Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S010827019901598X/qa0190sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S010827019901598X/qa0190Isup2.hkl |
CCDC reference: 140851
Tetrakis(2-methyl-2-phenylpropyl)stannane was prepared from the Gringnard reagent, from PhCMe2CH2Cl and Mg in Et2O and SnCl4 in benzene. It was recrystallized as colourless crystals from petroleum ether (60–80°C) and had a melting point of 94–96°C.
Molecule (1) crystallized in the monoclinic system; space group P21/c from the systematic absences. H atoms were treated as riding atoms with C—H 0.90–0.98 Å.
Data collection: KappaCCD Server Software (Nonius, 1997); cell refinement: DENZO (Otwinowski & Minor, 1997); data reduction: DENZO (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997b); software used to prepare material for publication: SHELXL97 and WORDPERFECT macro PRPKAPPA (Ferguson, 1999).
[Sn(C10H13)4] | F(000) = 1368 |
Mr = 651.51 | Dx = 1.255 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 13.9224 (4) Å | Cell parameters from 7414 reflections |
b = 9.9590 (2) Å | θ = 1.5–27.5° |
c = 25.6952 (6) Å | µ = 0.77 mm−1 |
β = 104.5178 (14)° | T = 150 K |
V = 3448.96 (15) Å3 | Lath, colourless |
Z = 4 | 0.30 × 0.10 × 0.03 mm |
KappaCCD diffractometer | 7414 independent reflections |
Radiation source: fine-focus sealed X-ray tube | 5147 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.064 |
ϕ scans and ω scans with κ offsets | θmax = 27.5°, θmin = 1.5° |
Absorption correction: multi-scan (SORTAV; Blessing, 1995, 1997) | h = −17→17 |
Tmin = 0.927, Tmax = 0.973 | k = −12→12 |
24777 measured reflections | l = −30→31 |
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)] = 0.038 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.088 | H-atom parameters constrained |
S = 0.99 | w = 1/[σ2(Fo2) + (0.0265P)2 + 1.4792P] where P = (Fo2 + 2Fc2)/3 |
7414 reflections | (Δ/σ)max = 0.004 |
378 parameters | Δρmax = 0.83 e Å−3 |
0 restraints | Δρmin = −0.74 e Å−3 |
[Sn(C10H13)4] | V = 3448.96 (15) Å3 |
Mr = 651.51 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 13.9224 (4) Å | µ = 0.77 mm−1 |
b = 9.9590 (2) Å | T = 150 K |
c = 25.6952 (6) Å | 0.30 × 0.10 × 0.03 mm |
β = 104.5178 (14)° |
KappaCCD diffractometer | 7414 independent reflections |
Absorption correction: multi-scan (SORTAV; Blessing, 1995, 1997) | 5147 reflections with I > 2σ(I) |
