PMCCPMCCPMCC

Search tips
Search criteria 

Advanced

 
Logo of actaeInternational Union of Crystallographysearchopen accessarticle submissionjournal home pagethis article
 
Acta Crystallogr Sect E Struct Rep Online. 2010 November 1; 66(Pt 11): m1372.
Published online 2010 October 9. doi:  10.1107/S1600536810039450
PMCID: PMC3009232

Tribenzylbis(triphenyl­arsine oxide-κO)tin(IV) tetra­phenyl­borate

Abstract

The crystal structure of the title salt, [Sn(C7H7)3(C18H15AsO)2][B(C6H5)4], consists of discrete cations and anions; the tin atom of the cation is five-coordinated in a distorted trans-C3SnO2 trigonal-bipyramidal geometry [summation of C–Sn–C angles 360.0 (3)° and O–Sn–O angle 173.1 (1)°]. The structure contains voids of 113 (19) Å3, but no solvent mol­ecule could reasonably be located there.

Related literature

For the structure of a related triorganotin tetra­phenyl­borate, see: Ng et al. (1989 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-66-m1372-scheme1.jpg

Experimental

Crystal data

  • [Sn(C7H7)3(C18H15AsO)2](C24H20B)
  • M r = 1355.72
  • Triclinic, An external file that holds a picture, illustration, etc.
Object name is e-66-m1372-efi1.jpg
  • a = 14.3288 (7) Å
  • b = 14.9477 (7) Å
  • c = 19.0994 (9) Å
  • α = 69.220 (1)°
  • β = 73.972 (1)°
  • γ = 62.683 (1)°
  • V = 3366.4 (3) Å3
  • Z = 2
  • Mo Kα radiation
  • μ = 1.40 mm−1
  • T = 100 K
  • 0.1 × 0.1 × 0.1 mm

Data collection

  • Bruker SMART APEX diffractometer
  • Absorption correction: multi-scan (TWINABS; Bruker, 2009 [triangle]) T min = 0.788, T max = 1.000
  • 76329 measured reflections
  • 17932 independent reflections
  • 12383 reflections with I > 2σ(I)
  • R int = 0.068

Refinement

  • R[F 2 > 2σ(F 2)] = 0.050
  • wR(F 2) = 0.170
  • S = 0.99
  • 17932 reflections
  • 629 parameters
  • H-atom parameters constrained
  • Δρmax = 2.06 e Å−3
  • Δρmin = −1.10 e Å−3

Data collection: APEX2 (Bruker, 2009 [triangle]); cell refinement: SAINT (Bruker, 2009 [triangle]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: X-SEED (Barbour, 2001 [triangle]); software used to prepare material for publication: publCIF (Westrip, 2010 [triangle]).

Table 1
Selected geometric parameters (Å, °)

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810039450/xu5034sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810039450/xu5034Isup2.hkl

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

Acknowledgments

We thank the University of Malaya (RG020/00AFr) for supporting this study.

supplementary crystallographic information

Comment

A suggestion for improving the aqueous solubility of triorganotin(IV) compounds, R3SnX, involves exchanging the X residue by the non-nucleophilic tetraphenylborate anion to generate a salt. However, to prevent aggregation into an oligopolymer, the triorganotin species itself must be stabilized by coordination by two neutral ligands. Of the number of such compounds synthesized, the crystal structure of only one, namely, [(p-ClC6H4)Ph2Sn(Ph3AsO)2][BPh4], has been reported (Ng et al., 1989). The compound exists as non-interacting cations and anions; the tin atom of the cation is five-coordinate in a trans-C3SnO2 trigonal bipyramidal geometry. The title tribenzyltin adduct (Scheme I, Figs. 1 & 2) is a similar non-interacting salt. The trans angle at tin is nearly linear, and the Sn–O–As skeleton is also nearly linear (Table 1).

Experimental

Tribenzyltin chloride (0.21 g, 0.5 mmol), triphenylarsine oxide (0.32 g, 1 mmol) and sodium tetraphenylborate (0.17 g, 0.5 mmol) were dissolved in ethanol (100 ml). The solution was heated for an hour. Then the mixture was filtered and the filtrate evaporated at room temperature to obtain the colorless crystals.

Refinement

Carbon-bound H-atoms were placed in calculated positions (C—H 0.95 Å) and were included in the refinement in the riding model approximation, with U(H) set to 1.2U(C). All aromatic rings were refined as rigid hexagons of 1.39 Å sides.

The final difference Fourier map had a high peak at 3.22 Å from H39 and hole at 0.83 Å from Sn1. The peak could not be refined as a water O atom, and is probably an artifical of twinning. The structure contains a voids of 113 (19) Å3, but no solvent molecule(s) could be located there reasonably.

Figures

Fig. 1.
Thermal ellipsoid plot (Barbour, 2001) of the cation of [Sn(C7H7)3(C18H15AsO)2] [B(C6H5)4] at the 70% probability level; hydrogen atoms are drawn as spheres of arbitrary radius.
Fig. 2.
Thermal ellipsoid plot (Barbour, 2001) of the anion of [Sn(C7H7)3(C18H15AsO)2] [B(C6H5)4] at the 70% probability level; hydrogen atoms are drawn as spheres of arbitrary radius.

