Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100008945/qa0338sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270100008945/qa0338Isup2.hkl |
CCDC reference: 150373
The title compound was prepared from Ph3Sb and [Me3O][BF4], following a published procedure (Henry & Wittig, 1960). The material was recrystallized from aqueous EtOH (m.p. 408–409 K).
Compound (I) crystallized in the triclinic system; space group P1 was assumed and confirmed by the analysis. The BF4 anions and the phenyl rings showed large librational effects and were accordingly refined as rigid groups with anisotropic displacement parameters. The F-atom positions of the BF4 anions were restrained using the DFIX option of SHELXL97 (Sheldrick, 1997), based on difference-map peaks. All H atoms were placed in calculated positions. In the case of the methyl H atoms, these were placed as six half-H atoms at the corners of a regular hexagon, and refined as riding atoms. The C—H distances were 0.93 and 0.96 Å. The largest peaks on the difference map were adjacent to B3, 1.25–1.46 Å, and its adjacent F atoms, and to the Sb atoms, 1.17–1.28 Å.
Data collection: CAD-4-PC Software (Enraf-Nonius, 1992); cell refinement: SET4 and CELDIM in CAD-4-PC Software; data reduction: DATRD2 in NRCVAX (Gabe et al., 1989); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); software used to prepare material for publication: NRCVAX, SHELXL97 and WORDPERFECT macro PREP8 (Ferguson, 1998).
[Sb(CH3)(C6H5)3]BF4 | Z = 8 |
Mr = 454.90 | F(000) = 1792 |
Triclinic, P1 | Dx = 1.583 Mg m−3 |
a = 12.874 (4) Å | Mo Kα radiation, λ = 0.70930 Å |
b = 13.760 (5) Å | Cell parameters from 25 reflections |
c = 24.974 (7) Å | θ = 9.5–11.9° |
α = 98.82 (3)° | µ = 1.48 mm−1 |
β = 93.97 (2)° | T = 293 K |
γ = 117.80 (3)° | Block, colourless |
V = 3817 (2) Å3 | 0.42 × 0.28 × 0.26 mm |
Enraf-Nonius CAD-4 diffractometer | 8121 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | θmax = 25.4°, θmin = 2.0° |
Graphite monochromator | h = −15→13 |
ω/2θ scans | k = 0→16 |
Absorption correction: gaussian (NRCVAX; Gabe et al., 1989) | l = −30→29 |
Tmin = 0.689, Tmax = 0.715 | 3 standard reflections every 120 min |
14181 measured reflections | intensity decay: 3% |
14181 independent 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)] = 0.057 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.181 | H-atom parameters constrained |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0943P)2 + 4.9573P] where P = (Fo2 + 2Fc2)/3 |
14181 reflections | (Δ/σ)max = 0.005 |
722 parameters | Δρmax = 1.15 e Å−3 |
0 restraints | Δρmin = −0.78 e Å−3 |
[Sb(CH3)(C6H5)3]BF4 | γ = 117.80 (3)° |
Mr = 454.90 | V = 3817 (2) Å3 |
Triclinic, P1 | Z = 8 |
a = 12.874 (4) Å | Mo Kα radiation |
b = 13.760 (5) Å | µ = 1.48 mm−1 |
c = 24.974 (7) Å | T = 293 K |
α = 98.82 (3)° | 0.42 × 0.28 × 0.26 mm |
β = 93.97 (2)° |
Enraf-Nonius CAD-4 diffractometer | 14181 independent reflections |
Absorption correction: gaussian (NRCVAX; Gabe et al., 1989) | 8121 reflections with I > 2σ(I) |
Tmin = 0.689, Tmax = 0.715 | 3 standard reflections every 120 min |
14181 measured reflections | intensity decay: 3% |
R[F2 > 2σ(F2)] = 0.057 | 0 restraints |
wR(F2) = 0.181 | H-atom parameters constrained |
S = 1.03 | Δρmax = 1.15 e Å−3 |
14181 reflections | Δρmin = −0.78 e Å−3 |
722 parameters |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Sb1 | 0.60137 (6) | 0.15922 (5) | 0.11741 (2) | 0.07008 (19) | |
Sb2 | 0.92577 (6) | 0.81482 (6) | 0.08202 (3) | 0.07138 (19) | |
Sb3 | 0.20603 (5) | 0.08417 (5) | 0.43431 (2) | 0.05697 (16) | |
Sb4 | 0.83974 (5) | 0.39753 (5) | 0.38364 (2) | 0.06388 (18) | |
C17 | 0.5375 (9) | −0.0145 (8) | 0.0938 (4) | 0.095 (3) | |
C111 | 0.7691 (5) | 0.2341 (6) | 0.1656 (3) | 0.073 (2) | |
C112 | 0.8369 (7) | 0.1796 (5) | 0.1642 (3) | 0.098 (3) | |
C113 | 0.9519 (7) | 0.2340 (8) | 0.1932 (4) | 0.120 (4) | |
C114 | 0.9993 (5) | 0.3430 (9) | 0.2237 (3) | 0.118 (5) | |
C115 | 0.9315 (7) | 0.3975 (6) | 0.2251 (3) | 0.113 (4) | |
C116 | 0.8165 (7) | 0.3431 (6) | 0.1960 (3) | 0.102 (3) | |
C121 | 0.6228 (7) | 0.2524 (6) | 0.0570 (2) | 0.078 (3) | |
C122 | 0.7360 (6) | 0.3149 (7) | 0.0448 (3) | 0.108 (4) | |
C123 | 0.7529 (7) | 0.3798 (7) | 0.0054 (4) | 0.133 (5) | |
C124 | 0.6564 (9) | 0.3822 (7) | −0.0218 (3) | 0.129 (5) | |
C125 | 0.5432 (8) | 0.3197 (8) | −0.0096 (3) | 0.118 (4) | |
C126 | 0.5263 (5) | 0.2548 (6) | 0.0298 (3) | 0.093 (3) | |
C131 | 0.4800 (5) | 0.1783 (6) | 0.1637 (2) | 0.075 (3) | |
C132 | 0.4888 (6) | 0.2833 (5) | 0.1806 (3) | 0.093 (3) | |
C133 | 0.4074 (7) | 0.2943 (6) | 0.2113 (3) | 0.099 (4) | |
C134 | 0.3173 (6) | 0.2003 (8) | 0.2252 (3) | 0.118 (5) | |
C135 | 0.3085 (6) | 0.0953 (7) | 0.2083 (3) | 0.113 (4) | |
C136 | 0.3899 (7) | 0.0843 (5) | 0.1776 (3) | 0.097 (3) | |
C27 | 0.9939 (9) | 0.9877 (8) | 0.0945 (4) | 0.090 (3) | |
C211 | 0.8840 (6) | 0.7387 (6) | −0.0009 (2) | 0.076 (3) | |
C212 | 0.7983 (7) | 0.7477 (7) | −0.0336 (4) | 0.123 (5) | |
