii—Y1—F1 | 80.23 (13) |
F1—K1—F2iv | 150.70 (7) | F2xiii—Y1—F1 | 141.94 (5) |
F1i—K1—F2iv | 99.83 (7) | F2xiv—Y1—F1 | 141.94 (5) |
F1ii—K1—F2iv | 58.574 (19) | F1xv—Y1—F1 | 101.8 (2) |
F1iii—K1—F2iv | 58.574 (19) | F2xi—Y1—F1xvi | 141.94 (5) |
F1—K1—F2v | 150.70 (7) | F2xii—Y1—F1xvi | 80.23 (13) |
F1i—K1—F2v | 58.574 (19) | F2xiii—Y1—F1xvi | 80.23 (13) |
F1ii—K1—F2v | 58.574 (19) | F2xiv—Y1—F1xvi | 141.94 (5) |
F1iii—K1—F2v | 99.83 (7) | F1xv—Y1—F1xvi | 66.58 (13) |
F2iv—K1—F2v | 50.16 (11) | F1—Y1—F1xvi | 66.58 (13) |
F1—K1—F2vi | 150.70 (7) | F2xi—Y1—F1xvii | 80.23 (13) |
F1i—K1—F2vi | 58.574 (19) | F2xii—Y1—F1xvii | 141.94 (5) |
F1ii—K1—F2vi | 99.83 (7) | F2xiii—Y1—F1xvii | 141.94 (5) |
F1iii—K1—F2vi | 58.574 (19) | F2xiv—Y1—F1xvii | 80.23 (13) |
F2iv—K1—F2vi | 50.16 (11) | F1xv—Y1—F1xvii | 66.58 (13) |
F2v—K1—F2vi | 50.16 (11) | F1—Y1—F1xvii | 66.58 (13) |
F1—K1—F2vii | 58.574 (19) | F1xvi—Y1—F1xvii | 101.8 (2) |
F1i—K1—F2vii | 58.574 (19) | F2xi—Y1—Y1xviii | 164.33 (10) |
F1ii—K1—F2vii | 150.70 (7) | F2xii—Y1—Y1xviii | 110.27 (7) |
F1iii—K1—F2vii | 99.83 (7) | F2xiii—Y1—Y1xviii | 74.33 (10) |
F2iv—K1—F2vii | 144.64 (9) | F2xiv—Y1—Y1xviii | 110.27 (7) |
F2v—K1—F2vii | 117.15 (4) | F1xv—Y1—Y1xviii | 33.50 (5) |
F2vi—K1—F2vii | 95.29 (3) | F1—Y1—Y1xviii | 86.70 (10) |
F1—K1—F2viii | 58.574 (19) | F1xvi—Y1—Y1xviii | 33.50 (5) |
F1i—K1—F2viii | 58.574 (19) | F1xvii—Y1—Y1xviii | 86.70 (10) |
F1ii—K1—F2viii | 99.83 (7) | F2xi—Y1—Y1xix | 110.27 (7) |
F1iii—K1—F2viii | 150.70 (7) | F2xii—Y1—Y1xix | 164.33 (10) |
F2iv—K1—F2viii | 144.64 (9) | F2xiii—Y1—Y1xix | 110.27 (7) |
F2v—K1—F2viii | 95.29 (3) | F2xiv—Y1—Y1xix | 74.33 (10) |
F2vi—K1—F2viii | 117.15 (4) | F1xv—Y1—Y1xix | 33.50 (5) |
F2vii—K1—F2viii | 50.86 (13) | F1—Y1—Y1xix | 86.70 (10) |
F1—K1—F2ix | 58.574 (19) | F1xvi—Y1—Y1xix | 86.70 (10) |
F1i—K1—F2ix | 99.83 (7) | F1xvii—Y1—Y1xix | 33.50 (5) |
F1ii—K1—F2ix | 150.70 (7) | Y1xviii—Y1—Y1xix | 60.0 |
F1iii—K1—F2ix | 58.574 (19) | F2xi—Y1—Y1xx | 74.33 (10) |
F2iv—K1—F2ix | 117.15 (4) | F2xii—Y1—Y1xx | 110.27 (7) |
F2v—K1—F2ix | 144.64 (9) | F2xiii—Y1—Y1xx | 164.33 (10) |
F2vi—K1—F2ix | 95.29 (3) | F2xiv—Y1—Y1xx | 110.27 (7) |
F2vii—K1—F2ix | 50.16 (11) | F1xv—Y1—Y1xx | 86.70 (10) |
F2viii—K1—F2ix | 95.29 (3) | F1—Y1—Y1xx | 33.50 (5) |
F1—K1—F2x | 58.574 (19) | F1xvi—Y1—Y1xx | 86.70 (10) |
F1i—K1—F2x | 99.83 (7) | F1xvii—Y1—Y1xx | 33.50 (5) |
F1ii—K1—F2x | 58.574 (19) | Y1xviii—Y1—Y1xx | 90.0 |
F1iii—K1—F2x | 150.70 (7) | Y1xix—Y1—Y1xx | 60.0 |
F2iv—K1—F2x | 117.15 (4) | F2xi—Y1—Y1xxi | 110.27 (7) |
F2v—K1—F2x | 95.29 (3) | F2xii—Y1—Y1xxi | 74.33 (10) |
F2vi—K1—F2x | 144.64 (9) | F2xiii—Y1—Y1xxi | 110.27 (7) |
F2vii—K1—F2x | 95.29 (3) | F2xiv—Y1—Y1xxi | 164.33 (10) |
F2viii—K1—F2x | 50.16 (11) | F1xv—Y1—Y1xxi | 86.70 (10) |
F2ix—K1—F2x | 117.15 (4) | F1—Y1—Y1xxi | 33.50 (5) |
F1—K1—F2xi | 58.574 (19) | F1xvi—Y1—Y1xxi | 33.50 (5) |
F1i—K1—F2xi | 150.70 (7) | F1xvii—Y1—Y1xxi | 86.70 (10) |
F1ii—K1—F2xi | 99.83 (7) | Y1xviii—Y1—Y1xxi | 60.0 |
F1iii—K1—F2xi | 58.574 (19) | Y1xix—Y1—Y1xxi | 90.0 |
F2iv—K1—F2xi | 95.29 (3) | Y1xx—Y1—Y1xxi | 60.0 |
F2v—K1—F2xi | 144.64 (9) | Y1xxi—F1—Y1xx | 113.00 (10) |
F2vi—K1—F2xi | 117.15 (4) | Y1xxi—F1—Y1 | 113.00 (10) |
F2vii—K1—F2xi | 95.29 (3) | Y1xx—F1—Y1 | 113.00 (10) |
F2viii—K1—F2xi | 117.15 (4) | Y1xxi—F1—K1 | 105.66 (12) |
F2ix—K1—F2xi | 50.86 (13) | Y1xx—F1—K1 | 105.66 (12) |
F2x—K1—F2xi | 95.29 (3) | Y1—F1—K1 | 105.66 (12) |
F2xi—Y1—F2xii | 76.11 (9) | Y1xxii—F2—Y1xxiii | 148.7 (2) |
F2xi—Y1—F2xiii | 121.3 (2) | Y1xxii—F2—K1xxiv | 96.66 (3) |
F2xii—Y1—F2xiii | 76.11 (9) | Y1xxiii—F2—K1xxiv | 96.66 (3) |
F2xi—Y1—F2xiv | 76.11 (9) | Y1xxii—F2—K1xxv | 96.66 (3) |
F2xii—Y1—F2xiv | 121.3 (2) | Y1xxiii—F2—K1xxv | 96.66 (3) |
F2xiii—Y1—F2xiv | 76.11 (9) | K1xxiv—F2—K1xxv | 129.14 (13) |
Symmetry codes: (i) x, −y−1/2, −z−1/2; (ii) −x−1/2, y, −z−1/2; (iii) −x−1/2, −y−1/2, z; (iv) x−1, y−1/2, z−1/2; (v) y−1/2, z−1/2, x−1; (vi) z−1/2, x−1, y−1/2; (vii) x−1/2, y−1/2, −z; (viii) −x+1/2, −y, z−1/2; (ix) −y, z−1/2, −x+1/2; (x) −z, x−1/2, y−1/2; (xi) y−1/2, −z, x−1/2; (xii) z−1/2, −x+1/2, −y; (xiii) y−1/2, z, x−1/2; (xiv) z−1/2, x−1/2, 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. |
F10RbY3 | Dx = 4.624 Mg m−3 |
Mr = 542.20 | Mo Kα radiation, λ = 0.71073 Å |
Hexagonal, P63mc | Cell parameters from 3303 reflections |
a = 8.1976 (12) Å | θ = 2.9–26.7° |
c = 13.384 (3) Å | µ = 28.51 mm−1 |
V = 778.9 (2) Å3 | T = 293 K |
Z = 4 | Block, colorless |
F(000) = 976 | 0.22 × 0.12 × 0.10 mm |
Rigaku AFC8S diffractometer | 557 independent reflections |
Radiation source: fine-focus sealed tube | 522 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.057 |
Detector resolution: 14.6199 pixels mm-1 | θmax = 25.2°, θmin = 2.9° |
ω scans | h = −9→9 |
Absorption correction: multi-scan REQAB, CrystalClear | k = −9→9 |
Tmin = 0.692, Tmax = 1.000 | l = −14→16 |
6434 measured reflections |
Refinement on F2 | Secondary 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) = 0.086 | Δρmax = 1.17 e Å−3 |
S = 1.16 | Δρmin = −0.86 e Å−3 |
557 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
60 parameters | Extinction coefficient: 0.0057 (5) |
1 restraint | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.21 (3) |
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. |
x | y | z | Uiso*/Ueq | ||
Rb1 | 0.3333 | 0.6667 | 0.95169 (17) | 0.0163 (6) | |
Rb2 | 0.0000 | 1.0000 | 0.70814 (19) | 0.0209 (9) | |
Y1 | 0.01072 (15) | 0.50536 (7) | 0.69776 (8) | 0.0085 (3) | |
Y2 | 0.34722 (14) | 0.17361 (7) | 0.95759 (8) | 0.0083 (4) | |
F1 | 0.3333 | 0.6667 | 0.7412 (12) | 0.017 (3) | |
F2 | 0.6667 | 0.3333 | 0.9128 (11) | 0.010 (3) | |
F3 | 0.0435 (9) | 0.5217 (5) | 0.5225 (6) | 0.0115 (15) | |
F4 | 0.3664 (10) | 0.1832 (5) | 1.1334 (7) | 0.0136 (17) | |
F5 | 0.3396 (7) | 0.0032 (9) | 0.8284 (9) | 0.0188 (8) | |
F6 | −0.2218 (5) | 0.2218 (5) | 0.6594 (7) | 0.0167 (15) | |
F7 | 0.1105 (5) | −0.1105 (5) | 0.9894 (7) | 0.0177 (16) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Rb1 | 0.0172 (7) | 0.0172 (7) | 0.0145 (15) | 0.0086 (4) | 0.000 | 0.000 |
Rb2 | 0.0164 (6) | 0.0164 (6) | 0.030 (3) | 0.0082 (3) | 0.000 | 0.000 |
Y1 | 0.0097 (6) | 0.0094 (4) | 0.0066 (7) | 0.0048 (3) | 0.0003 (7) | 0.0001 (3) |
Y2 | 0.0085 (6) | 0.0085 (4) | 0.0079 (7) | 0.0042 (3) | 0.0017 (8) | 0.0009 (4) |
F1 | 0.016 (5) | 0.016 (5) | 0.019 (7) | 0.008 (3) | 0.000 | 0.000 |