Tmin = 0.927, Tmax = 0.973 | Rint = 0.064 |
24777 measured reflections |
R[F2 > 2σ(F2)] = 0.038 | 0 restraints |
wR(F2) = 0.088 | H-atom parameters constrained |
S = 0.99 | Δρmax = 0.83 e Å−3 |
7414 reflections | Δρmin = −0.74 e Å−3 |
378 parameters |
Experimental. KappaCCD diffractometer using the following programs. Collect: Data collection software, Hooft (1998) [Hooft, R., Nonius B·V., (1998). Delft, The Netherlands] is a graphical user interface written by Enraf–Nonius which encompasses the following programs. DENZO (Otwinowski and Minor, 1997) and indexing and data collection software package and a scaling package, SCALEPACK both of which programs are produced by the company HKL. Absorption corrections are performed by the SORTAV package (Blessing, 1995, 1997). High redundancy data were used in the scaling program hence the 'multi-scan' code word was used. No transmission coefficients are available from the program (only scale factors for each frame). The scale factors in the experimental table are calculated from the 'size' command in the SHELXL97 input file. Low temperature data is collected using an Oxford Cryosystems cryostream, Cosier and Glazer (1986) [Cosier, J. and Glazer, A·M., J. Appl. Cryst. (1986), 19, 105–107]. |
x | y | z | Uiso*/Ueq | ||
Sn1 | 0.228713 (15) | 0.29327 (2) | 0.112097 (8) | 0.02055 (8) | |
C1A | 0.3145 (2) | 0.2547 (3) | 0.19360 (13) | 0.0266 (8) | |
C2A | 0.3860 (2) | 0.1341 (3) | 0.20645 (13) | 0.0273 (8) | |
C21A | 0.4418 (3) | 0.1423 (4) | 0.26652 (13) | 0.0368 (9) | |
C22A | 0.3263 (3) | 0.0035 (3) | 0.19885 (15) | 0.0418 (10) | |
C11A | 0.4635 (2) | 0.1369 (3) | 0.17340 (13) | 0.0277 (8) | |
C12A | 0.4942 (3) | 0.0236 (4) | 0.15103 (16) | 0.0487 (11) | |
C13A | 0.5680 (3) | 0.0304 (6) | 0.12299 (19) | 0.0722 (16) | |
C14A | 0.6111 (3) | 0.1505 (7) | 0.11730 (17) | 0.0682 (15) | |
C15A | 0.5823 (3) | 0.2638 (5) | 0.13862 (17) | 0.0549 (12) | |
C16A | 0.5094 (3) | 0.2571 (4) | 0.16642 (15) | 0.0375 (9) | |
C1B | 0.2386 (2) | 0.1222 (3) | 0.06066 (12) | 0.0234 (7) | |
C2B | 0.2122 (2) | 0.1386 (3) | −0.00105 (12) | 0.0248 (7) | |
C21B | 0.1036 (2) | 0.1818 (3) | −0.02118 (13) | 0.0320 (8) | |
C22B | 0.2232 (3) | −0.0002 (3) | −0.02649 (14) | 0.0330 (8) | |
C11B | 0.2834 (2) | 0.2357 (3) | −0.01873 (12) | 0.0259 (7) | |
C12B | 0.3851 (3) | 0.2169 (4) | −0.00005 (14) | 0.0345 (8) | |