C213 | 0.7633 (8) | 0.6931 (9) | −0.0885 (3) | 0.164 (8) | |
C214 | 0.8139 (10) | 0.6295 (8) | −0.1107 (2) | 0.173 (10) | |
C215 | 0.8996 (9) | 0.6205 (7) | −0.0780 (4) | 0.184 (9) | |
C216 | 0.9346 (7) | 0.6751 (7) | −0.0231 (3) | 0.112 (4) | |
C221 | 0.7637 (5) | 0.7367 (6) | 0.1101 (3) | 0.080 (3) | |
C222 | 0.7271 (6) | 0.7939 (5) | 0.1483 (3) | 0.103 (4) | |
C223 | 0.6193 (7) | 0.7362 (8) | 0.1665 (3) | 0.116 (4) | |
C224 | 0.5482 (5) | 0.6213 (8) | 0.1465 (4) | 0.115 (4) | |
C225 | 0.5848 (7) | 0.5642 (5) | 0.1082 (4) | 0.123 (4) | |
C226 | 0.6926 (7) | 0.6219 (6) | 0.0900 (3) | 0.110 (4) | |
C231 | 1.0413 (7) | 0.7700 (8) | 0.1206 (3) | 0.088 (3) | |
C232 | 1.1501 (8) | 0.7937 (8) | 0.1042 (4) | 0.140 (6) | |
C233 | 1.2225 (8) | 0.7586 (10) | 0.1295 (5) | 0.163 (7) | |
C234 | 1.1860 (12) | 0.6998 (11) | 0.1712 (5) | 0.191 (9) | |
C235 | 1.0772 (13) | 0.6761 (12) | 0.1876 (5) | 0.274 (16) | |
C236 | 1.0048 (9) | 0.7112 (11) | 0.1623 (4) | 0.196 (9) | |
C37 | 0.0205 (7) | −0.0083 (8) | 0.4161 (4) | 0.073 (2) | |
C311 | 0.2901 (4) | −0.0073 (4) | 0.4061 (2) | 0.0579 (19) | |
C312 | 0.2372 (4) | −0.0971 (5) | 0.3612 (2) | 0.079 (3) | |
C313 | 0.2961 (6) | −0.1560 (5) | 0.3439 (2) | 0.096 (3) | |
C314 | 0.4080 (6) | −0.1252 (5) | 0.3715 (3) | 0.082 (3) | |
C315 | 0.4609 (4) | −0.0355 (5) | 0.4164 (2) | 0.077 (3) | |
C316 | 0.4020 (5) | 0.0235 (4) | 0.4337 (2) | 0.065 (2) | |
C321 | 0.2649 (5) | 0.1370 (4) | 0.51910 (17) | 0.0540 (18) | |
C322 | 0.2593 (5) | 0.0587 (4) | 0.5496 (3) | 0.069 (2) | |
C323 | 0.2909 (6) | 0.0905 (6) | 0.6063 (2) | 0.092 (3) | |
C324 | 0.3281 (6) | 0.2007 (7) | 0.63267 (17) | 0.085 (3) | |
C325 | 0.3338 (6) | 0.2790 (5) | 0.6022 (2) | 0.104 (4) | |
C326 | 0.3021 (6) | 0.2472 (4) | 0.5454 (2) | 0.082 (3) | |
C331 | 0.2774 (5) | 0.2276 (4) | 0.4013 (2) | 0.0572 (19) | |
C332 | 0.2061 (4) | 0.2564 (5) | 0.3703 (2) | 0.079 (3) | |
C333 | 0.2579 (7) | 0.3493 (6) | 0.3464 (2) | 0.093 (3) | |
C334 | 0.3810 (7) | 0.4134 (5) | 0.3533 (3) | 0.092 (3) | |
C335 | 0.4523 (5) | 0.3845 (5) | 0.3842 (3) | 0.089 (3) | |
C336 | 0.4005 (5) | 0.2917 (5) | 0.4082 (2) | 0.073 (2) | |
C47 | 1.0216 (8) | 0.4480 (9) | 0.4003 (4) | 0.085 (3) | |
C411 | 0.8191 (5) | 0.5072 (4) | 0.3395 (2) | 0.062 (2) | |
C412 | 0.7118 (4) | 0.4713 (4) | 0.3059 (2) | 0.073 (2) | |
C413 | 0.6985 (5) | 0.5428 (6) | 0.2757 (2) | 0.086 (3) | |
C414 | 0.7923 (7) | 0.6502 (5) | 0.2792 (3) | 0.089 (3) | |
C415 | 0.8995 (6) | 0.6861 (4) | 0.3128 (3) | 0.109 (4) | |
C416 | 0.9129 (4) | 0.6146 (5) | 0.3430 (3) | 0.097 (3) | |
C421 | 0.7425 (5) | 0.2357 (4) | 0.3354 (2) | 0.066 (2) | |
C422 | 0.7977 (5) | 0.1769 (6) | 0.3126 (2) | 0.076 (3) | |
C423 | 0.7294 (8) | 0.0683 (6) | 0.2816 (3) | 0.096 (3) | |
C424 | 0.6060 (8) | 0.0185 (4) | 0.2733 (2) | 0.109 (4) | |
C425 | 0.5509 (5) | 0.0774 (6) | 0.2960 (3) | 0.096 (3) | |
C426 | 0.6191 (5) | 0.1859 (6) | 0.3271 (3) | 0.084 (3) | |
C431 | 0.7541 (5) | 0.3912 (5) | 0.4512 (2) | 0.059 (2) | |
C432 | 0.7202 (6) | 0.2995 (4) | 0.4761 (3) | 0.084 (3) | |
C433 | 0.6639 (6) | 0.2946 (5) | 0.5219 (3) | 0.095 (3) | |
C434 | 0.6416 (6) | 0.3814 (7) | 0.5429 (2) | 0.101 (4) | |
C435 | 0.6755 (6) | 0.4731 (5) | 0.5180 (3) | 0.095 (3) | |
C436 | 0.7318 (6) | 0.4780 (4) | 0.4722 (2) | 0.073 (2) | |
B1 | 0.7574 (4) | 0.0216 (4) | 0.00319 (19) | 0.086 (3) | |
F11 | 0.7430 (5) | −0.0564 (5) | 0.0321 (3) | 0.131 (2) | |
F12 | 0.8599 (5) | 0.0566 (6) | −0.0156 (3) | 0.165 (3) | |
F13 | 0.6683 (5) | −0.0215 (7) | −0.0385 (3) | 0.210 (6) | |
F14 | 0.7573 (8) | 0.1080 (5) | 0.0354 (3) | 0.201 (5) | |
B2 | 0.9775 (3) | 0.2502 (3) | 0.49727 (15) | 0.077 (3) | |
F21 | 1.0063 (5) | 0.3543 (3) | 0.5221 (2) | 0.114 (2) | |
F22 | 0.9116 (5) | 0.2224 (4) | 0.44831 (16) | 0.118 (2) | |
F23 | 0.9154 (6) | 0.1787 (4) | 0.5280 (2) | 0.145 (3) | |
F24 | 1.0763 (4) | 0.2442 (5) | 0.4910 (3) | 0.154 (3) | |
B3 | 0.3642 (7) | 0.6080 (5) | 0.2625 (3) | 0.110 (5) | |
F31 | 0.4144 (7) | 0.7095 (5) | 0.2509 (3) | 0.146 (3) | |
F32 | 0.4387 (13) | 0.5661 (10) | 0.2587 (5) | 0.306 (11) | |
F33 | 0.3385 (13) | 0.6139 (8) | 0.3130 (4) | 0.299 (10) | |
F34 | 0.2653 (11) | 0.5404 (8) | 0.2269 (6) | 0.441 (18) | |
B4 | −0.0009 (4) | −0.0196 (4) | 0.25962 (18) | 0.087 (3) | |
F41 | 0.0892 (5) | −0.0085 (6) | 0.2943 (2) | 0.136 (3) | |
F42 | −0.1033 (4) | −0.0784 (6) | 0.2770 (3) | 0.149 (3) | |
F43 | −0.0031 (6) | −0.0727 (9) | 0.21017 (19) | 0.221 (6) | |
F44 | 0.0134 (7) | 0.0814 (5) | 0.2570 (4) | 0.254 (7) | |
H17A | 0.5022 | −0.0503 | 0.1228 | 0.143* | 0.50 |
H17B | 0.6022 | −0.0283 | 0.0865 | 0.143* | 0.50 |
H17C | 0.4789 | −0.0444 | 0.0613 | 0.143* | 0.50 |
H17D | 0.5534 | −0.0317 | 0.0575 | 0.143* | 0.50 |
H17E | 0.4533 | −0.0537 | 0.0939 | 0.143* | 0.50 |
H17F | 0.5766 | −0.0376 | 0.1191 | 0.143* | 0.50 |
H112 | 0.8052 | 0.1067 | 0.1438 | 0.118* | |
H113 | 0.9973 | 0.1975 | 0.1923 | 0.144* | |
H114 | 1.0763 | 0.3794 | 0.2431 | 0.141* | |
H115 | 0.9632 | 0.4704 | 0.2454 | 0.135* | |
