Dibromidodi-μ-hydroxido-di-μ(3)-oxido-octa-phenyl-tetra-tin(IV).

In the centrosymmetric title compound, [Sn(4)Br(2)(C(6)H(5))(8)O(2)(OH)(2)], the four tin(IV) atoms are bridged by the hydroxo and oxo ligands, forming a ladder-like array of three edge-connected Sn(2)O(2) squares. The two independent tin atoms show distorted trigonal-bipyramidal SnC(2)O(3) and SnC(2)O(2)Br coordination geometries.

Related literature

For other [Sn4 X 2(O)2(OH)2 R 8] (X = halogen, R = organic group) structures, see: Baumeister et al. (2002 ▶); Beckmann et al. (2001 ▶); Cox & Tiekink (1994 ▶); Kresinski et al. (1994 ▶); Lo & Ng (2009 ▶); Mohamed et al. (2004 ▶); Puff et al. (1983 ▶); Tiekink (1991 ▶); Vollano et al. (1984 ▶).

Experimental

Crystal data

[Sn4Br2(C6H5)8O2(OH)2]

M = 1317.40

Triclinic,

a = 10.3759 (1) Å

b = 10.8247 (1) Å

c = 12.0341 (2) Å

α = 77.1809 (7)°

β = 65.4426 (7)°

γ = 75.2040 (7)°

V = 1178.26 (3) Å3

Z = 1

Mo Kα radiation

μ = 3.83 mm−1

T = 293 K

0.25 × 0.25 × 0.25 mm

Data collection

Bruker SMART APEX diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.539, T max = 0.746

10751 measured reflections

5309 independent reflections

4449 reflections with I > 2σ(I)

R int = 0.028

Refinement

R[F 2 > 2σ(F 2)] = 0.042

wR(F 2) = 0.160

S = 1.06

5309 reflections

262 parameters

H-atom parameters constrained

Δρmax = 2.39 e Å−3

Δρmin = −1.38 e Å−3

Data collection: APEX2 software (Bruker, 2008 ▶); cell refinement: SAINT (Bruker, 2008 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: X-SEED (Barbour, 2001 ▶); software used to prepare material for publication: publCIF (Westrip, 2009 ▶).

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809051691/hb5234sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809051691/hb5234Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Sn4Br2(C6H5)8O2(OH)2]	Z = 1
Mr = 1317.40	F(000) = 632
Triclinic, P1	Dx = 1.857 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 10.3759 (1) Å	Cell parameters from 7354 reflections
b = 10.8247 (1) Å	θ = 2.2–28.5°
c = 12.0341 (2) Å	µ = 3.83 mm−1
α = 77.1809 (7)°	T = 293 K
β = 65.4426 (7)°	Block, colourless
γ = 75.2040 (7)°	0.25 × 0.25 × 0.25 mm
V = 1178.26 (3) Å3

Bruker SMART APEX diffractometer	5309 independent reflections
Radiation source: fine-focus sealed tube	4449 reflections with I > 2σ(I)
graphite	Rint = 0.028
ω scans	θmax = 27.5°, θmin = 1.9°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −13→13
Tmin = 0.539, Tmax = 0.746	k = −14→13
10751 measured reflections	l = −15→15

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)] = 0.042	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.160	H-atom parameters constrained
S = 1.06	w = 1/[σ2(Fo2) + (0.0952P)2 + 4.7584P] where P = (Fo2 + 2Fc2)/3
5309 reflections	(Δ/σ)max = 0.001
262 parameters	Δρmax = 2.38 e Å−3
0 restraints	Δρmin = −1.38 e Å−3