C13B | 0.4518 (3) | 0.2996 (4) | −0.01619 (16) | 0.0478 (10) | |
C14B | 0.4184 (3) | 0.4043 (4) | −0.05149 (15) | 0.0504 (11) | |
C15B | 0.3180 (3) | 0.4247 (4) | −0.06990 (14) | 0.0425 (10) | |
C16B | 0.2513 (3) | 0.3415 (3) | −0.05390 (13) | 0.0335 (9) | |
C1C | 0.2971 (2) | 0.4691 (3) | 0.08648 (13) | 0.0249 (7) | |
C2C | 0.2438 (2) | 0.6066 (3) | 0.08068 (12) | 0.0246 (7) | |
C21C | 0.3163 (3) | 0.7144 (3) | 0.07046 (14) | 0.0362 (9) | |
C22C | 0.1540 (3) | 0.6015 (4) | 0.03161 (13) | 0.0382 (9) | |
C11C | 0.2137 (2) | 0.6470 (3) | 0.13183 (12) | 0.0218 (7) | |
C12C | 0.2792 (3) | 0.6268 (3) | 0.18195 (13) | 0.0307 (8) | |
C13C | 0.2570 (3) | 0.6695 (4) | 0.22865 (15) | 0.0439 (10) | |
C14C | 0.1695 (4) | 0.7335 (4) | 0.22699 (17) | 0.0503 (12) | |
C15C | 0.1027 (3) | 0.7544 (4) | 0.17833 (19) | 0.0489 (11) | |
C16C | 0.1252 (3) | 0.7116 (3) | 0.13118 (14) | 0.0332 (8) | |
C1D | 0.0742 (2) | 0.3340 (3) | 0.10973 (13) | 0.0244 (7) | |
C2D | 0.0191 (2) | 0.2460 (3) | 0.14255 (13) | 0.0251 (7) | |
C21D | −0.0897 (2) | 0.2939 (4) | 0.13127 (13) | 0.0351 (8) | |
C22D | 0.0186 (3) | 0.0998 (3) | 0.12357 (13) | 0.0332 (8) | |
C11D | 0.0673 (2) | 0.2595 (3) | 0.20301 (12) | 0.0234 (7) | |
C12D | 0.0885 (2) | 0.3862 (3) | 0.22603 (12) | 0.0283 (8) | |
C13D | 0.1371 (3) | 0.4013 (4) | 0.27984 (13) | 0.0346 (9) | |
C14D | 0.1651 (3) | 0.2905 (4) | 0.31226 (14) | 0.0388 (9) | |
C15D | 0.1415 (3) | 0.1654 (4) | 0.29076 (14) | 0.0382 (9) | |
C16D | 0.0927 (2) | 0.1494 (4) | 0.23682 (13) | 0.0320 (8) | |
H1A1 | 0.3533 | 0.3347 | 0.2058 | 0.032* | |
H1A2 | 0.2677 | 0.2456 | 0.2157 | 0.032* | |
H21A | 0.4801 | 0.2235 | 0.2729 | 0.055* | |
H21B | 0.4852 | 0.0664 | 0.2758 | 0.055* | |
H21C | 0.3948 | 0.1421 | 0.2882 | 0.055* | |
H22A | 0.2753 | 0.0091 | 0.2179 | 0.063* | |
H22B | 0.3696 | −0.0703 | 0.2126 | 0.063* | |
H22C | 0.2966 | −0.0103 | 0.1613 | 0.063* | |
H12A | 0.4652 | −0.0588 | 0.1547 | 0.058* | |
H13A | 0.5876 | −0.0470 | 0.1082 | 0.087* | |
H14A | 0.6604 | 0.1549 | 0.0987 | 0.082* | |
H15A | 0.6116 | 0.3457 | 0.1345 | 0.066* | |
H16A | 0.4905 | 0.3354 | 0.1809 | 0.045* | |
H1B1 | 0.3061 | 0.0888 | 0.0715 | 0.028* | |
H1B2 | 0.1962 | 0.0521 | 0.0688 | 0.028* | |
H21D | 0.0961 | 0.2720 | −0.0096 | 0.048* | |
H21E | 0.0623 | 0.1225 | −0.0068 | 0.048* | |
H21F | 0.0844 | 0.1780 | −0.0597 | 0.048* | |