H116 | 0.7711 | 0.3796 | 0.1970 | 0.122* | |
H122 | 0.8006 | 0.3133 | 0.0630 | 0.129* | |
H123 | 0.8287 | 0.4216 | −0.0028 | 0.160* | |
H124 | 0.6677 | 0.4256 | −0.0482 | 0.154* | |
H125 | 0.4786 | 0.3213 | −0.0278 | 0.141* | |
H126 | 0.4505 | 0.2129 | 0.0380 | 0.111* | |
H132 | 0.5491 | 0.3461 | 0.1713 | 0.112* | |
H133 | 0.4133 | 0.3646 | 0.2226 | 0.119* | |
H134 | 0.2629 | 0.2077 | 0.2457 | 0.142* | |
H135 | 0.2482 | 0.0325 | 0.2176 | 0.136* | |
H136 | 0.3840 | 0.0140 | 0.1663 | 0.116* | |
H27A | 1.0498 | 1.0171 | 0.0699 | 0.134* | 0.50 |
H27B | 1.0333 | 1.0217 | 0.1317 | 0.134* | 0.50 |
H27C | 0.9302 | 1.0042 | 0.0875 | 0.134* | 0.50 |
H27D | 0.9591 | 1.0116 | 0.1228 | 0.134* | 0.50 |
H27E | 0.9755 | 1.0070 | 0.0611 | 0.134* | 0.50 |
H27F | 1.0787 | 1.0245 | 0.1053 | 0.134* | 0.50 |
H212 | 0.7645 | 0.7903 | −0.0187 | 0.148* | |
H213 | 0.7060 | 0.6992 | −0.1104 | 0.197* | |
H214 | 0.7905 | 0.5930 | −0.1475 | 0.208* | |
H215 | 0.9334 | 0.5779 | −0.0929 | 0.220* | |
H216 | 0.9919 | 0.6691 | −0.0012 | 0.134* | |
H222 | 0.7747 | 0.8708 | 0.1618 | 0.124* | |
H223 | 0.5948 | 0.7745 | 0.1921 | 0.139* | |
H224 | 0.4761 | 0.5827 | 0.1586 | 0.138* | |
H225 | 0.5372 | 0.4873 | 0.0948 | 0.148* | |
H226 | 0.7171 | 0.5836 | 0.0644 | 0.132* | |
H232 | 1.1745 | 0.8330 | 0.0763 | 0.168* | |
H233 | 1.2953 | 0.7744 | 0.1185 | 0.196* | |
H234 | 1.2344 | 0.6763 | 0.1881 | 0.229* | |
H235 | 1.0528 | 0.6368 | 0.2155 | 0.329* | |
H236 | 0.9320 | 0.6954 | 0.1733 | 0.235* | |
H37A | −0.0123 | 0.0415 | 0.4232 | 0.110* | 0.50 |
H37B | −0.0083 | −0.0631 | 0.4387 | 0.110* | 0.50 |
H37C | −0.0030 | −0.0456 | 0.3781 | 0.110* | 0.50 |
H37D | −0.0034 | −0.0863 | 0.4035 | 0.110* | 0.50 |
H37E | −0.0074 | 0.0183 | 0.3880 | 0.110* | 0.50 |
H37F | −0.0127 | 0.0008 | 0.4486 | 0.110* | 0.50 |
H312 | 0.1624 | −0.1177 | 0.3428 | 0.095* | |
H313 | 0.2607 | −0.2161 | 0.3139 | 0.115* | |
H314 | 0.4474 | −0.1647 | 0.3599 | 0.098* | |
H315 | 0.5357 | −0.0149 | 0.4349 | 0.092* | |
H316 | 0.4374 | 0.0835 | 0.4638 | 0.078* | |
H322 | 0.2344 | −0.0150 | 0.5320 | 0.083* | |
H323 | 0.2872 | 0.0381 | 0.6267 | 0.110* | |
H324 | 0.3493 | 0.2219 | 0.6707 | 0.102* | |
H325 | 0.3587 | 0.3527 | 0.6198 | 0.125* | |
H326 | 0.3059 | 0.2996 | 0.5250 | 0.098* | |
H332 | 0.1237 | 0.2136 | 0.3657 | 0.094* | |
H333 | 0.2102 | 0.3686 | 0.3257 | 0.112* | |
H334 | 0.4157 | 0.4755 | 0.3372 | 0.110* | |
H335 | 0.5347 | 0.4274 | 0.3889 | 0.107* | |
H336 | 0.4482 | 0.2724 | 0.4289 | 0.088* | |
H47A | 1.0339 | 0.3850 | 0.3883 | 0.127* | 0.50 |
H47B | 1.0491 | 0.4758 | 0.4390 | 0.127* | 0.50 |
H47C | 1.0650 | 0.5063 | 0.3811 | 0.127* | 0.50 |
H47D | 1.0648 | 0.5264 | 0.4173 | 0.127* | 0.50 |
H47E | 1.0495 | 0.4356 | 0.3666 | 0.127* | 0.50 |
H47F | 1.0337 | 0.4051 | 0.4245 | 0.127* | 0.50 |
H412 | 0.6491 | 0.3994 | 0.3035 | 0.087* | |
H413 | 0.6267 | 0.5188 | 0.2532 | 0.103* | |
H414 | 0.7833 | 0.6980 | 0.2590 | 0.107* | |
H415 | 0.9623 | 0.7579 | 0.3152 | 0.131* | |
H416 | 0.9847 | 0.6386 | 0.3655 | 0.117* | |
H422 | 0.8802 | 0.2102 | 0.3182 | 0.091* | |
H423 | 0.7663 | 0.0289 | 0.2664 | 0.115* | |
H424 | 0.5603 | −0.0541 | 0.2525 | 0.131* | |
H425 | 0.4683 | 0.0441 | 0.2905 | 0.115* | |
H426 | 0.5823 | 0.2253 | 0.3423 | 0.101* | |
H432 | 0.7351 | 0.2414 | 0.4621 | 0.100* | |
H433 | 0.6412 | 0.2333 | 0.5386 | 0.114* | |
H434 | 0.6039 | 0.3781 | 0.5736 | 0.121* | |
H435 | 0.6606 | 0.5311 | 0.5320 | 0.114* | |
H436 | 0.7545 | 0.5393 | 0.4556 | 0.087* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Sb1 | 0.0705 (4) | 0.0741 (4) | 0.0631 (4) | 0.0342 (3) | 0.0150 (3) | 0.0078 (3) |
Sb2 | 0.0713 (4) | 0.0766 (4) | 0.0653 (4) | 0.0356 (3) | 0.0099 (3) | 0.0133 (3) |
Sb3 | 0.0502 (3) | 0.0615 (3) | 0.0595 (3) | 0.0284 (3) | 0.0094 (2) | 0.0087 (3) |
Sb4 | 0.0623 (4) | 0.0666 (4) | 0.0596 (3) | 0.0288 (3) | 0.0095 (3) | 0.0127 (3) |
C17 | 0.088 (7) | 0.076 (7) | 0.098 (8) | 0.026 (6) | 0.032 (6) | −0.005 (6) |
C111 | 0.071 (6) | 0.084 (7) | 0.060 (5) | 0.035 (5) | 0.016 (4) | 0.013 (5) |
C112 | 0.085 (8) | 0.109 (9) | 0.109 (8) | 0.051 (7) | 0.015 (6) | 0.034 (7) |
C113 | 0.090 (9) | 0.154 (13) | 0.138 (12) | 0.071 (9) | 0.019 (8) | 0.051 (10) |
C114 | 0.089 (9) | 0.165 (14) | 0.073 (7) | 0.038 (10) | 0.011 (6) | 0.034 (8) |
C115 | 0.092 (9) | 0.112 (10) | 0.089 (8) | 0.022 (8) | 0.001 (7) | −0.002 (7) |
C116 | 0.080 (7) | 0.107 (9) | 0.106 (8) | 0.044 (7) | 0.010 (6) | −0.004 (7) |
C121 | 0.094 (7) | 0.082 (7) | 0.062 (5) | 0.046 (6) | 0.020 (5) | 0.013 (5) |
C122 | 0.111 (9) | 0.135 (11) | 0.110 (9) | 0.074 (9) | 0.041 (7) | 0.055 (8) |
C123 | 0.126 (11) | 0.146 (12) | 0.169 (14) | 0.076 (10) | 0.073 (10) | 0.090 (11) |
C124 | 0.169 (14) | 0.142 (12) | 0.107 (10) | 0.089 (12) | 0.038 (10) | 0.062 (9) |
C125 | 0.112 (10) | 0.121 (10) | 0.100 (9) | 0.042 (9) | −0.013 (8) | 0.028 (8) |
C126 | 0.092 (8) | 0.107 (8) | 0.075 (7) | 0.046 (7) | 0.004 (6) | 0.022 (6) |
C131 | 0.076 (6) | 0.107 (8) | 0.046 (5) | 0.051 (6) | 0.010 (4) | 0.007 (5) |
