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Volume 65 
Part 9 
Pages m1103-m1104  
September 2009  

Received 6 August 2009
Accepted 14 August 2009
Online 19 August 2009

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Key indicators
Single-crystal X-ray study
T = 100 K
Mean [sigma](C-C) = 0.007 Å
Disorder in main residue
R = 0.027
wR = 0.072
Data-to-parameter ratio = 21.5
Details
Open access

Dichlorido{[mu]3-6,6'-diethoxy-2,2'-[ethane-1,2-diylbis(nitrilomethylidyne)]diphenolato}octamethyldi-[mu]3-oxido-tetratin(IV)

See Mun Lee,a Kong Mun Loa and Seik Weng Nga*

aDepartment of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia
Correspondence e-mail: seikweng@um.edu.my

In the title tetranuclear tin(IV) complex, [Sn4(CH3)8(C20H22N2O4)Cl2O2], there are three completely different tin-atom coordinations. One metal atom (site symmetry 2) adopts a distorted pentagonal-bipyramidal SnC2N2O3 coordination arising from the N,N',O,O'-tetradentate deprotonated Schiff base, two methyl groups in the axial sites and a [mu]3-O atom that also bonds to two further Sn atoms. Two symmetry-equivalent Sn atoms adopt very distorted SnC2O4 arrangements that could be described as pentagonal-bipyramidal with one equatorial vertex missing and the C atoms in the axial site. The final Sn atom (site symmetry 2) adopts an SnC2Cl2O trigonal-bipyramidal arrangement, with Cl atoms in the axial sites. As well as the two Sn atoms, one O atom lies on a twofold rotation rotation axis, and another is disordered about the axis. The terminal ethoxy group is disordered over two sets of sites with equal occupancy.

Related literature

For other organotin derivatives of 6,6'-dialkoxy-2,2'-[ethane-1,2-diylbis(nitrilomethylidyne)]diphenol, see: Cunningham et al. (2004[Cunningham, D., Gilligan, K., Hannon, M., Kelly, C., McArdle, P. & O'Malley, A. (2004). Organometallics, 23, 984-994.]). For the crystal structure of 6,6'-diethoxy-2,2'-[ethane-1,2-diylbis(nitrilomethylidyne)]diphenol, see: Bermejo et al. (2007[Bermejo, M. R., Fernández, M. I., Gómez-Fórneas, E., González-Noya, A., Maneiro, M., Pedrido, R. & Rodríguez, M. J. (2007). Eur. J. Inorg. Chem. pp. 3789-3797.]).

[Scheme 1]

Experimental

Crystal data

  • [Sn4(CH3)8(C20H22N2O4)Cl2O2]

  • Mr = 1052.33

  • Tetragonal, P 43 21 2

  • a = 9.8723 (1) Å

  • c = 38.0217 (5) Å

  • V = 3705.68 (6) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 2.85 mm-1

  • T = 100 K

  • 0.20 × 0.18 × 0.15 mm
Data collection

  • Bruker SMART APEX diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.]) Tmin = 0.863, Tmax = 1.000 (expected range = 0.563-0.652)

  • 68779 measured reflections

  • 4259 independent reflections

  • 4089 reflections with I > 2[sigma](I)

  • Rint = 0.029
Refinement

  • R[F2 > 2[sigma](F2)] = 0.027

  • wR(F2) = 0.072

  • S = 1.07

  • 4259 reflections

  • 198 parameters

  • 10 restraints

  • H-atom parameters constrained

  • [Delta][rho]max = 0.42 e Å-3

  • [Delta][rho]min = -0.69 e Å-3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 1694 Friedel pairs

  • Flack parameter: 0.00 (4)

Table 1
Selected geometric parameters (Å, °)

Sn1-O3 2.072 (4)
Sn1-C1 2.112 (5)
Sn1-O1 2.410 (3)
Sn1-N1 2.426 (4)
Sn2-O1 2.463 (3)
Sn2-O2 2.791 (4)
Sn2-O3 2.006 (2)
Sn2-C2 2.091 (5)
Sn2-C3 2.100 (5)
Sn2-O4 2.125 (17)
Sn3-O4 1.964 (5)
Sn3-C4 2.114 (5)
Sn3-Cl1 2.5829 (15)
C1i-Sn1-C1 173.9 (3)
C2-Sn2-C3 147.8 (2)
C4-Sn3-C4i 132.6 (3)
Symmetry code: (i) y, x, -z.

Data collection: APEX2 (Bruker, 2008[Bruker (2008). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2008[Bruker (2008). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: X-SEED (Barbour, 2001[Barbour, L. J. (2001). J. Supramol. Chem. 1, 189-191.]); software used to prepare material for publication: publCIF (Westrip, 2009[Westrip, S. P. (2009). publCIF. In preparation.]).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HB5035 ).

Acknowledgements

We thank the University of Malaya (RG020/09AFR) for supporting this study.

References

Barbour, L. J. (2001). J. Supramol. Chem. 1, 189-191.  [CrossRef] [ChemPort]
Bermejo, M. R., Fernández, M. I., Gómez-Fórneas, E., González-Noya, A., Maneiro, M., Pedrido, R. & Rodríguez, M. J. (2007). Eur. J. Inorg. Chem. pp. 3789-3797.  [ISI] [CSD] [CrossRef]
Bruker (2008). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Cunningham, D., Gilligan, K., Hannon, M., Kelly, C., McArdle, P. & O'Malley, A. (2004). Organometallics, 23, 984-994.  [CrossRef] [ChemPort]
Flack, H. D. (1983). Acta Cryst. A39, 876-881.  [CrossRef] [details]
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Westrip, S. P. (2009). publCIF. In preparation.

Acta Cryst (2009). E65, m1103-m1104   [ doi:10.1107/S1600536809032255 ]

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