Literature DB >> 21582660

Di-μ-hydroxido-bis-[bromidodi-p-tolyl-tin(IV)].

Kong Mun Lo1, Seik Weng Ng.   

Abstract

The Sn atoms in the dinuclear title compound, [Sn(2)Br(2)(C(7)H(7))(4)(OH)(2)], exist in distorted trigonal-bipyramidal BrSnC(2)O(2) coordination geometries. Each of the two independent dinuclear mol-ecules comprising the asymmetric unit is disposed about a center of inversion. In the crystal, molecules are linked by an O-H⋯ hydrogen bond.

Entities:  

Year:  2009        PMID: 21582660      PMCID: PMC2969444          DOI: 10.1107/S1600536809019758

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN: 1600-5368


Related literature

For other dihalo-di-μ-hydoxotetra­organylditins, see: Anacona et al. (2003 ▶); Barba et al. (2007 ▶); Puff et al. (1984 ▶).

Experimental

Crystal data

[Sn2Br2(C7H7)4(OH)2] M = 795.72 Triclinic, a = 10.9971 (3) Å b = 11.5391 (3) Å c = 12.1969 (3) Å α = 77.092 (2)° β = 86.552 (2)° γ = 68.204 (2)° V = 1400.34 (6) Å3 Z = 2 Mo Kα radiation μ = 4.66 mm−1 T = 100 K 0.35 × 0.05 × 0.05 mm

Data collection

Bruker SMART APEX diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.292, T max = 0.800 9026 measured reflections 4871 independent reflections 3367 reflections with I > 2σ(I) R int = 0.056