C132 | 0.085 (7) | 0.083 (7) | 0.097 (8) | 0.034 (6) | 0.023 (6) | −0.004 (6) |
C133 | 0.093 (8) | 0.107 (9) | 0.079 (7) | 0.047 (7) | 0.006 (6) | −0.023 (6) |
C134 | 0.086 (8) | 0.182 (14) | 0.083 (8) | 0.076 (10) | 0.008 (6) | −0.018 (9) |
C135 | 0.096 (9) | 0.127 (11) | 0.116 (9) | 0.049 (8) | 0.044 (7) | 0.028 (8) |
C136 | 0.093 (8) | 0.103 (8) | 0.097 (8) | 0.048 (7) | 0.036 (6) | 0.016 (6) |
C27 | 0.090 (7) | 0.077 (7) | 0.099 (8) | 0.042 (6) | 0.012 (6) | 0.008 (6) |
C211 | 0.072 (6) | 0.080 (6) | 0.064 (6) | 0.023 (5) | 0.021 (5) | 0.024 (5) |
C212 | 0.157 (13) | 0.130 (11) | 0.079 (8) | 0.071 (10) | −0.008 (8) | 0.023 (7) |
C213 | 0.161 (15) | 0.199 (18) | 0.070 (9) | 0.039 (13) | −0.007 (9) | 0.028 (10) |
C214 | 0.148 (15) | 0.174 (17) | 0.063 (8) | −0.028 (13) | 0.023 (9) | 0.013 (9) |
C215 | 0.164 (16) | 0.175 (16) | 0.116 (12) | 0.016 (13) | 0.077 (12) | −0.035 (12) |
C216 | 0.087 (8) | 0.141 (11) | 0.085 (8) | 0.048 (8) | 0.013 (6) | −0.012 (7) |
C221 | 0.089 (7) | 0.082 (7) | 0.067 (6) | 0.036 (6) | 0.019 (5) | 0.027 (5) |
C222 | 0.082 (8) | 0.115 (9) | 0.085 (7) | 0.030 (7) | 0.016 (6) | 0.000 (7) |
C223 | 0.082 (8) | 0.158 (13) | 0.094 (8) | 0.050 (9) | 0.024 (7) | 0.010 (8) |
C224 | 0.094 (9) | 0.137 (12) | 0.099 (9) | 0.035 (9) | 0.030 (7) | 0.047 (8) |
C225 | 0.115 (11) | 0.108 (10) | 0.133 (11) | 0.033 (9) | 0.038 (9) | 0.050 (9) |
C226 | 0.108 (9) | 0.106 (10) | 0.112 (9) | 0.044 (8) | 0.041 (8) | 0.027 (8) |
C231 | 0.102 (8) | 0.113 (8) | 0.068 (6) | 0.066 (7) | 0.005 (5) | 0.028 (6) |
C232 | 0.086 (9) | 0.159 (13) | 0.193 (15) | 0.063 (9) | −0.003 (9) | 0.078 (12) |
C233 | 0.126 (12) | 0.162 (15) | 0.199 (18) | 0.081 (12) | −0.036 (12) | 0.022 (13) |
C234 | 0.20 (2) | 0.24 (2) | 0.172 (18) | 0.14 (2) | −0.040 (15) | 0.061 (16) |
C235 | 0.24 (3) | 0.31 (3) | 0.33 (3) | 0.15 (3) | −0.03 (3) | 0.18 (3) |
C236 | 0.192 (18) | 0.25 (2) | 0.203 (19) | 0.125 (18) | 0.052 (15) | 0.151 (18) |
C37 | 0.054 (5) | 0.090 (7) | 0.071 (6) | 0.033 (5) | 0.007 (4) | 0.009 (5) |
C311 | 0.055 (5) | 0.059 (5) | 0.065 (5) | 0.033 (4) | 0.008 (4) | 0.008 (4) |
C312 | 0.064 (6) | 0.071 (6) | 0.089 (7) | 0.030 (5) | 0.004 (5) | −0.006 (5) |
C313 | 0.095 (8) | 0.079 (7) | 0.096 (8) | 0.041 (6) | 0.000 (6) | −0.019 (6) |
C314 | 0.091 (7) | 0.071 (6) | 0.097 (7) | 0.048 (6) | 0.026 (6) | 0.020 (6) |
C315 | 0.079 (6) | 0.094 (7) | 0.079 (6) | 0.059 (6) | 0.012 (5) | 0.022 (5) |
C316 | 0.071 (6) | 0.061 (5) | 0.067 (5) | 0.035 (5) | 0.016 (4) | 0.010 (4) |
C321 | 0.039 (4) | 0.052 (4) | 0.060 (5) | 0.016 (4) | 0.007 (3) | 0.003 (4) |
C322 | 0.061 (5) | 0.064 (5) | 0.088 (7) | 0.030 (4) | 0.011 (5) | 0.027 (5) |
C323 | 0.087 (7) | 0.136 (10) | 0.084 (7) | 0.071 (7) | 0.025 (6) | 0.051 (7) |
C324 | 0.082 (7) | 0.107 (8) | 0.062 (6) | 0.045 (7) | 0.010 (5) | 0.010 (6) |
C325 | 0.119 (9) | 0.089 (8) | 0.085 (8) | 0.043 (7) | 0.021 (7) | −0.012 (6) |
C326 | 0.108 (8) | 0.060 (6) | 0.075 (6) | 0.040 (6) | 0.023 (6) | 0.011 (5) |
C331 | 0.067 (5) | 0.063 (5) | 0.049 (4) | 0.038 (4) | 0.011 (4) | 0.011 (4) |
C332 | 0.088 (7) | 0.087 (7) | 0.068 (6) | 0.051 (6) | 0.004 (5) | 0.010 (5) |
C333 | 0.130 (10) | 0.101 (8) | 0.066 (6) | 0.072 (8) | 0.001 (6) | 0.017 (6) |
C334 | 0.123 (10) | 0.092 (8) | 0.061 (6) | 0.050 (8) | 0.021 (6) | 0.019 (5) |
C335 | 0.096 (8) | 0.093 (7) | 0.082 (7) | 0.042 (6) | 0.032 (6) | 0.032 (6) |
C336 | 0.070 (6) | 0.075 (6) | 0.083 (6) | 0.037 (5) | 0.018 (5) | 0.029 (5) |
C47 | 0.065 (6) | 0.105 (8) | 0.080 (6) | 0.041 (6) | −0.002 (5) | 0.012 (6) |
C411 | 0.068 (5) | 0.061 (5) | 0.049 (4) | 0.027 (4) | 0.006 (4) | 0.005 (4) |
C412 | 0.076 (6) | 0.066 (6) | 0.064 (5) | 0.026 (5) | 0.010 (5) | 0.013 (4) |
C413 | 0.092 (7) | 0.095 (8) | 0.067 (6) | 0.050 (7) | −0.010 (5) | 0.003 (5) |
C414 | 0.116 (9) | 0.073 (7) | 0.087 (7) | 0.051 (7) | 0.016 (6) | 0.022 (6) |
C415 | 0.104 (9) | 0.056 (6) | 0.136 (10) | 0.014 (6) | −0.014 (8) | 0.032 (6) |
C416 | 0.077 (7) | 0.070 (7) | 0.115 (9) | 0.016 (6) | −0.017 (6) | 0.019 (6) |
C421 | 0.078 (6) | 0.067 (5) | 0.057 (5) | 0.037 (5) | 0.016 (4) | 0.013 (4) |
C422 | 0.091 (7) | 0.074 (6) | 0.058 (5) | 0.036 (6) | 0.009 (5) | 0.016 (5) |
C423 | 0.153 (11) | 0.085 (8) | 0.071 (7) | 0.073 (8) | 0.034 (7) | 0.015 (6) |
C424 | 0.176 (14) | 0.067 (7) | 0.066 (7) | 0.044 (9) | 0.020 (8) | 0.014 (5) |
C425 | 0.093 (8) | 0.070 (7) | 0.083 (7) | 0.007 (6) | −0.005 (6) | 0.016 (6) |
C426 | 0.086 (7) | 0.078 (7) | 0.083 (7) | 0.035 (6) | 0.018 (5) | 0.015 (5) |
C431 | 0.059 (5) | 0.055 (5) | 0.053 (5) | 0.018 (4) | 0.011 (4) | 0.015 (4) |
C432 | 0.097 (7) | 0.077 (7) | 0.078 (6) | 0.041 (6) | 0.018 (6) | 0.022 (5) |
C433 | 0.103 (8) | 0.071 (7) | 0.092 (8) | 0.021 (6) | 0.020 (6) | 0.034 (6) |
C434 | 0.093 (8) | 0.117 (10) | 0.061 (6) | 0.026 (7) | 0.022 (5) | 0.016 (6) |
C435 | 0.099 (8) | 0.095 (8) | 0.077 (7) | 0.042 (7) | 0.021 (6) | −0.009 (6) |
C436 | 0.075 (6) | 0.060 (5) | 0.066 (5) | 0.019 (5) | 0.013 (5) | 0.014 (4) |