F2 | 0.003 (4) | 0.003 (4) | 0.023 (8) | 0.001 (2) | 0.000 | 0.000 |
F3 | 0.013 (4) | 0.014 (3) | 0.007 (4) | 0.0063 (19) | −0.001 (3) | −0.0007 (13) |
F4 | 0.011 (4) | 0.013 (3) | 0.016 (4) | 0.0053 (18) | 0.000 (3) | 0.0002 (15) |
F5 | 0.025 (3) | 0.017 (2) | 0.0113 (17) | 0.008 (3) | 0.0042 (17) | −0.0007 (16) |
F6 | 0.016 (3) | 0.016 (3) | 0.015 (4) | 0.005 (3) | 0.0009 (15) | −0.0009 (15) |
F7 | 0.015 (3) | 0.015 (3) | 0.016 (4) | 0.003 (3) | −0.0004 (16) | 0.0004 (16) |
Rb1—F1 | 2.817 (16) | Y1—Y1xv | 3.9670 (19) |
Rb1—F3i | 2.838 (7) | Y1—Y1xviii | 3.9670 (19) |
Rb1—F3ii | 2.838 (7) | Y2—F7 | 2.203 (2) |
Rb1—F3iii | 2.838 (7) | Y2—F7v | 2.203 (2) |
Rb1—F5iv | 3.192 (9) | Y2—F5 | 2.204 (10) |
Rb1—F5v | 3.192 (9) | Y2—F5viii | 2.204 (10) |
Rb1—F5vi | 3.192 (9) | Y2—F3iii | 2.338 (4) |
Rb1—F5vii | 3.192 (9) | Y2—F3xix | 2.338 (4) |
Rb1—F5viii | 3.192 (9) | Y2—F2 | 2.346 (4) |
Rb1—F5ix | 3.192 (9) | Y2—F4 | 2.357 (9) |
Rb1—F6ii | 3.199 (10) | Y2—Y2ix | 3.9281 (19) |
Rb1—F6i | 3.199 (10) | Y2—Y2xx | 3.9280 (18) |
Rb2—F4x | 2.787 (8) | Y2—Y1iii | 3.9405 (15) |
Rb2—F4xi | 2.787 (7) | Y2—Y1xix | 3.9405 (15) |
Rb2—F4xii | 2.787 (8) | F1—Y1xv | 2.363 (4) |
Rb2—F5xiii | 3.205 (8) | F1—Y1xviii | 2.363 (4) |
Rb2—F5xiv | 3.205 (8) | F2—Y2xx | 2.346 (4) |
Rb2—F5xv | 3.205 (8) | F2—Y2ix | 2.346 (4) |
Rb2—F5vi | 3.205 (8) | F3—Y2xvii | 2.338 (4) |
Rb2—F5xvi | 3.205 (8) | F3—Y2xi | 2.338 (4) |
Rb2—F5iv | 3.205 (8) | F3—Rb1x | 2.838 (7) |
Rb2—F6xiv | 3.216 (8) | F4—Y1iii | 2.377 (4) |
Rb2—F6xv | 3.216 (8) | F4—Y1xix | 2.377 (4) |
Rb2—F6vi | 3.216 (8) | F4—Rb2ii | 2.787 (7) |
Y1—F5iv | 2.198 (10) | F5—Y1xxi | 2.198 (10) |
Y1—F5v | 2.198 (10) | F5—Rb1xxii | 3.192 (9) |
Y1—F6 | 2.207 (3) | F5—Rb2xxii | 3.205 (8) |
Y1—F6xiv | 2.207 (3) | F6—Y1xxiii | 2.207 (3) |
Y1—F3 | 2.357 (8) | F6—Rb1x | 3.199 (10) |
Y1—F1 | 2.363 (4) | F6—Rb2xxii | 3.216 (8) |
Y1—F4xi | 2.377 (4) | F7—Y2xxi | 2.203 (2) |
Y1—F4xvii | 2.377 (4) | F7—Rb1xxii | 3.204 (7) |
Y1—Y2xvii | 3.9405 (15) | F7—Rb2ii | 3.321 (10) |
Y1—Y2xi | 3.9405 (15) | ||
F1—Rb1—F3i | 109.51 (19) | F1—Y1—F4xi | 65.8 (2) |
F1—Rb1—F3ii | 109.51 (19) | F5iv—Y1—F4xvii | 141.3 (3) |
F3i—Rb1—F3ii | 109.43 (19) | F5v—Y1—F4xvii | 80.9 (3) |
F1—Rb1—F3iii | 109.51 (19) | F6—Y1—F4xvii | 79.5 (2) |
F3i—Rb1—F3iii | 109.43 (19) | F6xiv—Y1—F4xvii | 141.6 (3) |
F3ii—Rb1—F3iii | 109.43 (19) | F3—Y1—F4xvii | 65.7 (2) |
F1—Rb1—F5iv | 58.9 (2) | F1—Y1—F4xvii | 65.8 (2) |
F3i—Rb1—F5iv | 100.71 (13) | F4xi—Y1—F4xvii | 101.9 (4) |
F3ii—Rb1—F5iv | 57.8 (2) | F5iv—Y1—Y2xvii | 164.43 (18) |
F3iii—Rb1—F5iv | 149.85 (15) | F5v—Y1—Y2xvii | 111.2 (2) |
F1—Rb1—F5v | 58.9 (2) | F6—Y1—Y2xvii | 73.7 (2) |
F3i—Rb1—F5v | 149.85 (15) | F6xiv—Y1—Y2xvii | 109.8 (2) |
F3ii—Rb1—F5v | 57.8 (2) | F3—Y1—Y2xvii | 32.78 (6) |
F3iii—Rb1—F5v | 100.71 (13) | F1—Y1—Y2xvii | 85.2 (3) |
F5iv—Rb1—F5v | 49.1 (2) | F4xi—Y1—Y2xvii | 86.6 (2) |
F1—Rb1—F5vi | 58.9 (2) | F4xvii—Y1—Y2xvii | 33.5 (2) |
F3i—Rb1—F5vi | 57.8 (2) | F5iv—Y1—Y2xi | 111.2 (2) |
F3ii—Rb1—F5vi | 100.71 (13) | F5v—Y1—Y2xi | 164.43 (18) |
F3iii—Rb1—F5vi | 149.85 (15) | F6—Y1—Y2xi | 109.8 (2) |
F5iv—Rb1—F5vi | 52.2 (2) | F6xiv—Y1—Y2xi | 73.7 (2) |
F5v—Rb1—F5vi | 95.7 (3) | F3—Y1—Y2xi | 32.78 (6) |
F1—Rb1—F5vii | 58.9 (2) | F1—Y1—Y2xi | 85.2 (3) |
F3i—Rb1—F5vii | 57.8 (2) | F4xi—Y1—Y2xi | 33.5 (2) |
F3ii—Rb1—F5vii | 149.85 (15) | F4xvii—Y1—Y2xi | 86.6 (2) |
F3iii—Rb1—F5vii | 100.71 (13) | Y2xvii—Y1—Y2xi | 59.79 (4) |
F5iv—Rb1—F5vii | 95.7 (3) | F5iv—Y1—Y1xv | 74.74 (18) |
F5v—Rb1—F5vii | 117.7 (4) | F5v—Y1—Y1xv | 109.9 (2) |
F5vi—Rb1—F5vii | 49.1 (2) | F6—Y1—Y1xv | 163.4 (2) |
F1—Rb1—F5viii | 58.9 (2) | F6xiv—Y1—Y1xv | 109.70 (19) |
F3i—Rb1—F5viii | 149.85 (15) | F3—Y1—Y1xv | 85.10 (14) |
F3ii—Rb1—F5viii | 100.71 (13) | F1—Y1—Y1xv | 32.93 (14) |
F3iii—Rb1—F5viii | 57.8 (2) | F4xi—Y1—Y1xv | 33.44 (15) |
F5iv—Rb1—F5viii | 95.7 (3) | F4xvii—Y1—Y1xv | 86.69 (15) |
F5v—Rb1—F5viii | 52.2 (2) | Y2xvii—Y1—Y1xv | 89.72 (2) |
F5vi—Rb1—F5viii | 117.7 (4) | Y2xi—Y1—Y1xv | 59.777 (17) |
F5vii—Rb1—F5viii | 95.7 (3) | F5iv—Y1—Y1xviii | 109.93 (19) |
F1—Rb1—F5ix | 58.9 (2) | F5v—Y1—Y1xviii | 74.74 (17) |
F3i—Rb1—F5ix | 100.71 (13) | F6—Y1—Y1xviii | 109.70 (19) |
F3ii—Rb1—F5ix | 149.85 (15) | F6xiv—Y1—Y1xviii | 163.4 (2) |
F3iii—Rb1—F5ix | 57.8 (2) | F3—Y1—Y1xviii | 85.10 (14) |
F5iv—Rb1—F5ix | 117.7 (4) | F1—Y1—Y1xviii | 32.93 (14) |
F5v—Rb1—F5ix | 95.7 (3) | F4xi—Y1—Y1xviii | 86.69 (15) |
F5vi—Rb1—F5ix | 95.7 (3) | F4xvii—Y1—Y1xviii | 33.44 (15) |
F5vii—Rb1—F5ix | 52.2 (2) | Y2xvii—Y1—Y1xviii | 59.777 (17) |
F5viii—Rb1—F5ix | 49.1 (2) | Y2xi—Y1—Y1xviii | 89.72 (2) |
F1—Rb1—F6ii | 150.33 (15) | Y1xv—Y1—Y1xviii | 60.0 |
F3i—Rb1—F6ii | 58.44 (15) | F7—Y2—F7v | 76.2 (4) |
F3ii—Rb1—F6ii | 58.44 (15) | F7—Y2—F5 | 75.6 (3) |
F3iii—Rb1—F6ii | 100.2 (3) | F7v—Y2—F5 | 121.0 (3) |
F5iv—Rb1—F6ii | 94.9 (2) | F7—Y2—F5viii | 121.0 (3) |
F5v—Rb1—F6ii | 116.24 (18) | F7v—Y2—F5viii | 75.6 (3) |
F5vi—Rb1—F6ii | 94.9 (2) | F5—Y2—F5viii | 76.6 (5) |
F5vii—Rb1—F6ii | 116.24 (18) | F7—Y2—F3iii | 143.4 (3) |
F5viii—Rb1—F6ii | 145.0 (2) | F7v—Y2—F3iii | 82.1 (3) |
F5ix—Rb1—F6ii | 145.0 (2) | F5—Y2—F3iii | 141.0 (3) |
F1—Rb1—F6i | 150.33 (15) | F5viii—Y2—F3iii | 80.3 (3) |
F3i—Rb1—F6i | 58.44 (15) | F7—Y2—F3xix | 82.1 (3) |
F3ii—Rb1—F6i | 100.2 (3) | F7v—Y2—F3xix | 143.4 (3) |
F3iii—Rb1—F6i | 58.44 (15) | F5—Y2—F3xix | 80.3 (3) |
F5iv—Rb1—F6i | 145.0 (2) | F5viii—Y2—F3xix | 141.0 (3) |
F5v—Rb1—F6i | 145.0 (2) | F3iii—Y2—F3xix | 99.3 (3) |
F5vi—Rb1—F6i | 116.24 (18) | F7—Y2—F2 | 141.91 (19) |
F5vii—Rb1—F6i | 94.9 (2) | F7v—Y2—F2 | 141.9 (2) |
F5viii—Rb1—F6i | 116.24 (18) | F5—Y2—F2 | 79.8 (3) |
F5ix—Rb1—F6i | 94.9 (2) | F5viii—Y2—F2 | 79.8 (3) |
F6ii—Rb1—F6i | 50.8 (2) | F3iii—Y2—F2 | 65.3 (2) |
F4x—Rb2—F4xi | 107.9 (2) | F3xix—Y2—F2 | 65.3 (2) |
F4x—Rb2—F4xii | 107.9 (2) | F7—Y2—F4 | 81.4 (3) |
F4xi—Rb2—F4xii | 107.9 (2) | F7v—Y2—F4 | 81.4 (3) |
F4x—Rb2—F5xiii | 151.95 (15) | F5—Y2—F4 | 141.7 (2) |
F4xi—Rb2—F5xiii | 100.01 (16) | F5viii—Y2—F4 | 141.7 (2) |
F4xii—Rb2—F5xiii | 59.0 (2) | F3iii—Y2—F4 | 66.3 (2) |
F4x—Rb2—F5xiv | 100.01 (16) | F3xix—Y2—F4 | 66.3 (2) |
F4xi—Rb2—F5xiv | 151.95 (15) | F2—Y2—F4 | 101.5 (4) |
F4xii—Rb2—F5xiv | 59.0 (2) | F7—Y2—Y2ix | 165.7 (2) |
F5xiii—Rb2—F5xiv | 52.0 (3) | F7v—Y2—Y2ix | 110.63 (19) |
F4x—Rb2—F5xv | 59.0 (2) | F5—Y2—Y2ix | 109.33 (18) |
F4xi—Rb2—F5xv | 100.01 (16) | F5viii—Y2—Y2ix | 73.22 (15) |