Crystal data

[Sn(C7H7)3(C18H15AsO)](C24H20B)Z = 2
Mr = 1355.72F(000) = 1388
Triclinic, P1Dx = 1.337 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 14.3288 (7) ÅCell parameters from 4476 reflections
b = 14.9477 (7) Åθ = 2.3–28.2°
c = 19.0994 (9) ŵ = 1.40 mm1
α = 69.220 (1)°T = 100 K
β = 73.972 (1)°Cube, colorless
γ = 62.683 (1)°0.1 × 0.1 × 0.1 mm
V = 3366.4 (3) Å3

Data collection

Bruker SMART APEX diffractometer17932 independent reflections
Radiation source: fine-focus sealed tube12383 reflections with I > 2σ(I)
graphiteRint = 0.068
ω scansθmax = 27.5°, θmin = 1.2°
Absorption correction: multi-scan (TWINABS; Bruker, 2009)h = −17→18
Tmin = 0.788, Tmax = 1.000k = −17→19
76329 measured reflectionsl = 0→24

Refinement

Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.050Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.170H-atom parameters constrained
S = 0.99w = 1/[σ2(Fo2) + (0.1059P)2] where P = (Fo2 + 2Fc2)/3
17932 reflections(Δ/σ)max = 0.001
629 parametersΔρmax = 2.06 e Å3
0 restraintsΔρmin = −1.10 e Å3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

