catena-Poly[[triphenyltin(IV)]-[mu]-hydroxo-[kappa]²O:O] at 120 K

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.

Computing details

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]

Crystal data

[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) Å^3	Block, colourless
Z = 4	0.40 × 0.22 × 0.20 mm

Data collection

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

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.025	H-atom parameters constrained
wR(F^2) = 0.060	w = 1/[σ^2(Fo^2) + (0.0221P)^2 + 1.0158P] where P = (Fo^2 + 2Fc^2)/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

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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

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—O1^i	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—O1^i	176.842 (12)	C26—C21—C22	118.6 (3)
Sn1—O1—Sn1^ii	137.66 (10)	C26—C21—Sn1	119.3 (2)
Sn1—O1—H1	106.0	C22—C21—Sn1	122.1 (2)
Sn1^ii—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—O1^i	90.36 (9)	C25—C24—H24	120.2
C21—Sn1—O1^i	85.43 (9)	C23—C24—H24	120.2
C31—Sn1—O1^i	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)
O1^i—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)
O1^i—Sn1—C11—C12	−33.1 (2)	C11—Sn1—C31—C36	129.9 (2)
O1^i—Sn1—C21—C22	−98.3 (2)	O1—Sn1—C31—C36	−136.6 (2)
O1^i—Sn1—C31—C32	−137.3 (2)	O1^i—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—Sn1^ii	5.14 (16)
C11—Sn1—C21—C26	−9.2 (3)	C31—Sn1—O1—Sn1^ii	125.45 (16)
O1—Sn1—C21—C26	−104.0 (2)	C11—Sn1—O1—Sn1^ii	−111.97 (16)
O1^i—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)

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···O1^i	0.95	2.69	3.178 (4)	113
C36—H36···O1^i	0.95	2.71	3.134 (4)	108

Symmetry code: (i) x+1/2, −y+1/2, −z.