Trichlorido(tetra­hydro­furan){(1,2,3,3a,7a-η)-1-[2-(1-trimethyl­silyl-1H-imidazol-2-yl-κN3)-1-methyl­prop­yl]inden­yl}zirconium(IV)

Guan, S.; Nie, W.; Borzov, M.V.

doi:10.1107/S1600536811012037

Volume 67
Part 5
Pages m540-m541
May 2011

Received 21 March 2011
Accepted 31 March 2011
Online 7 April 2011

Key indicators
Single-crystal X-ray study
T = 296 K
Mean (C-C) = 0.006 Å
R = 0.037
wR = 0.093
Data-to-parameter ratio = 17.0
Details

Trichlorido(tetrahydrofuran){(1,2,3,3a,7a-)-1-[2-(1-trimethylsilyl-1H-imidazol-2-yl-N³)-1-methylpropyl]indenyl}zirconium(IV)

Shengzhou Guan,^a ⁺ Wanli Nie ^a ^* and Maxim V. Borzov ^a

^aKey Laboratory of Synthetic and Natural Chemistry of the Ministry of Education, College of Chemistry and Material Science, the North-West University of Xi'an, Taibai Bei Avenue 229, Xi'an 710069, Shaanxi Province, People's Republic of China
Correspondence e-mail: niewl126@126.com

The title compound, [ZrCl₃(C₁₉H₂₅N₂Si)(C₄H₈O)], was prepared from bis(N,N-dimethylamido- [kappa] N)(2-{2-[(1,2,3,3a,7a- [eta] )-indenyl]-2-methylpropyl}-1H-imidazolido- [kappa] N¹)zirconium(IV) [(C₁₆H₁₆N₂)Zr(NMe₂)] by reaction with excess Me₃SiCl in tetrahydrofuran (THF) at elevated temperature. The crystal studied contained a minor non-merohedral twin contaminant [6.3 (4)%] which was taken into account during the refinement. The coordination polyhedron of the Zr^IV atom is a distorted octahedron [assuming that the five-membered ring of the indenyl group (Cp) occupies one coordination site], with the Cp group and a THF O atom at the apical positions and the three Cl and ligating N atoms at the equatorial positions. The Zr, Si and the methylene C atoms deviate noticeably from the imidazole ring plane [by -0.197 (5), -0.207 (5) and 0.119 (6) Å, respectively]. The THF ligand adopts an envelope conformation.

Related literature

For general practical utility of geometry-constrained complexes, including those derived from group 4 transition metals, see: Erker (2006); Braunschweig & Breitling (2006). For the geometric parameters of similar Zr^IV complexes, see: Nifant'ev et al. (1998); Paolucci et al. (2003); Krut'ko et al. (2004, 2007); Enders et al. (1996); Nie et al. (2008). For Ti^IV analogues of the title compound, see: Ge et al. (2010) and references cited therein. For procedures used in the preparation, see: Curtis & Brown (1980); Chisholm et al. (1988); Diamond et al. (1996); Weizmann et al. (1950); Armarego & Perrin (1997). For a description of the Cambridge Structural Database, see: Allen (2002).

Experimental

Crystal data

[ZrCl₃(C₁₉H₂₅N₂Si)(C₄H₈O)]
M_r = 579.17
Triclinic, $[P \overline 1]$
a = 10.6274 (8) Å
b = 10.9496 (7) Å
c = 13.1397 (9) Å
= 102.720 (1)°
= 101.416 (1)°
= 110.456 (1)°
V = 1332.73 (16) Å³
Z = 2
Mo K radiation
= 0.78 mm^-1
T = 296 K
0.35 × 0.24 × 0.14 mm

Data collection

Bruker SMART APEXII diffractometer
Absorption correction: multi-scan (TWINABS; Sheldrick, 2006) T_min = 0.773, T_max = 0.899
4871 measured reflections
4871 independent reflections
3757 reflections with I > 2(I)

Refinement

R[F² > 2(F²)] = 0.037
wR(F²) = 0.093
S = 1.00
4871 reflections
286 parameters
H-atom parameters constrained
_max = 0.42 e Å^-3
_min = -0.52 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: SHELXTL (Sheldrick, 2008) and OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: SHELXTL and OLEX2.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: DN2668 ).

Acknowledgements

Financial support from the National Natural Science Foundation of China (project Nos. 20702041 and 21072157) and Shaanxi Province Administration of Foreign Experts Bureau Foundation (grant No. 20106100079) is gratefully acknowledged. The authors are thankful to Mr Wang Minchang and Mr Su Pengfei (Xi'an Modern Chemistry Research Institute) for their help in carrying out the NMR spectroscopicl and X-ray diffraction experiments.

References

Allen, F. H. (2002). Acta Cryst. B58, 380-388.
Armarego, W. L. F. & Perrin, D. D. (1997). Purification of Laboratory Chemicals, 4th ed. Oxford: Pergamon.
Braunschweig, H. & Breitling, F. M. (2006). Coord. Chem. Rev. 250, 2691-2720.
Bruker (2007). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Chisholm, M. H., Hammond, C. E. & Huffman, J. C. (1988). Polyhedron, 7, 2515-2520.
Curtis, N. J. & Brown, R. S. (1980). J. Org. Chem. 45, 4038-4040.
Diamond, G. M., Jordan, R. F. & Petersen, J. L. (1996). J. Am. Chem. Soc. 118, 8024-8033.
Dolomanov, O. V., Bourhis, L. J., Gildea, R. J., Howard, J. A. K. & Puschmann, H. (2009). J. Appl. Cryst. 42, 339-341.
Enders, M., Rudolph, R. & Pritzkow, H. (1996). Chem. Ber. 129, 459-463.
Erker, G. (2006). Coord. Chem. Rev. 250, 1056-1070.
Ge, F., Nie, W., Borzov, M. V. & Churakov, A. V. (2010). Acta Cryst. E66, m546-m547.
Krut'ko, D. P., Borzov, M. V., Kirsanov, R. S., Antipin, M. Y. & Churakov, A. V. (2004). J. Organomet. Chem. 689, 595-604.
Krut'ko, D. P., Kirsanov, R. S., Belov, S. A., Borzov, M. V. & Churakov, A. V. (2007). J. Organomet. Chem. 692, 1465-1471.
Nie, W., Liao, L., Xu, W., Borzov, M. V., Krut'ko, D. P., Churakov, A. V., Howard, J. A. K. & Lemenovskii, D. A. (2008). J. Organomet. Chem. 693, 2355-2368.
Nifant'ev, I. E., Ivchenko, P. V., Bagrov, V. V. & Kuz'mina, L. G. (1998). Organometallics, 17, 4734-4738.
Paolucci, G., Vignola, M., Coletto, L., Pitteri, B. & Benetollo, F. (2003). J. Organomet. Chem. 687, 161-170.
Sheldrick, G. M. (2006). TWINABS. University of Göttingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Weizmann, C., Bergmann, E. & Sulzbacher, M. (1950). J. Org. Chem. 15, 918-929.

metal-organic compounds

Trichlorido(tetrahydrofuran){(1,2,3,3a,7a-)-1-[2-(1-trimethylsilyl-1H-imidazol-2-yl-N3)-1-methylpropyl]indenyl}zirconium(IV)