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Acta Crystallogr Sect E Struct Rep Online. 2008 November 1; 64(Pt 11): m1410.
Published online 2008 October 15. doi:  10.1107/S1600536808032790
PMCID: PMC2959511

Tetra­kis(4-methyl-2-thien­yl)tin(IV)

Abstract

The mol­ecule of the title compound, [Sn(C5H5S)4], lies on a special position of An external file that holds a picture, illustration, etc.
Object name is e-64-m1410-efi1.jpg site symmetry. The SnIV atom shows a slightly distorted tetra­hedral coordination.

Related literature

For the structure of tetra­kis(2-thien­yl)tin, see: Karipides et al. (1977 [triangle]). For the synthesis, see: Kumar Das et al. (1987 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-64-m1410-scheme1.jpg

Experimental

Crystal data

  • [Sn(C5H5S)4]
  • M r = 507.29
  • Tetragonal, An external file that holds a picture, illustration, etc.
Object name is e-64-m1410-efi2.jpg
  • a = 11.6286 (9) Å
  • c = 7.5918 (6) Å
  • V = 1026.6 (1) Å3
  • Z = 2
  • Mo Kα radiation
  • μ = 1.65 mm−1
  • T = 100 (2) K
  • 0.30 × 0.25 × 0.10 mm

Data collection

  • Bruker SMART APEX diffractometer
  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996 [triangle]) T min = 0.637, T max = 0.852
  • 2948 measured reflections
  • 1151 independent reflections
  • 1149 reflections with I > 2σ(I)
  • R int = 0.014

Refinement

  • R[F 2 > 2σ(F 2)] = 0.012
  • wR(F 2) = 0.028
  • S = 1.01
  • 1151 reflections
  • 58 parameters
  • H-atom parameters constrained
  • Δρmax = 0.45 e Å−3
  • Δρmin = −0.21 e Å−3
  • Absolute structure: Flack (1983 [triangle]), 513 Friedel pairs
  • Flack parameter: 0.005 (14)

Data collection: APEX2 (Bruker, 2007 [triangle]); cell refinement: SAINT (Bruker, 2007 [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, 2008 [triangle]).

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808032790/ci2670sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808032790/ci2670Isup2.hkl

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

Acknowledgments

The authors thank the University of Malaya for funding this study (grant No. FR155/2007A) and also for the purchase of the diffractometer.

supplementary crystallographic information

Experimental

The title compound was synthesized as reported previously (Kumar Das et al., 1987). Single crystals were obtained upon recrystallization from chloroform.

Refinement

H-atoms were placed in calculated positions (C-H = 0.95-0.98 Å) and were included in the refinement in the riding model approximation, with U(H) set to 1.2–1.5Ueq(C).

Figures

Fig. 1.
Displacement ellipsoid plot (Barbour, 2001) of [Sn(C5H5S)4] at the 70% probability level. H atoms are drawn as spheres of arbitrary radii.

Crystal data

[Sn(C5H5S)4]Dx = 1.641 Mg m3
Mr = 507.29Mo Kα radiation, λ = 0.71073 Å
Tetragonal, I4Cell parameters from 2958 reflections
Hall symbol: I -4θ = 2.5–28.3°
a = 11.6286 (9) ŵ = 1.65 mm1
c = 7.5918 (6) ÅT = 100 K
V = 1026.6 (1) Å3Prism, colourless
Z = 20.30 × 0.25 × 0.10 mm
F(000) = 508

Data collection

Bruker SMART APEX diffractometer1151 independent reflections
Radiation source: fine-focus sealed tube1149 reflections with I > 2σ(I)
graphiteRint = 0.014
ω scansθmax = 27.5°, θmin = 2.5°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −15→14
Tmin = 0.637, Tmax = 0.852k = −15→13
2948 measured reflectionsl = −9→8

Refinement

Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.012H-atom parameters constrained
wR(F2) = 0.028w = 1/[σ2(Fo2) + (0.0145P)2] where P = (Fo2 + 2Fc2)/3
S = 1.01(Δ/σ)max = 0.001
1151 reflectionsΔρmax = 0.45 e Å3
58 parametersΔρmin = −0.21 e Å3
0 restraintsAbsolute structure: Flack (1983), 513 Friedel pairs
Primary atom site location: structure-invariant direct methodsFlack parameter: 0.005 (14)