F4xii—Rb2—F5xv | 151.95 (15) | F3iii—Y2—Y2ix | 32.85 (16) |
F5xiii—Rb2—F5xv | 119.7 (4) | F3xix—Y2—Y2ix | 85.53 (15) |
F5xiv—Rb2—F5xv | 97.0 (3) | F2—Y2—Y2ix | 33.15 (14) |
F4x—Rb2—F5vi | 151.95 (15) | F4—Y2—Y2ix | 87.13 (15) |
F4xi—Rb2—F5vi | 59.0 (2) | F7—Y2—Y2xx | 110.63 (18) |
F4xii—Rb2—F5vi | 100.01 (16) | F7v—Y2—Y2xx | 165.7 (2) |
F5xiii—Rb2—F5vi | 50.5 (2) | F5—Y2—Y2xx | 73.22 (15) |
F5xiv—Rb2—F5vi | 97.0 (3) | F5viii—Y2—Y2xx | 109.33 (18) |
F5xv—Rb2—F5vi | 97.0 (3) | F3iii—Y2—Y2xx | 85.53 (15) |
F4x—Rb2—F5xvi | 59.0 (2) | F3xix—Y2—Y2xx | 32.85 (16) |
F4xi—Rb2—F5xvi | 151.95 (15) | F2—Y2—Y2xx | 33.15 (14) |
F4xii—Rb2—F5xvi | 100.01 (16) | F4—Y2—Y2xx | 87.13 (15) |
F5xiii—Rb2—F5xvi | 97.0 (3) | Y2ix—Y2—Y2xx | 60.0 |
F5xiv—Rb2—F5xvi | 50.5 (2) | F7—Y2—Y1iii | 111.7 (3) |
F5xv—Rb2—F5xvi | 52.0 (3) | F7v—Y2—Y1iii | 75.5 (2) |
F5vi—Rb2—F5xvi | 119.7 (4) | F5—Y2—Y1iii | 163.49 (15) |
F4x—Rb2—F5iv | 100.01 (16) | F5viii—Y2—Y1iii | 109.6 (2) |
F4xi—Rb2—F5iv | 59.0 (2) | F3iii—Y2—Y1iii | 33.09 (19) |
F4xii—Rb2—F5iv | 151.95 (15) | F3xix—Y2—Y1iii | 85.96 (19) |
F5xiii—Rb2—F5iv | 97.0 (3) | F2—Y2—Y1iii | 86.2 (3) |
F5xiv—Rb2—F5iv | 119.7 (4) | F4—Y2—Y1iii | 33.81 (7) |
F5xv—Rb2—F5iv | 50.5 (2) | Y2ix—Y2—Y1iii | 60.104 (18) |
F5vi—Rb2—F5iv | 52.0 (3) | Y2xx—Y2—Y1iii | 90.28 (2) |
F5xvi—Rb2—F5iv | 97.0 (3) | F7—Y2—Y1xix | 75.5 (2) |
F4x—Rb2—F6xiv | 58.01 (6) | F7v—Y2—Y1xix | 111.7 (3) |
F4xi—Rb2—F6xiv | 58.01 (6) | F5—Y2—Y1xix | 109.6 (2) |
F4xii—Rb2—F6xiv | 147.3 (3) | F5viii—Y2—Y1xix | 163.49 (15) |
F5xiii—Rb2—F6xiv | 146.3 (2) | F3iii—Y2—Y1xix | 85.96 (19) |
F5xiv—Rb2—F6xiv | 146.3 (2) | F3xix—Y2—Y1xix | 33.09 (19) |
F5xv—Rb2—F6xiv | 50.60 (19) | F2—Y2—Y1xix | 86.2 (3) |
F5vi—Rb2—F6xiv | 96.25 (14) | F4—Y2—Y1xix | 33.81 (7) |
F5xvi—Rb2—F6xiv | 96.25 (15) | Y2ix—Y2—Y1xix | 90.28 (2) |
F5iv—Rb2—F6xiv | 50.60 (19) | Y2xx—Y2—Y1xix | 60.104 (18) |
F4x—Rb2—F6xv | 147.3 (3) | Y1iii—Y2—Y1xix | 60.45 (3) |
F4xi—Rb2—F6xv | 58.01 (6) | Y1—F1—Y1xv | 114.1 (3) |
F4xii—Rb2—F6xv | 58.01 (6) | Y1—F1—Y1xviii | 114.1 (3) |
F5xiii—Rb2—F6xv | 50.60 (19) | Y1xv—F1—Y1xviii | 114.1 (3) |
F5xiv—Rb2—F6xv | 96.25 (15) | Y1—F1—Rb1 | 104.3 (4) |
F5xv—Rb2—F6xv | 146.3 (2) | Y1xv—F1—Rb1 | 104.3 (4) |
F5vi—Rb2—F6xv | 50.60 (19) | Y1xviii—F1—Rb1 | 104.3 (4) |
F5xvi—Rb2—F6xv | 146.3 (2) | Y2xx—F2—Y2ix | 113.7 (3) |
F5iv—Rb2—F6xv | 96.25 (14) | Y2xx—F2—Y2 | 113.7 (3) |
F6xiv—Rb2—F6xv | 115.99 (12) | Y2ix—F2—Y2 | 113.7 (3) |
F4x—Rb2—F6vi | 58.01 (6) | Y2xvii—F3—Y2xi | 114.3 (3) |
F4xi—Rb2—F6vi | 147.3 (3) | Y2xvii—F3—Y1 | 114.1 (2) |
F4xii—Rb2—F6vi | 58.01 (6) | Y2xi—F3—Y1 | 114.1 (2) |
F5xiii—Rb2—F6vi | 96.25 (14) | Y2xvii—F3—Rb1x | 104.4 (2) |
F5xiv—Rb2—F6vi | 50.60 (19) | Y2xi—F3—Rb1x | 104.4 (2) |
F5xv—Rb2—F6vi | 96.25 (14) | Y1—F3—Rb1x | 103.8 (3) |
F5vi—Rb2—F6vi | 146.3 (2) | Y2—F4—Y1iii | 112.7 (2) |
F5xvi—Rb2—F6vi | 50.60 (19) | Y2—F4—Y1xix | 112.7 (2) |
F5iv—Rb2—F6vi | 146.3 (2) | Y1iii—F4—Y1xix | 113.1 (3) |
F6xiv—Rb2—F6vi | 115.99 (13) | Y2—F4—Rb2ii | 107.7 (3) |
F6xv—Rb2—F6vi | 115.99 (13) | Y1iii—F4—Rb2ii | 104.9 (2) |
F5iv—Y1—F5v | 74.3 (4) | Y1xix—F4—Rb2ii | 104.9 (2) |
F5iv—Y1—F6 | 121.8 (3) | Y1xxi—F5—Y2 | 145.4 (3) |
F5v—Y1—F6 | 77.1 (3) | Y1xxi—F5—Rb1xxii | 97.26 (19) |
F5iv—Y1—F6xiv | 77.1 (3) | Y2—F5—Rb1xxii | 97.2 (4) |
F5v—Y1—F6xiv | 121.8 (3) | Y1xxi—F5—Rb2xxii | 97.0 (4) |
F6—Y1—F6xiv | 76.9 (4) | Y2—F5—Rb2xxii | 98.52 (18) |
F5iv—Y1—F3 | 142.8 (2) | Rb1xxii—F5—Rb2xxii | 127.9 (2) |
F5v—Y1—F3 | 142.8 (2) | Y1—F6—Y1xxiii | 146.9 (4) |
F6—Y1—F3 | 80.9 (3) | Y1—F6—Rb1x | 96.9 (2) |
F6xiv—Y1—F3 | 80.9 (3) | Y1xxiii—F6—Rb1x | 96.9 (2) |
F5iv—Y1—F1 | 81.2 (4) | Y1—F6—Rb2xxii | 96.5 (2) |
F5v—Y1—F1 | 81.2 (4) | Y1xxiii—F6—Rb2xxii | 96.5 (2) |
F6—Y1—F1 | 141.5 (2) | Rb1x—F6—Rb2xxii | 131.4 (3) |
F6xiv—Y1—F1 | 141.5 (2) | Y2xxi—F7—Y2 | 151.5 (4) |
F3—Y1—F1 | 98.6 (4) | Y2xxi—F7—Rb1xxii | 96.9 (2) |
F5iv—Y1—F4xi | 80.9 (3) | Y2—F7—Rb1xxii | 96.9 (2) |
F5v—Y1—F4xi | 141.3 (3) | Y2xxi—F7—Rb2ii | 95.6 (2) |
F6—Y1—F4xi | 141.6 (3) | Y2—F7—Rb2ii | 95.6 (2) |
F6xiv—Y1—F4xi | 79.5 (2) | Rb1xxii—F7—Rb2ii | 127.2 (3) |
F3—Y1—F4xi | 65.7 (2) |
Symmetry codes: (i) x−y+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, x−y, z; (vi) x, y+1, z; (vii) −x+y+1, y+1, z; (viii) x, x−y, z; (ix) −x+y+1, −x+1, z; (x) −x, −y+1, z−1/2; (xi) y, −x+y+1, z−1/2; (xii) x−y, x+1, z−1/2; (xiii) x, x−y+1, z; (xiv) −y, x−y+1, z; (xv) −x+y, −x+1, z; (xvi) −x+y, y+1, z; (xvii) x−y, x, z−1/2; (xviii) −y+1, x−y+1, z; (xix) x−y+1, x, z+1/2; (xx) −y+1, x−y, z; (xxi) −x+y, −x, z; (xxii) x, y−1, z; (xxiii) −x+y−1, −x, z. |
F10RbSm3 | Mo Kα radiation, λ = 0.71073 Å |
Mr = 726.52 | Cell parameters from 3876 reflections |
Cubic, Fm3m | θ = 3.0–26.7° |
a = 11.8576 (14) Å | µ = 26.78 mm−1 |
V = 1667.2 (3) Å3 | T = 293 K |
Z = 8 | Block, yellow |
F(000) = 2504 | 0.18 × 0.15 × 0.15 mm |
Dx = 5.789 Mg m−3 |
Rigaku AFC8S diffractometer | 103 independent reflections |
Radiation source: fine-focus sealed tube | 103 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.060 |
Detector resolution: 14.6199 pixels mm-1 | θmax = 25.1°, θmin = 3.0° |
ω scans | h = −14→14 |
Absorption correction: multi-scan REQAB, CrystalClear | k = −14→12 |
Tmin = 0.681, Tmax = 1.000 | l = −14→14 |
3438 measured reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary 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 = 1.18 | Δρmax = 1.77 e Å−3 |
103 reflections | Δρmin = −1.06 e Å−3 |
13 parameters | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints |
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. |
x | y | z | Uiso*/Ueq | ||
Rb1 | −0.2500 | −0.2500 | −0.2500 | 0.0157 (12) | |
Sm1 | −0.24234 (12) | 0.0000 | 0.0000 | 0.0084 (9) | |
F1 | −0.1107 (6) | −0.1107 (6) | −0.1107 (6) | 0.016 (3) | |
F2 | 0.5000 | 0.1686 (9) | 0.1686 (9) | 0.042 (4) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Rb1 | 0.0157 (12) | 0.0157 (12) | 0.0157 (12) | 0.000 | 0.000 | 0.000 |
Sm1 | 0.0105 (10) | 0.0074 (9) | 0.0074 (9) | 0.000 | 0.000 | 0.000 |
F1 | 0.016 (3) | 0.016 (3) | 0.016 (3) | −0.001 (3) | −0.001 (3) | −0.001 (3) |
F2 | 0.043 (8) | 0.042 (5) | 0.042 (5) | 0.000 | 0.000 | 0.012 (7) |
Rb1—F1 | 2.861 (13) | Sm1—F2xiii | 2.261 (4) |
Rb1—F1i | 2.861 (13) | Sm1—F1xiv | 2.425 (4) |
Rb1—F1ii | 2.861 (13) | Sm1—F1 | 2.425 (4) |
Rb1—F1iii | 2.861 (13) | Sm1—F1xv | 2.425 (4) |
Rb1—F2iv | 3.264 (6) | Sm1—F1xvi | 2.425 (4) |
Rb1—F2v | 3.264 (6) | Sm1—Sm1xvii | 4.064 (2) |