H22D | 0.2066 | 0.0080 | −0.0649 | 0.049* | |
H22E | 0.1794 | −0.0636 | −0.0162 | 0.049* | |
H22F | 0.2904 | −0.0309 | −0.0140 | 0.049* | |
H12B | 0.4088 | 0.1472 | 0.0238 | 0.041* | |
H13B | 0.5195 | 0.2850 | −0.0033 | 0.057* | |
H14B | 0.4631 | 0.4599 | −0.0626 | 0.061* | |
H15B | 0.2946 | 0.4952 | −0.0934 | 0.051* | |
H16B | 0.1836 | 0.3567 | −0.0669 | 0.040* | |
H1C1 | 0.3612 | 0.4810 | 0.1117 | 0.030* | |
H1C2 | 0.3097 | 0.4480 | 0.0519 | 0.030* | |
H21G | 0.3338 | 0.6951 | 0.0374 | 0.054* | |
H21H | 0.3750 | 0.7145 | 0.0996 | 0.054* | |
H21I | 0.2851 | 0.8010 | 0.0680 | 0.054* | |
H22G | 0.1045 | 0.5426 | 0.0390 | 0.057* | |
H22H | 0.1747 | 0.5688 | 0.0010 | 0.057* | |
H22I | 0.1267 | 0.6900 | 0.0242 | 0.057* | |
H12C | 0.3392 | 0.5836 | 0.1840 | 0.037* | |
H13C | 0.3020 | 0.6546 | 0.2616 | 0.053* | |
H14C | 0.1552 | 0.7628 | 0.2586 | 0.060* | |
H15C | 0.0427 | 0.7970 | 0.1769 | 0.059* | |
H16C | 0.0797 | 0.7267 | 0.0984 | 0.040* | |
H1D1 | 0.0704 | 0.4262 | 0.1213 | 0.029* | |
H1D2 | 0.0371 | 0.3294 | 0.0724 | 0.029* | |
H21J | −0.1205 | 0.2863 | 0.0935 | 0.053* | |
H21K | −0.0913 | 0.3859 | 0.1422 | 0.053* | |
H21L | −0.1249 | 0.2394 | 0.1511 | 0.053* | |
H22J | 0.0852 | 0.0654 | 0.1327 | 0.050* | |
H22K | −0.0076 | 0.0960 | 0.0853 | 0.050* | |
H22L | −0.0220 | 0.0466 | 0.1408 | 0.050* | |
H12D | 0.0697 | 0.4622 | 0.2049 | 0.034* | |
H13D | 0.1508 | 0.4870 | 0.2942 | 0.041* | |
H14D | 0.1994 | 0.3005 | 0.3481 | 0.047* | |
H15D | 0.1583 | 0.0901 | 0.3125 | 0.046* | |
H16D | 0.0769 | 0.0634 | 0.2232 | 0.038* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Sn1 | 0.02045 (12) | 0.02029 (12) | 0.02082 (12) | −0.00004 (10) | 0.00504 (8) | 0.00072 (10) |
C1A | 0.0189 (17) | 0.0298 (17) | 0.0297 (19) | 0.0015 (14) | 0.0036 (14) | 0.0068 (14) |
C2A | 0.0216 (18) | 0.0250 (18) | 0.0318 (19) | −0.0031 (14) | 0.0001 (14) | 0.0044 (15) |
C21A | 0.029 (2) | 0.042 (2) | 0.035 (2) | 0.0003 (17) | 0.0006 (16) | 0.0104 (17) |
C22A | 0.038 (2) | 0.029 (2) | 0.053 (3) | −0.0062 (17) | 0.0004 (18) | 0.0155 (17) |
C11A | 0.0212 (18) | 0.0296 (19) | 0.0281 (19) | 0.0055 (15) | −0.0018 (14) | 0.0023 (15) |
C12A | 0.037 (2) | 0.044 (2) | 0.059 (3) | 0.0097 (19) | 0.000 (2) | −0.015 (2) |
C13A | 0.047 (3) | 0.103 (4) | 0.063 (3) | 0.032 (3) | 0.006 (2) | −0.034 (3) |
C14A | 0.038 (3) | 0.130 (5) | 0.037 (3) | 0.020 (3) | 0.010 (2) | 0.007 (3) |