Refinement

R[F 2 > 2σ(F 2)] = 0.076 wR(F 2) = 0.227 S = 1.05 4871 reflections 311 parameters 180 restraints H-atom parameters constrained Δρmax = 2.96 e Å−3 Δρmin = −3.19 e Å−3 Data collection: APEX2 (Bruker, 2007 ▶); cell refinement: SAINT (Bruker, 2007 ▶); 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/S1600536809019758/tk2460sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809019758/tk2460Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Sn2Br2(C7H7)4(OH)2]Z = 2
Mr = 795.72F(000) = 768
Triclinic, P1Dx = 1.887 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 10.9971 (3) ÅCell parameters from 3015 reflections
b = 11.5391 (3) Åθ = 2.2–28.0°
c = 12.1969 (3) ŵ = 4.66 mm1
α = 77.092 (2)°T = 100 K
β = 86.552 (2)°Plate, colorless
γ = 68.204 (2)°0.35 × 0.05 × 0.05 mm
V = 1400.34 (6) Å3
Bruker SMART APEX diffractometer4871 independent reflections
Radiation source: fine-focus sealed tube3367 reflections with I > 2σ(I)
graphiteRint = 0.056
ω scansθmax = 25.0°, θmin = 1.7°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −13→13
Tmin = 0.292, Tmax = 0.800k = −12→13
9026 measured reflectionsl = −14→14
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.076Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.227H-atom parameters constrained
S = 1.05w = 1/[σ2(Fo2) + (0.1452P)2] where P = (Fo2 + 2Fc2)/3
4871 reflections(Δ/σ)max = 0.001
311 parametersΔρmax = 2.96 e Å3
180 restraintsΔρmin = −3.19 e Å3
xyzUiso*/Ueq
Sn10.62921 (7)0.55224 (9)0.51125 (6)0.0230 (3)
Sn20.64941 (7)0.38277 (9)0.05546 (6)0.0247 (3)
Br10.68040 (11)0.63918 (14)0.67783 (9)0.0280 (4)
Br20.67660 (12)0.23425 (14)0.25580 (10)0.0302 (4)
O10.4708 (7)0.5278 (8)0.5909 (6)0.0248 (19)
H10.44580.54530.65380.030*
O20.4555 (7)0.4658 (8)0.0890 (6)0.0244 (19)
H20.42060.44510.14960.029*
C10.5776 (11)0.7262 (12)0.3905 (10)0.024 (3)
C20.6189 (12)0.7250 (13)0.2814 (10)0.029 (3)
H2a0.66890.64690.25990.035*
C30.5850 (12)0.8423 (14)0.2031 (11)0.031 (3)
H30.61530.84160.12850.038*
C40.5107 (11)0.9574 (13)0.2283 (10)0.029 (3)
C50.4709 (12)0.9557 (13)0.3400 (10)0.029 (3)
H50.41971.03400.36060.034*
C60.5041 (11)0.8434 (13)0.4206 (10)0.028 (3)
H60.47770.84490.49600.033*
C70.4664 (13)1.0812 (15)0.1414 (11)0.039 (3)
H7A0.53651.08170.08790.058*
H7B0.44581.15300.17860.058*
H7C0.38811.08950.10110.058*
C80.8096 (11)0.3956 (13)0.5251 (10)0.026 (3)
C90.8241 (12)0.2834 (13)0.4902 (10)0.031 (3)
H90.74960.27430.46310.037*
C100.9453 (13)0.1859 (15)0.4946 (11)0.036 (3)
H100.95350.11070.47020.043*
C111.0547 (12)0.1972 (14)0.5344 (10)0.031 (3)
C121.0404 (13)0.3050 (15)0.5719 (12)0.040 (4)
H121.11430.31200.60250.048*
C130.9190 (13)0.4043 (16)0.5658 (12)0.041 (4)
H130.91170.47920.59010.049*
C141.1892 (13)0.0913 (16)0.5399 (13)0.045 (4)
H14A1.24570.12050.48440.067*
H14B1.18020.01550.52340.067*
H14C1.22820.06980.61540.067*
C150.7678 (11)0.4819 (14)0.0875 (10)0.028 (3)
C160.8608 (11)0.4277 (12)0.1749 (9)0.023 (3)
