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The structure of the title compound, [Sn(C6H5)3(OH)]n, has been re-investigated at 120 (2) K. The hydroxyl H atom was readily located and the threefold coordination about the O atom is planar. There are no hydrogen bonds involving the hydroxyl group, either as donor or as acceptor.
Supporting information
CCDC reference: 184453
Data collection: KappaCCD Server Software (Nonius, 1997); cell refinement: DENZO-SMN (Otwinowski & Minor, 1997); data reduction: DENZO-SMN; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2002); software used to prepare material for publication: SHELXL97 and PRPKAPPA (Ferguson, 1999).
catena-Poly[[triphenyltin(IV)]-µ-hydroxo-
κ2O:
O]
top
Crystal data top
[Sn(C6H5)3OH] | F(000) = 728 |
Mr = 367.00 | Dx = 1.632 Mg m−3 |
Orthorhombic, P212121 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2ac 2ab | Cell parameters from 3376 reflections |
a = 8.2573 (2) Å | θ = 3.0–27.5° |
b = 10.2229 (2) Å | µ = 1.70 mm−1 |
c = 17.6996 (5) Å | T = 120 K |
V = 1494.09 (6) Å3 | Block, colourless |
Z = 4 | 0.40 × 0.22 × 0.20 mm |
Data collection top
Nonius KappaCCD area-detector diffractometer | 3376 independent reflections |
Radiation source: fine-focus sealed X-ray tube | 3120 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.062 |
φ scans, and ω scans with κ offsets | θmax = 27.5°, θmin = 3.0° |
Absorption correction: multi-scan (DENZO-SMN; Otwinowski & Minor, 1997) | h = −9→10 |
Tmin = 0.554, Tmax = 0.712 | k = −13→11 |
10366 measured reflections | l = −18→22 |
Refinement top
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)] = 0.025 | H-atom parameters constrained |
wR(F2) = 0.060 | w = 1/[σ2(Fo2) + (0.0221P)2 + 1.0158P] where P = (Fo2 + 2Fc2)/3 |
S = 1.00 | (Δ/σ)max = 0.001 |
3376 reflections | Δρmax = 0.68 e Å−3 |
181 parameters | Δρmin = −1.06 e Å−3 |
0 restraints | Absolute structure: Flack (1983), 1408 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.01 (3) |
Special details top
Experimental. The program DENZO-SMN (Otwinowski & Minor, 1997) uses a scaling algorithm
[Fox, G. C. & Holmes, K. C. (1966). Acta Cryst. 20, 886–891] which
effectively corrects for absorption effects. High-redundancy data were used in
the scaling program, hence the `multi-scan' code word was used. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Sn1 | 0.565990 (18) | 0.247677 (16) | 0.003450 (8) | 0.01350 (7) | |
C11 | 0.6051 (3) | 0.1461 (3) | 0.10708 (16) | 0.0187 (6) | |
C12 | 0.7054 (4) | 0.0355 (3) | 0.10904 (18) | 0.0238 (7) | |
C13 | 0.7341 (4) | −0.0293 (3) | 0.1767 (2) | 0.0317 (8) | |