xyzUiso*/Ueq
Sn10.68359 (3)0.68691 (2)0.973010 (17)0.01457 (9)
As10.58668 (4)0.62392 (4)1.18383 (3)0.01939 (13)
As20.77629 (4)0.73481 (4)0.76041 (3)0.01624 (12)
O10.6109 (3)0.6565 (3)1.09025 (18)0.0275 (9)
O20.7611 (3)0.6987 (3)0.85374 (18)0.0239 (8)
B10.8611 (5)0.8755 (5)0.3893 (3)0.0213 (12)
C10.6220 (5)0.8523 (4)0.9593 (3)0.0271 (12)
H1A0.64720.88620.90750.033*
H1B0.54360.88130.96520.033*
C20.6556 (3)0.8774 (3)1.01589 (17)0.0260 (12)
C30.5848 (2)0.9025 (3)1.07932 (19)0.0261 (12)
H30.51510.90591.08600.031*
C40.6159 (2)0.9228 (3)1.13289 (16)0.0298 (13)
H40.56750.93991.17620.036*
C50.7177 (3)0.9179 (3)1.12305 (18)0.0300 (13)
H50.73900.93171.15970.036*
C60.7885 (2)0.8927 (3)1.0596 (2)0.0324 (13)
H60.85820.88941.05290.039*
C70.7574 (2)0.8725 (3)1.00605 (16)0.0283 (12)
H70.80580.85530.96270.034*
C80.8415 (4)0.6017 (4)1.0023 (3)0.0193 (10)
H8A0.89030.62740.96130.023*
H8B0.84340.61501.04890.023*
C90.8804 (3)0.48387 (18)1.01481 (17)0.0211 (11)
C100.8659 (3)0.4197 (2)1.08652 (14)0.0295 (13)
H100.83470.44841.12870.035*
C110.8970 (3)0.3137 (2)1.09650 (15)0.0364 (14)
H110.88710.26981.14550.044*
C120.9425 (3)0.27177 (18)1.0348 (2)0.0321 (13)
H120.96380.19931.04160.038*
C130.9570 (3)0.3359 (2)0.96306 (16)0.0270 (12)
H130.98820.30730.92090.032*
C140.9259 (3)0.4420 (2)0.95308 (13)0.0233 (11)
H140.93580.48580.90410.028*
C150.5900 (4)0.6224 (4)0.9532 (3)0.0204 (10)
H15A0.59390.63640.89800.024*
H15B0.62080.54570.97470.024*
C160.4742 (2)0.6659 (3)0.98714 (18)0.0210 (11)
C170.4353 (3)0.6003 (2)1.04697 (19)0.0319 (13)
H170.48090.52951.06600.038*
C180.3298 (3)0.6384 (3)1.07905 (18)0.0447 (17)
H180.30320.59351.11990.054*
C190.2631 (2)0.7420 (3)1.0513 (2)0.0452 (17)
H190.19100.76801.07320.054*
C200.3020 (2)0.8076 (2)0.9914 (2)0.0382 (15)
H200.25640.87840.97250.046*
C210.4075 (3)0.7696 (2)0.95937 (16)0.0302 (13)
H210.43410.81440.91850.036*
C220.4714 (2)0.7369 (3)1.21711 (19)0.0233 (11)
C230.4759 (3)0.7645 (3)1.2780 (2)0.0311 (13)
H230.53790.72841.30210.037*
C240.3896 (3)0.8448 (3)1.3037 (2)0.0439 (16)
H240.39260.86371.34530.053*
C250.2988 (3)0.8977 (3)1.2684 (2)0.054 (2)
H250.23980.95261.28600.065*
C260.2943 (3)0.8701 (3)1.2075 (2)0.0545 (19)
H260.23220.90621.18350.065*
C270.3806 (3)0.7897 (3)1.18188 (19)0.0414 (15)
H270.37750.77091.14030.050*
C280.7089 (2)0.5866 (3)1.22728 (17)0.0220 (11)
C290.7405 (3)0.4986 (2)1.28777 (18)0.0271 (12)
H290.70030.45711.30860.032*
C300.8308 (3)0.4715 (2)1.31782 (16)0.0334 (14)
H300.85230.41141.35920.040*
C310.8896 (2)0.5323 (3)1.28739 (19)0.0302 (13)
H310.95130.51381.30790.036*
C320.8581 (3)0.6202 (3)1.22690 (18)0.0297 (13)
H320.89830.66181.20610.036*
C330.7678 (3)0.6474 (2)1.19685 (15)0.0236 (11)
H330.74620.70751.15550.028*
C340.5484 (3)0.5070 (2)1.22101 (19)0.0230 (11)
C350.6048 (3)0.4222 (3)1.19022 (19)0.0374 (14)
H350.65990.42411.14910.045*
C360.5808 (3)0.3347 (2)1.2196 (2)0.0441 (16)
H360.61940.27671.19860.053*
C370.5003 (3)0.3319 (3)1.2798 (2)0.0420 (16)
H370.48380.27211.29990.050*
C380.4438 (3)0.4167 (3)1.31061 (19)0.0428 (16)
H380.38880.41481.35180.051*
C390.4678 (3)0.5043 (2)1.2812 (2)0.0345 (14)
H390.42920.56221.30230.041*
C400.8874 (2)0.7819 (3)0.72386 (17)0.0203 (10)
C410.9008 (3)0.8327 (3)0.76640 (15)0.0293 (12)
H410.85620.84100.81280.035*
C420.9793 (3)0.8713 (3)0.74100 (19)0.0344 (14)
H420.98840.90610.77010.041*
C431.0445 (2)0.8591 (3)0.67305 (19)0.0308 (13)
H431.09820.88560.65570.037*
C441.0311 (3)0.8083 (3)0.63051 (15)0.0321 (13)
H441.07570.80000.58410.038*
C450.9526 (3)0.7696 (3)0.65592 (16)0.0257 (12)
H450.94350.73490.62680.031*
C460.8060 (3)0.61942 (19)0.72419 (16)0.0176 (10)
C470.8266 (3)0.5212 (2)0.77497 (12)0.0217 (11)
H470.82390.51260.82710.026*
C480.8510 (3)0.43569 (18)0.74944 (15)0.0254 (11)
H480.86510.36860.78410.030*
C490.8549 (3)0.4483 (2)0.67314 (17)0.0246 (11)
H490.87160.38990.65570.030*
