Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100015067/qa0440sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270100015067/qa0440Isup2.hkl |
CCDC reference: 156195
The title compound was prepared from the corresponding oxide and HCl. Crystals were obtained by the slow evaporation of a CHCl3 solution [m.p. 389–390 K;. literature value: m.p. 389.5–390.5 K (Zimmer et al., 1966)].
Molecule (I) crystallized in the cubic system; space group I43 d from the systematic absences. H atoms were treated as riding atoms with C—H = 0.95–0.98 Å. Examination of the structure with PLATON (Spek, 2000) showed that there were no solvent-accessible voids in the crystal lattice.
Data collection: KappaCCD Server Software (Nonius, 1997); cell refinement: DENZO (Otwinowski & Minor, 1997); data reduction: DENZO; 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: SHELXL97 and WORDPERFECT macro PRPKAPPA (Ferguson, 1999).
[SnCl(C10H13)3] | Mo Kα radiation, λ = 0.71073 Å |
Mr = 553.75 | Cell parameters from 2073 reflections |
Cubic, I43d | θ = 3.4–27.4° |
a = 22.3858 (4) Å | µ = 1.02 mm−1 |
V = 11218.1 (3) Å3 | T = 150 K |
Z = 16 | Block, colourless |
F(000) = 4576 | 0.38 × 0.25 × 0.13 mm |
Dx = 1.311 Mg m−3 |
KappaCCD diffractometer | 2073 independent reflections |
Radiation source: fine-focus sealed X-ray tube | 1602 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.032 |
ϕ scans and ω scans with κ offsets | θmax = 27.4°, θmin = 3.4° |
Absorption correction: multi-scan (SORTAV; lessing, 1995, 1997) | h = −9→29 |
Tmin = 0.701, Tmax = 0.883 | k = −23→29 |
11754 measured reflections | l = −24→26 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.042 | H-atom parameters constrained |
wR(F2) = 0.123 | w = 1/[σ2(Fo2) + (0.0747P)2 + 4.8319P] where P = (Fo2 + 2Fc2)/3 |
S = 1.04 | (Δ/σ)max = 0.004 |
2073 reflections | Δρmax = 0.43 e Å−3 |
99 parameters | Δρmin = −0.59 e Å−3 |
0 restraints | Absolute structure: Flack (1983), 927 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.06 (6) |
[SnCl(C10H13)3] | Z = 16 |
Mr = 553.75 | Mo Kα radiation |
Cubic, I43d | µ = 1.02 mm−1 |
a = 22.3858 (4) Å | T = 150 K |
V = 11218.1 (3) Å3 | 0.38 × 0.25 × 0.13 mm |
KappaCCD diffractometer | 2073 independent reflections |
Absorption correction: multi-scan (SORTAV; lessing, 1995, 1997) | 1602 reflections with I > 2σ(I) |
Tmin = 0.701, Tmax = 0.883 | Rint = 0.032 |
11754 measured reflections |
R[F2 > 2σ(F2)] = 0.042 | H-atom parameters constrained |
wR(F2) = 0.123 | Δρmax = 0.43 e Å−3 |
S = 1.04 | Δρmin = −0.59 e Å−3 |
2073 reflections | Absolute structure: Flack (1983), 927 Friedel pairs |
99 parameters | Absolute structure parameter: −0.06 (6) |
0 restraints |
x | y | z | Uiso*/Ueq | ||
Sn1 | 0.402092 (13) | 0.597908 (13) | 0.097908 (13) | 0.0578 (2) | |