B1 | 0.072 (8) | 0.101 (10) | 0.094 (9) | 0.046 (7) | 0.025 (7) | 0.024 (8) |
F11 | 0.109 (5) | 0.131 (6) | 0.170 (7) | 0.061 (5) | 0.024 (5) | 0.068 (5) |
F12 | 0.109 (6) | 0.194 (9) | 0.205 (9) | 0.069 (6) | 0.075 (6) | 0.069 (7) |
F13 | 0.155 (8) | 0.187 (9) | 0.152 (7) | −0.032 (7) | −0.065 (6) | 0.089 (7) |
F14 | 0.261 (12) | 0.130 (7) | 0.244 (11) | 0.109 (8) | 0.139 (10) | 0.034 (7) |
B2 | 0.076 (7) | 0.052 (6) | 0.090 (8) | 0.019 (6) | −0.001 (6) | 0.020 (6) |
F21 | 0.112 (5) | 0.080 (4) | 0.136 (5) | 0.038 (4) | 0.014 (4) | 0.012 (4) |
F22 | 0.139 (6) | 0.114 (5) | 0.085 (4) | 0.054 (4) | −0.010 (4) | 0.016 (4) |
F23 | 0.170 (7) | 0.092 (5) | 0.101 (5) | 0.005 (5) | −0.003 (5) | 0.032 (4) |
F24 | 0.109 (6) | 0.122 (6) | 0.219 (9) | 0.065 (5) | −0.003 (6) | −0.014 (6) |
B3 | 0.149 (14) | 0.087 (10) | 0.138 (13) | 0.082 (11) | 0.058 (11) | 0.047 (9) |
F31 | 0.161 (7) | 0.132 (6) | 0.186 (8) | 0.083 (6) | 0.068 (6) | 0.083 (6) |
F32 | 0.59 (3) | 0.40 (2) | 0.260 (13) | 0.44 (2) | 0.258 (18) | 0.232 (15) |
F33 | 0.58 (3) | 0.163 (9) | 0.285 (14) | 0.234 (15) | 0.300 (18) | 0.111 (10) |
F34 | 0.31 (2) | 0.27 (2) | 0.42 (3) | −0.076 (17) | −0.19 (2) | 0.062 (19) |
B4 | 0.080 (8) | 0.096 (9) | 0.071 (8) | 0.033 (7) | 0.006 (6) | 0.017 (7) |
F41 | 0.117 (5) | 0.194 (8) | 0.114 (5) | 0.089 (6) | 0.002 (4) | 0.038 (5) |
F42 | 0.114 (6) | 0.174 (8) | 0.137 (6) | 0.047 (6) | 0.027 (5) | 0.050 (6) |
F43 | 0.148 (8) | 0.339 (16) | 0.084 (5) | 0.075 (9) | 0.004 (5) | −0.060 (7) |
F44 | 0.239 (13) | 0.128 (8) | 0.365 (18) | 0.073 (8) | −0.085 (12) | 0.081 (10) |
Sb1—C121 | 2.077 (5) | C37—H37A | 0.96 |
Sb1—C111 | 2.087 (5) | C37—H37B | 0.96 |
Sb1—C131 | 2.095 (5) | C37—H37C | 0.96 |
Sb1—C17 | 2.099 (10) | C37—H37D | 0.96 |
Sb2—C27 | 2.077 (10) | C37—H37E | 0.96 |
Sb2—C211 | 2.081 (5) | C37—H37F | 0.96 |
Sb2—C221 | 2.083 (5) | C311—C312 | 1.39 |
Sb2—C231 | 2.089 (6) | C311—C316 | 1.39 |
Sb3—C331 | 2.082 (4) | C312—C313 | 1.39 |
Sb3—C311 | 2.088 (4) | C312—H312 | 0.93 |
Sb3—C37 | 2.090 (8) | C313—C314 | 1.39 |
Sb3—C321 | 2.093 (4) | C313—H313 | 0.93 |
Sb4—C431 | 2.070 (4) | C314—C315 | 1.39 |
Sb4—C421 | 2.085 (5) | C314—H314 | 0.93 |
Sb4—C47 | 2.096 (9) | C315—C316 | 1.39 |
Sb4—C411 | 2.099 (4) | C315—H315 | 0.93 |
C17—H17A | 0.96 | C316—H316 | 0.93 |
C17—H17B | 0.96 | C321—C322 | 1.39 |
C17—H17C | 0.96 | C321—C326 | 1.39 |
C17—H17D | 0.96 | C322—C323 | 1.39 |
C17—H17E | 0.96 | C322—H322 | 0.93 |
C17—H17F | 0.96 | C323—C324 | 1.39 |
C111—C112 | 1.39 | C323—H323 | 0.93 |
C111—C116 | 1.39 | C324—C325 | 1.39 |
C112—C113 | 1.39 | C324—H324 | 0.93 |
C112—H112 | 0.93 | C325—C326 | 1.39 |
C113—C114 | 1.39 | C325—H325 | 0.93 |
C113—H113 | 0.93 | C326—H326 | 0.93 |
C114—C115 | 1.39 | C331—C332 | 1.39 |
C114—H114 | 0.93 | C331—C336 | 1.39 |
C115—C116 | 1.39 | C332—C333 | 1.39 |
C115—H115 | 0.93 | C332—H332 | 0.93 |
C116—H116 | 0.93 | C333—C334 | 1.39 |
C121—C122 | 1.39 | C333—H333 | 0.93 |
C121—C126 | 1.39 | C334—C335 | 1.39 |
C122—C123 | 1.39 | C334—H334 | 0.93 |
C122—H122 | 0.93 | C335—C336 | 1.39 |
C123—C124 | 1.39 | C335—H335 | 0.93 |
C123—H123 | 0.93 | C336—H336 | 0.93 |
C124—C125 | 1.39 | C47—H47A | 0.96 |
C124—H124 | 0.93 | C47—H47B | 0.96 |
C125—C126 | 1.39 | C47—H47C | 0.96 |
C125—H125 | 0.93 | C47—H47D | 0.96 |
C126—H126 | 0.93 | C47—H47E | 0.96 |
C131—C132 | 1.39 | C47—H47F | 0.96 |
C131—C136 | 1.39 | C411—C412 | 1.39 |
C132—C133 | 1.39 | C411—C416 | 1.39 |
C132—H132 | 0.93 | C412—C413 | 1.39 |
C133—C134 | 1.39 | C412—H412 | 0.93 |
C133—H133 | 0.93 | C413—C414 | 1.39 |
C134—C135 | 1.39 | C413—H413 | 0.93 |
C134—H134 | 0.93 | C414—C415 | 1.39 |
C135—C136 | 1.39 | C414—H414 | 0.93 |
C135—H135 | 0.93 | C415—C416 | 1.39 |
C136—H136 | 0.93 | C415—H415 | 0.93 |
C27—H27A | 0.96 | C416—H416 | 0.93 |
C27—H27B | 0.96 | C421—C422 | 1.39 |
C27—H27C | 0.96 | C421—C426 | 1.39 |
C27—H27D | 0.96 | C422—C423 | 1.39 |
C27—H27E | 0.96 | C422—H422 | 0.93 |
C27—H27F | 0.96 | C423—C424 | 1.39 |
C211—C212 | 1.39 | C423—H423 | 0.93 |
C211—C216 | 1.39 | C424—C425 | 1.39 |
C212—C213 | 1.39 | C424—H424 | 0.93 |
C212—H212 | 0.93 | C425—C426 | 1.39 |
C213—C214 | 1.39 | C425—H425 | 0.93 |
C213—H213 | 0.93 | C426—H426 | 0.93 |
C214—C215 | 1.39 | C431—C432 | 1.39 |
C214—H214 | 0.93 | C431—C436 | 1.39 |
C215—C216 | 1.39 | C432—C433 | 1.39 |
C215—H215 | 0.93 | C432—H432 | 0.93 |
C216—H216 | 0.93 | C433—C434 | 1.39 |
C221—C222 | 1.39 | C433—H433 | 0.93 |
C221—C226 | 1.39 | C434—C435 | 1.39 |
C222—C223 | 1.39 | C434—H434 | 0.93 |
C222—H222 | 0.93 | C435—C436 | 1.39 |
C223—C224 | 1.39 | C435—H435 | 0.93 |
C223—H223 | 0.93 | C436—H436 | 0.93 |
C224—C225 | 1.39 | B1—F12 | 1.3257 |
C224—H224 | 0.93 | B1—F13 | 1.3274 |
C225—C226 | 1.39 | B1—F14 | 1.3298 |
C225—H225 | 0.93 | B1—F11 | 1.3326 |
C226—H226 | 0.93 | B2—F22 | 1.3306 |
C231—C232 | 1.39 | B2—F24 | 1.3316 |
C231—C236 | 1.39 | B2—F21 | 1.3318 |
C232—C233 | 1.39 | B2—F23 | 1.3354 |
C232—H232 | 0.93 | B3—F33 | 1.3249 |
C233—C234 | 1.39 | B3—F34 | 1.3269 |