C15A | 0.036 (2) | 0.079 (3) | 0.051 (3) | 0.006 (2) | 0.013 (2) | 0.027 (2) |
C16A | 0.031 (2) | 0.043 (2) | 0.040 (2) | 0.0057 (17) | 0.0106 (16) | 0.0136 (17) |
C1B | 0.0264 (18) | 0.0217 (16) | 0.0232 (17) | −0.0001 (14) | 0.0082 (13) | −0.0014 (14) |
C2B | 0.0235 (18) | 0.0260 (17) | 0.0232 (17) | 0.0020 (14) | 0.0028 (13) | −0.0015 (14) |
C21B | 0.0289 (19) | 0.037 (2) | 0.0275 (19) | −0.0012 (16) | 0.0025 (14) | −0.0012 (15) |
C22B | 0.036 (2) | 0.0276 (19) | 0.033 (2) | −0.0010 (16) | 0.0050 (16) | −0.0093 (15) |
C11B | 0.0281 (19) | 0.0290 (18) | 0.0212 (17) | −0.0011 (15) | 0.0073 (13) | −0.0081 (14) |
C12B | 0.032 (2) | 0.041 (2) | 0.032 (2) | 0.0034 (18) | 0.0109 (15) | 0.0046 (17) |
C13B | 0.033 (2) | 0.068 (3) | 0.043 (2) | −0.011 (2) | 0.0120 (17) | 0.002 (2) |
C14B | 0.054 (3) | 0.063 (3) | 0.037 (2) | −0.026 (2) | 0.015 (2) | 0.001 (2) |
C15B | 0.056 (3) | 0.043 (2) | 0.026 (2) | −0.014 (2) | 0.0060 (18) | 0.0060 (17) |
C16B | 0.036 (2) | 0.038 (2) | 0.0253 (19) | −0.0048 (17) | 0.0039 (15) | −0.0028 (15) |
C1C | 0.0252 (18) | 0.0234 (17) | 0.0290 (19) | −0.0021 (14) | 0.0119 (14) | 0.0006 (14) |
C2C | 0.0273 (18) | 0.0208 (16) | 0.0267 (18) | −0.0011 (14) | 0.0084 (14) | 0.0044 (14) |
C21C | 0.047 (2) | 0.0276 (19) | 0.041 (2) | −0.0025 (18) | 0.0223 (17) | 0.0084 (17) |
C22C | 0.049 (2) | 0.037 (2) | 0.0258 (19) | 0.0061 (18) | 0.0043 (16) | 0.0042 (16) |
C11C | 0.0215 (17) | 0.0161 (15) | 0.0281 (18) | −0.0038 (13) | 0.0071 (13) | 0.0008 (13) |
C12C | 0.031 (2) | 0.0297 (19) | 0.0304 (19) | −0.0070 (16) | 0.0062 (15) | −0.0030 (16) |
C13C | 0.062 (3) | 0.038 (2) | 0.031 (2) | −0.019 (2) | 0.0114 (19) | −0.0067 (17) |
C14C | 0.088 (4) | 0.032 (2) | 0.045 (3) | −0.020 (2) | 0.043 (2) | −0.0103 (18) |
C15C | 0.055 (3) | 0.031 (2) | 0.075 (3) | 0.0028 (19) | 0.045 (2) | −0.005 (2) |
C16C | 0.032 (2) | 0.0291 (19) | 0.041 (2) | 0.0035 (17) | 0.0130 (16) | 0.0037 (17) |
C1D | 0.0225 (18) | 0.0281 (18) | 0.0229 (17) | 0.0033 (14) | 0.0060 (13) | 0.0011 (13) |
C2D | 0.0201 (18) | 0.0298 (17) | 0.0262 (18) | −0.0036 (14) | 0.0071 (13) | −0.0008 (14) |
C21D | 0.0237 (18) | 0.051 (2) | 0.031 (2) | 0.0001 (18) | 0.0079 (14) | 0.0032 (18) |
C22D | 0.032 (2) | 0.035 (2) | 0.033 (2) | −0.0101 (16) | 0.0099 (15) | −0.0038 (16) |
C11D | 0.0180 (17) | 0.0301 (18) | 0.0238 (18) | −0.0020 (13) | 0.0082 (13) | 0.0017 (14) |