Rb1—F2vi | 3.264 (6) | Sm1—Sm1xviii | 4.064 (2) |
Rb1—F2vii | 3.264 (6) | Sm1—Sm1xix | 4.064 (2) |
Rb1—F2viii | 3.264 (6) | Sm1—Sm1xx | 4.064 (2) |
Rb1—F2ix | 3.264 (6) | F1—Sm1xx | 2.425 (4) |
Rb1—F2x | 3.264 (6) | F1—Sm1xix | 2.425 (4) |
Rb1—F2xi | 3.264 (6) | F2—Sm1xxi | 2.261 (4) |
Sm1—F2ix | 2.261 (4) | F2—Sm1xxii | 2.261 (4) |
Sm1—F2x | 2.261 (4) | F2—Rb1xxiii | 3.264 (6) |
Sm1—F2xii | 2.261 (4) | F2—Rb1xxiv | 3.264 (6) |
F1—Rb1—F1i | 109.5 | F2ix—Sm1—F1xiv | 141.19 (18) |
F1—Rb1—F1ii | 109.5 | F2x—Sm1—F1xiv | 141.19 (18) |
F1i—Rb1—F1ii | 109.471 (1) | F2xii—Sm1—F1xiv | 79.8 (4) |
F1—Rb1—F1iii | 109.5 | F2xiii—Sm1—F1xiv | 79.8 (4) |
F1i—Rb1—F1iii | 109.5 | F2ix—Sm1—F1 | 79.8 (4) |
F1ii—Rb1—F1iii | 109.5 | F2x—Sm1—F1 | 79.8 (4) |
F1—Rb1—F2iv | 150.0 (2) | F2xii—Sm1—F1 | 141.19 (18) |
F1i—Rb1—F2iv | 58.37 (7) | F2xiii—Sm1—F1 | 141.19 (18) |
F1ii—Rb1—F2iv | 100.5 (2) | F1xiv—Sm1—F1 | 99.9 (6) |
F1iii—Rb1—F2iv | 58.37 (7) | F2ix—Sm1—F1xv | 141.19 (18) |
F1—Rb1—F2v | 150.0 (2) | F2x—Sm1—F1xv | 79.8 (4) |
F1i—Rb1—F2v | 100.5 (2) | F2xii—Sm1—F1xv | 79.8 (4) |
F1ii—Rb1—F2v | 58.37 (7) | F2xiii—Sm1—F1xv | 141.19 (18) |
F1iii—Rb1—F2v | 58.37 (7) | F1xiv—Sm1—F1xv | 65.5 (3) |
F2iv—Rb1—F2v | 51.3 (4) | F1—Sm1—F1xv | 65.5 (3) |
F1—Rb1—F2vi | 150.0 (2) | F2ix—Sm1—F1xvi | 79.8 (4) |
F1i—Rb1—F2vi | 58.37 (7) | F2x—Sm1—F1xvi | 141.19 (18) |
F1ii—Rb1—F2vi | 58.37 (7) | F2xii—Sm1—F1xvi | 141.19 (18) |
F1iii—Rb1—F2vi | 100.5 (2) | F2xiii—Sm1—F1xvi | 79.8 (4) |
F2iv—Rb1—F2vi | 51.3 (4) | F1xiv—Sm1—F1xvi | 65.5 (3) |
F2v—Rb1—F2vi | 51.3 (4) | F1—Sm1—F1xvi | 65.5 (3) |
F1—Rb1—F2vii | 58.37 (7) | F1xv—Sm1—F1xvi | 99.9 (6) |
F1i—Rb1—F2vii | 150.0 (2) | F2ix—Sm1—Sm1xvii | 162.9 (4) |
F1ii—Rb1—F2vii | 58.37 (7) | F2x—Sm1—Sm1xvii | 109.3 (2) |
F1iii—Rb1—F2vii | 100.5 (2) | F2xii—Sm1—Sm1xvii | 72.9 (4) |
F2iv—Rb1—F2vii | 145.6 (3) | F2xiii—Sm1—Sm1xvii | 109.3 (2) |
F2v—Rb1—F2vii | 95.02 (9) | F1xiv—Sm1—Sm1xvii | 33.10 (12) |
F2vi—Rb1—F2vii | 116.74 (14) | F1—Sm1—Sm1xvii | 85.9 (3) |
F1—Rb1—F2viii | 58.37 (7) | F1xv—Sm1—Sm1xvii | 33.10 (12) |
F1i—Rb1—F2viii | 58.37 (7) | F1xvi—Sm1—Sm1xvii | 85.9 (3) |
F1ii—Rb1—F2viii | 150.0 (2) | F2ix—Sm1—Sm1xviii | 109.3 (2) |
F1iii—Rb1—F2viii | 100.5 (2) | F2x—Sm1—Sm1xviii | 162.9 (4) |
F2iv—Rb1—F2viii | 95.02 (9) | F2xii—Sm1—Sm1xviii | 109.3 (2) |
F2v—Rb1—F2viii | 145.6 (3) | F2xiii—Sm1—Sm1xviii | 72.9 (4) |
F2vi—Rb1—F2viii | 116.74 (14) | F1xiv—Sm1—Sm1xviii | 33.10 (12) |
F2vii—Rb1—F2viii | 116.74 (14) | F1—Sm1—Sm1xviii | 85.9 (3) |
F1—Rb1—F2ix | 58.37 (7) | F1xv—Sm1—Sm1xviii | 85.9 (3) |
F1i—Rb1—F2ix | 100.5 (2) | F1xvi—Sm1—Sm1xviii | 33.10 (12) |
F1ii—Rb1—F2ix | 58.37 (7) | Sm1xvii—Sm1—Sm1xviii | 60.0 |
F1iii—Rb1—F2ix | 150.0 (2) | F2ix—Sm1—Sm1xix | 72.9 (4) |
F2iv—Rb1—F2ix | 145.6 (3) | F2x—Sm1—Sm1xix | 109.3 (2) |
F2v—Rb1—F2ix | 116.74 (14) | F2xii—Sm1—Sm1xix | 162.9 (4) |
F2vi—Rb1—F2ix | 95.02 (9) | F2xiii—Sm1—Sm1xix | 109.3 (2) |
F2vii—Rb1—F2ix | 49.5 (5) | F1xiv—Sm1—Sm1xix | 85.9 (3) |
F2viii—Rb1—F2ix | 95.02 (9) | F1—Sm1—Sm1xix | 33.10 (12) |
F1—Rb1—F2x | 58.37 (7) | F1xv—Sm1—Sm1xix | 85.9 (3) |
F1i—Rb1—F2x | 58.37 (7) | F1xvi—Sm1—Sm1xix | 33.10 (12) |
F1ii—Rb1—F2x | 100.5 (2) | Sm1xvii—Sm1—Sm1xix | 90.0 |
F1iii—Rb1—F2x | 150.0 (2) | Sm1xviii—Sm1—Sm1xix | 60.0 |
F2iv—Rb1—F2x | 116.74 (14) | F2ix—Sm1—Sm1xx | 109.3 (2) |
F2v—Rb1—F2x | 145.6 (3) | F2x—Sm1—Sm1xx | 72.9 (4) |
F2vi—Rb1—F2x | 95.02 (9) | F2xii—Sm1—Sm1xx | 109.3 (2) |
F2vii—Rb1—F2x | 95.02 (9) | F2xiii—Sm1—Sm1xx | 162.9 (4) |
F2viii—Rb1—F2x | 49.5 (5) | F1xiv—Sm1—Sm1xx | 85.9 (3) |
F2ix—Rb1—F2x | 51.3 (4) | F1—Sm1—Sm1xx | 33.10 (12) |
F1—Rb1—F2xi | 58.37 (7) | F1xv—Sm1—Sm1xx | 33.10 (12) |
F1i—Rb1—F2xi | 150.0 (2) | F1xvi—Sm1—Sm1xx | 85.9 (3) |
F1ii—Rb1—F2xi | 100.5 (2) | Sm1xvii—Sm1—Sm1xx | 60.0 |
F1iii—Rb1—F2xi | 58.37 (7) | Sm1xviii—Sm1—Sm1xx | 90.0 |
F2iv—Rb1—F2xi | 116.74 (14) | Sm1xix—Sm1—Sm1xx | 60.0 |
F2v—Rb1—F2xi | 95.02 (9) | Sm1xx—F1—Sm1xix | 113.8 (2) |
F2vi—Rb1—F2xi | 145.6 (3) | Sm1xx—F1—Sm1 | 113.8 (2) |
F2vii—Rb1—F2xi | 51.3 (4) | Sm1xix—F1—Sm1 | 113.8 (2) |
F2viii—Rb1—F2xi | 95.02 (9) | Sm1xx—F1—Rb1 | 104.7 (3) |
F2ix—Rb1—F2xi | 95.02 (9) | Sm1xix—F1—Rb1 | 104.7 (3) |
F2x—Rb1—F2xi | 116.74 (14) | Sm1—F1—Rb1 | 104.7 (3) |
F2ix—Sm1—F2x | 77.4 (3) | Sm1xxi—F2—Sm1xxii | 145.7 (7) |
F2ix—Sm1—F2xii | 124.3 (7) | Sm1xxi—F2—Rb1xxiii | 97.08 (8) |
F2x—Sm1—F2xii | 77.4 (3) | Sm1xxii—F2—Rb1xxiii | 97.08 (8) |
F2ix—Sm1—F2xiii | 77.4 (3) | Sm1xxi—F2—Rb1xxiv | 97.08 (8) |
F2x—Sm1—F2xiii | 124.3 (7) | Sm1xxii—F2—Rb1xxiv | 97.08 (8) |
F2xii—Sm1—F2xiii | 77.4 (3) | Rb1xxiii—F2—Rb1xxiv | 130.5 (5) |
Symmetry codes: (i) −x−1/2, y, −z−1/2; (ii) −x−1/2, −y−1/2, z; (iii) x, −y−1/2, −z−1/2; (iv) y−1/2, z−1/2, x−1; (v) z−1/2, x−1, y−1/2; (vi) x−1, y−1/2, z−1/2; (vii) −y, z−1/2, −x+1/2; (viii) −z, x−1/2, y−1/2; (ix) y−1/2, −z, x−1/2; (x) z−1/2, −x+1/2, −y; (xi) x−1/2, y−1/2, −z; (xii) y−1/2, z, x−1/2; (xiii) z−1/2, x−1/2, 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. |
F10Gd3Rb | Dx = 6.017 Mg m−3 |
Mr = 747.22 | Mo Kα radiation, λ = 0.71073 Å |
Hexagonal, P63mc | Cell parameters from 5211 reflections |
a = 8.3540 (12) Å | θ = 2.8–25.4° |
c = 13.649 (3) Å | µ = 29.83 mm−1 |
V = 824.9 (2) Å3 | T = 293 K |
Z = 4 | Block, colorless |
F(000) = 1276 | 0.25 × 0.23 × 0.20 mm |
Rigaku AFC8S diffractometer | 613 independent reflections |
Radiation source: fine-focus sealed tube | 611 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.075 |
Detector resolution: 14.6199 pixels mm-1 | θmax = 25.4°, θmin = 2.8° |
ω scans | h = −10→10 |
Absorption correction: multi-scan REQAB,RIGAKU/MSC,The Woodlands,TX,USA,1999. | k = −9→9 |
Tmin = 0.456, Tmax = 1.000 | l = −16→16 |
6420 measured reflections |
Refinement on F2 | Secondary 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) = 0.083 | Δρmax = 2.30 e Å−3 |
S = 1.18 | Δρmin = −1.44 e Å−3 |
613 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
59 parameters | Extinction coefficient: 0.0112 (5) |
25 restraints | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.11 (9) |
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. |
x | y | z | Uiso*/Ueq | ||
Gd1 | 0.50576 (7) | −0.50576 (7) | −0.01044 (7) | 0.0052 (3) | |
Gd2 | 0.17390 (7) | −0.17390 (7) | 0.24930 (7) | 0.0051 (4) | |
Rb2 | 0.0000 | 0.0000 | −0.0069 (10) | 0.0198 (10) | |
Rb1 | 0.3333 | −0.3333 | 0.7436 (8) | 0.0161 (12) | |
F5 | 0.3339 (14) | 0.3357 (14) | 0.1141 (15) | 0.0166 (19) | |