H160.86760.34920.22450.027*
C170.9444 (12)0.4905 (13)0.1889 (10)0.030 (3)
H171.00810.45280.24860.035*
C180.9376 (12)0.6030 (14)0.1205 (11)0.032 (3)
C190.8446 (12)0.6556 (15)0.0312 (11)0.035 (3)
H190.83850.7338−0.01860.042*
C200.7623 (12)0.5951 (13)0.0151 (10)0.031 (3)
H200.70100.6314−0.04630.037*
C211.0280 (13)0.6689 (15)0.1349 (12)0.040 (4)
H21A1.05360.70540.06090.060*
H21B1.10630.60700.17830.060*
H21C0.98330.73730.17510.060*
C220.7048 (11)0.2359 (13)−0.0370 (10)0.027 (3)
C230.6804 (12)0.2653 (14)−0.1532 (10)0.030 (3)
H230.62830.3495−0.19090.036*
C240.7342 (13)0.1684 (14)−0.2122 (10)0.033 (3)
H240.71310.1866−0.29010.039*
C250.8156 (13)0.0490 (15)−0.1629 (11)0.035 (3)
C260.8421 (13)0.0196 (15)−0.0484 (12)0.037 (3)
H260.8979−0.0639−0.01230.045*
C270.7869 (12)0.1125 (13)0.0126 (10)0.031 (3)
H270.80530.09180.09120.037*
C280.8804 (14)−0.0516 (15)−0.2323 (12)0.041 (4)
H28A0.9194−0.0147−0.29870.061*
H28B0.8146−0.0799−0.25630.061*
H28C0.9490−0.1248−0.18660.061*
U11U22U33U12U13U23
Sn10.0242 (4)0.0333 (6)0.0114 (4)−0.0063 (4)0.0016 (3)−0.0123 (4)
Sn20.0272 (5)0.0359 (6)0.0117 (4)−0.0082 (4)0.0011 (3)−0.0127 (4)
Br10.0312 (6)0.0416 (9)0.0135 (6)−0.0108 (6)0.0014 (5)−0.0155 (6)
Br20.0346 (7)0.0402 (9)0.0134 (6)−0.0085 (6)0.0002 (5)−0.0104 (6)
O10.027 (4)0.037 (5)0.012 (4)−0.009 (4)0.005 (3)−0.014 (4)
O20.024 (4)0.034 (5)0.014 (4)−0.007 (3)0.003 (3)−0.012 (3)
C10.025 (5)0.025 (6)0.017 (5)−0.002 (5)−0.005 (4)−0.004 (5)
C20.031 (6)0.031 (7)0.022 (6)−0.008 (5)−0.002 (4)−0.005 (5)
C30.033 (6)0.039 (7)0.023 (6)−0.010 (5)0.003 (5)−0.014 (5)
C40.029 (5)0.036 (7)0.022 (5)−0.007 (5)−0.005 (4)−0.014 (5)
C50.029 (5)0.034 (7)0.024 (6)−0.008 (5)−0.001 (4)−0.016 (5)
C60.029 (5)0.036 (7)0.016 (5)−0.005 (5)−0.001 (4)−0.013 (5)
C70.038 (6)0.046 (7)0.030 (6)−0.013 (5)0.000 (5)−0.009 (6)
C80.024 (5)0.036 (7)0.015 (5)−0.002 (5)0.004 (4)−0.014 (5)
C90.033 (6)0.033 (7)0.024 (6)−0.006 (5)−0.004 (5)−0.010 (5)
C100.043 (6)0.042 (7)0.026 (6)−0.011 (5)−0.002 (5)−0.020 (5)
C110.031 (6)0.040 (7)0.018 (5)−0.010 (5)0.002 (4)−0.005 (5)
C120.034 (6)0.051 (8)0.035 (6)−0.009 (5)−0.002 (5)−0.018 (6)
C130.038 (6)0.047 (8)0.042 (7)−0.015 (6)0.003 (5)−0.019 (6)
C140.042 (6)0.046 (8)0.040 (7)−0.005 (6)−0.001 (5)−0.014 (6)
C150.023 (5)0.040 (7)0.024 (6)−0.011 (5)0.005 (4)−0.018 (5)
C160.028 (5)0.025 (6)0.014 (5)−0.005 (5)0.001 (4)−0.011 (5)
C170.030 (5)0.039 (7)0.021 (5)−0.010 (5)0.004 (4)−0.017 (5)
C180.033 (6)0.038 (7)0.027 (6)−0.008 (5)0.009 (5)−0.019 (5)
C190.037 (6)0.041 (7)0.027 (6)−0.015 (5)0.003 (5)−0.008 (5)
C200.032 (6)0.041 (7)0.016 (5)−0.004 (5)−0.009 (4)−0.011 (5)
C210.040 (6)0.051 (8)0.036 (6)−0.020 (6)−0.003 (5)−0.016 (6)
C220.030 (5)0.032 (7)0.022 (5)−0.007 (5)−0.002 (4)−0.018 (5)
C230.038 (6)0.036 (7)0.014 (5)−0.010 (5)−0.003 (4)−0.009 (5)
C240.043 (6)0.036 (7)0.020 (5)−0.007 (5)−0.003 (5)−0.019 (5)
C250.041 (6)0.045 (7)0.025 (6)−0.014 (5)0.000 (5)−0.022 (5)
C260.034 (6)0.039 (7)0.037 (6)−0.009 (5)0.000 (5)−0.012 (6)