C233—H233 | 0.93 | B3—F31 | 1.3275 |
C234—C235 | 1.39 | B3—F32 | 1.3311 |
C234—H234 | 0.93 | B4—F43 | 1.3261 |
C235—C236 | 1.39 | B4—F44 | 1.3266 |
C235—H235 | 0.93 | B4—F42 | 1.3316 |
C236—H236 | 0.93 | B4—F41 | 1.3317 |
C121—Sb1—C111 | 104.9 (3) | Sb3—C37—H37A | 109.5 |
C121—Sb1—C131 | 107.3 (3) | Sb3—C37—H37B | 109.5 |
C111—Sb1—C131 | 110.1 (3) | H37A—C37—H37B | 109.5 |
C121—Sb1—C17 | 119.0 (4) | Sb3—C37—H37C | 109.5 |
C111—Sb1—C17 | 109.4 (4) | H37A—C37—H37C | 109.5 |
C131—Sb1—C17 | 106.1 (3) | H37B—C37—H37C | 109.5 |
C27—Sb2—C211 | 112.3 (4) | Sb3—C37—H37D | 109.5 |
C27—Sb2—C221 | 111.9 (4) | H37A—C37—H37D | 141.1 |
C211—Sb2—C221 | 103.3 (3) | H37B—C37—H37D | 56.3 |
C27—Sb2—C231 | 112.7 (4) | H37C—C37—H37D | 56.3 |
C211—Sb2—C231 | 108.4 (3) | Sb3—C37—H37E | 109.5 |
C221—Sb2—C231 | 107.8 (3) | H37A—C37—H37E | 56.3 |
C331—Sb3—C311 | 106.1 (2) | H37B—C37—H37E | 141.1 |
C331—Sb3—C37 | 113.3 (3) | H37C—C37—H37E | 56.3 |
C311—Sb3—C37 | 113.4 (3) | H37D—C37—H37E | 109.5 |
C331—Sb3—C321 | 106.9 (2) | Sb3—C37—H37F | 109.5 |
C311—Sb3—C321 | 105.2 (2) | H37A—C37—H37F | 56.3 |
C37—Sb3—C321 | 111.5 (3) | H37B—C37—H37F | 56.3 |
C431—Sb4—C421 | 104.0 (2) | H37C—C37—H37F | 141.1 |
C431—Sb4—C47 | 116.0 (3) | H37D—C37—H37F | 109.5 |
C421—Sb4—C47 | 112.0 (3) | H37E—C37—H37F | 109.5 |
C431—Sb4—C411 | 108.7 (2) | C312—C311—C316 | 120 |
C421—Sb4—C411 | 107.4 (2) | C312—C311—Sb3 | 121.9 (3) |
C47—Sb4—C411 | 108.4 (3) | C316—C311—Sb3 | 118.1 (3) |
Sb1—C17—H17A | 109.5 | C311—C312—C313 | 120 |
Sb1—C17—H17B | 109.5 | C311—C312—H312 | 120 |
H17A—C17—H17B | 109.5 | C313—C312—H312 | 120 |
Sb1—C17—H17C | 109.5 | C314—C313—C312 | 120 |
H17A—C17—H17C | 109.5 | C314—C313—H313 | 120 |
H17B—C17—H17C | 109.5 | C312—C313—H313 | 120 |
Sb1—C17—H17D | 109.5 | C313—C314—C315 | 120 |
H17A—C17—H17D | 141.1 | C313—C314—H314 | 120 |
H17B—C17—H17D | 56.3 | C315—C314—H314 | 120 |
H17C—C17—H17D | 56.3 | C316—C315—C314 | 120 |
Sb1—C17—H17E | 109.5 | C316—C315—H315 | 120 |
H17A—C17—H17E | 56.3 | C314—C315—H315 | 120 |
H17B—C17—H17E | 141.1 | C315—C316—C311 | 120 |
H17C—C17—H17E | 56.3 | C315—C316—H316 | 120 |
H17D—C17—H17E | 109.5 | C311—C316—H316 | 120 |
Sb1—C17—H17F | 109.5 | C322—C321—C326 | 120 |
H17A—C17—H17F | 56.3 | C322—C321—Sb3 | 119.1 (3) |
H17B—C17—H17F | 56.3 | C326—C321—Sb3 | 120.8 (3) |
H17C—C17—H17F | 141.1 | C323—C322—C321 | 120 |
H17D—C17—H17F | 109.5 | C323—C322—H322 | 120 |
H17E—C17—H17F | 109.5 | C321—C322—H322 | 120 |
C112—C111—C116 | 120 | C322—C323—C324 | 120 |
C112—C111—Sb1 | 120.7 (4) | C322—C323—H323 | 120 |
C116—C111—Sb1 | 119.1 (4) | C324—C323—H323 | 120 |
C111—C112—C113 | 120 | C323—C324—C325 | 120 |
C111—C112—H112 | 120 | C323—C324—H324 | 120 |
C113—C112—H112 | 120 | C325—C324—H324 | 120 |
C112—C113—C114 | 120 | C326—C325—C324 | 120 |
C112—C113—H113 | 120 | C326—C325—H325 | 120 |
C114—C113—H113 | 120 | C324—C325—H325 | 120 |
C115—C114—C113 | 120 | C325—C326—C321 | 120 |
C115—C114—H114 | 120 | C325—C326—H326 | 120 |
C113—C114—H114 | 120 | C321—C326—H326 | 120 |
C114—C115—C116 | 120 | C332—C331—C336 | 120 |
C114—C115—H115 | 120 | C332—C331—Sb3 | 122.0 (3) |
C116—C115—H115 | 120 | C336—C331—Sb3 | 117.9 (3) |
C115—C116—C111 | 120 | C333—C332—C331 | 120 |
C115—C116—H116 | 120 | C333—C332—H332 | 120 |
C111—C116—H116 | 120 | C331—C332—H332 | 120 |
C122—C121—C126 | 120 | C334—C333—C332 | 120 |
C122—C121—Sb1 | 119.0 (4) | C334—C333—H333 | 120 |
C126—C121—Sb1 | 121.0 (4) | C332—C333—H333 | 120 |
C123—C122—C121 | 120 | C333—C334—C335 | 120 |
C123—C122—H122 | 120 | C333—C334—H334 | 120 |
C121—C122—H122 | 120 | C335—C334—H334 | 120 |
C124—C123—C122 | 120 | C334—C335—C336 | 120 |
C124—C123—H123 | 120 | C334—C335—H335 | 120 |
C122—C123—H123 | 120 | C336—C335—H335 | 120 |
C123—C124—C125 | 120 | C335—C336—C331 | 120 |
C123—C124—H124 | 120 | C335—C336—H336 | 120 |
C125—C124—H124 | 120 | C331—C336—H336 | 120 |
C126—C125—C124 | 120 | Sb4—C47—H47A | 109.5 |
C126—C125—H125 | 120 | Sb4—C47—H47B | 109.5 |
C124—C125—H125 | 120 | H47A—C47—H47B | 109.5 |
C125—C126—C121 | 120 | Sb4—C47—H47C | 109.5 |
C125—C126—H126 | 120 | H47A—C47—H47C | 109.5 |
C121—C126—H126 | 120 | H47B—C47—H47C | 109.5 |
C132—C131—C136 | 120 | Sb4—C47—H47D | 109.5 |
C132—C131—Sb1 | 120.8 (4) | H47A—C47—H47D | 141.1 |
C136—C131—Sb1 | 119.2 (4) | H47B—C47—H47D | 56.3 |
C133—C132—C131 | 120 | H47C—C47—H47D | 56.3 |
C133—C132—H132 | 120 | Sb4—C47—H47E | 109.5 |
C131—C132—H132 | 120 | H47A—C47—H47E | 56.3 |
C134—C133—C132 | 120 | H47B—C47—H47E | 141.1 |
C134—C133—H133 | 120 | H47C—C47—H47E | 56.3 |
C132—C133—H133 | 120 | H47D—C47—H47E | 109.5 |
C133—C134—C135 | 120 | Sb4—C47—H47F | 109.5 |
C133—C134—H134 | 120 | H47A—C47—H47F | 56.3 |
C135—C134—H134 | 120 | H47B—C47—H47F | 56.3 |
C136—C135—C134 | 120 | H47C—C47—H47F | 141.1 |
C136—C135—H135 | 120 | H47D—C47—H47F | 109.5 |
C134—C135—H135 | 120 | H47E—C47—H47F | 109.5 |
C135—C136—C131 | 120 | C412—C411—C416 | 120 |
C135—C136—H136 | 120 | C412—C411—Sb4 | 119.8 (3) |