F6 | 0.2209 (11) | −0.2209 (11) | 0.9523 (11) | 0.016 (3) | |
F4 | 0.1836 (10) | −0.1836 (10) | 0.4266 (11) | 0.013 (3) | |
F7 | 0.1090 (10) | −0.1090 (10) | 0.7827 (11) | 0.015 (3) | |
F2 | 0.3333 | −0.3333 | 0.2082 (17) | 0.0044 (13) | |
F1 | 0.3333 | −0.3333 | 0.540 (2) | 0.021 (6) | |
F3 | 0.4794 (9) | −0.4794 (9) | 0.3168 (10) | 0.006 (3) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Gd1 | 0.0060 (4) | 0.0060 (4) | 0.0044 (5) | 0.0035 (4) | 0.0008 (4) | −0.0008 (4) |
Gd2 | 0.0056 (4) | 0.0056 (4) | 0.0044 (6) | 0.0030 (4) | 0.0007 (5) | −0.0007 (5) |
Rb2 | 0.0168 (11) | 0.0168 (11) | 0.026 (3) | 0.0084 (5) | 0.000 | 0.000 |
Rb1 | 0.0162 (12) | 0.0162 (12) | 0.016 (3) | 0.0081 (6) | 0.000 | 0.000 |
F5 | 0.027 (5) | 0.022 (5) | 0.007 (4) | 0.017 (4) | 0.008 (4) | 0.007 (4) |
F6 | 0.009 (4) | 0.009 (4) | 0.022 (6) | −0.003 (5) | −0.002 (3) | 0.002 (3) |
F4 | 0.011 (4) | 0.011 (4) | 0.018 (5) | 0.006 (4) | −0.004 (2) | 0.004 (2) |
F7 | 0.011 (3) | 0.011 (3) | 0.023 (5) | 0.007 (4) | 0.000 (2) | 0.000 (2) |
F2 | 0.0043 (12) | 0.0043 (12) | 0.0047 (17) | 0.0021 (6) | 0.000 | 0.000 |
F1 | 0.015 (8) | 0.015 (8) | 0.032 (14) | 0.007 (4) | 0.000 | 0.000 |
F3 | 0.004 (4) | 0.004 (4) | 0.003 (5) | −0.002 (5) | −0.001 (3) | 0.001 (3) |
Gd1—F5i | 2.192 (17) | Rb2—F5xii | 3.248 (19) |
Gd1—F5ii | 2.192 (17) | Rb1—F1 | 2.77 (3) |
Gd1—F6iii | 2.252 (4) | Rb1—F3xvi | 2.888 (15) |
Gd1—F6iv | 2.252 (4) | Rb1—F3xvii | 2.888 (15) |
Gd1—F3v | 2.368 (13) | Rb1—F3xxv | 2.888 (15) |
Gd1—F4vi | 2.410 (8) | Rb1—F6 | 3.28 (2) |
Gd1—F4vii | 2.410 (8) | Rb1—F6xv | 3.28 (2) |
Gd1—F1v | 2.430 (8) | Rb1—F6xiv | 3.28 (2) |
Gd1—Gd2vi | 4.0155 (13) | Rb1—F7 | 3.289 (14) |
Gd1—Gd2vii | 4.0155 (13) | Rb1—F7xv | 3.289 (14) |
Gd1—Gd1viii | 4.0327 (18) | Rb1—F7xiv | 3.289 (14) |
Gd1—Gd1ix | 4.0327 (18) | Rb1—F5xxvi | 3.302 (18) |
Gd2—F7x | 2.249 (4) | Rb1—F5xxvii | 3.302 (19) |
Gd2—F7xi | 2.249 (4) | F5—Gd1xxviii | 2.192 (17) |
Gd2—F5xii | 2.310 (18) | F5—Gd2xxiv | 2.310 (18) |
Gd2—F5xiii | 2.310 (18) | F5—Rb1xxix | 3.302 (18) |
Gd2—F2 | 2.374 (5) | F6—Gd1xxx | 2.252 (4) |
Gd2—F3xiv | 2.400 (7) | F6—Gd1xxxi | 2.252 (4) |
Gd2—F3xv | 2.400 (7) | F6—Rb2xxxii | 3.244 (16) |
Gd2—F4 | 2.424 (16) | F4—Gd1xvi | 2.410 (8) |
Gd2—Gd2xv | 3.9957 (18) | F4—Gd1xvii | 2.410 (8) |
Gd2—Gd2xiv | 3.9957 (18) | F4—Rb2xxxiii | 2.807 (16) |
Gd2—Gd1xvi | 4.0155 (13) | F7—Gd2xxxiv | 2.249 (4) |
Gd2—Gd1xvii | 4.0155 (13) | F7—Gd2xxxv | 2.249 (4) |
Rb2—F4xi | 2.807 (16) | F7—Rb2xxxii | 3.28 (2) |
Rb2—F4x | 2.807 (16) | F2—Gd2xv | 2.374 (5) |
Rb2—F4xviii | 2.807 (16) | F2—Gd2xiv | 2.374 (5) |
Rb2—F6xix | 3.244 (16) | F1—Gd1xvii | 2.430 (8) |
Rb2—F6xx | 3.244 (16) | F1—Gd1xvi | 2.430 (8) |
Rb2—F6xxi | 3.244 (16) | F1—Gd1xxv | 2.430 (8) |
Rb2—F5 | 3.248 (19) | F3—Gd1xxv | 2.368 (13) |
Rb2—F5xxii | 3.248 (19) | F3—Gd2xiv | 2.400 (7) |
Rb2—F5xiii | 3.248 (19) | F3—Gd2xv | 2.400 (7) |
Rb2—F5xxiii | 3.248 (19) | F3—Rb1v | 2.888 (15) |
Rb2—F5xxiv | 3.248 (19) | ||
F5i—Gd1—F5ii | 78.0 (8) | F6xxi—Rb2—F5 | 95.2 (3) |
F5i—Gd1—F6iii | 122.4 (5) | F4xi—Rb2—F5xxii | 150.7 (4) |
F5ii—Gd1—F6iii | 75.4 (5) | F4x—Rb2—F5xxii | 99.2 (3) |
F5i—Gd1—F6iv | 75.4 (5) | F4xviii—Rb2—F5xxii | 57.4 (4) |
F5ii—Gd1—F6iv | 122.4 (5) | F6xix—Rb2—F5xxii | 95.2 (3) |
F6iii—Gd1—F6iv | 77.5 (8) | F6xx—Rb2—F5xxii | 49.5 (3) |
F5i—Gd1—F3v | 140.9 (4) | F6xxi—Rb2—F5xxii | 145.1 (5) |
F5ii—Gd1—F3v | 140.9 (4) | F5—Rb2—F5xxii | 50.6 (4) |
F6iii—Gd1—F3v | 81.0 (5) | F4xi—Rb2—F5xiii | 99.2 (3) |
F6iv—Gd1—F3v | 81.0 (5) | F4x—Rb2—F5xiii | 57.4 (4) |
F5i—Gd1—F4vi | 142.1 (5) | F4xviii—Rb2—F5xiii | 150.7 (4) |
F5ii—Gd1—F4vi | 79.0 (5) | F6xix—Rb2—F5xiii | 145.1 (5) |
F6iii—Gd1—F4vi | 79.5 (5) | F6xx—Rb2—F5xiii | 95.2 (3) |
F6iv—Gd1—F4vi | 142.4 (5) | F6xxi—Rb2—F5xiii | 49.5 (3) |
F3v—Gd1—F4vi | 66.3 (4) | F5—Rb2—F5xiii | 51.4 (5) |
F5i—Gd1—F4vii | 79.0 (5) | F5xxii—Rb2—F5xiii | 96.4 (6) |
F5ii—Gd1—F4vii | 142.1 (5) | F4xi—Rb2—F5xxiii | 57.4 (4) |
F6iii—Gd1—F4vii | 142.4 (5) | F4x—Rb2—F5xxiii | 150.7 (4) |
F6iv—Gd1—F4vii | 79.5 (5) | F4xviii—Rb2—F5xxiii | 99.2 (3) |
F3v—Gd1—F4vii | 66.3 (4) | F6xix—Rb2—F5xxiii | 49.5 (3) |
F4vi—Gd1—F4vii | 102.3 (7) | F6xx—Rb2—F5xxiii | 145.1 (5) |
F5i—Gd1—F1v | 79.7 (6) | F6xxi—Rb2—F5xxiii | 95.2 (3) |
F5ii—Gd1—F1v | 79.7 (6) | F5—Rb2—F5xxiii | 118.9 (9) |
F6iii—Gd1—F1v | 141.3 (4) | F5xxii—Rb2—F5xxiii | 96.4 (6) |
F6iv—Gd1—F1v | 141.3 (4) | F5xiii—Rb2—F5xxiii | 96.4 (6) |
F3v—Gd1—F1v | 101.4 (7) | F4xi—Rb2—F5xxiv | 99.2 (3) |
F4vi—Gd1—F1v | 66.9 (4) | F4x—Rb2—F5xxiv | 150.7 (4) |
F4vii—Gd1—F1v | 66.9 (4) | F4xviii—Rb2—F5xxiv | 57.4 (4) |
F5i—Gd1—Gd2vi | 163.6 (3) | F6xix—Rb2—F5xxiv | 49.5 (3) |
F5ii—Gd1—Gd2vi | 109.4 (4) | F6xx—Rb2—F5xxiv | 95.2 (3) |
F6iii—Gd1—Gd2vi | 73.9 (4) | F6xxi—Rb2—F5xxiv | 145.1 (5) |
F6iv—Gd1—Gd2vi | 110.2 (4) | F5—Rb2—F5xxiv | 96.4 (6) |
F3v—Gd1—Gd2vi | 32.89 (13) | F5xxii—Rb2—F5xxiv | 51.4 (5) |
F4vi—Gd1—Gd2vi | 34.0 (4) | F5xiii—Rb2—F5xxiv | 118.9 (9) |
F4vii—Gd1—Gd2vi | 86.9 (4) | F5xxiii—Rb2—F5xxiv | 50.6 (4) |
F1v—Gd1—Gd2vi | 87.3 (6) | F4xi—Rb2—F5xii | 57.4 (4) |
F5i—Gd1—Gd2vii | 109.4 (4) | F4x—Rb2—F5xii | 99.2 (3) |
F5ii—Gd1—Gd2vii | 163.6 (3) | F4xviii—Rb2—F5xii | 150.7 (4) |
F6iii—Gd1—Gd2vii | 110.2 (4) | F6xix—Rb2—F5xii | 95.2 (3) |
F6iv—Gd1—Gd2vii | 73.9 (4) | F6xx—Rb2—F5xii | 145.1 (5) |
F3v—Gd1—Gd2vii | 32.89 (13) | F6xxi—Rb2—F5xii | 49.5 (3) |
F4vi—Gd1—Gd2vii | 86.9 (4) | F5—Rb2—F5xii | 96.4 (6) |
F4vii—Gd1—Gd2vii | 34.0 (4) | F5xxii—Rb2—F5xii | 118.9 (9) |
F1v—Gd1—Gd2vii | 87.3 (6) | F5xiii—Rb2—F5xii | 50.6 (4) |
Gd2vi—Gd1—Gd2vii | 59.67 (3) | F5xxiii—Rb2—F5xii | 51.4 (5) |
F5i—Gd1—Gd1viii | 73.9 (3) | F5xxiv—Rb2—F5xii | 96.4 (6) |
F5ii—Gd1—Gd1viii | 110.7 (3) | F1—Rb1—F3xvi | 110.2 (4) |
F6iii—Gd1—Gd1viii | 163.6 (4) | F1—Rb1—F3xvii | 110.2 (4) |
F6iv—Gd1—Gd1viii | 109.5 (4) | F3xvi—Rb1—F3xvii | 108.7 (4) |
F3v—Gd1—Gd1viii | 85.5 (3) | F1—Rb1—F3xxv | 110.2 (4) |
F4vi—Gd1—Gd1viii | 86.7 (3) | F3xvi—Rb1—F3xxv | 108.7 (4) |
F4vii—Gd1—Gd1viii | 33.2 (3) | F3xvii—Rb1—F3xxv | 108.7 (4) |
F1v—Gd1—Gd1viii | 33.9 (3) | F1—Rb1—F6 | 150.3 (3) |
Gd2vi—Gd1—Gd1viii | 89.736 (18) | F3xvi—Rb1—F6 | 57.8 (3) |
Gd2vii—Gd1—Gd1viii | 59.858 (16) | F3xvii—Rb1—F6 | 57.8 (3) |
F5i—Gd1—Gd1ix | 110.7 (3) | F3xxv—Rb1—F6 | 99.5 (6) |
F5ii—Gd1—Gd1ix | 73.9 (3) | F1—Rb1—F6xv | 150.3 (3) |
F6iii—Gd1—Gd1ix | 109.5 (4) | F3xvi—Rb1—F6xv | 57.8 (3) |
F6iv—Gd1—Gd1ix | 163.6 (4) | F3xvii—Rb1—F6xv | 99.5 (6) |