Cl1 | 0.34066 (7) | 0.65934 (7) | 0.15934 (7) | 0.1127 (13) | |
C1 | 0.3382 (2) | 0.5305 (2) | 0.0735 (3) | 0.0739 (14) | |
C2 | 0.3405 (3) | 0.4703 (3) | 0.1068 (2) | 0.0796 (17) | |
C3 | 0.3289 (5) | 0.4824 (5) | 0.1742 (3) | 0.147 (5) | |
C4 | 0.2920 (3) | 0.4299 (4) | 0.0823 (3) | 0.100 (3) | |
C5 | 0.4002 (3) | 0.4399 (2) | 0.0977 (2) | 0.0725 (14) | |
C6 | 0.4251 (3) | 0.4369 (3) | 0.0412 (3) | 0.0750 (15) | |
C7 | 0.4779 (3) | 0.4084 (3) | 0.0254 (4) | 0.096 (2) | |
C8 | 0.5078 (5) | 0.3803 (4) | 0.0657 (4) | 0.119 (3) | |
C9 | 0.4916 (5) | 0.3788 (3) | 0.1219 (5) | 0.110 (3) | |
C10 | 0.4365 (6) | 0.4099 (3) | 0.1415 (4) | 0.131 (4) | |
H1A | 0.2978 | 0.5476 | 0.0791 | 0.089* | |
H1B | 0.3431 | 0.5223 | 0.0303 | 0.089* | |
H3A | 0.3218 | 0.4444 | 0.1948 | 0.220* | |
H3B | 0.2937 | 0.5081 | 0.1786 | 0.220* | |
H3C | 0.3637 | 0.5022 | 0.1917 | 0.220* | |
H4A | 0.2983 | 0.4239 | 0.0394 | 0.150* | |
H4B | 0.2529 | 0.4484 | 0.0888 | 0.150* | |
H4C | 0.2935 | 0.3912 | 0.1028 | 0.150* | |
H6 | 0.4039 | 0.4564 | 0.0100 | 0.090* | |
H7 | 0.4917 | 0.4095 | −0.0147 | 0.115* | |
H8 | 0.5432 | 0.3600 | 0.0542 | 0.143* | |
H9 | 0.5151 | 0.3576 | 0.1501 | 0.132* | |
H10 | 0.4253 | 0.4100 | 0.1824 | 0.157* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Sn1 | 0.0578 (2) | 0.0578 (2) | 0.0578 (2) | 0.00548 (14) | 0.00548 (14) | −0.00548 (14) |
Cl1 | 0.1127 (13) | 0.1127 (13) | 0.1127 (13) | 0.0326 (10) | 0.0326 (10) | −0.0326 (10) |
C1 | 0.060 (3) | 0.089 (4) | 0.072 (3) | −0.015 (3) | 0.009 (2) | −0.007 (3) |
C2 | 0.094 (4) | 0.083 (3) | 0.061 (3) | −0.037 (3) | 0.028 (3) | −0.010 (3) |
C3 | 0.221 (10) | 0.139 (7) | 0.081 (5) | −0.093 (7) | 0.091 (6) | −0.035 (4) |
C4 | 0.091 (5) | 0.112 (5) | 0.097 (5) | −0.047 (4) | 0.039 (4) | −0.032 (4) |
C5 | 0.105 (4) | 0.056 (2) | 0.057 (3) | −0.025 (3) | −0.022 (4) | −0.003 (2) |
C6 | 0.064 (3) | 0.077 (4) | 0.084 (4) | −0.015 (3) | 0.002 (3) | −0.014 (3) |
C7 | 0.089 (4) | 0.089 (4) | 0.109 (5) | −0.008 (4) | 0.003 (4) | −0.007 (4) |
C8 | 0.164 (9) | 0.092 (5) | 0.100 (6) | −0.040 (6) | −0.026 (6) | −0.012 (5) |
C9 | 0.127 (6) | 0.053 (3) | 0.151 (8) | −0.001 (4) | −0.070 (6) | 0.002 (4) |
C10 | 0.225 (11) | 0.072 (4) | 0.095 (5) | −0.043 (6) | −0.054 (6) | 0.010 (4) |
Sn1—C1 | 2.149 (5) | C4—H4B | 0.9800 |
Sn1—C1i | 2.149 (5) | C4—H4C | 0.9800 |
Sn1—C1ii | 2.149 (5) | C5—C6 | 1.385 (9) |
Sn1—Cl1 | 2.382 (3) | C5—C10 | 1.439 (11) |
C1—C2 | 1.541 (8) | C6—C7 | 1.389 (9) |
C1—H1A | 0.9900 | C6—H6 | 0.9500 |
C1—H1B | 0.9900 | C7—C8 | 1.288 (11) |
C2—C5 | 1.513 (9) | C7—H7 | 0.9500 |
C2—C4 | 1.517 (9) | C8—C9 | 1.310 (14) |
C2—C3 | 1.555 (8) | C8—H8 | 0.9500 |
C3—H3A | 0.9800 | C9—C10 | 1.483 (15) |
C3—H3B | 0.9800 | C9—H9 | 0.9500 |
C3—H3C | 0.9800 | C10—H10 | 0.9500 |
C4—H4A | 0.9800 | ||