C500.8344 (3)0.5465 (2)0.62236 (12)0.0253 (12)
H500.83700.55510.57020.030*
C510.8099 (3)0.63205 (18)0.64788 (14)0.0230 (11)
H510.79580.69920.61320.028*
C520.6509 (2)0.8450 (2)0.72226 (17)0.0182 (10)
C530.5530 (2)0.8515 (2)0.76437 (14)0.0231 (11)
H530.54950.80380.81270.028*
C540.46027 (19)0.9277 (3)0.73580 (17)0.0263 (12)
H540.39340.93210.76460.032*
C550.4654 (2)0.9974 (2)0.66512 (18)0.0274 (12)
H550.40201.04950.64560.033*
C560.5633 (3)0.9910 (2)0.62301 (14)0.0281 (12)
H560.56681.03870.57470.034*
C570.6561 (2)0.9148 (3)0.65158 (16)0.0225 (11)
H570.72300.91040.62280.027*
C580.9777 (2)0.7831 (2)0.41918 (18)0.0221 (11)
C591.0692 (3)0.8022 (2)0.39184 (17)0.0251 (11)
H591.06690.86540.35490.030*
C601.1642 (2)0.7287 (3)0.41855 (19)0.0301 (13)
H601.22680.74170.39990.036*
C611.1677 (2)0.6362 (2)0.47260 (19)0.0319 (13)
H611.23260.58600.49090.038*
C621.0762 (3)0.6172 (2)0.49995 (16)0.0270 (12)
H621.07850.55400.53690.032*
C630.9812 (2)0.6906 (2)0.47324 (17)0.0227 (11)
H630.91860.67760.49190.027*
C640.7728 (2)0.8193 (2)0.41460 (17)0.0193 (10)
C650.6996 (3)0.8321 (2)0.47932 (16)0.0221 (11)
H650.69830.87310.50810.027*
C660.6283 (2)0.7847 (3)0.50194 (15)0.0284 (12)
H660.57830.79350.54620.034*
C670.6303 (3)0.7246 (3)0.45982 (19)0.0303 (13)
H670.58160.69230.47530.036*
C680.7035 (3)0.7119 (3)0.39510 (19)0.0312 (13)
H680.70480.67080.36630.037*
C690.7747 (2)0.7592 (3)0.37248 (16)0.0268 (12)
H690.82470.75050.32820.032*
C700.8132 (2)0.9726 (2)0.43254 (17)0.0189 (10)
C710.7171 (2)1.0564 (2)0.41706 (17)0.0223 (11)
H710.67721.05760.38420.027*
C720.6794 (2)1.1384 (2)0.44967 (19)0.0278 (12)
H720.61371.19570.43910.033*
C730.7378 (3)1.1367 (2)0.49776 (18)0.0294 (13)
H730.71201.19280.52000.035*
C740.8339 (3)1.0529 (3)0.51324 (17)0.0294 (13)
H740.87381.05170.54610.035*
C750.8716 (2)0.9708 (2)0.48063 (18)0.0233 (11)
H750.93730.91350.49120.028*
C760.8834 (3)0.9200 (2)0.29298 (12)0.0216 (11)
C770.9541 (3)0.84763 (19)0.25304 (17)0.0276 (12)
H770.98790.77630.27920.033*
C780.9755 (3)0.8796 (2)0.17476 (17)0.0329 (14)
H781.02380.83010.14750.040*
C790.9261 (3)0.9839 (3)0.13641 (12)0.0314 (13)
H790.94071.00580.08290.038*
C800.8553 (3)1.05630 (19)0.17636 (16)0.0267 (12)
H800.82161.12760.15020.032*
C810.8340 (2)1.0244 (2)0.25464 (16)0.0210 (11)
H810.78561.07380.28190.025*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Sn10.01473 (17)0.01544 (17)0.01310 (16)−0.00479 (13)−0.00460 (12)−0.00301 (13)
As10.0186 (3)0.0259 (3)0.0140 (3)−0.0083 (2)−0.0023 (2)−0.0063 (2)
As20.0163 (3)0.0201 (3)0.0120 (2)−0.0081 (2)−0.00233 (19)−0.0025 (2)
O10.030 (2)0.041 (2)0.0141 (18)−0.0184 (19)−0.0009 (15)−0.0061 (17)
O20.025 (2)0.031 (2)0.0131 (17)−0.0127 (17)−0.0052 (15)0.0002 (15)
B10.028 (3)0.021 (3)0.018 (3)−0.010 (3)−0.007 (2)−0.005 (2)
C10.030 (3)0.022 (3)0.028 (3)−0.007 (2)−0.009 (2)−0.008 (2)
C20.026 (3)0.016 (3)0.033 (3)−0.006 (2)−0.007 (2)−0.006 (2)
C30.021 (3)0.015 (3)0.037 (3)−0.001 (2)−0.011 (2)−0.005 (2)
C40.035 (3)0.024 (3)0.033 (3)−0.012 (3)−0.001 (3)−0.013 (2)
C50.037 (3)0.031 (3)0.034 (3)−0.017 (3)−0.009 (3)−0.014 (3)
C60.026 (3)0.033 (3)0.047 (4)−0.011 (3)−0.009 (3)−0.019 (3)
C70.026 (3)0.026 (3)0.033 (3)−0.009 (2)−0.001 (2)−0.013 (2)
C80.017 (3)0.025 (3)0.018 (2)−0.011 (2)−0.006 (2)−0.002 (2)
C90.018 (3)0.021 (3)0.019 (3)−0.003 (2)−0.008 (2)−0.002 (2)
C100.022 (3)0.031 (3)0.023 (3)−0.003 (2)−0.002 (2)−0.003 (2)
C110.034 (3)0.024 (3)0.036 (3)−0.008 (3)0.000 (3)0.001 (3)
C120.028 (3)0.022 (3)0.040 (3)−0.010 (2)−0.003 (3)−0.003 (3)
C130.023 (3)0.030 (3)0.032 (3)−0.008 (2)−0.005 (2)−0.014 (2)
C140.022 (3)0.023 (3)0.020 (3)−0.005 (2)−0.009 (2)−0.002 (2)
C150.020 (3)0.024 (3)0.020 (3)−0.012 (2)−0.002 (2)−0.006 (2)
C160.021 (3)0.030 (3)0.020 (3)−0.015 (2)−0.004 (2)−0.008 (2)
C170.039 (3)0.039 (3)0.026 (3)−0.026 (3)0.007 (3)−0.012 (3)
C180.044 (4)0.055 (4)0.045 (4)−0.038 (4)0.019 (3)−0.019 (3)