C131—C136—H136 | 120 | C416—C411—Sb4 | 120.2 (3) |
Sb2—C27—H27A | 109.5 | C413—C412—C411 | 120 |
Sb2—C27—H27B | 109.5 | C413—C412—H412 | 120 |
H27A—C27—H27B | 109.5 | C411—C412—H412 | 120 |
Sb2—C27—H27C | 109.5 | C412—C413—C414 | 120 |
H27A—C27—H27C | 109.5 | C412—C413—H413 | 120 |
H27B—C27—H27C | 109.5 | C414—C413—H413 | 120 |
Sb2—C27—H27D | 109.5 | C413—C414—C415 | 120 |
H27A—C27—H27D | 141.1 | C413—C414—H414 | 120 |
H27B—C27—H27D | 56.3 | C415—C414—H414 | 120 |
H27C—C27—H27D | 56.3 | C416—C415—C414 | 120 |
Sb2—C27—H27E | 109.5 | C416—C415—H415 | 120 |
H27A—C27—H27E | 56.3 | C414—C415—H415 | 120 |
H27B—C27—H27E | 141.1 | C415—C416—C411 | 120 |
H27C—C27—H27E | 56.3 | C415—C416—H416 | 120 |
H27D—C27—H27E | 109.5 | C411—C416—H416 | 120 |
Sb2—C27—H27F | 109.5 | C422—C421—C426 | 120 |
H27A—C27—H27F | 56.3 | C422—C421—Sb4 | 121.9 (4) |
H27B—C27—H27F | 56.3 | C426—C421—Sb4 | 118.1 (4) |
H27C—C27—H27F | 141.1 | C423—C422—C421 | 120 |
H27D—C27—H27F | 109.5 | C423—C422—H422 | 120 |
H27E—C27—H27F | 109.5 | C421—C422—H422 | 120 |
C212—C211—C216 | 120 | C422—C423—C424 | 120 |
C212—C211—Sb2 | 118.2 (5) | C422—C423—H423 | 120 |
C216—C211—Sb2 | 121.7 (5) | C424—C423—H423 | 120 |
C211—C212—C213 | 120 | C425—C424—C423 | 120 |
C211—C212—H212 | 120 | C425—C424—H424 | 120 |
C213—C212—H212 | 120 | C423—C424—H424 | 120 |
C212—C213—C214 | 120 | C426—C425—C424 | 120 |
C212—C213—H213 | 120 | C426—C425—H425 | 120 |
C214—C213—H213 | 120 | C424—C425—H425 | 120 |
C215—C214—C213 | 120 | C425—C426—C421 | 120 |
C215—C214—H214 | 120 | C425—C426—H426 | 120 |
C213—C214—H214 | 120 | C421—C426—H426 | 120 |
C214—C215—C216 | 120 | C432—C431—C436 | 120 |
C214—C215—H215 | 120 | C432—C431—Sb4 | 119.3 (3) |
C216—C215—H215 | 120 | C436—C431—Sb4 | 120.7 (3) |
C215—C216—C211 | 120 | C433—C432—C431 | 120 |
C215—C216—H216 | 120 | C433—C432—H432 | 120 |
C211—C216—H216 | 120 | C431—C432—H432 | 120 |
C222—C221—C226 | 120 | C432—C433—C434 | 120 |
C222—C221—Sb2 | 122.9 (4) | C432—C433—H433 | 120 |
C226—C221—Sb2 | 117.1 (4) | C434—C433—H433 | 120 |
C221—C222—C223 | 120 | C435—C434—C433 | 120 |
C221—C222—H222 | 120 | C435—C434—H434 | 120 |
C223—C222—H222 | 120 | C433—C434—H434 | 120 |
C224—C223—C222 | 120 | C436—C435—C434 | 120 |
C224—C223—H223 | 120 | C436—C435—H435 | 120 |
C222—C223—H223 | 120 | C434—C435—H435 | 120 |
C223—C224—C225 | 120 | C435—C436—C431 | 120 |
C223—C224—H224 | 120 | C435—C436—H436 | 120 |
C225—C224—H224 | 120 | C431—C436—H436 | 120 |
C226—C225—C224 | 120 | F12—B1—F13 | 109.8 |
C226—C225—H225 | 120 | F12—B1—F14 | 109.4 |
C224—C225—H225 | 120 | F13—B1—F14 | 109.2 |
C225—C226—C221 | 120 | F12—B1—F11 | 109.8 |
C225—C226—H226 | 120 | F13—B1—F11 | 109.4 |
C221—C226—H226 | 120 | F14—B1—F11 | 109.2 |
C232—C231—C236 | 120 | F22—B2—F24 | 109.3 |
C232—C231—Sb2 | 121.7 (5) | F22—B2—F21 | 110.4 |
C236—C231—Sb2 | 118.2 (5) | F24—B2—F21 | 109.4 |
C233—C232—C231 | 120 | F22—B2—F23 | 109.0 |
C233—C232—H232 | 120 | F24—B2—F23 | 109.5 |
C231—C232—H232 | 120 | F21—B2—F23 | 109.3 |
C234—C233—C232 | 120 | F33—B3—F34 | 109.6 |
C234—C233—H233 | 120 | F33—B3—F31 | 110.1 |
C232—C233—H233 | 120 | F34—B3—F31 | 109.6 |
C233—C234—C235 | 120 | F33—B3—F32 | 109.3 |
C233—C234—H234 | 120 | F34—B3—F32 | 108.8 |
C235—C234—H234 | 120 | F31—B3—F32 | 109.5 |
C236—C235—C234 | 120 | F43—B4—F44 | 109.5 |
C236—C235—H235 | 120 | F43—B4—F42 | 109.3 |
C234—C235—H235 | 120 | F44—B4—F42 | 109.3 |
C235—C236—C231 | 120 | F43—B4—F41 | 109.5 |
C235—C236—H236 | 120 | F44—B4—F41 | 109.3 |
C231—C236—H236 | 120 | F42—B4—F41 | 109.9 |
C121—Sb1—C111—C112 | −109.2 (4) | C331—Sb3—C311—C312 | −98.3 (4) |
C131—Sb1—C111—C112 | 135.7 (4) | C37—Sb3—C311—C312 | 26.6 (5) |
C17—Sb1—C111—C112 | 19.5 (5) | C321—Sb3—C311—C312 | 148.6 (3) |
C121—Sb1—C111—C116 | 65.9 (4) | C331—Sb3—C311—C316 | 81.9 (4) |
C131—Sb1—C111—C116 | −49.2 (4) | C37—Sb3—C311—C316 | −153.2 (4) |
C17—Sb1—C111—C116 | −165.3 (4) | C321—Sb3—C311—C316 | −31.2 (4) |
C116—C111—C112—C113 | 0.0 | C316—C311—C312—C313 | 0.0 |
Sb1—C111—C112—C113 | 175.1 (5) | Sb3—C311—C312—C313 | −179.8 (4) |
C111—C112—C113—C114 | 0.0 | C311—C312—C313—C314 | 0.0 |
C112—C113—C114—C115 | 0.0 | C312—C313—C314—C315 | 0.0 |
C113—C114—C115—C116 | 0.0 | C313—C314—C315—C316 | 0.0 |
C114—C115—C116—C111 | 0.0 | C314—C315—C316—C311 | 0.0 |
C112—C111—C116—C115 | 0.0 | C312—C311—C316—C315 | 0.0 |
Sb1—C111—C116—C115 | −175.1 (4) | Sb3—C311—C316—C315 | 179.8 (4) |
C111—Sb1—C121—C122 | 21.8 (5) | C331—Sb3—C321—C322 | −162.2 (3) |
C131—Sb1—C121—C122 | 138.8 (4) | C311—Sb3—C321—C322 | −49.7 (4) |
C17—Sb1—C121—C122 | −101.0 (5) | C37—Sb3—C321—C322 | 73.6 (4) |
C111—Sb1—C121—C126 | −156.8 (4) | C331—Sb3—C321—C326 | 21.9 (4) |
C131—Sb1—C121—C126 | −39.8 (5) | C311—Sb3—C321—C326 | 134.4 (3) |
C17—Sb1—C121—C126 | 80.4 (5) | C37—Sb3—C321—C326 | −102.4 (4) |
C126—C121—C122—C123 | 0.0 | C326—C321—C322—C323 | 0.0 |
Sb1—C121—C122—C123 | −178.6 (5) | Sb3—C321—C322—C323 | −176.0 (4) |
C121—C122—C123—C124 | 0.0 | C321—C322—C323—C324 | 0.0 |