F3v—Gd1—Gd1ix | 85.5 (3) | F3xxv—Rb1—F6xv | 57.8 (3) |
F4vi—Gd1—Gd1ix | 33.2 (3) | F6—Rb1—F6xv | 50.9 (5) |
F4vii—Gd1—Gd1ix | 86.7 (3) | F1—Rb1—F6xiv | 150.3 (3) |
F1v—Gd1—Gd1ix | 33.9 (3) | F3xvi—Rb1—F6xiv | 99.5 (6) |
Gd2vi—Gd1—Gd1ix | 59.858 (16) | F3xvii—Rb1—F6xiv | 57.8 (3) |
Gd2vii—Gd1—Gd1ix | 89.736 (18) | F3xxv—Rb1—F6xiv | 57.8 (3) |
Gd1viii—Gd1—Gd1ix | 60.0 | F6—Rb1—F6xiv | 50.9 (5) |
F7x—Gd2—F7xi | 74.8 (7) | F6xv—Rb1—F6xiv | 50.9 (5) |
F7x—Gd2—F5xii | 119.8 (5) | F1—Rb1—F7 | 99.3 (4) |
F7xi—Gd2—F5xii | 76.6 (5) | F3xvi—Rb1—F7 | 58.73 (12) |
F7x—Gd2—F5xiii | 76.6 (5) | F3xvii—Rb1—F7 | 58.73 (12) |
F7xi—Gd2—F5xiii | 119.8 (5) | F3xxv—Rb1—F7 | 150.4 (7) |
F5xii—Gd2—F5xiii | 73.8 (8) | F6—Rb1—F7 | 50.9 (4) |
F7x—Gd2—F2 | 142.6 (4) | F6xv—Rb1—F7 | 96.0 (5) |
F7xi—Gd2—F2 | 142.6 (3) | F6xiv—Rb1—F7 | 96.0 (5) |
F5xii—Gd2—F2 | 81.3 (5) | F1—Rb1—F7xv | 99.3 (4) |
F5xiii—Gd2—F2 | 81.3 (5) | F3xvi—Rb1—F7xv | 58.73 (12) |
F7x—Gd2—F3xiv | 81.9 (4) | F3xvii—Rb1—F7xv | 150.4 (7) |
F7xi—Gd2—F3xiv | 141.8 (5) | F3xxv—Rb1—F7xv | 58.73 (12) |
F5xii—Gd2—F3xiv | 141.6 (4) | F6—Rb1—F7xv | 96.0 (5) |
F5xiii—Gd2—F3xiv | 82.4 (5) | F6xv—Rb1—F7xv | 50.9 (4) |
F2—Gd2—F3xiv | 65.5 (4) | F6xiv—Rb1—F7xv | 96.0 (5) |
F7x—Gd2—F3xv | 141.8 (5) | F7—Rb1—F7xv | 117.4 (2) |
F7xi—Gd2—F3xv | 81.9 (4) | F1—Rb1—F7xiv | 99.3 (4) |
F5xii—Gd2—F3xv | 82.4 (5) | F3xvi—Rb1—F7xiv | 150.4 (7) |
F5xiii—Gd2—F3xv | 141.6 (4) | F3xvii—Rb1—F7xiv | 58.73 (12) |
F2—Gd2—F3xv | 65.5 (4) | F3xxv—Rb1—F7xiv | 58.73 (12) |
F3xiv—Gd2—F3xv | 99.4 (6) | F6—Rb1—F7xiv | 96.0 (5) |
F7x—Gd2—F4 | 80.9 (5) | F6xv—Rb1—F7xiv | 96.0 (5) |
F7xi—Gd2—F4 | 80.9 (5) | F6xiv—Rb1—F7xiv | 50.9 (4) |
F5xii—Gd2—F4 | 143.1 (4) | F7—Rb1—F7xiv | 117.4 (2) |
F5xiii—Gd2—F4 | 143.1 (4) | F7xv—Rb1—F7xiv | 117.4 (2) |
F2—Gd2—F4 | 100.4 (6) | F1—Rb1—F5xxvi | 57.6 (4) |
F3xiv—Gd2—F4 | 65.6 (3) | F3xvi—Rb1—F5xxvi | 100.9 (2) |
F3xv—Gd2—F4 | 65.6 (3) | F3xvii—Rb1—F5xxvi | 59.7 (4) |
F7x—Gd2—Gd2xv | 111.2 (3) | F3xxv—Rb1—F5xxvi | 150.4 (3) |
F7xi—Gd2—Gd2xv | 165.7 (3) | F6—Rb1—F5xxvi | 95.9 (4) |
F5xii—Gd2—Gd2xv | 109.5 (3) | F6xv—Rb1—F5xxvi | 146.0 (5) |
F5xiii—Gd2—Gd2xv | 74.5 (3) | F6xiv—Rb1—F5xxvi | 117.5 (4) |
F2—Gd2—Gd2xv | 32.7 (2) | F7—Rb1—F5xxvi | 50.8 (3) |
F3xiv—Gd2—Gd2xv | 33.7 (3) | F7xv—Rb1—F5xxvi | 144.2 (5) |
F3xv—Gd2—Gd2xv | 86.0 (3) | F7xiv—Rb1—F5xxvi | 94.7 (2) |
F4—Gd2—Gd2xv | 87.1 (3) | F1—Rb1—F5xxvii | 57.6 (4) |
F7x—Gd2—Gd2xiv | 165.7 (3) | F3xvi—Rb1—F5xxvii | 150.4 (3) |
F7xi—Gd2—Gd2xiv | 111.2 (3) | F3xvii—Rb1—F5xxvii | 59.7 (4) |
F5xii—Gd2—Gd2xiv | 74.5 (3) | F3xxv—Rb1—F5xxvii | 100.9 (2) |
F5xiii—Gd2—Gd2xiv | 109.5 (3) | F6—Rb1—F5xxvii | 117.5 (4) |
F2—Gd2—Gd2xiv | 32.7 (2) | F6xv—Rb1—F5xxvii | 146.0 (5) |
F3xiv—Gd2—Gd2xiv | 86.0 (3) | F6xiv—Rb1—F5xxvii | 95.9 (4) |
F3xv—Gd2—Gd2xiv | 33.7 (3) | F7—Rb1—F5xxvii | 94.7 (2) |
F4—Gd2—Gd2xiv | 87.1 (3) | F7xv—Rb1—F5xxvii | 144.2 (5) |
Gd2xv—Gd2—Gd2xiv | 60.0 | F7xiv—Rb1—F5xxvii | 50.8 (3) |
F7x—Gd2—Gd1xvi | 75.4 (3) | F5xxvi—Rb1—F5xxvii | 49.4 (4) |
F7xi—Gd2—Gd1xvi | 111.0 (4) | Gd1xxviii—F5—Gd2xxiv | 144.2 (5) |
F5xii—Gd2—Gd1xvi | 164.7 (3) | Gd1xxviii—F5—Rb2 | 98.5 (8) |
F5xiii—Gd2—Gd1xvi | 111.2 (4) | Gd2xxiv—F5—Rb2 | 100.3 (4) |
F2—Gd2—Gd1xvi | 85.2 (5) | Gd1xxviii—F5—Rb1xxix | 96.9 (4) |
F3xiv—Gd2—Gd1xvi | 32.4 (3) | Gd2xxiv—F5—Rb1xxix | 94.6 (7) |
F3xv—Gd2—Gd1xvi | 85.5 (3) | Rb2—F5—Rb1xxix | 129.0 (3) |
F4—Gd2—Gd1xvi | 33.73 (14) | Gd1xxx—F6—Gd1xxxi | 147.3 (7) |
Gd2xv—Gd2—Gd1xvi | 60.163 (15) | Gd1xxx—F6—Rb2xxxii | 97.3 (4) |
Gd2xiv—Gd2—Gd1xvi | 90.264 (18) | Gd1xxxi—F6—Rb2xxxii | 97.3 (4) |
F7x—Gd2—Gd1xvii | 111.0 (4) | Gd1xxx—F6—Rb1 | 96.5 (4) |
F7xi—Gd2—Gd1xvii | 75.4 (4) | Gd1xxxi—F6—Rb1 | 96.5 (4) |
F5xii—Gd2—Gd1xvii | 111.2 (4) | Rb2xxxii—F6—Rb1 | 129.6 (7) |
F5xiii—Gd2—Gd1xvii | 164.7 (3) | Gd1xvi—F4—Gd1xvii | 113.6 (6) |
F2—Gd2—Gd1xvii | 85.2 (5) | Gd1xvi—F4—Gd2 | 112.3 (4) |
F3xiv—Gd2—Gd1xvii | 85.5 (3) | Gd1xvii—F4—Gd2 | 112.3 (4) |
F3xv—Gd2—Gd1xvii | 32.4 (3) | Gd1xvi—F4—Rb2xxxiii | 106.2 (4) |
F4—Gd2—Gd1xvii | 33.73 (14) | Gd1xvii—F4—Rb2xxxiii | 106.2 (4) |
Gd2xv—Gd2—Gd1xvii | 90.264 (18) | Gd2—F4—Rb2xxxiii | 105.6 (6) |
Gd2xiv—Gd2—Gd1xvii | 60.163 (15) | Gd2xxxiv—F7—Gd2xxxv | 151.3 (7) |
Gd1xvi—Gd2—Gd1xvii | 60.28 (3) | Gd2xxxiv—F7—Rb2xxxii | 96.3 (4) |
F4xi—Rb2—F4x | 110.1 (4) | Gd2xxxv—F7—Rb2xxxii | 96.3 (4) |
F4xi—Rb2—F4xviii | 110.1 (4) | Gd2xxxiv—F7—Rb1 | 96.2 (4) |
F4x—Rb2—F4xviii | 110.1 (4) | Gd2xxxv—F7—Rb1 | 96.2 (4) |
F4xi—Rb2—F6xix | 58.56 (12) | Rb2xxxii—F7—Rb1 | 128.1 (6) |
F4x—Rb2—F6xix | 151.3 (8) | Gd2—F2—Gd2xv | 114.6 (4) |
F4xviii—Rb2—F6xix | 58.56 (12) | Gd2—F2—Gd2xiv | 114.6 (4) |
F4xi—Rb2—F6xx | 151.3 (8) | Gd2xv—F2—Gd2xiv | 114.6 (4) |
F4x—Rb2—F6xx | 58.56 (12) | Gd1xvii—F1—Gd1xvi | 112.2 (6) |
F4xviii—Rb2—F6xx | 58.56 (12) | Gd1xvii—F1—Gd1xxv | 112.2 (6) |
F6xix—Rb2—F6xx | 117.1 (3) | Gd1xvi—F1—Gd1xxv | 112.2 (6) |
F4xi—Rb2—F6xxi | 58.56 (12) | Gd1xvii—F1—Rb1 | 106.6 (6) |
F4x—Rb2—F6xxi | 58.56 (12) | Gd1xvi—F1—Rb1 | 106.6 (6) |
F4xviii—Rb2—F6xxi | 151.3 (8) | Gd1xxv—F1—Rb1 | 106.6 (6) |
F6xix—Rb2—F6xxi | 117.1 (3) | Gd1xxv—F3—Gd2xiv | 114.7 (3) |
F6xx—Rb2—F6xxi | 117.1 (3) | Gd1xxv—F3—Gd2xv | 114.7 (3) |
F4xi—Rb2—F5 | 150.7 (4) | Gd2xiv—F3—Gd2xv | 112.7 (5) |
F4x—Rb2—F5 | 57.4 (4) | Gd1xxv—F3—Rb1v | 105.0 (5) |
F4xviii—Rb2—F5 | 99.2 (3) | Gd2xiv—F3—Rb1v | 104.0 (4) |
F6xix—Rb2—F5 | 145.1 (5) | Gd2xv—F3—Rb1v | 104.0 (4) |
F6xx—Rb2—F5 | 49.5 (3) |
Symmetry codes: (i) −y+1, −x, z; (ii) x, y−1, z; (iii) −y, x−y−1, z−1; (iv) −x+y+1, −x, z−1; (v) −x+1, −y−1, z−1/2; (vi) x−y, x−1, z−1/2; (vii) y+1, −x+y, z−1/2; (viii) −x+y+2, −x, z; (ix) −y, x−y−2, z; (x) x−y, x, z−1/2; (xi) y, −x+y, z−1/2; (xii) −x+y, −x, z; (xiii) x, x−y, z; (xiv) −y, x−y−1, z; (xv) −x+y+1, −x, z; (xvi) y+1, −x+y+1, z+1/2; (xvii) x−y−1, x−1, z+1/2; (xviii) −x, −y, z−1/2; (xix) −x+y, −x, z−1; (xx) −y, x−y, z−1; (xxi) x, y, z−1; (xxii) −x+y, y, z; (xxiii) −y, −x, z; (xxiv) −y, x−y, z; (xxv) −x+1, −y−1, z+1/2; (xxvi) x−y, −y, z+1/2; (xxvii) x−y, x−1, z+1/2; (xxviii) x, y+1, z; (xxix) −x+1, −y, z−1/2; (xxx) −y, x−y−1, 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) x−y, x, z+1/2. |
F10KLu3 | Dx = 6.798 Mg m−3 |
Mr = 754.01 | Mo Kα radiation, λ = 0.71073 Å |
Hexagonal, P63mc | Cell parameters from 3712 reflections |
a = 8.0420 (11) Å | θ = 2.9–25.9° |
c = 13.154 (3) Å | µ = 40.59 mm−1 |
V = 736.8 (2) Å3 | T = 293 K |
Z = 4 | Block, colorless |