C190.020 (3)0.072 (5)0.059 (4)−0.026 (3)0.009 (3)−0.036 (4)
C200.022 (3)0.047 (4)0.043 (4)−0.007 (3)−0.011 (3)−0.012 (3)
C210.031 (3)0.042 (3)0.021 (3)−0.017 (3)−0.004 (2)−0.009 (3)
C220.024 (3)0.024 (3)0.021 (3)−0.012 (2)0.002 (2)−0.006 (2)
C230.035 (3)0.034 (3)0.029 (3)−0.020 (3)0.003 (2)−0.012 (3)
C240.050 (4)0.039 (4)0.042 (4)−0.015 (3)0.007 (3)−0.023 (3)
C250.055 (5)0.038 (4)0.053 (4)−0.012 (4)0.013 (4)−0.018 (3)
C260.027 (4)0.049 (4)0.064 (5)0.000 (3)−0.005 (3)−0.011 (4)
C270.037 (4)0.049 (4)0.035 (4)−0.014 (3)−0.005 (3)−0.013 (3)
C280.023 (3)0.025 (3)0.019 (3)−0.009 (2)−0.003 (2)−0.007 (2)
C290.033 (3)0.028 (3)0.025 (3)−0.014 (3)−0.006 (2)−0.007 (2)
C300.026 (3)0.038 (3)0.027 (3)0.000 (3)−0.016 (2)−0.007 (3)
C310.017 (3)0.043 (3)0.029 (3)−0.006 (3)−0.006 (2)−0.014 (3)
C320.029 (3)0.046 (4)0.022 (3)−0.021 (3)−0.002 (2)−0.011 (3)
C330.031 (3)0.024 (3)0.016 (2)−0.012 (2)−0.002 (2)−0.005 (2)
C340.022 (3)0.027 (3)0.020 (3)−0.008 (2)−0.006 (2)−0.005 (2)
C350.037 (4)0.036 (3)0.037 (3)−0.015 (3)0.003 (3)−0.014 (3)
C360.051 (4)0.030 (3)0.053 (4)−0.014 (3)−0.008 (3)−0.015 (3)
C370.051 (4)0.037 (4)0.045 (4)−0.026 (3)−0.009 (3)−0.004 (3)
C380.045 (4)0.045 (4)0.038 (4)−0.026 (3)0.005 (3)−0.009 (3)
C390.034 (3)0.041 (4)0.034 (3)−0.021 (3)0.006 (3)−0.016 (3)
C400.020 (3)0.023 (3)0.016 (2)−0.009 (2)−0.006 (2)0.000 (2)
C410.032 (3)0.034 (3)0.024 (3)−0.016 (3)0.001 (2)−0.009 (2)
C420.037 (4)0.039 (3)0.038 (3)−0.024 (3)−0.013 (3)−0.004 (3)
C430.029 (3)0.030 (3)0.031 (3)−0.019 (3)−0.015 (3)0.011 (2)
C440.033 (3)0.037 (3)0.024 (3)−0.022 (3)−0.002 (2)0.004 (2)
C450.024 (3)0.034 (3)0.021 (3)−0.016 (2)−0.002 (2)−0.004 (2)
C460.020 (3)0.012 (2)0.021 (2)−0.004 (2)−0.011 (2)−0.0016 (19)
C470.021 (3)0.027 (3)0.016 (2)−0.010 (2)−0.005 (2)−0.002 (2)
C480.027 (3)0.021 (3)0.027 (3)−0.012 (2)−0.004 (2)−0.002 (2)
C490.026 (3)0.024 (3)0.025 (3)−0.011 (2)−0.001 (2)−0.009 (2)
C500.031 (3)0.028 (3)0.019 (3)−0.013 (2)−0.003 (2)−0.006 (2)
C510.029 (3)0.024 (3)0.013 (2)−0.012 (2)0.000 (2)−0.003 (2)
C520.020 (3)0.016 (2)0.020 (2)−0.004 (2)−0.009 (2)−0.006 (2)
C530.023 (3)0.022 (3)0.018 (3)−0.005 (2)−0.006 (2)−0.002 (2)
C540.015 (3)0.034 (3)0.028 (3)−0.007 (2)−0.002 (2)−0.012 (2)
C550.035 (3)0.017 (3)0.031 (3)−0.002 (2)−0.022 (3)−0.006 (2)
C560.033 (3)0.026 (3)0.021 (3)−0.013 (3)−0.006 (2)0.002 (2)
C570.020 (3)0.023 (3)0.018 (3)−0.008 (2)−0.003 (2)−0.001 (2)
C580.029 (3)0.022 (3)0.016 (2)−0.008 (2)−0.003 (2)−0.008 (2)
C590.019 (3)0.028 (3)0.031 (3)−0.011 (2)−0.004 (2)−0.010 (2)
C600.024 (3)0.038 (3)0.037 (3)−0.013 (3)−0.011 (2)−0.014 (3)
C610.030 (3)0.035 (3)0.028 (3)−0.002 (3)−0.016 (3)−0.010 (3)
C620.037 (3)0.030 (3)0.012 (2)−0.011 (3)−0.008 (2)−0.002 (2)
C630.022 (3)0.028 (3)0.018 (3)−0.009 (2)−0.003 (2)−0.007 (2)
C640.014 (2)0.019 (2)0.022 (3)−0.002 (2)−0.010 (2)−0.003 (2)
C650.027 (3)0.023 (3)0.015 (2)−0.011 (2)−0.008 (2)0.002 (2)
C660.036 (3)0.034 (3)0.019 (3)−0.020 (3)−0.006 (2)0.000 (2)
C670.026 (3)0.028 (3)0.040 (3)−0.017 (3)−0.009 (3)−0.002 (3)
C680.032 (3)0.034 (3)0.038 (3)−0.015 (3)−0.005 (3)−0.019 (3)
C690.018 (3)0.029 (3)0.037 (3)−0.009 (2)−0.002 (2)−0.015 (3)
C700.023 (3)0.023 (3)0.017 (2)−0.017 (2)−0.003 (2)−0.002 (2)
C710.022 (3)0.030 (3)0.023 (3)−0.016 (2)0.000 (2)−0.011 (2)
C720.028 (3)0.026 (3)0.027 (3)−0.009 (2)−0.001 (2)−0.009 (2)
C730.035 (3)0.038 (3)0.027 (3)−0.025 (3)0.013 (2)−0.020 (3)
C740.039 (3)0.035 (3)0.023 (3)−0.024 (3)0.001 (2)−0.008 (2)
C750.022 (3)0.032 (3)0.022 (3)−0.018 (2)−0.003 (2)−0.006 (2)
C760.015 (3)0.026 (3)0.021 (3)−0.003 (2)−0.004 (2)−0.010 (2)
C770.028 (3)0.025 (3)0.022 (3)−0.005 (2)−0.005 (2)−0.005 (2)
C780.031 (3)0.045 (4)0.020 (3)−0.010 (3)−0.001 (2)−0.014 (3)
C790.031 (3)0.051 (4)0.014 (3)−0.023 (3)−0.002 (2)−0.003 (3)
C800.037 (3)0.028 (3)0.023 (3)−0.019 (3)−0.010 (2)−0.002 (2)
C810.025 (3)0.019 (3)0.021 (3)−0.008 (2)−0.007 (2)−0.005 (2)

