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Volume 68 
Part 7 
Page m893  
July 2012  

Received 25 May 2012
Accepted 31 May 2012
Online 13 June 2012

Key indicators
Single-crystal X-ray study
T = 223 K
Mean [sigma](C-C) = 0.009 Å
R = 0.040
wR = 0.100
Data-to-parameter ratio = 24.0
Details
Open access

Dichlorido-1[kappa]Cl,3[kappa]Cl-hexakis[1,1,2,2,3,3([eta]5)-cyclopentadienyl]di-[mu]2-oxido-1:2[kappa]2O:O;2:3[kappa]2O:O-trizirconium(IV)

aDepartment of Chemistry, St. John Fisher College, Rochester, NY 14618, USA, and bDepartment of Chemistry, University of Rochester, Rochester, NY 14627, USA
Correspondence e-mail: bkraft@sjfc.edu

The title compound, [Zr3(C5H5)6Cl2O2], exists as discrete molecules possessing a series of three Cp2Zr units (Cp is cyclopentadienyl) bridged by oxide ligands and end-capped by chloride ligands. The Cp planes in the central and terminal zirconocene units form dihedral angles of 53.3 (2) and 53.5 (2)°, respectively. The two Zr-O-Zr bridge angles are nearly linear and form a planar Zr3O2 core. The molecule bears C2 symmetry with the central Zr atom lying on a crystallographic twofold axis.

Related literature

For closely related Zr molecules with only one oxo bridge, see: Reid et al. (1965[Reid, A. F., Shannon, J. S., Swan, J. M. & Wailes, P. C. (1965). Aust. J. Chem. 18, 173-181.]); Clarke & Drew (1974[Clarke, J. F. & Drew, G. B. (1974). Acta Cryst. B30, 2267-2269.]); Kuz'mina et al. (1988[Kuz'mina, L. G., Struchkov, Yu. T., Minacheva, M. Kh. & Brainina, E. M. (1988). Russ. J. Coord. Chem. 14, 1257-1261.]); Nieger et al. (1999[Nieger, M., Niecke, E. & Loew, A. (1999). Private communication (refcode CPZROX02). CCDC, Cambridge, England.]); Spletstoser et al. (2007[Spletstoser, J. T., White, J. M., Tunoori, A. R. & Georg, G. I. (2007). J. Am. Chem. Soc. 129, 3408-3419.]). For cyclic trimeric oxozirconocenes, see: Arnold et al. (2011[Arnold, T., Braunschweig, H. & Gruss, K. (2011). Acta Cryst. E67, m391.]); Boutonnet et al. (1995[Boutonnet, F., Zablocka, M., Igau, A., Jaud, J., Majoral, J., Schamberger, J., Erker, G., Werner, S. & Krüger, C. (1995). J. Chem. Soc. Chem. Commun. pp. 823-824.]); Mikhailova et al. (1993[Mikhailova, O. A., Minacheva, M. H., Burlakov, V. V., Shur, V. B., Pisarevsky, A. P., Yanovsky, A. I. & Struchkov, Yu. T. (1993). Acta Cryst. C49, 1345-1347.]). For similar structures with terminal Zr-Cl bonds, see: Corey et al. (1995[Corey, J. Y., Zhu, X.-H., Brammer, L. & Rath, N. P. (1995). Acta Cryst. C51, 565-567.]); Reddy & Petersen (1989[Reddy, K. P. & Petersen, J. L. (1989). Organometallics, 8, 2107-2113.]). For the Hf analog, but with methyl-substituted cyclopentadienyl rings, see: Wisniewska et al. (2008[Wisniewska, A., Baranowska, K. & Pikies, J. (2008). Acta Cryst. E64, m361.]).