C14 | 0.6675 (4) | 0.0145 (4) | 0.2428 (2) | 0.0391 (9) | |
C15 | 0.5652 (4) | 0.1226 (3) | 0.24182 (18) | 0.0347 (8) | |
C16 | 0.5352 (4) | 0.1866 (3) | 0.17407 (17) | 0.0273 (7) | |
C26 | 0.4913 (3) | −0.0019 (3) | −0.08508 (18) | 0.0244 (7) | |
C21 | 0.4901 (3) | 0.1339 (3) | −0.09059 (16) | 0.0169 (6) | |
C22 | 0.4456 (4) | 0.1906 (3) | −0.15902 (16) | 0.0253 (6) | |
C23 | 0.3999 (4) | 0.1134 (4) | −0.21958 (18) | 0.0354 (8) | |
C24 | 0.3995 (4) | −0.0221 (4) | −0.2130 (2) | 0.0395 (9) | |
C25 | 0.4458 (4) | −0.0788 (3) | −0.14645 (19) | 0.0329 (8) | |
C31 | 0.6261 (3) | 0.4483 (3) | −0.01089 (17) | 0.0177 (5) | |
C32 | 0.5807 (4) | 0.5435 (3) | 0.04118 (19) | 0.0290 (7) | |
C33 | 0.6265 (4) | 0.6737 (3) | 0.0318 (3) | 0.0380 (9) | |
C34 | 0.7172 (4) | 0.7099 (3) | −0.0299 (3) | 0.0383 (9) | |
C35 | 0.7619 (4) | 0.6170 (3) | −0.0827 (2) | 0.0303 (7) | |
C36 | 0.7174 (4) | 0.4865 (3) | −0.07307 (18) | 0.0234 (6) | |
O1 | 0.3191 (2) | 0.30112 (18) | 0.03424 (12) | 0.0181 (4) | |
H12 | 0.7540 | 0.0047 | 0.0638 | 0.029* | |
H13 | 0.8008 | −0.1051 | 0.1771 | 0.038* | |
H14 | 0.6910 | −0.0286 | 0.2891 | 0.047* | |
H15 | 0.5161 | 0.1524 | 0.2872 | 0.042* | |
H16 | 0.4649 | 0.2602 | 0.1737 | 0.033* | |
H26 | 0.5233 | −0.0424 | −0.0391 | 0.029* | |
H22 | 0.4467 | 0.2831 | −0.1642 | 0.030* | |
H23 | 0.3687 | 0.1531 | −0.2659 | 0.043* | |
H24 | 0.3672 | −0.0750 | −0.2544 | 0.047* | |
H25 | 0.4470 | −0.1714 | −0.1421 | 0.039* | |
H32 | 0.5176 | 0.5194 | 0.0838 | 0.035* | |
H33 | 0.5949 | 0.7374 | 0.0680 | 0.046* | |
H34 | 0.7491 | 0.7985 | −0.0362 | 0.046* | |
H35 | 0.8232 | 0.6422 | −0.1257 | 0.036* | |
H36 | 0.7498 | 0.4231 | −0.1093 | 0.028* | |
H1 | 0.3274 | 0.3731 | 0.0630 | 0.022* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Sn1 | 0.01138 (10) | 0.01108 (10) | 0.01804 (10) | −0.00002 (6) | −0.00070 (6) | −0.00076 (10) |
C11 | 0.0159 (14) | 0.0176 (14) | 0.0225 (14) | −0.0024 (11) | −0.0050 (11) | 0.0024 (11) |
C12 | 0.0226 (15) | 0.0183 (15) | 0.0306 (17) | −0.0033 (13) | −0.0060 (13) | −0.0005 (13) |
C13 | 0.0354 (19) | 0.0171 (15) | 0.043 (2) | −0.0013 (14) | −0.0143 (16) | 0.0101 (14) |
C14 | 0.046 (2) | 0.039 (2) | 0.032 (2) | −0.0101 (18) | −0.0119 (16) | 0.0181 (17) |
C15 | 0.0400 (19) | 0.040 (2) | 0.0236 (16) | −0.0042 (17) | 0.0025 (15) | 0.0035 (14) |
C16 | 0.0254 (16) | 0.0308 (16) | 0.0256 (16) | −0.0022 (13) | −0.0008 (12) | 0.0008 (13) |
C26 | 0.0236 (15) | 0.0229 (15) | 0.0267 (16) | −0.0025 (13) | 0.0007 (12) | −0.0034 (13) |
C21 | 0.0130 (13) | 0.0152 (14) | 0.0226 (14) | −0.0008 (11) | 0.0020 (10) | −0.0021 (11) |
C22 | 0.0242 (15) | 0.0277 (16) | 0.0241 (15) | 0.0072 (13) | 0.0009 (13) | −0.0012 (12) |