Geometric parameters (Å, °)

Sn1—C12.150 (5)C36—C371.3900
Sn1—C82.145 (5)C36—H360.9500
Sn1—C152.144 (5)C37—C381.3900
Sn1—O12.175 (3)C37—H370.9500
Sn1—O22.225 (3)C38—C391.3900
As1—O11.657 (3)C38—H380.9500
As1—C221.899 (3)C39—H390.9500
As1—C341.909 (3)C40—C411.3900
As1—C281.909 (2)C40—C451.3900
As2—O21.651 (3)C41—C421.3900
As2—C401.893 (2)C41—H410.9500
As2—C521.904 (2)C42—C431.3900
As2—C461.909 (2)C42—H420.9500
B1—C581.695 (6)C43—C441.3900
B1—C701.697 (6)C43—H430.9500
B1—C641.701 (6)C44—C451.3900
B1—C761.712 (6)C44—H440.9500
C1—C21.511 (5)C45—H450.9500
C1—H1A0.9900C46—C471.3900
C1—H1B0.9900C46—C511.3900
C2—C31.3900C47—C481.3900
C2—C71.3900C47—H470.9500
C3—C41.3900C48—C491.3900
C3—H30.9500C48—H480.9500
C4—C51.3900C49—C501.3900
C4—H40.9500C49—H490.9500
C5—C61.3900C50—C511.3900
C5—H50.9500C50—H500.9500
C6—C71.3900C51—H510.9500
C6—H60.9500C52—C531.3900
C7—H70.9500C52—C571.3900
C8—C91.531 (5)C53—C541.3900
C8—H8A0.9900C53—H530.9500
C8—H8B0.9900C54—C551.3900
C9—C101.3900C54—H540.9500
C9—C141.3900C55—C561.3900
C10—C111.3900C55—H550.9500
C10—H100.9500C56—C571.3900
C11—C121.3900C56—H560.9500
C11—H110.9500C57—H570.9500
C12—C131.3900C58—C591.3900
C12—H120.9500C58—C631.3900
C13—C141.3900C59—C601.3900
C13—H130.9500C59—H590.9500
C14—H140.9500C60—C611.3900
C15—C161.520 (5)C60—H600.9500
C15—H15A0.9900C61—C621.3900
C15—H15B0.9900C61—H610.9500
C16—C171.3900C62—C631.3900
C16—C211.3900C62—H620.9500
C17—C181.3900C63—H630.9500
C17—H170.9500C64—C651.3900
C18—C191.3900C64—C691.3900
C18—H180.9500C65—C661.3900
C19—C201.3900C65—H650.9500
C19—H190.9500C66—C671.3900
C20—C211.3900C66—H660.9500
C20—H200.9500C67—C681.3900
C21—H210.9500C67—H670.9500
C22—C231.3900C68—C691.3900
C22—C271.3900C68—H680.9500
C23—C241.3900C69—H690.9500
C23—H230.9500C70—C711.3900
C24—C251.3900C70—C751.3900
C24—H240.9500C71—C721.3900
C25—C261.3900C71—H710.9500
C25—H250.9500C72—C731.3900
C26—C271.3900C72—H720.9500
C26—H260.9500C73—C741.3900
C27—H270.9500C73—H730.9500
C28—C291.3900C74—C751.3900
C28—C331.3900C74—H740.9500
C29—C301.3900C75—H750.9500
C29—H290.9500C76—C771.3900
C30—C311.3900C76—C811.3900
C30—H300.9500C77—C781.3900
C31—C321.3900C77—H770.9500
C31—H310.9500C78—C791.3900
C32—C331.3900C78—H780.9500
C32—H320.9500C79—C801.3900
C33—H330.9500C79—H790.9500
C34—C351.3900C80—C811.3900
C34—C391.3900C80—H800.9500
C35—C361.3900C81—H810.9500
C35—H350.9500
C1—Sn1—C8114.4 (2)C34—C35—C36120.0
C1—Sn1—C15119.7 (2)C34—C35—H35120.0
C8—Sn1—C15125.9 (2)C36—C35—H35120.0
C15—Sn1—O186.24 (16)C35—C36—C37120.0
C8—Sn1—O193.12 (16)C35—C36—H36120.0
C1—Sn1—O193.11 (18)C37—C36—H36120.0
C15—Sn1—O288.98 (16)C38—C37—C36120.0
C8—Sn1—O285.65 (16)C38—C37—H37120.0
C1—Sn1—O293.57 (17)C36—C37—H37120.0
O1—Sn1—O2173.1 (1)C37—C38—C39120.0
O1—As1—C22109.92 (17)C37—C38—H38120.0
O1—As1—C34111.14 (16)C39—C38—H38120.0
C22—As1—C34107.37 (16)C38—C39—C34120.0
O1—As1—C28110.98 (16)C38—C39—H39120.0
C22—As1—C28109.80 (15)C34—C39—H39120.0
C34—As1—C28107.54 (15)C41—C40—C45120.0
O2—As2—C40109.27 (16)C41—C40—As2117.73 (17)
O2—As2—C52111.94 (16)C45—C40—As2122.25 (17)
C40—As2—C52108.31 (14)C40—C41—C42120.0
O2—As2—C46109.16 (15)C40—C41—H41120.0
C40—As2—C46111.20 (14)C42—C41—H41120.0
C52—As2—C46106.96 (14)C43—C42—C41120.0
As1—O1—Sn1165.3 (2)C43—C42—H42120.0
As2—O2—Sn1160.3 (2)C41—C42—H42120.0
C58—B1—C70109.7 (3)C44—C43—C42120.0
C58—B1—C64108.3 (4)C44—C43—H43120.0
C70—B1—C64108.3 (4)C42—C43—H43120.0
C58—B1—C76107.9 (4)C43—C44—C45120.0
C70—B1—C76112.3 (4)C43—C44—H44120.0
C64—B1—C76110.3 (3)C45—C44—H44120.0
C2—C1—Sn1112.2 (3)C44—C45—C40120.0
C2—C1—H1A109.2C44—C45—H45120.0
Sn1—C1—H1A109.2C40—C45—H45120.0
C2—C1—H1B109.2C47—C46—C51120.0
Sn1—C1—H1B109.2C47—C46—As2119.09 (16)
H1A—C1—H1B107.9C51—C46—As2120.89 (16)
C3—C2—C7120.0C46—C47—C48120.0
C3—C2—C1119.5 (3)C46—C47—H47120.0
C7—C2—C1120.5 (3)C48—C47—H47120.0
C4—C3—C2120.0C49—C48—C47120.0
C4—C3—H3120.0C49—C48—H48120.0
C2—C3—H3120.0C47—C48—H48120.0
C3—C4—C5120.0C50—C49—C48120.0
C3—C4—H4120.0C50—C49—H49120.0
C5—C4—H4120.0C48—C49—H49120.0
C4—C5—C6120.0C49—C50—C51120.0