	x	y	z	Uiso*/Ueq
Sn1	0.38584 (4)	0.45011 (4)	0.46172 (4)	0.03147 (14)
Sn2	0.52171 (5)	0.20525 (4)	0.63535 (4)	0.03495 (15)
Br1	0.70321 (9)	0.23768 (8)	0.72424 (7)	0.0508 (2)
O1	0.4796 (5)	0.6078 (4)	0.4416 (4)	0.0315 (8)
O2	0.3774 (5)	0.2494 (4)	0.5377 (4)	0.0364 (9)
H2O	0.3312	0.2022	0.5311	0.044*
C1	0.4869 (8)	0.4083 (7)	0.2777 (6)	0.0437 (15)
C2	0.6000 (10)	0.4680 (9)	0.1951 (7)	0.062 (2)
H2	0.6262	0.5303	0.2198	0.074*
C3	0.6748 (14)	0.4366 (14)	0.0765 (9)	0.092 (4)
H3	0.7537	0.4739	0.0230	0.111*
C4	0.6308 (17)	0.3499 (15)	0.0393 (11)	0.104 (5)
H4	0.6786	0.3303	−0.0410	0.125*
C5	0.5169 (15)	0.2913 (12)	0.1190 (11)	0.088 (4)
H5	0.4865	0.2338	0.0921	0.106*
C6	0.4471 (11)	0.3183 (9)	0.2404 (8)	0.060 (2)
H6	0.3736	0.2753	0.2959	0.072*
C7	0.1737 (7)	0.5207 (7)	0.5813 (6)	0.0379 (13)
C8	0.0633 (8)	0.4546 (8)	0.6167 (8)	0.0524 (18)
H8	0.0782	0.3810	0.5819	0.063*
C9	−0.0724 (10)	0.4978 (12)	0.7057 (10)	0.075 (3)
H9	−0.1485	0.4550	0.7284	0.090*
C10	−0.0900 (10)	0.6034 (13)	0.7578 (9)	0.082 (3)
H10	−0.1780	0.6296	0.8196	0.098*
C11	0.0158 (11)	0.6711 (12)	0.7228 (11)	0.084 (3)
H11	−0.0008	0.7451	0.7576	0.100*
C12	0.1506 (9)	0.6298 (9)	0.6340 (8)	0.0554 (19)
H12	0.2247	0.6754	0.6103	0.067*
C13	0.3559 (8)	0.1680 (7)	0.8092 (6)	0.0453 (15)
C14	0.3843 (12)	0.0721 (11)	0.8954 (9)	0.077 (3)
H14	0.4784	0.0286	0.8804	0.093*
C15	0.2745 (16)	0.0389 (14)	1.0052 (10)	0.103 (4)
H15	0.2949	−0.0282	1.0623	0.123*
C16	0.1375 (15)	0.1039 (13)	1.0295 (10)	0.091 (4)
H16	0.0637	0.0796	1.1022	0.109*
C17	0.1077 (13)	0.2043 (14)	0.9484 (10)	0.094 (4)
H17	0.0144	0.2512	0.9670	0.113*
C18	0.2175 (10)	0.2370 (10)	0.8367 (8)	0.065 (2)
H18	0.1971	0.3056	0.7809	0.078*
C19	0.6770 (7)	0.0737 (6)	0.5153 (6)	0.0388 (13)
C20	0.7810 (9)	−0.0145 (8)	0.5494 (8)	0.0527 (18)
H20	0.7787	−0.0227	0.6288	0.063*
C21	0.8893 (9)	−0.0909 (9)	0.4642 (9)	0.062 (2)
H21	0.9578	−0.1515	0.4879	0.074*
C22	0.8961 (9)	−0.0784 (8)	0.3475 (9)	0.059 (2)
H22	0.9705	−0.1285	0.2911	0.071*
C23	0.7926 (9)	0.0089 (8)	0.3123 (8)	0.0541 (19)
H23	0.7975	0.0177	0.2321	0.065*
C24	0.6816 (9)	0.0834 (7)	0.3962 (7)	0.0495 (17)
H24	0.6101	0.1399	0.3732	0.059*