F(000) = 1288 | 0.26 × 0.21 × 0.20 mm |
Rigaku AFC8S diffractometer | 547 independent reflections |
Radiation source: fine-focus sealed tube | 542 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.086 |
Detector resolution: 14.6199 pixels mm-1 | θmax = 25.2°, θmin = 2.9° |
ω scans | h = −9→9 |
Absorption correction: multi-scan REQAB,RIGAKU/MSC,The Woodlands,TX,USA,1999. | k = −9→8 |
Tmin = 0.308, Tmax = 1.000 | l = −15→15 |
5397 measured reflections |
Refinement on F2 | Secondary 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) = 0.076 | Δρmax = 2.74 e Å−3 |
S = 1.19 | Δρmin = −1.92 e Å−3 |
547 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
59 parameters | Extinction coefficient: 0.0025 (2) |
25 restraints | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.02 (6) |
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. |
x | y | z | Uiso*/Ueq | ||
K1 | 0.6667 | 0.3333 | 0.0482 (16) | 0.0097 (18) | |
K2 | 1.0000 | 0.0000 | 0.3016 (18) | 0.0132 (15) | |
Lu1 | 0.98918 (12) | 0.49459 (6) | 0.30267 (5) | 0.0067 (3) | |
Lu2 | 0.65254 (9) | 0.82627 (5) | 0.04309 (7) | 0.0059 (3) | |
F1 | 0.6667 | 0.3333 | 0.2564 (15) | 0.011 (3) | |
F2 | 0.3333 | 0.6667 | 0.0886 (13) | 0.002 (3) | |
F3 | 0.9664 (15) | 0.4832 (7) | 0.4769 (10) | 0.007 (3) | |
F4 | 0.6323 (15) | 0.8161 (8) | −0.1329 (10) | 0.012 (3) | |
F5 | 0.6626 (11) | 0.9970 (11) | 0.1693 (16) | 0.0178 (14) | |
F6 | 1.2229 (8) | 0.7771 (8) | 0.3416 (8) | 0.014 (2) | |
F7 | 0.8881 (9) | 1.1119 (9) | 0.0106 (8) | 0.016 (2) |
U11 | U22 | U33 | U12 | U13 | U23 | |
K1 | 0.013 (2) | 0.013 (2) | 0.004 (4) | 0.0063 (11) | 0.000 | 0.000 |
K2 | 0.014 (2) | 0.014 (2) | 0.011 (4) | 0.0070 (10) | 0.000 | 0.000 |
Lu1 | 0.0087 (4) | 0.0085 (4) | 0.0030 (5) | 0.0043 (2) | −0.0005 (5) | −0.0002 (2) |
Lu2 | 0.0075 (4) | 0.0071 (4) | 0.0034 (4) | 0.0037 (2) | 0.0004 (6) | 0.0002 (3) |
F1 | 0.013 (4) | 0.013 (4) | 0.009 (5) | 0.0065 (19) | 0.000 | 0.000 |
F2 | 0.003 (3) | 0.003 (3) | 0.002 (5) | 0.0013 (17) | 0.000 | 0.000 |
F3 | 0.009 (5) | 0.005 (4) | 0.009 (6) | 0.004 (3) | 0.006 (4) | 0.003 (2) |
F4 | 0.011 (5) | 0.017 (5) | 0.006 (6) | 0.005 (2) | −0.002 (4) | −0.0008 (19) |
F5 | 0.021 (3) | 0.019 (3) | 0.007 (3) | 0.004 (3) | 0.004 (2) | −0.002 (3) |
F6 | 0.016 (4) | 0.016 (4) | 0.008 (5) | 0.007 (5) | 0.000 (2) | 0.000 (2) |
F7 | 0.016 (4) | 0.016 (4) | 0.011 (5) | 0.004 (5) | 0.002 (2) | −0.002 (2) |
K1—F3i | 2.722 (14) | Lu1—Lu1xii | 3.8905 (16) |
K1—F3ii | 2.722 (14) | Lu1—Lu1xv | 3.8905 (16) |
K1—F3iii | 2.722 (14) | Lu2—F5 | 2.130 (17) |
K1—F1 | 2.74 (3) | Lu2—F5xvi | 2.130 (17) |
K1—F6ii | 3.12 (2) | Lu2—F7vi | 2.167 (3) |
K1—F6i | 3.12 (2) | Lu2—F7 | 2.167 (3) |
K1—F6iii | 3.12 (2) | Lu2—F2 | 2.302 (4) |
K1—F7iv | 3.124 (13) | Lu2—F4 | 2.320 (13) |
K1—F7v | 3.124 (13) | Lu2—F3xvii | 2.327 (6) |
K1—F7vi | 3.124 (13) | Lu2—F3iii | 2.327 (6) |
K1—F5vii | 3.125 (18) | Lu2—Lu2v | 3.8505 (12) |
K1—F5vi | 3.125 (18) | Lu2—Lu2xviii | 3.8505 (12) |
K2—F4viii | 2.702 (14) | Lu2—Lu1xvii | 3.8725 (12) |
K2—F4ix | 2.702 (14) | Lu2—Lu1iii | 3.8725 (12) |
K2—F4x | 2.702 (14) | F1—Lu1xii | 2.327 (5) |
K2—F6xi | 3.148 (12) | F1—Lu1xv | 2.327 (5) |
K2—F6xii | 3.148 (12) | F2—Lu2xviii | 2.302 (4) |
K2—F6iv | 3.148 (12) | F2—Lu2v | 2.302 (4) |
K2—F7x | 3.16 (3) | F3—Lu2x | 2.327 (6) |
K2—F7viii | 3.16 (3) | F3—Lu2xiv | 2.327 (6) |
K2—F7ix | 3.16 (3) | F3—K1viii | 2.722 (14) |
K2—F5xiii | 3.21 (2) | F4—Lu1xvii | 2.328 (6) |
K2—F5iv | 3.21 (2) | F4—Lu1iii | 2.328 (6) |
K2—F5xi | 3.21 (2) | F4—K2ii | 2.702 (14) |
Lu1—F6xi | 2.165 (3) | F5—Lu1xix | 2.197 (17) |
Lu1—F6 | 2.165 (3) | F5—K1xx | 3.125 (18) |
Lu1—F5vii | 2.197 (17) | F5—K2xx | 3.21 (2) |
Lu1—F5vi | 2.197 (17) | F6—Lu1xxi | 2.165 (3) |
Lu1—F3 | 2.298 (13) | F6—K1viii | 3.12 (2) |
Lu1—F1 | 2.327 (5) | F6—K2xx | 3.148 (12) |
Lu1—F4x | 2.328 (6) | F7—Lu2xix | 2.167 (3) |
Lu1—F4xiv | 2.328 (6) | F7—K1xx | 3.124 (13) |
Lu1—Lu2x | 3.8725 (12) | F7—K2ii | 3.16 (3) |
Lu1—Lu2xiv | 3.8725 (12) | ||
F3i—K1—F3ii | 108.8 (5) | F1—Lu1—F4x | 66.2 (3) |
F3i—K1—F3iii | 108.8 (5) | F6xi—Lu1—F4xiv | 141.2 (4) |
F3ii—K1—F3iii | 108.8 (5) | F6—Lu1—F4xiv | 80.0 (4) |
F3i—K1—F1 | 110.1 (5) | F5vii—Lu1—F4xiv | 141.1 (4) |
F3ii—K1—F1 | 110.1 (5) | F5vi—Lu1—F4xiv | 81.3 (4) |
F3iii—K1—F1 | 110.1 (5) | F3—Lu1—F4xiv | 66.5 (3) |
F3i—K1—F6ii | 57.9 (4) | F1—Lu1—F4xiv | 66.2 (3) |
F3ii—K1—F6ii | 57.9 (4) | F4x—Lu1—F4xiv | 101.5 (6) |
F3iii—K1—F6ii | 99.4 (8) | F6xi—Lu1—Lu2x | 73.8 (3) |
F1—K1—F6ii | 150.5 (3) | F6—Lu1—Lu2x | 109.5 (3) |
F3i—K1—F6i | 57.9 (4) | F5vii—Lu1—Lu2x | 111.5 (4) |
F3ii—K1—F6i | 99.4 (8) | F5vi—Lu1—Lu2x | 164.5 (2) |
F3iii—K1—F6i | 57.9 (4) | F3—Lu1—Lu2x | 33.39 (11) |
F1—K1—F6i | 150.5 (3) | F1—Lu1—Lu2x | 86.0 (4) |
F6ii—K1—F6i | 50.5 (5) | F4x—Lu1—Lu2x | 33.5 (3) |
F3i—K1—F6iii | 99.4 (8) | F4xiv—Lu1—Lu2x | 86.3 (3) |
F3ii—K1—F6iii | 57.9 (4) | F6xi—Lu1—Lu2xiv | 109.5 (3) |
F3iii—K1—F6iii | 57.9 (4) | F6—Lu1—Lu2xiv | 73.8 (3) |
F1—K1—F6iii | 150.5 (3) | F5vii—Lu1—Lu2xiv | 164.5 (2) |
F6ii—K1—F6iii | 50.5 (5) | F5vi—Lu1—Lu2xiv | 111.5 (4) |
F6i—K1—F6iii | 50.5 (5) | F3—Lu1—Lu2xiv | 33.39 (11) |
F3i—K1—F7iv | 58.81 (15) | F1—Lu1—Lu2xiv | 86.0 (4) |
F3ii—K1—F7iv | 58.81 (15) | F4x—Lu1—Lu2xiv | 86.3 (3) |
F3iii—K1—F7iv | 150.8 (10) | F4xiv—Lu1—Lu2xiv | 33.5 (3) |
F1—K1—F7iv | 99.1 (5) | Lu2x—Lu1—Lu2xiv | 59.63 (3) |
F6ii—K1—F7iv | 51.4 (3) | F6xi—Lu1—Lu1xii | 110.1 (3) |
F6i—K1—F7iv | 96.1 (6) | F6—Lu1—Lu1xii | 163.5 (3) |
F6iii—K1—F7iv | 96.1 (6) | F5vii—Lu1—Lu1xii | 74.8 (2) |
F3i—K1—F7v | 58.81 (15) | F5vi—Lu1—Lu1xii | 109.8 (3) |
F3ii—K1—F7v | 150.8 (10) | F3—Lu1—Lu1xii | 86.6 (2) |
F3iii—K1—F7v | 58.81 (15) | F1—Lu1—Lu1xii | 33.30 (19) |
F1—K1—F7v | 99.1 (5) | F4x—Lu1—Lu1xii | 33.3 (2) |
F6ii—K1—F7v | 96.1 (6) | F4xiv—Lu1—Lu1xii | 86.5 (2) |
F6i—K1—F7v | 51.4 (3) | Lu2x—Lu1—Lu1xii | 59.846 (14) |
F6iii—K1—F7v | 96.1 (6) | Lu2xiv—Lu1—Lu1xii | 89.705 (14) |
F7iv—K1—F7v | 117.6 (3) | F6xi—Lu1—Lu1xv | 163.5 (3) |
F3i—K1—F7vi | 150.8 (10) | F6—Lu1—Lu1xv | 110.1 (3) |
F3ii—K1—F7vi | 58.81 (15) | F5vii—Lu1—Lu1xv | 109.8 (3) |
F3iii—K1—F7vi | 58.81 (15) | F5vi—Lu1—Lu1xv | 74.8 (2) |
F1—K1—F7vi | 99.1 (5) | F3—Lu1—Lu1xv | 86.6 (2) |
F6ii—K1—F7vi | 96.1 (6) | F1—Lu1—Lu1xv | 33.30 (19) |
F6i—K1—F7vi | 96.1 (6) | F4x—Lu1—Lu1xv | 86.5 (2) |
F6iii—K1—F7vi | 51.4 (3) | F4xiv—Lu1—Lu1xv | 33.3 (2) |
F7iv—K1—F7vi | 117.6 (3) | Lu2x—Lu1—Lu1xv | 89.705 (14) |