C12D | 0.0305 (19) | 0.0300 (18) | 0.0261 (19) | 0.0014 (15) | 0.0104 (14) | 0.0023 (15) |
C13D | 0.039 (2) | 0.038 (2) | 0.028 (2) | −0.0089 (17) | 0.0111 (16) | −0.0056 (16) |
C14D | 0.037 (2) | 0.053 (2) | 0.0266 (19) | −0.008 (2) | 0.0074 (15) | 0.0054 (19) |
C15D | 0.040 (2) | 0.044 (2) | 0.031 (2) | −0.0031 (18) | 0.0083 (17) | 0.0160 (17) |
C16D | 0.031 (2) | 0.0325 (19) | 0.034 (2) | −0.0076 (16) | 0.0122 (16) | 0.0018 (16) |
Sn1—C1A | 2.169 (3) | C14B—C15B | 1.374 (5) |
Sn1—C1C | 2.173 (3) | C15B—C16B | 1.382 (5) |
Sn1—C1D | 2.175 (3) | C1C—C2C | 1.546 (4) |
Sn1—C1B | 2.182 (3) | C2C—C11C | 1.530 (4) |
C1A—C2A | 1.542 (4) | C2C—C22C | 1.538 (4) |
C2A—C22A | 1.529 (4) | C2C—C21C | 1.541 (4) |
C2A—C11A | 1.532 (5) | C11C—C16C | 1.386 (4) |
C2A—C21A | 1.547 (4) | C11C—C12C | 1.394 (4) |
C11A—C12A | 1.382 (5) | C12C—C13C | 1.379 (5) |
C11A—C16A | 1.390 (5) | C13C—C14C | 1.366 (6) |
C12A—C13A | 1.396 (6) | C14C—C15C | 1.374 (6) |
C13A—C14A | 1.362 (7) | C15C—C16C | 1.392 (5) |
C14A—C15A | 1.358 (7) | C1D—C2D | 1.547 (4) |
C15A—C16A | 1.381 (5) | C2D—C22D | 1.534 (4) |
C1B—C2B | 1.544 (4) | C2D—C11D | 1.536 (4) |
C2B—C21B | 1.532 (4) | C2D—C21D | 1.545 (4) |
C2B—C11B | 1.532 (4) | C11D—C16D | 1.389 (4) |
C2B—C22B | 1.553 (4) | C11D—C12D | 1.393 (4) |
C11B—C16B | 1.387 (5) | C12D—C13D | 1.387 (4) |
C11B—C12B | 1.390 (5) | C13D—C14D | 1.379 (5) |
C12B—C13B | 1.380 (5) | C14D—C15D | 1.369 (5) |
C13B—C14B | 1.383 (5) | C15D—C16D | 1.391 (5) |
C1A—Sn1—C1C | 104.97 (12) | C15B—C14B—C13B | 118.9 (4) |
C1A—Sn1—C1D | 111.19 (12) | C14B—C15B—C16B | 120.7 (4) |
C1C—Sn1—C1D | 110.27 (12) | C15B—C16B—C11B | 121.2 (3) |
C1A—Sn1—C1B | 110.08 (12) | C2C—C1C—Sn1 | 120.4 (2) |
C1C—Sn1—C1B | 110.30 (12) | C11C—C2C—C22C | 111.8 (3) |
C1D—Sn1—C1B | 109.94 (12) | C11C—C2C—C21C | 107.2 (3) |
C2A—C1A—Sn1 | 121.0 (2) | C22C—C2C—C21C | 108.4 (3) |
C22A—C2A—C11A | 112.4 (3) | C11C—C2C—C1C | 112.2 (3) |
C22A—C2A—C1A | 109.5 (3) | C22C—C2C—C1C | 108.8 (3) |
C11A—C2A—C1A | 111.9 (3) | C21C—C2C—C1C | 108.3 (3) |
C22A—C2A—C21A | 107.1 (3) | C16C—C11C—C12C | 116.9 (3) |
C11A—C2A—C21A | 107.7 (3) | C16C—C11C—C2C | 123.1 (3) |
C1A—C2A—C21A | 108.0 (3) | C12C—C11C—C2C | 119.9 (3) |
C12A—C11A—C16A | 116.7 (4) | C13C—C12C—C11C | 121.5 (4) |
C12A—C11A—C2A | 123.3 (3) | C14C—C13C—C12C | 120.6 (4) |