C122—C123—C124—C125 | 0.0 | C322—C323—C324—C325 | 0.0 |
C123—C124—C125—C126 | 0.0 | C323—C324—C325—C326 | 0.0 |
C124—C125—C126—C121 | 0.0 | C324—C325—C326—C321 | 0.0 |
C122—C121—C126—C125 | 0.0 | C322—C321—C326—C325 | 0.0 |
Sb1—C121—C126—C125 | 178.6 (5) | Sb3—C321—C326—C325 | 175.9 (4) |
C121—Sb1—C131—C132 | −44.5 (4) | C311—Sb3—C331—C332 | 125.0 (3) |
C111—Sb1—C131—C132 | 69.1 (4) | C37—Sb3—C331—C332 | −0.1 (4) |
C17—Sb1—C131—C132 | −172.6 (5) | C321—Sb3—C331—C332 | −123.2 (3) |
C121—Sb1—C131—C136 | 135.5 (4) | C311—Sb3—C331—C336 | −51.3 (3) |
C111—Sb1—C131—C136 | −110.9 (4) | C37—Sb3—C331—C336 | −176.3 (4) |
C17—Sb1—C131—C136 | 7.4 (5) | C321—Sb3—C331—C336 | 60.6 (3) |
C136—C131—C132—C133 | 0.0 | C336—C331—C332—C333 | 0.0 |
Sb1—C131—C132—C133 | −180.0 (5) | Sb3—C331—C332—C333 | −176.2 (4) |
C131—C132—C133—C134 | 0.0 | C331—C332—C333—C334 | 0.0 |
C132—C133—C134—C135 | 0.0 | C332—C333—C334—C335 | 0.0 |
C133—C134—C135—C136 | 0.0 | C333—C334—C335—C336 | 0.0 |
C134—C135—C136—C131 | 0.0 | C334—C335—C336—C331 | 0.0 |
C132—C131—C136—C135 | 0.0 | C332—C331—C336—C335 | 0.0 |
Sb1—C131—C136—C135 | 180.0 (4) | Sb3—C331—C336—C335 | 176.3 (4) |
C27—Sb2—C211—C212 | −61.4 (5) | C431—Sb4—C411—C412 | −77.6 (4) |
C221—Sb2—C211—C212 | 59.4 (5) | C421—Sb4—C411—C412 | 34.3 (4) |
C231—Sb2—C211—C212 | 173.5 (5) | C47—Sb4—C411—C412 | 155.5 (4) |
C27—Sb2—C211—C216 | 122.1 (5) | C431—Sb4—C411—C416 | 103.7 (4) |
C221—Sb2—C211—C216 | −117.1 (5) | C421—Sb4—C411—C416 | −144.4 (4) |
C231—Sb2—C211—C216 | −3.0 (5) | C47—Sb4—C411—C416 | −23.2 (5) |
C216—C211—C212—C213 | 0.0 | C416—C411—C412—C413 | 0.0 |
Sb2—C211—C212—C213 | −176.6 (5) | Sb4—C411—C412—C413 | −178.7 (4) |
C211—C212—C213—C214 | 0.0 | C411—C412—C413—C414 | 0.0 |
C212—C213—C214—C215 | 0.0 | C412—C413—C414—C415 | 0.0 |
C213—C214—C215—C216 | 0.0 | C413—C414—C415—C416 | 0.0 |
C214—C215—C216—C211 | 0.0 | C414—C415—C416—C411 | 0.0 |
C212—C211—C216—C215 | 0.0 | C412—C411—C416—C415 | 0.0 |
Sb2—C211—C216—C215 | 176.5 (5) | Sb4—C411—C416—C415 | 178.7 (4) |
C27—Sb2—C221—C222 | −20.5 (5) | C431—Sb4—C421—C422 | −133.0 (3) |
C211—Sb2—C221—C222 | −141.5 (4) | C47—Sb4—C421—C422 | −6.9 (5) |
C231—Sb2—C221—C222 | 103.9 (5) | C411—Sb4—C421—C422 | 112.0 (4) |
C27—Sb2—C221—C226 | 161.3 (5) | C431—Sb4—C421—C426 | 45.8 (4) |
C211—Sb2—C221—C226 | 40.3 (4) | C47—Sb4—C421—C426 | 171.9 (4) |
C231—Sb2—C221—C226 | −74.3 (5) | C411—Sb4—C421—C426 | −69.3 (3) |
C226—C221—C222—C223 | 0.0 | C426—C421—C422—C423 | 0.0 |
Sb2—C221—C222—C223 | −178.2 (5) | Sb4—C421—C422—C423 | 178.8 (4) |
C221—C222—C223—C224 | 0.0 | C421—C422—C423—C424 | 0.0 |
C222—C223—C224—C225 | 0.0 | C422—C423—C424—C425 | 0.0 |
C223—C224—C225—C226 | 0.0 | C423—C424—C425—C426 | 0.0 |
C224—C225—C226—C221 | 0.0 | C424—C425—C426—C421 | 0.0 |
C222—C221—C226—C225 | 0.0 | C422—C421—C426—C425 | 0.0 |
Sb2—C221—C226—C225 | 178.3 (5) | Sb4—C421—C426—C425 | −178.8 (4) |
C27—Sb2—C231—C232 | −66.5 (7) | C421—Sb4—C431—C432 | 44.3 (4) |
C211—Sb2—C231—C232 | 58.4 (7) | C47—Sb4—C431—C432 | −79.2 (5) |
C221—Sb2—C231—C232 | 169.5 (6) | C411—Sb4—C431—C432 | 158.5 (3) |
C27—Sb2—C231—C236 | 116.0 (6) | C421—Sb4—C431—C436 | −136.5 (4) |
C211—Sb2—C231—C236 | −119.1 (6) | C47—Sb4—C431—C436 | 100.0 (5) |
C221—Sb2—C231—C236 | −8.0 (6) | C411—Sb4—C431—C436 | −22.3 (4) |
C236—C231—C232—C233 | 0.0 | C436—C431—C432—C433 | 0.0 |
Sb2—C231—C232—C233 | −177.4 (7) | Sb4—C431—C432—C433 | 179.2 (4) |
C231—C232—C233—C234 | 0.0 | C431—C432—C433—C434 | 0.0 |
C232—C233—C234—C235 | 0.0 | C432—C433—C434—C435 | 0.0 |
C233—C234—C235—C236 | 0.0 | C433—C434—C435—C436 | 0.0 |
C234—C235—C236—C231 | 0.0 | C434—C435—C436—C431 | 0.0 |
C232—C231—C236—C235 | 0.0 | C432—C431—C436—C435 | 0.0 |
Sb2—C231—C236—C235 | 177.5 (6) | Sb4—C431—C436—C435 | −179.2 (4) |
Experimental details
Crystal data | |
Chemical formula | [Sb(CH3)(C6H5)3]BF4 |
Mr | 454.90 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 12.874 (4), 13.760 (5), 24.974 (7) |
α, β, γ (°) | 98.82 (3), 93.97 (2), 117.80 (3) |
V (Å3) | 3817 (2) |
Z | 8 |
Radiation type | Mo Kα |
µ (mm−1) | 1.48 |
Crystal size (mm) | 0.42 × 0.28 × 0.26 |
Data collection | |
Diffractometer | Enraf-Nonius CAD-4 diffractometer |
Absorption correction | Gaussian (NRCVAX; Gabe et al., 1989) |
Tmin, Tmax | 0.689, 0.715 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 14181, 14181, 8121 |
Rint | ? |
(sin θ/λ)max (Å−1) | 0.605 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.057, 0.181, 1.03 |
No. of reflections | 14181 |
No. of parameters | 722 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.15, −0.78 |
Computer programs: CAD-4-PC Software (Enraf-Nonius, 1992), SET4 and CELDIM in CAD-4-PC Software, DATRD2 in NRCVAX (Gabe et al., 1989), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), NRCVAX, SHELXL97 and WORDPERFECT macro PREP8 (Ferguson, 1998).
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Examination of the structure with PLATON (Spek, 2000) showed that there were no solvent-accessible voids in the crystal lattice.