C270.043 (6)0.031 (7)0.016 (5)−0.008 (5)−0.007 (5)−0.009 (5)
C280.048 (6)0.044 (7)0.031 (6)−0.013 (6)0.005 (5)−0.021 (6)
Sn1—O12.024 (8)C11—C141.523 (18)
Sn1—C82.115 (12)C12—C131.39 (2)
Sn1—C12.111 (12)C12—H120.9500
Sn1—O1i2.248 (8)C13—H130.9500
Sn1—Br12.6304 (14)C14—H14A0.9800
Sn2—O22.046 (8)C14—H14B0.9800
Sn2—C222.126 (13)C14—H14C0.9800
Sn2—C152.127 (13)C15—C201.386 (19)
Sn2—O2ii2.205 (8)C15—C161.390 (16)
Sn2—Br22.6141 (15)C16—C171.402 (18)
O1—Sn1i2.248 (8)C16—H160.9500
O1—H10.8400C17—C181.357 (19)
O2—Sn2ii2.205 (8)C17—H170.9500
O2—H20.8400C18—C191.406 (18)
C1—C21.381 (17)C18—C211.496 (19)
C1—C61.411 (18)C19—C201.378 (19)
C2—C31.405 (18)C19—H190.9500
C2—H2a0.9500C20—H200.9500
C3—C41.368 (19)C21—H21A0.9800
C3—H30.9500C21—H21B0.9800
C4—C51.404 (17)C21—H21C0.9800
C4—C71.507 (19)C22—C271.391 (18)
C5—C61.380 (18)C22—C231.400 (16)
C5—H50.9500C23—C241.390 (19)
C6—H60.9500C23—H230.9500
C7—H7A0.9800C24—C251.357 (19)
C7—H7B0.9800C24—H240.9500
C7—H7C0.9800C25—C261.383 (19)
C8—C131.374 (18)C25—C281.525 (19)
C8—C91.403 (19)C26—C271.37 (2)
C9—C101.383 (18)C26—H260.9500
C9—H90.9500C27—H270.9500
C10—C111.384 (18)C28—H28A0.9800
C10—H100.9500C28—H28B0.9800
C11—C121.37 (2)C28—H28C0.9800
O1—Sn1—C8119.8 (4)C10—C11—C14121.3 (14)
O1—Sn1—C1112.0 (4)C11—C12—C13120.8 (13)
C8—Sn1—C1126.5 (5)C11—C12—H12119.6
O1—Sn1—O1i69.1 (3)C13—C12—H12119.6
C8—Sn1—O1i94.3 (4)C8—C13—C12121.1 (15)
C1—Sn1—O1i91.6 (4)C8—C13—H13119.5
O1—Sn1—Br190.9 (2)C12—C13—H13119.5
C8—Sn1—Br195.4 (3)C11—C14—H14A109.5
C1—Sn1—Br196.5 (3)C11—C14—H14B109.5
O1i—Sn1—Br1160.0 (2)H14A—C14—H14B109.5
O2—Sn2—C22118.3 (4)C11—C14—H14C109.5
O2—Sn2—C15114.3 (4)H14A—C14—H14C109.5
C22—Sn2—C15126.0 (5)H14B—C14—H14C109.5
O2—Sn2—O2ii69.2 (4)C20—C15—C16119.0 (12)
C22—Sn2—O2ii93.8 (4)C20—C15—Sn2120.5 (9)
C15—Sn2—O2ii93.7 (4)C16—C15—Sn2120.3 (10)
O2—Sn2—Br287.4 (2)C15—C16—C17119.1 (12)
C22—Sn2—Br296.9 (3)C15—C16—H16120.4
C15—Sn2—Br296.7 (3)C17—C16—H16120.4
O2ii—Sn2—Br2156.6 (2)C18—C17—C16122.4 (12)
Sn1—O1—Sn1i110.9 (3)C18—C17—H17118.8
Sn1—O1—H1124.6C16—C17—H17118.8
Sn1i—O1—H1124.6C17—C18—C19117.8 (13)
Sn2—O2—Sn2ii110.8 (4)C17—C18—C21122.2 (12)
Sn2—O2—H2124.6C19—C18—C21119.9 (13)
Sn2ii—O2—H2124.6C20—C19—C18120.8 (14)
C2—C1—C6119.9 (11)C20—C19—H19119.6
C2—C1—Sn1119.4 (10)C18—C19—H19119.6
C6—C1—Sn1120.7 (9)C19—C20—C15120.8 (11)
C1—C2—C3118.2 (13)C19—C20—H20119.6
C1—C2—H2a120.9C15—C20—H20119.6
C3—C2—H2a120.9C18—C21—H21A109.5
C4—C3—C2123.6 (12)C18—C21—H21B109.5
C4—C3—H3118.2H21A—C21—H21B109.5
C2—C3—H3118.2C18—C21—H21C109.5
C3—C4—C5116.9 (13)H21A—C21—H21C109.5
C3—C4—C7123.0 (12)H21B—C21—H21C109.5
C5—C4—C7120.0 (13)C27—C22—C23118.1 (12)
C6—C5—C4121.7 (13)C27—C22—Sn2120.1 (9)
C6—C5—H5119.2C23—C22—Sn2120.8 (10)
C4—C5—H5119.2C24—C23—C22118.5 (12)
C5—C6—C1119.7 (11)C24—C23—H23120.8
C5—C6—H6120.2C22—C23—H23120.8
C1—C6—H6120.2C25—C24—C23122.6 (12)
C4—C7—H7A109.5C25—C24—H24118.7
C4—C7—H7B109.5C23—C24—H24118.7
H7A—C7—H7B109.5C24—C25—C26119.2 (13)