[Scheme 1]

Experimental

Crystal data
  • [Zr3(C5H5)6Cl2O2]

  • Mr = 767.10

  • Orthorhombic, P b c n

  • a = 7.8809 (4) Å

  • b = 18.0518 (10) Å

  • c = 20.1883 (11) Å

  • V = 2872.1 (3) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 1.28 mm-1

  • T = 223 K

  • 0.20 × 0.18 × 0.04 mm

Data collection
  • Bruker SMART APEXII CCD Platform diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 2008b[Sheldrick, G. M. (2008b). SADABS. University of Göttingen, Germany.]) Tmin = 0.784, Tmax = 0.951

  • 34715 measured reflections

  • 4032 independent reflections

  • 2569 reflections with I > 2[sigma](I)

  • Rint = 0.099

Refinement
  • R[F2 > 2[sigma](F2)] = 0.040

  • wR(F2) = 0.100

  • S = 1.01

  • 4032 reflections

  • 168 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 0.52 e Å-3

  • [Delta][rho]min = -0.48 e Å-3

Table 1
Selected geometric parameters (Å, °)

Zr1-O1 1.921 (3)
Zr1-Cl1 2.4857 (12)
Zr2-O1 1.980 (3)
Zr2-O1i 1.980 (2)
O1-Zr1-Cl1 97.23 (8)
O1-Zr2-O1i 102.43 (15)
Zr1-O1-Zr2 171.43 (15)
Symmetry code: (i) [-x+1, y, -z+{\script{1\over 2}}].

Data collection: APEX2 (Bruker, 2011[Bruker (2011). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2009[Bruker (2009). SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SIR97 (Altomare et al., 1999[Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008a[Sheldrick, G. M. (2008a). Acta Cryst. A64, 112-122.]); molecular graphics: SHELXTL (Sheldrick, 2008a[Sheldrick, G. M. (2008a). 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: PK2418 ).


References

Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119.  [ISI] [CrossRef] [ChemPort] [details]
Arnold, T., Braunschweig, H. & Gruss, K. (2011). Acta Cryst. E67, m391.  [CSD] [CrossRef] [details]
Boutonnet, F., Zablocka, M., Igau, A., Jaud, J., Majoral, J., Schamberger, J., Erker, G., Werner, S. & Krüger, C. (1995). J. Chem. Soc. Chem. Commun. pp. 823-824.  [CrossRef] [ISI]
Bruker (2009). SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Bruker (2011). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.
Clarke, J. F. & Drew, G. B. (1974). Acta Cryst. B30, 2267-2269.  [CrossRef] [details] [ISI]
Corey, J. Y., Zhu, X.-H., Brammer, L. & Rath, N. P. (1995). Acta Cryst. C51, 565-567.  [CrossRef] [details]
Kuz'mina, L. G., Struchkov, Yu. T., Minacheva, M. Kh. & Brainina, E. M. (1988). Russ. J. Coord. Chem. 14, 1257-1261.  [ChemPort]
Mikhailova, O. A., Minacheva, M. H., Burlakov, V. V., Shur, V. B., Pisarevsky, A. P., Yanovsky, A. I. & Struchkov, Yu. T. (1993). Acta Cryst. C49, 1345-1347.  [CrossRef] [details]
Nieger, M., Niecke, E. & Loew, A. (1999). Private communication (refcode CPZROX02). CCDC, Cambridge, England.
Reddy, K. P. & Petersen, J. L. (1989). Organometallics, 8, 2107-2113.  [CrossRef] [ChemPort]
Reid, A. F., Shannon, J. S., Swan, J. M. & Wailes, P. C. (1965). Aust. J. Chem. 18, 173-181.  [CrossRef] [ChemPort]
Sheldrick, G. M. (2008a). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Sheldrick, G. M. (2008b). SADABS. University of Göttingen, Germany.
Spletstoser, J. T., White, J. M., Tunoori, A. R. & Georg, G. I. (2007). J. Am. Chem. Soc. 129, 3408-3419.  [ISI] [CSD] [CrossRef] [PubMed] [ChemPort]
Wisniewska, A., Baranowska, K. & Pikies, J. (2008). Acta Cryst. E64, m361.  [CSD] [CrossRef] [details]


Acta Cryst (2012). E68, m893  [ doi:10.1107/S1600536812024968 ]

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