C4—C5—H5120.0C49—C50—H50120.0
C6—C5—H5120.0C51—C50—H50120.0
C7—C6—C5120.0C50—C51—C46120.0
C7—C6—H6120.0C50—C51—H51120.0
C5—C6—H6120.0C46—C51—H51120.0
C6—C7—C2120.0C53—C52—C57120.0
C6—C7—H7120.0C53—C52—As2118.93 (17)
C2—C7—H7120.0C57—C52—As2120.97 (17)
C9—C8—Sn1112.6 (3)C52—C53—C54120.0
C9—C8—H8A109.1C52—C53—H53120.0
Sn1—C8—H8A109.1C54—C53—H53120.0
C9—C8—H8B109.1C53—C54—C55120.0
Sn1—C8—H8B109.1C53—C54—H54120.0
H8A—C8—H8B107.8C55—C54—H54120.0
C10—C9—C14120.0C56—C55—C54120.0
C10—C9—C8120.6 (3)C56—C55—H55120.0
C14—C9—C8119.3 (3)C54—C55—H55120.0
C11—C10—C9120.0C57—C56—C55120.0
C11—C10—H10120.0C57—C56—H56120.0
C9—C10—H10120.0C55—C56—H56120.0
C10—C11—C12120.0C56—C57—C52120.0
C10—C11—H11120.0C56—C57—H57120.0
C12—C11—H11120.0C52—C57—H57120.0
C13—C12—C11120.0C59—C58—C63120.0
C13—C12—H12120.0C59—C58—B1119.7 (3)
C11—C12—H12120.0C63—C58—B1120.3 (3)
C12—C13—C14120.0C60—C59—C58120.0
C12—C13—H13120.0C60—C59—H59120.0
C14—C13—H13120.0C58—C59—H59120.0
C13—C14—C9120.0C59—C60—C61120.0
C13—C14—H14120.0C59—C60—H60120.0
C9—C14—H14120.0C61—C60—H60120.0
C16—C15—Sn1113.7 (3)C62—C61—C60120.0
C16—C15—H15A108.8C62—C61—H61120.0
Sn1—C15—H15A108.8C60—C61—H61120.0
C16—C15—H15B108.8C61—C62—C63120.0
Sn1—C15—H15B108.8C61—C62—H62120.0
H15A—C15—H15B107.7C63—C62—H62120.0
C17—C16—C21120.0C62—C63—C58120.0
C17—C16—C15118.9 (3)C62—C63—H63120.0
C21—C16—C15121.1 (3)C58—C63—H63120.0
C18—C17—C16120.0C65—C64—C69120.0
C18—C17—H17120.0C65—C64—B1119.1 (3)
C16—C17—H17120.0C69—C64—B1120.9 (3)
C17—C18—C19120.0C66—C65—C64120.0
C17—C18—H18120.0C66—C65—H65120.0
C19—C18—H18120.0C64—C65—H65120.0
C20—C19—C18120.0C65—C66—C67120.0
C20—C19—H19120.0C65—C66—H66120.0
C18—C19—H19120.0C67—C66—H66120.0
C21—C20—C19120.0C68—C67—C66120.0
C21—C20—H20120.0C68—C67—H67120.0
C19—C20—H20120.0C66—C67—H67120.0
C20—C21—C16120.0C67—C68—C69120.0
C20—C21—H21120.0C67—C68—H68120.0
C16—C21—H21120.0C69—C68—H68120.0
C23—C22—C27120.0C68—C69—C64120.0
C23—C22—As1120.4 (2)C68—C69—H69120.0
C27—C22—As1119.5 (2)C64—C69—H69120.0
C22—C23—C24120.0C71—C70—C75120.0
C22—C23—H23120.0C71—C70—B1119.6 (3)
C24—C23—H23120.0C75—C70—B1120.4 (3)
C23—C24—C25120.0C72—C71—C70120.0
C23—C24—H24120.0C72—C71—H71120.0
C25—C24—H24120.0C70—C71—H71120.0
C26—C25—C24120.0C71—C72—C73120.0
C26—C25—H25120.0C71—C72—H72120.0
C24—C25—H25120.0C73—C72—H72120.0
C25—C26—C27120.0C72—C73—C74120.0
C25—C26—H26120.0C72—C73—H73120.0
C27—C26—H26120.0C74—C73—H73120.0
C26—C27—C22120.0C75—C74—C73120.0
C26—C27—H27120.0C75—C74—H74120.0
C22—C27—H27120.0C73—C74—H74120.0
C29—C28—C33120.0C74—C75—C70120.0
C29—C28—As1120.76 (18)C74—C75—H75120.0
C33—C28—As1119.23 (18)C70—C75—H75120.0
C30—C29—C28120.0C77—C76—C81120.0
C30—C29—H29120.0C77—C76—B1117.6 (3)
C28—C29—H29120.0C81—C76—B1122.4 (3)
C29—C30—C31120.0C76—C77—C78120.0
C29—C30—H30120.0C76—C77—H77120.0
C31—C30—H30120.0C78—C77—H77120.0
C32—C31—C30120.0C77—C78—C79120.0
C32—C31—H31120.0C77—C78—H78120.0
C30—C31—H31120.0C79—C78—H78120.0
C31—C32—C33120.0C78—C79—C80120.0
C31—C32—H32120.0C78—C79—H79120.0
C33—C32—H32120.0C80—C79—H79120.0
C32—C33—C28120.0C81—C80—C79120.0
C32—C33—H33120.0C81—C80—H80120.0
C28—C33—H33120.0C79—C80—H80120.0
C35—C34—C39120.0C80—C81—C76120.0
C35—C34—As1119.74 (19)C80—C81—H81120.0
C39—C34—As1120.18 (19)C76—C81—H81120.0
C22—As1—O1—Sn1126.5 (9)C52—As2—C40—C4188.5 (2)
C34—As1—O1—Sn1−114.8 (9)C46—As2—C40—C41−154.27 (18)
C28—As1—O1—Sn14.8 (9)O2—As2—C40—C45148.1 (2)
C15—Sn1—O1—As1139.5 (9)C52—As2—C40—C45−89.7 (2)
C8—Sn1—O1—As113.6 (9)C46—As2—C40—C4527.6 (2)
C1—Sn1—O1—As1−101.0 (9)C45—C40—C41—C420.0
C40—As2—O2—Sn1128.4 (6)As2—C40—C41—C42−178.2 (2)
C52—As2—O2—Sn18.4 (7)C40—C41—C42—C430.0
C46—As2—O2—Sn1−109.8 (6)C41—C42—C43—C440.0
C15—Sn1—O2—As262.7 (6)C42—C43—C44—C450.0
C8—Sn1—O2—As2−171.2 (6)C43—C44—C45—C400.0
C1—Sn1—O2—As2−57.0 (6)C41—C40—C45—C440.0
C15—Sn1—C1—C2144.6 (3)As2—C40—C45—C44178.1 (3)
C8—Sn1—C1—C2−37.7 (4)O2—As2—C46—C47−9.3 (2)
O1—Sn1—C1—C257.2 (4)C40—As2—C46—C47111.3 (2)
O2—Sn1—C1—C2−124.5 (3)C52—As2—C46—C47−130.62 (19)
Sn1—C1—C2—C3−100.8 (3)O2—As2—C46—C51172.3 (2)