F7v—K1—F7vi | 117.6 (3) | Lu2xiv—Lu1—Lu1xv | 59.846 (14) |
F3i—K1—F5vii | 100.6 (2) | Lu1xii—Lu1—Lu1xv | 60.0 |
F3ii—K1—F5vii | 58.1 (4) | F5—Lu2—F5xvi | 77.4 (8) |
F3iii—K1—F5vii | 150.5 (4) | F5—Lu2—F7vi | 121.2 (4) |
F1—K1—F5vii | 59.3 (5) | F5xvi—Lu2—F7vi | 74.9 (4) |
F6ii—K1—F5vii | 94.5 (4) | F5—Lu2—F7 | 74.9 (4) |
F6i—K1—F5vii | 144.4 (6) | F5xvi—Lu2—F7 | 121.2 (4) |
F6iii—K1—F5vii | 116.1 (4) | F7vi—Lu2—F7 | 77.1 (6) |
F7iv—K1—F5vii | 49.4 (3) | F5—Lu2—F2 | 80.2 (4) |
F7v—K1—F5vii | 145.1 (6) | F5xvi—Lu2—F2 | 80.2 (4) |
F7vi—K1—F5vii | 94.1 (2) | F7vi—Lu2—F2 | 141.5 (3) |
F3i—K1—F5vi | 150.5 (4) | F7—Lu2—F2 | 141.5 (3) |
F3ii—K1—F5vi | 58.1 (4) | F5—Lu2—F4 | 141.3 (4) |
F3iii—K1—F5vi | 100.6 (2) | F5xvi—Lu2—F4 | 141.3 (4) |
F1—K1—F5vi | 59.3 (5) | F7vi—Lu2—F4 | 81.3 (4) |
F6ii—K1—F5vi | 116.1 (4) | F7—Lu2—F4 | 81.3 (4) |
F6i—K1—F5vi | 144.4 (6) | F2—Lu2—F4 | 101.6 (5) |
F6iii—K1—F5vi | 94.5 (4) | F5—Lu2—F3xvii | 79.8 (5) |
F7iv—K1—F5vi | 94.1 (2) | F5xvi—Lu2—F3xvii | 142.6 (4) |
F7v—K1—F5vi | 145.1 (6) | F7vi—Lu2—F3xvii | 142.5 (4) |
F7vi—K1—F5vi | 49.4 (3) | F7—Lu2—F3xvii | 80.0 (4) |
F5vii—K1—F5vi | 50.0 (4) | F2—Lu2—F3xvii | 66.9 (3) |
F4viii—K2—F4ix | 110.3 (6) | F4—Lu2—F3xvii | 66.2 (3) |
F4viii—K2—F4x | 110.3 (6) | F5—Lu2—F3iii | 142.6 (4) |
F4ix—K2—F4x | 110.3 (6) | F5xvi—Lu2—F3iii | 79.8 (5) |
F4viii—K2—F6xi | 58.64 (15) | F7vi—Lu2—F3iii | 80.0 (4) |
F4ix—K2—F6xi | 151.8 (11) | F7—Lu2—F3iii | 142.5 (4) |
F4x—K2—F6xi | 58.64 (15) | F2—Lu2—F3iii | 66.9 (3) |
F4viii—K2—F6xii | 151.8 (11) | F4—Lu2—F3iii | 66.2 (3) |
F4ix—K2—F6xii | 58.64 (15) | F3xvii—Lu2—F3iii | 101.9 (6) |
F4x—K2—F6xii | 58.64 (15) | F5—Lu2—Lu2v | 110.0 (3) |
F6xi—K2—F6xii | 117.3 (3) | F5xvi—Lu2—Lu2v | 73.5 (2) |
F4viii—K2—F6iv | 58.64 (15) | F7vi—Lu2—Lu2v | 110.1 (3) |
F4ix—K2—F6iv | 58.64 (15) | F7—Lu2—Lu2v | 165.3 (3) |
F4x—K2—F6iv | 151.8 (11) | F2—Lu2—Lu2v | 33.26 (17) |
F6xi—K2—F6iv | 117.3 (3) | F4—Lu2—Lu2v | 87.0 (2) |
F6xii—K2—F6iv | 117.3 (3) | F3xvii—Lu2—Lu2v | 87.1 (2) |
F4viii—K2—F7x | 59.3 (4) | F3iii—Lu2—Lu2v | 34.2 (2) |
F4ix—K2—F7x | 101.0 (8) | F5—Lu2—Lu2xviii | 73.5 (2) |
F4x—K2—F7x | 59.3 (4) | F5xvi—Lu2—Lu2xviii | 110.0 (3) |
F6xi—K2—F7x | 50.8 (4) | F7vi—Lu2—Lu2xviii | 165.3 (3) |
F6xii—K2—F7x | 95.6 (6) | F7—Lu2—Lu2xviii | 110.1 (3) |
F6iv—K2—F7x | 95.6 (6) | F2—Lu2—Lu2xviii | 33.26 (17) |
F4viii—K2—F7viii | 59.3 (4) | F4—Lu2—Lu2xviii | 87.0 (2) |
F4ix—K2—F7viii | 59.3 (4) | F3xvii—Lu2—Lu2xviii | 34.2 (2) |
F4x—K2—F7viii | 101.0 (8) | F3iii—Lu2—Lu2xviii | 87.1 (2) |
F6xi—K2—F7viii | 95.6 (6) | Lu2v—Lu2—Lu2xviii | 60.0 |
F6xii—K2—F7viii | 95.6 (6) | F5—Lu2—Lu1xvii | 109.4 (4) |
F6iv—K2—F7viii | 50.8 (4) | F5xvi—Lu2—Lu1xvii | 163.8 (3) |
F7x—K2—F7viii | 50.6 (5) | F7vi—Lu2—Lu1xvii | 111.5 (3) |
F4viii—K2—F7ix | 101.0 (8) | F7—Lu2—Lu1xvii | 75.0 (3) |
F4ix—K2—F7ix | 59.3 (4) | F2—Lu2—Lu1xvii | 86.5 (3) |
F4x—K2—F7ix | 59.3 (4) | F4—Lu2—Lu1xvii | 33.65 (11) |
F6xi—K2—F7ix | 95.6 (6) | F3xvii—Lu2—Lu1xvii | 32.9 (3) |
F6xii—K2—F7ix | 50.8 (4) | F3iii—Lu2—Lu1xvii | 86.6 (3) |
F6iv—K2—F7ix | 95.6 (6) | Lu2v—Lu2—Lu1xvii | 90.295 (15) |
F7x—K2—F7ix | 50.6 (5) | Lu2xviii—Lu2—Lu1xvii | 60.187 (13) |
F7viii—K2—F7ix | 50.6 (5) | F5—Lu2—Lu1iii | 163.8 (3) |
F4viii—K2—F5xiii | 150.0 (5) | F5xvi—Lu2—Lu1iii | 109.4 (4) |
F4ix—K2—F5xiii | 59.0 (4) | F7vi—Lu2—Lu1iii | 75.0 (3) |
F4x—K2—F5xiii | 99.6 (3) | F7—Lu2—Lu1iii | 111.5 (3) |
F6xi—K2—F5xiii | 143.6 (6) | F2—Lu2—Lu1iii | 86.5 (3) |
F6xii—K2—F5xiii | 50.9 (3) | F4—Lu2—Lu1iii | 33.65 (11) |
F6iv—K2—F5xiii | 95.5 (3) | F3xvii—Lu2—Lu1iii | 86.6 (3) |
F7x—K2—F5xiii | 146.0 (6) | F3iii—Lu2—Lu1iii | 32.9 (3) |
F7viii—K2—F5xiii | 118.3 (4) | Lu2v—Lu2—Lu1iii | 60.187 (13) |
F7ix—K2—F5xiii | 96.3 (4) | Lu2xviii—Lu2—Lu1iii | 90.295 (14) |
F4viii—K2—F5iv | 150.0 (5) | Lu1xvii—Lu2—Lu1iii | 60.31 (3) |
F4ix—K2—F5iv | 99.6 (3) | Lu1—F1—Lu1xii | 113.4 (4) |
F4x—K2—F5iv | 59.0 (4) | Lu1—F1—Lu1xv | 113.4 (4) |
F6xi—K2—F5iv | 95.5 (3) | Lu1xii—F1—Lu1xv | 113.4 (4) |
F6xii—K2—F5iv | 50.9 (3) | Lu1—F1—K1 | 105.2 (5) |
F6iv—K2—F5iv | 143.6 (6) | Lu1xii—F1—K1 | 105.2 (5) |
F7x—K2—F5iv | 118.3 (4) | Lu1xv—F1—K1 | 105.2 (5) |
F7viii—K2—F5iv | 146.0 (6) | Lu2xviii—F2—Lu2v | 113.5 (3) |
F7ix—K2—F5iv | 96.3 (4) | Lu2xviii—F2—Lu2 | 113.5 (3) |
F5xiii—K2—F5iv | 49.0 (4) | Lu2v—F2—Lu2 | 113.5 (3) |
F4viii—K2—F5xi | 99.6 (3) | Lu1—F3—Lu2x | 113.7 (3) |
F4ix—K2—F5xi | 59.0 (4) | Lu1—F3—Lu2xiv | 113.7 (3) |
F4x—K2—F5xi | 150.0 (5) | Lu2x—F3—Lu2xiv | 111.6 (5) |
F6xi—K2—F5xi | 143.6 (6) | Lu1—F3—K1viii | 106.2 (6) |
F6xii—K2—F5xi | 95.5 (3) | Lu2x—F3—K1viii | 105.4 (4) |
F6iv—K2—F5xi | 50.9 (3) | Lu2xiv—F3—K1viii | 105.4 (4) |
F7x—K2—F5xi | 146.0 (6) | Lu2—F4—Lu1xvii | 112.8 (4) |
F7viii—K2—F5xi | 96.3 (4) | Lu2—F4—Lu1iii | 112.8 (4) |
F7ix—K2—F5xi | 118.3 (4) | Lu1xvii—F4—Lu1iii | 113.3 (5) |
F5xiii—K2—F5xi | 50.4 (4) | Lu2—F4—K2ii | 105.1 (6) |
F5iv—K2—F5xi | 93.4 (7) | Lu1xvii—F4—K2ii | 105.9 (5) |
F6xi—Lu1—F6 | 76.0 (6) | Lu1iii—F4—K2ii | 105.9 (5) |
F6xi—Lu1—F5vii | 77.6 (4) | Lu2—F5—Lu1xix | 144.8 (4) |
F6—Lu1—F5vii | 121.7 (4) | Lu2—F5—K1xx | 98.1 (8) |
F6xi—Lu1—F5vi | 121.7 (4) | Lu1xix—F5—K1xx | 96.9 (4) |
F6—Lu1—F5vi | 77.6 (4) | Lu2—F5—K2xx | 100.8 (4) |
F5vii—Lu1—F5vi | 73.8 (7) | Lu1xix—F5—K2xx | 94.1 (8) |
F6xi—Lu1—F3 | 79.4 (3) | K1xx—F5—K2xx | 128.8 (3) |
F6—Lu1—F3 | 79.4 (4) | Lu1xxi—F6—Lu1 | 147.0 (6) |
F5vii—Lu1—F3 | 143.1 (4) | Lu1xxi—F6—K1viii | 97.4 (3) |
F5vi—Lu1—F3 | 143.1 (4) | Lu1—F6—K1viii | 97.4 (3) |
F6xi—Lu1—F1 | 141.9 (3) | Lu1xxi—F6—K2xx | 96.6 (3) |
F6—Lu1—F1 | 141.9 (3) | Lu1—F6—K2xx | 96.6 (3) |
F5vii—Lu1—F1 | 80.4 (4) | K1viii—F6—K2xx | 129.1 (8) |
F5vi—Lu1—F1 | 80.4 (4) | Lu2xix—F7—Lu2 | 150.5 (6) |
F3—Lu1—F1 | 101.2 (5) | Lu2xix—F7—K1xx | 97.3 (3) |
F6xi—Lu1—F4x | 80.0 (4) | Lu2—F7—K1xx | 97.3 (3) |
F6—Lu1—F4x | 141.2 (4) | Lu2xix—F7—K2ii | 95.3 (3) |
F5vii—Lu1—F4x | 81.3 (5) | Lu2—F7—K2ii | 95.3 (3) |
F5vi—Lu1—F4x | 141.1 (4) | K1xx—F7—K2ii | 128.6 (8) |
F3—Lu1—F4x | 66.5 (3) |
Symmetry codes: (i) x−y, x−1, z−1/2; (ii) −x+2, −y+1, z−1/2; (iii) y, −x+y+1, z−1/2; (iv) x, y−1, z; (v) −x+y, −x+1, z; (vi) −y+2, x−y+1, z; (vii) −y+2, −x+1, z; (viii) −x+2, −y+1, z+1/2; (ix) x−y+1, x−1, z+1/2; (x) y, −x+y, z+1/2; (xi) −y+2, x−y, z; (xii) −x+y+1, −x+1, z; (xiii) x, x−y, z; (xiv) x−y+1, x, z+1/2; (xv) −y+1, x−y, z; (xvi) x, x−y+1, z; (xvii) x−y, x, z−1/2; (xviii) −y+1, x−y+1, z; (xix) −x+y+1, −x+2, z; (xx) x, y+1, z; (xxi) −x+y+2, −x+2, z. |