C23 | 0.0336 (18) | 0.052 (2) | 0.0210 (15) | 0.0149 (17) | −0.0037 (14) | −0.0067 (15) |
C24 | 0.0321 (19) | 0.054 (2) | 0.0324 (19) | −0.0009 (17) | −0.0023 (15) | −0.0249 (18) |
C25 | 0.0371 (19) | 0.0196 (15) | 0.0419 (19) | −0.0043 (14) | 0.0057 (17) | −0.0128 (14) |
C31 | 0.0105 (12) | 0.0138 (12) | 0.0287 (15) | −0.0006 (10) | −0.0023 (11) | 0.0013 (12) |
C32 | 0.0199 (15) | 0.0210 (15) | 0.0461 (19) | −0.0014 (12) | 0.0037 (14) | −0.0075 (14) |
C33 | 0.0261 (17) | 0.0169 (15) | 0.071 (3) | 0.0012 (13) | 0.0023 (17) | −0.0133 (16) |
C34 | 0.0245 (15) | 0.0125 (13) | 0.078 (3) | −0.0013 (13) | −0.0061 (18) | 0.0062 (17) |
C35 | 0.0247 (16) | 0.0257 (16) | 0.0405 (19) | −0.0053 (13) | −0.0077 (14) | 0.0151 (15) |
C36 | 0.0182 (14) | 0.0222 (15) | 0.0297 (17) | 0.0014 (13) | −0.0057 (13) | 0.0063 (13) |
O1 | 0.0123 (9) | 0.0151 (9) | 0.0269 (12) | −0.0033 (7) | −0.0013 (7) | −0.0037 (9) |
Geometric parameters (Å, º) top
Sn1—C11 | 2.133 (3) | C22—C23 | 1.384 (4) |
Sn1—C21 | 2.125 (3) | C22—H22 | 0.9500 |
Sn1—C31 | 2.126 (3) | C23—C24 | 1.390 (5) |
Sn1—O1 | 2.1797 (17) | C23—H23 | 0.9500 |
Sn1—O1i | 2.2500 (17) | C24—C25 | 1.367 (5) |
C11—C16 | 1.382 (4) | C24—H24 | 0.9500 |
C11—C12 | 1.401 (4) | C25—H25 | 0.9500 |
C12—C13 | 1.389 (4) | C31—C36 | 1.390 (4) |
C12—H12 | 0.9500 | C31—C32 | 1.392 (4) |
C13—C14 | 1.369 (5) | C32—C33 | 1.393 (4) |
C13—H13 | 0.9500 | C32—H32 | 0.9500 |
C14—C15 | 1.391 (5) | C33—C34 | 1.375 (6) |
C14—H14 | 0.9500 | C33—H33 | 0.9500 |
C15—C16 | 1.388 (4) | C34—C35 | 1.382 (5) |
C15—H15 | 0.9500 | C34—H34 | 0.9500 |
C16—H16 | 0.9500 | C35—C36 | 1.394 (4) |
C26—C21 | 1.391 (4) | C35—H35 | 0.9500 |
C26—C25 | 1.393 (4) | C36—H36 | 0.9500 |
C26—H26 | 0.9500 | O1—H1 | 0.897 |
C21—C22 | 1.392 (4) | | |
| | | |
O1—Sn1—O1i | 176.842 (12) | C26—C21—C22 | 118.6 (3) |
Sn1—O1—Sn1ii | 137.66 (10) | C26—C21—Sn1 | 119.3 (2) |
Sn1—O1—H1 | 106.0 | C22—C21—Sn1 | 122.1 (2) |
Sn1ii—O1—H1 | 114.9 | C23—C22—C21 | 120.5 (3) |
C11—Sn1—C21 | 116.84 (11) | C23—C22—H22 | 119.7 |
C21—Sn1—C31 | 120.24 (11) | C21—C22—H22 | 119.7 |
C31—Sn1—C11 | 122.51 (11) | C22—C23—C24 | 120.3 (3) |
C11—Sn1—O1 | 92.79 (10) | C22—C23—H23 | 119.9 |
C21—Sn1—O1 | 93.29 (9) | C24—C23—H23 | 119.9 |
C31—Sn1—O1 | 90.36 (8) | C25—C24—C23 | 119.6 (3) |
C11—Sn1—O1i | 90.36 (9) | C25—C24—H24 | 120.2 |
C21—Sn1—O1i | 85.43 (9) | C23—C24—H24 | 120.2 |
C31—Sn1—O1i | 87.81 (8) | C24—C25—C26 | 120.5 (3) |
C16—C11—C12 | 117.9 (3) | C24—C25—H25 | 119.7 |
C16—C11—Sn1 | 121.9 (2) | C26—C25—H25 | 119.7 |
C12—C11—Sn1 | 120.2 (2) | C36—C31—C32 | 118.3 (3) |
C13—C12—C11 | 120.5 (3) | C36—C31—Sn1 | 119.5 (2) |