Sn1—C1—C2—C777.3 (4)C40—As2—C46—C51−67.0 (2)
C7—C2—C3—C40.0C52—As2—C46—C5151.0 (2)
C1—C2—C3—C4178.1 (4)C51—C46—C47—C480.0
C2—C3—C4—C50.0As2—C46—C47—C48−178.4 (2)
C3—C4—C5—C60.0C46—C47—C48—C490.0
C4—C5—C6—C70.0C47—C48—C49—C500.0
C5—C6—C7—C20.0C48—C49—C50—C510.0
C3—C2—C7—C60.0C49—C50—C51—C460.0
C1—C2—C7—C6−178.1 (4)C47—C46—C51—C500.0
C15—Sn1—C8—C9−4.9 (4)As2—C46—C51—C50178.3 (2)
C1—Sn1—C8—C9177.5 (3)O2—As2—C52—C53−30.3 (2)
O1—Sn1—C8—C982.7 (3)C40—As2—C52—C53−150.86 (18)
O2—Sn1—C8—C9−90.5 (3)C46—As2—C52—C5389.19 (19)
Sn1—C8—C9—C10−91.8 (3)O2—As2—C52—C57153.30 (19)
Sn1—C8—C9—C1485.1 (3)C40—As2—C52—C5732.8 (2)
C14—C9—C10—C110.0C46—As2—C52—C57−87.2 (2)
C8—C9—C10—C11176.9 (4)C57—C52—C53—C540.0
C9—C10—C11—C120.0As2—C52—C53—C54−176.4 (2)
C10—C11—C12—C130.0C52—C53—C54—C550.0
C11—C12—C13—C140.0C53—C54—C55—C560.0
C12—C13—C14—C90.0C54—C55—C56—C570.0
C10—C9—C14—C130.0C55—C56—C57—C520.0
C8—C9—C14—C13−176.9 (3)C53—C52—C57—C560.0
C8—Sn1—C15—C16138.9 (3)As2—C52—C57—C56176.3 (2)
C1—Sn1—C15—C16−43.7 (4)C70—B1—C58—C59−75.9 (4)
O1—Sn1—C15—C1647.7 (3)C64—B1—C58—C59166.1 (2)
O2—Sn1—C15—C16−137.2 (3)C76—B1—C58—C5946.7 (4)
Sn1—C15—C16—C17−112.3 (3)C70—B1—C58—C63101.3 (4)
Sn1—C15—C16—C2167.6 (4)C64—B1—C58—C63−16.7 (4)
C21—C16—C17—C180.0C76—B1—C58—C63−136.1 (3)
C15—C16—C17—C18179.9 (3)C63—C58—C59—C600.0
C16—C17—C18—C190.0B1—C58—C59—C60177.2 (3)
C17—C18—C19—C200.0C58—C59—C60—C610.0
C18—C19—C20—C210.0C59—C60—C61—C620.0
C19—C20—C21—C160.0C60—C61—C62—C630.0
C17—C16—C21—C200.0C61—C62—C63—C580.0
C15—C16—C21—C20−179.9 (3)C59—C58—C63—C620.0
O1—As1—C22—C23−136.7 (2)B1—C58—C63—C62−177.1 (3)
C34—As1—C22—C23102.3 (2)C58—B1—C64—C6598.9 (3)
C28—As1—C22—C23−14.4 (3)C70—B1—C64—C65−20.0 (4)
O1—As1—C22—C2745.6 (3)C76—B1—C64—C65−143.3 (3)
C34—As1—C22—C27−75.4 (2)C58—B1—C64—C69−79.6 (4)
C28—As1—C22—C27167.9 (2)C70—B1—C64—C69161.5 (3)
C27—C22—C23—C240.0C76—B1—C64—C6938.2 (4)
As1—C22—C23—C24−177.7 (3)C69—C64—C65—C660.0
C22—C23—C24—C250.0B1—C64—C65—C66−178.5 (3)
C23—C24—C25—C260.0C64—C65—C66—C670.0
C24—C25—C26—C270.0C65—C66—C67—C680.0
C25—C26—C27—C220.0C66—C67—C68—C690.0
C23—C22—C27—C260.0C67—C68—C69—C640.0
As1—C22—C27—C26177.7 (3)C65—C64—C69—C680.0
O1—As1—C28—C29−135.3 (2)B1—C64—C69—C68178.5 (3)
C22—As1—C28—C29103.0 (2)C58—B1—C70—C71−179.2 (3)
C34—As1—C28—C29−13.5 (2)C64—B1—C70—C71−61.2 (4)
O1—As1—C28—C3343.5 (2)C76—B1—C70—C7160.9 (4)
C22—As1—C28—C33−78.2 (2)C58—B1—C70—C753.6 (5)
C34—As1—C28—C33165.30 (19)C64—B1—C70—C75121.6 (3)
C33—C28—C29—C300.0C76—B1—C70—C75−116.3 (3)
As1—C28—C29—C30178.8 (2)C75—C70—C71—C720.0
C28—C29—C30—C310.0B1—C70—C71—C72−177.2 (3)
C29—C30—C31—C320.0C70—C71—C72—C730.0
C30—C31—C32—C330.0C71—C72—C73—C740.0
C31—C32—C33—C280.0C72—C73—C74—C750.0
C29—C28—C33—C320.0C73—C74—C75—C700.0
As1—C28—C33—C32−178.8 (2)C71—C70—C75—C740.0
O1—As1—C34—C3543.5 (3)B1—C70—C75—C74177.2 (3)
C22—As1—C34—C35163.8 (2)C58—B1—C76—C7737.5 (4)
C28—As1—C34—C35−78.1 (2)C70—B1—C76—C77158.5 (3)
O1—As1—C34—C39−139.7 (2)C64—B1—C76—C77−80.6 (4)
C22—As1—C34—C39−19.5 (3)C58—B1—C76—C81−142.3 (3)
C28—As1—C34—C3998.6 (2)C70—B1—C76—C81−21.3 (5)
C39—C34—C35—C360.0C64—B1—C76—C8199.7 (4)
As1—C34—C35—C36176.7 (3)C81—C76—C77—C780.0
C34—C35—C36—C370.0B1—C76—C77—C78−179.7 (4)
C35—C36—C37—C380.0C76—C77—C78—C790.0
C36—C37—C38—C390.0C77—C78—C79—C800.0
C37—C38—C39—C340.0C78—C79—C80—C810.0
C35—C34—C39—C380.0C79—C80—C81—C760.0
As1—C34—C39—C38−176.7 (3)C77—C76—C81—C800.0
O2—As2—C40—C41−33.7 (2)B1—C76—C81—C80179.7 (4)

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: XU5034).

References

  • Barbour, L. J. (2001). J. Supramol. Chem.1, 189–191.
  • Bruker (2009). APEX2, SAINT and TWINABS Bruker AXS Inc., Madison, Wisconsin, USA.
  • Ng, W. K., Chen, W., Kumar Das, V. G. & Butcher, R. J. (1989). J. Organomet. Chem.361, 53–61.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Westrip, S. P. (2010). J. Appl. Cryst.43, 920–925.

Articles from Acta Crystallographica Section E: Structure Reports Online are provided here courtesy of International Union of Crystallography