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

xyzUiso*/Ueq
Sn10.50000.50000.50000.01202 (5)
S10.36597 (3)0.74692 (3)0.61422 (5)0.02012 (9)
C10.46144 (12)0.63979 (12)0.6694 (2)0.0140 (3)
C20.50206 (12)0.65832 (13)0.8364 (2)0.0134 (3)
H20.55620.60880.89140.016*
C30.45677 (14)0.75770 (14)0.9212 (2)0.0154 (3)
C40.38176 (14)0.81447 (13)0.8139 (2)0.0192 (3)
H40.34290.88320.84590.023*
C50.48542 (16)0.79485 (16)1.1056 (2)0.0206 (4)
H5A0.49190.87881.10970.031*
H5B0.55860.76021.14140.031*
H5C0.42440.76971.18590.031*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Sn10.01360 (6)0.01360 (6)0.00885 (9)0.0000.0000.000
S10.0221 (2)0.0223 (2)0.0160 (2)0.00775 (16)−0.00468 (16)0.00016 (16)
C10.0138 (7)0.0138 (7)0.0144 (8)0.0010 (5)0.0011 (6)0.0019 (6)
C20.0133 (6)0.0140 (7)0.0129 (8)0.0000 (5)0.0011 (6)0.0020 (6)
C30.0165 (8)0.0151 (8)0.0146 (8)−0.0017 (6)0.0023 (6)0.0011 (6)
C40.0220 (8)0.0172 (8)0.0185 (9)0.0055 (6)0.0014 (7)−0.0008 (7)
C50.0267 (9)0.0213 (9)0.0139 (9)−0.0005 (7)0.0007 (7)−0.0030 (7)

Geometric parameters (Å, °)

Sn1—C1i2.1209 (15)C2—H20.95
Sn1—C12.1209 (15)C3—C41.364 (2)
Sn1—C1ii2.1209 (15)C3—C51.502 (2)
Sn1—C1iii2.1209 (15)C4—H40.95
S1—C41.7173 (16)C5—H5A0.98
S1—C11.7206 (15)C5—H5B0.98
C1—C21.370 (2)C5—H5C0.98
C2—C31.424 (2)
C1i—Sn1—C1111.58 (4)C4—C3—C2111.07 (15)
C1i—Sn1—C1ii105.32 (8)C4—C3—C5124.00 (16)
C1—Sn1—C1ii111.58 (4)C2—C3—C5124.92 (16)
C1i—Sn1—C1iii111.58 (4)C3—C4—S1111.98 (12)
C1—Sn1—C1iii105.32 (8)C3—C4—H4124.0
C1ii—Sn1—C1iii111.58 (4)S1—C4—H4124.0
C4—S1—C192.70 (8)C3—C5—H5A109.5
C2—C1—S1109.51 (12)C3—C5—H5B109.5
C2—C1—Sn1127.51 (11)H5A—C5—H5B109.5
S1—C1—Sn1122.93 (8)C3—C5—H5C109.5
C1—C2—C3114.74 (14)H5A—C5—H5C109.5
C1—C2—H2122.6H5B—C5—H5C109.5
C3—C2—H2122.6
C4—S1—C1—C20.03 (12)S1—C1—C2—C30.28 (17)
C4—S1—C1—Sn1177.81 (9)Sn1—C1—C2—C3−177.37 (11)
C1i—Sn1—C1—C2149.39 (12)C1—C2—C3—C4−0.54 (19)
C1ii—Sn1—C1—C2−93.09 (10)C1—C2—C3—C5178.39 (14)
C1iii—Sn1—C1—C228.15 (11)C2—C3—C4—S10.54 (17)
C1i—Sn1—C1—S1−27.98 (10)C5—C3—C4—S1−178.40 (12)
C1ii—Sn1—C1—S189.54 (12)C1—S1—C4—C3−0.34 (13)
C1iii—Sn1—C1—S1−149.22 (11)

Symmetry codes: (i) −y+1, x, −z+1; (ii) y, −x+1, −z+1; (iii) −x+1, −y+1, z.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: CI2670).

References

  • Barbour, L. J. (2001). J. Supramol. Chem.1, 189–191.
  • Bruker (2007). APEX2 and SAINT Bruker AXS Inc., Madison, Wisconsin, USA.
  • Flack, H. D. (1983). Acta Cryst. A39, 876–881.
  • Karipides, A., Reed, A. T., Haller, D. A. & Hayes, F. (1977). Acta Cryst. B33, 950–951.
  • Kumar Das, V. G., Lo, K. M. & Blunden, S. J. (1987). J. Organomet. Chem.334, 307–322.
  • Sheldrick, G. M. (1996). SADABS University of Göttingen, Germany.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Westrip, S. P. (2008). publCIF In preparation.

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