	U11	U22	U33	U12	U13	U23
Sn1	0.0317 (2)	0.0315 (2)	0.0317 (2)	−0.00616 (16)	−0.01214 (17)	−0.00462 (15)
Sn2	0.0381 (2)	0.0287 (2)	0.0345 (2)	−0.00560 (17)	−0.01235 (18)	−0.00091 (16)
Br1	0.0555 (4)	0.0517 (4)	0.0531 (4)	−0.0067 (3)	−0.0305 (3)	−0.0063 (3)
O1	0.033 (2)	0.026 (2)	0.036 (2)	−0.0070 (16)	−0.0157 (17)	0.0008 (16)
O2	0.040 (2)	0.030 (2)	0.045 (2)	−0.0123 (18)	−0.0197 (19)	−0.0005 (17)
C1	0.055 (4)	0.039 (3)	0.033 (3)	0.000 (3)	−0.017 (3)	−0.008 (3)
C2	0.068 (5)	0.070 (6)	0.040 (4)	−0.024 (5)	−0.006 (4)	−0.010 (4)
C3	0.104 (9)	0.114 (10)	0.041 (5)	−0.033 (8)	−0.002 (5)	−0.014 (5)
C4	0.127 (11)	0.120 (11)	0.050 (6)	−0.001 (9)	−0.019 (7)	−0.036 (6)
C5	0.123 (10)	0.082 (7)	0.080 (7)	0.005 (7)	−0.055 (7)	−0.046 (6)
C6	0.069 (5)	0.061 (5)	0.061 (5)	−0.005 (4)	−0.032 (4)	−0.024 (4)
C7	0.031 (3)	0.041 (3)	0.038 (3)	−0.005 (3)	−0.012 (2)	−0.004 (3)
C8	0.039 (4)	0.049 (4)	0.066 (5)	−0.010 (3)	−0.017 (3)	−0.005 (3)
C9	0.044 (5)	0.096 (8)	0.077 (6)	−0.024 (5)	−0.016 (4)	0.002 (6)
C10	0.044 (5)	0.114 (9)	0.061 (6)	−0.008 (5)	0.006 (4)	−0.018 (6)
C11	0.058 (6)	0.086 (8)	0.090 (7)	−0.003 (5)	−0.001 (5)	−0.046 (6)
C12	0.042 (4)	0.059 (5)	0.060 (5)	−0.011 (4)	−0.007 (3)	−0.021 (4)
C13	0.051 (4)	0.043 (4)	0.038 (3)	−0.016 (3)	−0.010 (3)	−0.003 (3)
C14	0.075 (6)	0.073 (6)	0.059 (5)	−0.011 (5)	−0.019 (5)	0.023 (5)
C15	0.110 (10)	0.107 (10)	0.058 (6)	−0.033 (8)	−0.015 (6)	0.033 (6)
C16	0.101 (9)	0.094 (8)	0.049 (5)	−0.038 (7)	0.010 (5)	−0.009 (5)
C17	0.069 (7)	0.115 (10)	0.065 (6)	−0.025 (7)	0.016 (5)	−0.024 (7)
C18	0.058 (5)	0.068 (6)	0.053 (5)	−0.009 (4)	−0.009 (4)	−0.005 (4)
C19	0.036 (3)	0.030 (3)	0.050 (4)	−0.007 (3)	−0.016 (3)	−0.008 (3)
C20	0.054 (4)	0.046 (4)	0.060 (5)	−0.002 (3)	−0.025 (4)	−0.012 (3)
C21	0.051 (5)	0.048 (5)	0.087 (6)	0.011 (4)	−0.031 (4)	−0.024 (4)
C22	0.040 (4)	0.051 (5)	0.081 (6)	−0.003 (3)	−0.013 (4)	−0.023 (4)
C23	0.054 (4)	0.058 (5)	0.048 (4)	−0.018 (4)	−0.009 (3)	−0.014 (3)
C24	0.052 (4)	0.038 (4)	0.055 (4)	−0.002 (3)	−0.019 (3)	−0.010 (3)