C13—C12—H12 | 119.8 | C32—C31—Sn1 | 122.2 (2) |
C11—C12—H12 | 119.8 | C31—C32—C33 | 121.1 (3) |
C14—C13—C12 | 120.8 (3) | C31—C32—H32 | 119.5 |
C14—C13—H13 | 119.6 | C33—C32—H32 | 119.5 |
C12—C13—H13 | 119.6 | C34—C33—C32 | 120.0 (3) |
C13—C14—C15 | 119.5 (3) | C34—C33—H33 | 120.0 |
C13—C14—H14 | 120.2 | C32—C33—H33 | 120.0 |
C15—C14—H14 | 120.2 | C33—C34—C35 | 119.8 (3) |
C16—C15—C14 | 119.6 (3) | C33—C34—H34 | 120.1 |
C16—C15—H15 | 120.2 | C35—C34—H34 | 120.1 |
C14—C15—H15 | 120.2 | C34—C35—C36 | 120.3 (3) |
C11—C16—C15 | 121.7 (3) | C34—C35—H35 | 119.9 |
C11—C16—H16 | 119.2 | C36—C35—H35 | 119.9 |
C15—C16—H16 | 119.2 | C31—C36—C35 | 120.5 (3) |
C21—C26—C25 | 120.5 (3) | C31—C36—H36 | 119.7 |
C21—C26—H26 | 119.8 | C35—C36—H36 | 119.7 |
C25—C26—H26 | 119.8 | | |
| | | |
C21—Sn1—C11—C16 | −128.8 (2) | C31—Sn1—C21—C22 | −13.5 (3) |
C31—Sn1—C11—C16 | 58.5 (3) | C11—Sn1—C21—C22 | 173.6 (2) |
O1—Sn1—C11—C16 | −33.7 (2) | C26—C21—C22—C23 | 1.5 (4) |
O1i—Sn1—C11—C16 | 146.2 (2) | Sn1—C21—C22—C23 | 178.7 (2) |
C21—Sn1—C11—C12 | 51.9 (2) | C21—C22—C23—C24 | −0.7 (5) |
C31—Sn1—C11—C12 | −120.8 (2) | C22—C23—C24—C25 | −0.5 (5) |
O1—Sn1—C11—C12 | 147.0 (2) | C23—C24—C25—C26 | 0.8 (5) |
O1—Sn1—C21—C22 | 78.8 (2) | C21—C26—C25—C24 | 0.0 (5) |
O1—Sn1—C31—C32 | 45.2 (2) | C21—Sn1—C31—C36 | −42.5 (2) |
O1i—Sn1—C11—C12 | −33.1 (2) | C11—Sn1—C31—C36 | 129.9 (2) |
O1i—Sn1—C21—C22 | −98.3 (2) | O1—Sn1—C31—C36 | −136.6 (2) |
O1i—Sn1—C31—C32 | −137.3 (2) | O1i—Sn1—C31—C36 | 40.9 (2) |
C16—C11—C12—C13 | −0.8 (4) | C21—Sn1—C31—C32 | 139.3 (2) |
Sn1—C11—C12—C13 | 178.6 (2) | C11—Sn1—C31—C32 | −48.3 (3) |
C11—C12—C13—C14 | −1.1 (5) | C36—C31—C32—C33 | −0.5 (5) |
C12—C13—C14—C15 | 2.3 (5) | Sn1—C31—C32—C33 | 177.7 (2) |
C13—C14—C15—C16 | −1.6 (5) | C31—C32—C33—C34 | 0.3 (5) |
C12—C11—C16—C15 | 1.4 (5) | C32—C33—C34—C35 | 0.4 (6) |
Sn1—C11—C16—C15 | −177.9 (3) | C33—C34—C35—C36 | −1.0 (5) |
C14—C15—C16—C11 | −0.2 (5) | C32—C31—C36—C35 | 0.0 (4) |
C25—C26—C21—C22 | −1.2 (4) | Sn1—C31—C36—C35 | −178.3 (2) |
C25—C26—C21—Sn1 | −178.5 (2) | C34—C35—C36—C31 | 0.8 (5) |
C31—Sn1—C21—C26 | 163.7 (2) | C21—Sn1—O1—Sn1ii | 5.14 (16) |
C11—Sn1—C21—C26 | −9.2 (3) | C31—Sn1—O1—Sn1ii | 125.45 (16) |
O1—Sn1—C21—C26 | −104.0 (2) | C11—Sn1—O1—Sn1ii | −111.97 (16) |
O1i—Sn1—C21—C26 | 78.9 (2) | | |
Symmetry codes: (i) x+1/2, −y+1/2, −z; (ii) x−1/2, −y+1/2, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1···C32 | 0.90 | 2.75 | 3.289 (4) | 120 |
C12—H12···O1i | 0.95 | 2.69 | 3.178 (4) | 113 |
C36—H36···O1i | 0.95 | 2.71 | 3.134 (4) | 108 |
Symmetry code: (i) x+1/2, −y+1/2, −z. |
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