C1—Sn1—C1i | 117.23 (9) | C2—C4—H4A | 109.5 |
C1—Sn1—C1ii | 117.24 (8) | C2—C4—H4B | 109.5 |
C1i—Sn1—C1ii | 117.24 (8) | H4A—C4—H4B | 109.5 |
C1—Sn1—Cl1 | 99.67 (15) | C2—C4—H4C | 109.5 |
C1i—Sn1—Cl1 | 99.67 (15) | H4A—C4—H4C | 109.5 |
C1ii—Sn1—Cl1 | 99.67 (15) | H4B—C4—H4C | 109.5 |
C2—C1—Sn1 | 118.0 (4) | C6—C5—C10 | 111.8 (7) |
C2—C1—H1A | 107.8 | C6—C5—C2 | 119.9 (5) |
Sn1—C1—H1A | 107.8 | C10—C5—C2 | 128.2 (7) |
C2—C1—H1B | 107.8 | C5—C6—C7 | 126.6 (7) |
Sn1—C1—H1B | 107.8 | C5—C6—H6 | 116.7 |
H1A—C1—H1B | 107.2 | C7—C6—H6 | 116.7 |
C5—C2—C4 | 108.4 (5) | C8—C7—C6 | 119.3 (9) |
C5—C2—C1 | 111.0 (4) | C8—C7—H7 | 120.3 |
C4—C2—C1 | 108.9 (6) | C6—C7—H7 | 120.3 |
C5—C2—C3 | 110.8 (7) | C7—C8—C9 | 122.7 (12) |
C4—C2—C3 | 109.5 (5) | C7—C8—H8 | 118.6 |
C1—C2—C3 | 108.2 (6) | C9—C8—H8 | 118.6 |
C2—C3—H3A | 109.5 | C8—C9—C10 | 120.2 (9) |
C2—C3—H3B | 109.5 | C8—C9—H9 | 119.9 |
H3A—C3—H3B | 109.5 | C10—C9—H9 | 119.9 |
C2—C3—H3C | 109.5 | C5—C10—C9 | 119.2 (8) |
H3A—C3—H3C | 109.5 | C5—C10—H10 | 120.4 |
H3B—C3—H3C | 109.5 | C9—C10—H10 | 120.4 |
C1i—Sn1—C1—C2 | 152.8 (2) | C1—C2—C5—C10 | 136.7 (6) |
C1ii—Sn1—C1—C2 | 5.2 (6) | C3—C2—C5—C10 | 16.5 (8) |
Cl1—Sn1—C1—C2 | −101.0 (4) | C10—C5—C6—C7 | 1.1 (9) |
Sn1—C1—C2—C5 | −60.6 (5) | C2—C5—C6—C7 | −176.9 (6) |
Sn1—C1—C2—C4 | −179.8 (4) | C5—C6—C7—C8 | 1.2 (11) |
Sn1—C1—C2—C3 | 61.3 (7) | C6—C7—C8—C9 | −1.9 (12) |
C4—C2—C5—C6 | 73.9 (7) | C7—C8—C9—C10 | 0.2 (12) |
C1—C2—C5—C6 | −45.6 (6) | C6—C5—C10—C9 | −2.7 (8) |
C3—C2—C5—C6 | −165.9 (5) | C2—C5—C10—C9 | 175.2 (5) |
C4—C2—C5—C10 | −103.8 (7) | C8—C9—C10—C5 | 2.3 (11) |
Symmetry codes: (i) −z+1/2, −x+1, y−1/2; (ii) −y+1, z+1/2, −x+1/2. |
Experimental details
Crystal data | |
Chemical formula | [SnCl(C10H13)3] |
Mr | 553.75 |
Crystal system, space group | Cubic, I43d |
Temperature (K) | 150 |
a (Å) | 22.3858 (4) |
V (Å3) | 11218.1 (3) |
Z | 16 |
Radiation type | Mo Kα |
µ (mm−1) | 1.02 |
Crystal size (mm) | 0.38 × 0.25 × 0.13 |
Data collection | |
Diffractometer | KappaCCD diffractometer |
Absorption correction | Multi-scan (SORTAV; lessing, 1995, 1997) |
Tmin, Tmax | 0.701, 0.883 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 11754, 2073, 1602 |
Rint | 0.032 |
(sin θ/λ)max (Å−1) | 0.647 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.042, 0.123, 1.04 |
No. of reflections | 2073 |
No. of parameters | 99 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.43, −0.59 |
Absolute structure | Flack (1983), 927 Friedel pairs |
Absolute structure parameter | −0.06 (6) |
Computer programs: KappaCCD Server Software (Nonius, 1997), DENZO (Otwinowski & Minor, 1997), DENZO, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXL97 and WORDPERFECT macro PRPKAPPA (Ferguson, 1999).
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