Sn1—O1i	2.068 (4)	C9—H9	0.9300
Sn1—O1	2.095 (4)	C10—C11	1.345 (16)
Sn1—C1	2.117 (6)	C10—H10	0.9300
Sn1—C7	2.120 (6)	C11—C12	1.396 (12)
Sn1—O2	2.171 (4)	C11—H11	0.9300
Sn2—O1i	2.029 (4)	C12—H12	0.9300
Sn2—C13	2.118 (7)	C13—C14	1.365 (11)
Sn2—C19	2.126 (7)	C13—C18	1.377 (12)
Sn2—O2	2.167 (4)	C14—C15	1.385 (14)
Sn2—Br1	2.6444 (9)	C14—H14	0.9300
O1—Sn2i	2.029 (4)	C15—C16	1.355 (18)
O1—Sn1i	2.068 (4)	C15—H15	0.9300
O2—H2O	0.8200	C16—C17	1.356 (19)
C1—C6	1.369 (11)	C16—H16	0.9300
C1—C2	1.384 (11)	C17—C18	1.397 (13)
C2—C3	1.384 (12)	C17—H17	0.9300
C2—H2	0.9300	C18—H18	0.9300
C3—C4	1.365 (19)	C19—C20	1.383 (10)
C3—H3	0.9300	C19—C24	1.394 (11)
C4—C5	1.37 (2)	C20—C21	1.393 (11)
C4—H4	0.9300	C20—H20	0.9300
C5—C6	1.395 (13)	C21—C22	1.355 (13)
C5—H5	0.9300	C21—H21	0.9300
C6—H6	0.9300	C22—C23	1.381 (12)
C7—C12	1.384 (10)	C22—H22	0.9300
C7—C8	1.373 (10)	C23—C24	1.385 (11)
C8—C9	1.407 (12)	C23—H23	0.9300
C8—H8	0.9300	C24—H24	0.9300
C9—C10	1.360 (16)
O1i—Sn1—O1	73.05 (18)	C9—C8—H8	119.9
O1i—Sn1—C1	113.5 (2)	C10—C9—C8	118.7 (9)
O1—Sn1—C1	98.9 (2)	C10—C9—H9	120.6
O1i—Sn1—C7	109.8 (2)	C8—C9—H9	120.6
O1—Sn1—C7	98.4 (2)	C11—C10—C9	122.1 (9)
C1—Sn1—C7	136.4 (3)	C11—C10—H10	118.9
O1i—Sn1—O2	72.57 (17)	C9—C10—H10	118.9
O1—Sn1—O2	145.58 (17)	C10—C11—C12	119.7 (10)
C1—Sn1—O2	93.1 (2)	C10—C11—H11	120.2
C7—Sn1—O2	94.7 (2)	C12—C11—H11	120.2
O1i—Sn2—C13	116.9 (2)	C7—C12—C11	119.8 (8)
O1i—Sn2—C19	113.2 (2)	C7—C12—H12	120.1
C13—Sn2—C19	129.4 (3)	C11—C12—H12	120.1
O1i—Sn2—O2	73.38 (17)	C14—C13—C18	118.6 (8)
C13—Sn2—O2	93.3 (2)	C14—C13—Sn2	120.1 (7)
C19—Sn2—O2	94.0 (2)	C18—C13—Sn2	121.3 (6)
O1i—Sn2—Br1	86.33 (12)	C13—C14—C15	120.8 (10)
C13—Sn2—Br1	95.6 (2)	C13—C14—H14	119.6
C19—Sn2—Br1	94.25 (18)	C15—C14—H14	119.6
O2—Sn2—Br1	159.71 (12)	C16—C15—C14	120.1 (11)
Sn2i—O1—Sn1i	111.45 (19)	C16—C15—H15	120.0
Sn2i—O1—Sn1	141.6 (2)	C14—C15—H15	120.0
Sn1i—O1—Sn1	106.95 (18)	C17—C16—C15	120.3 (10)
Sn2—O2—Sn1	102.60 (18)	C17—C16—H16	119.9
Sn2—O2—H2O	128.7	C15—C16—H16	119.9
Sn1—O2—H2O	128.7	C16—C17—C18	119.8 (12)
C6—C1—C2	119.3 (7)	C16—C17—H17	120.1
C6—C1—Sn1	121.1 (6)	C18—C17—H17	120.1
C2—C1—Sn1	119.5 (6)	C13—C18—C17	120.2 (10)
C3—C2—C1	121.1 (9)	C13—C18—H18	119.9
C3—C2—H2	119.5	C17—C18—H18	119.9
C1—C2—H2	119.5	C20—C19—C24	119.3 (7)
C4—C3—C2	119.0 (11)	C20—C19—Sn2	121.2 (5)
C4—C3—H3	120.5	C24—C19—Sn2	119.4 (5)
C2—C3—H3	120.5	C19—C20—C21	119.6 (8)
C3—C4—C5	120.9 (10)	C19—C20—H20	120.2
C3—C4—H4	119.6	C21—C20—H20	120.2
C5—C4—H4	119.6	C22—C21—C20	121.0 (8)
C4—C5—C6	119.7 (11)	C22—C21—H21	119.5
C4—C5—H5	120.1	C20—C21—H21	119.5