C4—C7—H7C109.5C24—C25—C28120.9 (12)
H7A—C7—H7C109.5C26—C25—C28119.8 (13)
H7B—C7—H7C109.5C27—C26—C25119.3 (13)
C13—C8—C9117.9 (12)C27—C26—H26120.4
C13—C8—Sn1119.5 (11)C25—C26—H26120.4
C9—C8—Sn1122.6 (9)C26—C27—C22122.2 (12)
C10—C9—C8120.9 (12)C26—C27—H27118.9
C10—C9—H9119.5C22—C27—H27118.9
C8—C9—H9119.5C25—C28—H28A109.5
C11—C10—C9120.3 (14)C25—C28—H28B109.5
C11—C10—H10119.8H28A—C28—H28B109.5
C9—C10—H10119.8C25—C28—H28C109.5
C12—C11—C10119.0 (12)H28A—C28—H28C109.5
C12—C11—C14119.6 (12)H28B—C28—H28C109.5
C8—Sn1—O1—Sn1i−82.8 (5)C14—C11—C12—C13178.7 (13)
C1—Sn1—O1—Sn1i83.0 (5)C9—C8—C13—C120(2)
O1i—Sn1—O1—Sn1i0.0Sn1—C8—C13—C12−177.5 (11)
Br1—Sn1—O1—Sn1i−179.6 (3)C11—C12—C13—C82(2)
C22—Sn2—O2—Sn2ii−82.9 (6)O2—Sn2—C15—C20−74.5 (10)
C15—Sn2—O2—Sn2ii84.5 (5)C22—Sn2—C15—C2091.8 (11)
O2ii—Sn2—O2—Sn2ii0.0O2ii—Sn2—C15—C20−5.6 (10)
Br2—Sn2—O2—Sn2ii−179.4 (3)Br2—Sn2—C15—C20−164.6 (10)
O1—Sn1—C1—C2−127.0 (9)O2—Sn2—C15—C16111.9 (10)
C8—Sn1—C1—C237.7 (12)C22—Sn2—C15—C16−81.8 (11)
O1i—Sn1—C1—C2−58.9 (10)O2ii—Sn2—C15—C16−179.3 (9)
Br1—Sn1—C1—C2139.4 (9)Br2—Sn2—C15—C1621.8 (10)
O1—Sn1—C1—C654.4 (11)C20—C15—C16—C171.4 (18)
C8—Sn1—C1—C6−140.9 (9)Sn2—C15—C16—C17175.2 (9)
O1i—Sn1—C1—C6122.5 (10)C15—C16—C17—C180.3 (19)
Br1—Sn1—C1—C6−39.3 (10)C16—C17—C18—C19−1.4 (19)
C6—C1—C2—C3−0.4 (18)C16—C17—C18—C21−179.3 (12)
Sn1—C1—C2—C3−179.0 (9)C17—C18—C19—C201(2)
C1—C2—C3—C4−1.6 (19)C21—C18—C19—C20178.7 (13)
C2—C3—C4—C52.0 (19)C18—C19—C20—C151(2)
C2—C3—C4—C7−175.1 (12)C16—C15—C20—C19−2.0 (19)
C3—C4—C5—C6−0.4 (19)Sn2—C15—C20—C19−175.8 (10)
C7—C4—C5—C6176.8 (11)O2—Sn2—C22—C27−116.7 (10)
C4—C5—C6—C1−1.4 (18)C15—Sn2—C22—C2777.5 (12)
C2—C1—C6—C51.8 (18)O2ii—Sn2—C22—C27174.9 (10)
Sn1—C1—C6—C5−179.6 (9)Br2—Sn2—C22—C27−25.9 (10)
O1—Sn1—C8—C13−123.0 (10)O2—Sn2—C22—C2375.3 (11)
C1—Sn1—C8—C1373.4 (12)C15—Sn2—C22—C23−90.5 (11)
O1i—Sn1—C8—C13168.7 (10)O2ii—Sn2—C22—C236.9 (10)
Br1—Sn1—C8—C13−28.8 (11)Br2—Sn2—C22—C23166.0 (10)
O1—Sn1—C8—C959.6 (11)C27—C22—C23—C243.0 (19)
C1—Sn1—C8—C9−104.0 (11)Sn2—C22—C23—C24171.3 (10)
O1i—Sn1—C8—C9−8.8 (10)C22—C23—C24—C25−4(2)
Br1—Sn1—C8—C9153.7 (10)C23—C24—C25—C263(2)
C13—C8—C9—C10−1.3 (19)C23—C24—C25—C28−175.5 (13)
Sn1—C8—C9—C10176.3 (10)C24—C25—C26—C27−1(2)
C8—C9—C10—C110(2)C28—C25—C26—C27177.6 (13)
C9—C10—C11—C122(2)C25—C26—C27—C220(2)
C9—C10—C11—C14−179.9 (12)C23—C22—C27—C26−1(2)
C10—C11—C12—C13−3(2)Sn2—C22—C27—C26−169.4 (11)
D—H···AD—HH···AD···AD—H···A
O2—H2···Br1i0.842.493.329 (8)173
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯ADAD—H⋯A
O2—H2⋯Br1i0.842.493.329 (8)173

Symmetry code: (i) .

  1 in total

1.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

  1 in total
  1 in total

1.  Di-tert-butyl-tin(IV)-hydroxide-iodide, t Bu2Sn(OH)I, the last missing member in the series of pure di-tert-butyl-tin(IV)-hydroxide-halides.

Authors:  Hans Reuter
Journal:  Acta Crystallogr E Crystallogr Commun       Date:  2022-05-20
  1 in total

北京卡尤迪生物科技股份有限公司 © 2022-2023.