C16A—C11A—C2A | 119.9 (3) | C13C—C14C—C15C | 119.6 (4) |
C11A—C12A—C13A | 121.3 (4) | C14C—C15C—C16C | 119.8 (4) |
C14A—C13A—C12A | 119.9 (5) | C11C—C16C—C15C | 121.6 (3) |
C15A—C14A—C13A | 120.3 (5) | C2D—C1D—Sn1 | 120.1 (2) |
C14A—C15A—C16A | 119.9 (5) | C22D—C2D—C11D | 111.8 (3) |
C15A—C16A—C11A | 122.0 (4) | C22D—C2D—C21D | 107.9 (3) |
C2B—C1B—Sn1 | 120.3 (2) | C11D—C2D—C21D | 108.7 (3) |
C21B—C2B—C11B | 112.3 (3) | C22D—C2D—C1D | 109.1 (3) |
C21B—C2B—C1B | 109.7 (3) | C11D—C2D—C1D | 110.6 (2) |
C11B—C2B—C1B | 111.5 (2) | C21D—C2D—C1D | 108.6 (3) |
C21B—C2B—C22B | 107.5 (3) | C16D—C11D—C12D | 117.1 (3) |
C11B—C2B—C22B | 107.3 (3) | C16D—C11D—C2D | 122.8 (3) |
C1B—C2B—C22B | 108.3 (3) | C12D—C11D—C2D | 120.1 (3) |
C16B—C11B—C12B | 117.5 (3) | C13D—C12D—C11D | 121.3 (3) |
C16B—C11B—C2B | 123.1 (3) | C14D—C13D—C12D | 120.6 (3) |
C12B—C11B—C2B | 119.5 (3) | C15D—C14D—C13D | 118.8 (3) |
C13B—C12B—C11B | 121.3 (3) | C14D—C15D—C16D | 121.0 (3) |
C12B—C13B—C14B | 120.4 (4) | C11D—C16D—C15D | 121.1 (3) |
C1C—Sn1—C1A—C2A | −107.7 (3) | C1A—Sn1—C1C—C2C | −107.7 (2) |
C1D—Sn1—C1A—C2A | 133.1 (2) | C1D—Sn1—C1C—C2C | 12.1 (3) |
C1B—Sn1—C1A—C2A | 11.0 (3) | C1B—Sn1—C1C—C2C | 133.7 (2) |
Sn1—C1A—C2A—C22A | −68.6 (3) | Sn1—C1C—C2C—C11C | 53.5 (3) |
Sn1—C1A—C2A—C11A | 56.7 (3) | Sn1—C1C—C2C—C22C | −70.8 (3) |
Sn1—C1A—C2A—C21A | 175.1 (2) | Sn1—C1C—C2C—C21C | 171.6 (2) |
C22A—C2A—C11A—C12A | −16.1 (4) | C22C—C2C—C11C—C16C | −19.2 (4) |
C1A—C2A—C11A—C12A | −139.8 (3) | C21C—C2C—C11C—C16C | 99.4 (3) |
C21A—C2A—C11A—C12A | 101.6 (4) | C1C—C2C—C11C—C16C | −141.8 (3) |
C22A—C2A—C11A—C16A | 166.4 (3) | C22C—C2C—C11C—C12C | 164.9 (3) |
C1A—C2A—C11A—C16A | 42.7 (4) | C21C—C2C—C11C—C12C | −76.4 (3) |
C21A—C2A—C11A—C16A | −75.9 (4) | C1C—C2C—C11C—C12C | 42.4 (4) |
C16A—C11A—C12A—C13A | 0.2 (5) | C16C—C11C—C12C—C13C | −0.2 (5) |
C2A—C11A—C12A—C13A | −177.4 (3) | C2C—C11C—C12C—C13C | 176.0 (3) |
C11A—C12A—C13A—C14A | 0.0 (6) | C11C—C12C—C13C—C14C | −0.1 (5) |
C12A—C13A—C14A—C15A | −0.2 (7) | C12C—C13C—C14C—C15C | 0.6 (6) |
C13A—C14A—C15A—C16A | 0.3 (6) | C13C—C14C—C15C—C16C | −0.7 (6) |
C14A—C15A—C16A—C11A | −0.2 (6) | C12C—C11C—C16C—C15C | 0.0 (5) |
C12A—C11A—C16A—C15A | −0.1 (5) | C2C—C11C—C16C—C15C | −176.0 (3) |
C2A—C11A—C16A—C15A | 177.6 (3) | C14C—C15C—C16C—C11C | 0.4 (5) |
C1A—Sn1—C1B—C2B | −161.4 (2) | C1A—Sn1—C1D—C2D | −44.1 (3) |