C6—C5—H5	120.1	C21—C22—C23	119.9 (8)
C1—C6—C5	119.9 (10)	C21—C22—H22	120.0
C1—C6—H6	120.0	C23—C22—H22	120.0
C5—C6—H6	120.0	C24—C23—C22	120.1 (8)
C12—C7—C8	119.5 (7)	C24—C23—H23	119.9
C12—C7—Sn1	118.4 (5)	C22—C23—H23	119.9
C8—C7—Sn1	121.8 (5)	C23—C24—C19	120.0 (7)
C7—C8—C9	120.1 (9)	C23—C24—H24	120.0
C7—C8—H8	119.9	C19—C24—H24	120.0
O1i—Sn1—O1—Sn2i	−177.8 (5)	C12—C7—C8—C9	0.2 (12)
C1—Sn1—O1—Sn2i	70.2 (4)	Sn1—C7—C8—C9	173.6 (7)
C7—Sn1—O1—Sn2i	−69.5 (4)	C7—C8—C9—C10	−1.9 (15)
O2—Sn1—O1—Sn2i	179.3 (3)	C8—C9—C10—C11	3.2 (19)
O1i—Sn1—O1—Sn1i	0.0	C9—C10—C11—C12	−3(2)
C1—Sn1—O1—Sn1i	−112.0 (2)	C8—C7—C12—C11	0.2 (13)
C7—Sn1—O1—Sn1i	108.2 (2)	Sn1—C7—C12—C11	−173.4 (8)
O2—Sn1—O1—Sn1i	−2.9 (4)	C10—C11—C12—C7	1.0 (17)
O1i—Sn2—O2—Sn1	−0.23 (16)	O1i—Sn2—C13—C14	−143.7 (8)
C13—Sn2—O2—Sn1	116.9 (3)	C19—Sn2—C13—C14	45.3 (9)
C19—Sn2—O2—Sn1	−113.2 (2)	O2—Sn2—C13—C14	143.2 (8)
Br1—Sn2—O2—Sn1	0.7 (5)	Br1—Sn2—C13—C14	−55.0 (8)
O1i—Sn1—O2—Sn2	0.23 (16)	O1i—Sn2—C13—C18	37.9 (8)
O1—Sn1—O2—Sn2	3.2 (4)	C19—Sn2—C13—C18	−133.2 (7)
C1—Sn1—O2—Sn2	113.9 (3)	O2—Sn2—C13—C18	−35.2 (7)
C7—Sn1—O2—Sn2	−109.1 (2)	Br1—Sn2—C13—C18	126.6 (7)
O1i—Sn1—C1—C6	112.1 (6)	C18—C13—C14—C15	4.3 (17)
O1—Sn1—C1—C6	−172.6 (6)	Sn2—C13—C14—C15	−174.2 (11)
C7—Sn1—C1—C6	−60.4 (8)	C13—C14—C15—C16	−2(2)
O2—Sn1—C1—C6	39.7 (7)	C14—C15—C16—C17	−2(2)
O1i—Sn1—C1—C2	−64.6 (7)	C15—C16—C17—C18	3(2)
O1—Sn1—C1—C2	10.7 (7)	C14—C13—C18—C17	−3.3 (16)
C7—Sn1—C1—C2	122.9 (7)	Sn2—C13—C18—C17	175.2 (9)
O2—Sn1—C1—C2	−137.0 (7)	C16—C17—C18—C13	−0.3 (19)
C6—C1—C2—C3	−1.1 (15)	O1i—Sn2—C19—C20	123.9 (6)
Sn1—C1—C2—C3	175.6 (9)	C13—Sn2—C19—C20	−64.8 (7)
C1—C2—C3—C4	3.3 (19)	O2—Sn2—C19—C20	−162.4 (6)
C2—C3—C4—C5	−2(2)	Br1—Sn2—C19—C20	36.1 (6)
C3—C4—C5—C6	−1(2)	O1i—Sn2—C19—C24	−50.8 (6)
C2—C1—C6—C5	−2.4 (13)	C13—Sn2—C19—C24	120.5 (6)
Sn1—C1—C6—C5	−179.1 (8)	O2—Sn2—C19—C24	22.9 (6)
C4—C5—C6—C1	3.7 (17)	Br1—Sn2—C19—C24	−138.6 (6)
O1i—Sn1—C7—C12	63.6 (6)	C24—C19—C20—C21	0.7 (12)
O1—Sn1—C7—C12	−11.3 (6)	Sn2—C19—C20—C21	−174.0 (6)
C1—Sn1—C7—C12	−123.7 (6)	C19—C20—C21—C22	1.4 (14)
O2—Sn1—C7—C12	136.8 (6)	C20—C21—C22—C23	−1.7 (14)
O1i—Sn1—C7—C8	−109.8 (6)	C21—C22—C23—C24	−0.2 (13)
O1—Sn1—C7—C8	175.3 (6)	C22—C23—C24—C19	2.3 (12)
C1—Sn1—C7—C8	62.9 (7)	C20—C19—C24—C23	−2.5 (12)
O2—Sn1—C7—C8	−36.7 (6)	Sn2—C19—C24—C23	172.3 (6)

Table 1

Selected bond lengths (Å)

Sn1—O1i	2.068 (4)
Sn1—O1	2.095 (4)
Sn1—C1	2.117 (6)
Sn1—C7	2.120 (6)
Sn1—O2	2.171 (4)
Sn2—O1i	2.029 (4)
Sn2—C13	2.118 (7)
Sn2—C19	2.126 (7)
Sn2—O2	2.167 (4)
Sn2—Br1	2.6444 (9)

Symmetry code: (i) .