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Volume 65 
Part 5 
Pages m558-m559  
May 2009  

Received 2 April 2009
Accepted 16 April 2009
Online 25 April 2009

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Key indicators
Single-crystal X-ray study
T = 173 K
Mean [sigma](C-C) = 0.007 Å
R = 0.036
wR = 0.083
Data-to-parameter ratio = 19.3
Details
Open access

Tricarbonyl(chlorodiphenylstannyl){[eta]5-[2-(dimethylamino)ethyl]cyclopentadienyl}molybdenum

Paul J. Fischer,a* Kristina M. Krohna and Victor G. Young Jrb

aChemistry Department, Macalester College, 1600 Grand Avenue, Saint Paul, MN 55105, USA, and bX-ray Crystallographic Laboratory, Department of Chemistry, University of Minnesota, 207 Pleasant Street SE, Minneapolis, MN 55455, USA
Correspondence e-mail: fischer@macalester.edu

Reaction of the tricarbonyl{[eta]5-[2-(dimethylamino)ethyl]cyclopentadienyl}molybdenum anion and dichloridodiphenylstannane affords the title compound, [MoSn(C6H5)2Cl(C9H14N)(CO)3], which exhibits a four-legged piano-stool geometry with chloridodiphenylstannyl ligands unperturbed by the pendant 2-(dimethylamino)ethyl groups. The Mo-Sn bond length [2.7584 (5) Å] and the distortion of the tetrahedral tin coordination geometry are similar to those observed in related tin-substituted tricarbonylmolybdenum and -tungsten complexes.

Related literature

The synthesis of Mo(SnMe2Cl)(CO)3([eta]5-Cp) was reported by Patil & Graham (1966[Patil, H. R. H. & Graham, W. A. G. (1966). Inorg. Chem. 5, 1401-1405.]). This methodolgy was extended to prepare Mo(SnPh2Cl)(CO)3([eta]5-Cp) by Marks & Seyam (1974[Marks, T. J. & Seyam, A. M. (1974). Inorg. Chem. 13, 1624-1627.]). Triphenyltin and tricyclohexyltin derivatives of [M(CO)3([eta]5-C5H4CH2CH2NMe2)]- (M = Mo and W) were reported by Fischer et al. (2005[Fischer, P. J., Krohn, K. M., Mwenda, E. T. & Young, V. G. Jr (2005). Organometallics, 24, 1776-1779.]). The structural characterization and reaction chemistry of a variety of half-sandwich molybdenum and tungsten chlorostannyl complexes have been reported by Braunschweig et al. (2007[Braunschweig, H., Bera, H., Geibel, B., Dörfler, R., Götz, D., Seeler, F., Kupfer, T. & Radacki, K. (2007). Eur. J. Inorg. Chem. pp. 3416-3424.], 2009[Braunschweig, H., Dörfler, R., Mager, J., Radacki, K. & Seeler, F. (2009). J. Organomet. Chem. 694, 1134-1137.]). The Lewis acidity of coordinatively saturated chlorostannyl ligands has been explored by Tang et al. (2005[Tang, L.-F., Zhao, X.-M., Zou, H.-B., Song, H.-B. & Zhai, Y.-P. (2005). J. Organomet. Chem. 690, 4124-4131.]). Structural parameters that define four-legged piano-stool geometries were detailed by Kubácek et al. (1982[Kubácek, P., Hoffmann, R. & Havias, Z. (1982). Organometallics, 1, 180-188.]).

[Scheme 1]

Experimental

Crystal data

  • [MoSn(C6H5)2Cl(C9H14N)(CO)3]

  • Mr = 624.52

  • Triclinic, [P \overline 1]

  • a = 8.8096 (8) Å

  • b = 9.3458 (8) Å

  • c = 16.1258 (14) Å

  • [alpha] = 89.392 (2)°

  • [beta] = 85.269 (2)°

  • [gamma] = 63.8560 (10)°

  • V = 1187.29 (18) Å3

  • Z = 2

  • Mo K[alpha] radiation

  • [mu] = 1.72 mm-1

  • T = 173 K

  • 0.25 × 0.12 × 0.04 mm
Data collection

  • Bruker SMART CCD area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2003[Bruker (2003). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.673, Tmax = 0.935

  • 14425 measured reflections

  • 5431 independent reflections

  • 4081 reflections with I > 2[sigma](I)

  • Rint = 0.056
Refinement

  • R[F2 > 2[sigma](F2)] = 0.036

  • wR(F2) = 0.083

  • S = 1.00

  • 5431 reflections

  • 282 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 0.71 e Å-3

  • [Delta][rho]min = -0.56 e Å-3

Table 1
Selected bond lengths (Å)

Sn1-C13 2.144 (4)
Sn1-C19 2.146 (4)
Sn1-Cl1 2.3914 (11)

Data collection: SMART (Bruker, 2003[Bruker (2003). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2003[Bruker (2003). SMART, SAINT and SADABS. 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: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: SI2168 ).

Acknowledgements

The donors of the Petroleum Research Fund, administered by the American Chemical Society (grant No. ACS-PRF 46626-B), and an award from Research Corporation (grant No. CC5932) supported this research.

References

Braunschweig, H., Bera, H., Geibel, B., Dörfler, R., Götz, D., Seeler, F., Kupfer, T. & Radacki, K. (2007). Eur. J. Inorg. Chem. pp. 3416-3424.  [ISI] [CSD] [CrossRef]
Braunschweig, H., Dörfler, R., Mager, J., Radacki, K. & Seeler, F. (2009). J. Organomet. Chem. 694, 1134-1137.  [CSD] [CrossRef] [ChemPort]
Bruker (2003). SMART, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Fischer, P. J., Krohn, K. M., Mwenda, E. T. & Young, V. G. Jr (2005). Organometallics, 24, 1776-1779.  [CSD] [CrossRef] [ChemPort]
Kubácek, P., Hoffmann, R. & Havias, Z. (1982). Organometallics, 1, 180-188.
Marks, T. J. & Seyam, A. M. (1974). Inorg. Chem. 13, 1624-1627.  [CrossRef] [ChemPort] [ISI]
Patil, H. R. H. & Graham, W. A. G. (1966). Inorg. Chem. 5, 1401-1405.  [CrossRef] [ChemPort] [ISI]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Tang, L.-F., Zhao, X.-M., Zou, H.-B., Song, H.-B. & Zhai, Y.-P. (2005). J. Organomet. Chem. 690, 4124-4131.  [CSD] [CrossRef] [ChemPort]

Acta Cryst (2009). E65, m558-m559   [ doi:10.1107/S1600536809014329 ]

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