C1C—Sn1—C1B—C2B | −46.0 (3) | C1C—Sn1—C1D—C2D | −160.1 (2) |
C1D—Sn1—C1B—C2B | 75.8 (3) | C1B—Sn1—C1D—C2D | 78.1 (3) |
Sn1—C1B—C2B—C21B | −61.2 (3) | Sn1—C1D—C2D—C22D | −60.2 (3) |
Sn1—C1B—C2B—C11B | 63.9 (3) | Sn1—C1D—C2D—C11D | 63.2 (3) |
Sn1—C1B—C2B—C22B | −178.3 (2) | Sn1—C1D—C2D—C21D | −177.6 (2) |
C21B—C2B—C11B—C16B | −6.7 (4) | C22D—C2D—C11D—C16D | −9.1 (4) |
C1B—C2B—C11B—C16B | −130.3 (3) | C21D—C2D—C11D—C16D | 109.9 (3) |
C22B—C2B—C11B—C16B | 111.2 (3) | C1D—C2D—C11D—C16D | −130.9 (3) |
C21B—C2B—C11B—C12B | 174.7 (3) | C22D—C2D—C11D—C12D | 170.1 (3) |
C1B—C2B—C11B—C12B | 51.1 (4) | C21D—C2D—C11D—C12D | −70.9 (4) |
C22B—C2B—C11B—C12B | −67.3 (4) | C1D—C2D—C11D—C12D | 48.3 (4) |
C16B—C11B—C12B—C13B | −0.5 (5) | C16D—C11D—C12D—C13D | 2.9 (5) |
C2B—C11B—C12B—C13B | 178.1 (3) | C2D—C11D—C12D—C13D | −176.2 (3) |
C11B—C12B—C13B—C14B | 0.2 (6) | C11D—C12D—C13D—C14D | −0.5 (5) |
C12B—C13B—C14B—C15B | 0.3 (6) | C12D—C13D—C14D—C15D | −1.9 (5) |
C13B—C14B—C15B—C16B | −0.6 (6) | C13D—C14D—C15D—C16D | 1.9 (6) |
C14B—C15B—C16B—C11B | 0.3 (5) | C12D—C11D—C16D—C15D | −3.0 (5) |
C12B—C11B—C16B—C15B | 0.3 (5) | C2D—C11D—C16D—C15D | 176.2 (3) |
C2B—C11B—C16B—C15B | −178.3 (3) | C14D—C15D—C16D—C11D | 0.6 (5) |
Experimental details
Crystal data | |
Chemical formula | [Sn(C10H13)4] |
Mr | 651.51 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 150 |
a, b, c (Å) | 13.9224 (4), 9.9590 (2), 25.6952 (6) |
β (°) | 104.5178 (14) |
V (Å3) | 3448.96 (15) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.77 |
Crystal size (mm) | 0.30 × 0.10 × 0.03 |
Data collection | |
Diffractometer | KappaCCD diffractometer |
Absorption correction | Multi-scan (SORTAV; Blessing, 1995, 1997) |
Tmin, Tmax | 0.927, 0.973 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 24777, 7414, 5147 |
Rint | 0.064 |
(sin θ/λ)max (Å−1) | 0.649 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.038, 0.088, 0.99 |
No. of reflections | 7414 |
No. of parameters | 378 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.83, −0.74 |
Computer programs: KappaCCD Server Software (Nonius, 1997), DENZO (Otwinowski & Minor, 1997), SHELXS97 (Sheldrick, 1997a), SHELXL97 (Sheldrick, 1997b), SHELXL97 and WORDPERFECT macro PRPKAPPA (Ferguson, 1999).
Examination of the structure with PLATON (Spek, 1999) showed that there were no solvent-accessible voids in the crystal lattice.