Tetra­chlorido[(diphenyl­phosphino)diphenyl­phosphine oxide-κO]zirconium(IV) benzene monosolvate

Ogawa, T.; Kajita, Y.; Masuda, H.

doi:10.1107/S1600536809031882

Volume 65
Part 9
Page m1129
September 2009

Received 10 August 2009
Accepted 12 August 2009
Online 22 August 2009

Key indicators
Single-crystal X-ray study
T = 173 K
Mean (C-C) = 0.006 Å
R = 0.045
wR = 0.151
Data-to-parameter ratio = 19.2
Details

ADDENDA AND ERRATA

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Tetrachlorido[(diphenylphosphino)diphenylphosphine oxide-O]zirconium(IV) benzene monosolvate

Takahiko Ogawa,^a Yuji Kajita ^a and Hideki Masuda ^a ^*

^aDepartment of Applied Chemistry, Nagoya Institute of Technology, Showa-ku, Nagoya 466-8555, Japan
Correspondence e-mail: masuda.hideki@nitech.ac.jp

In the title centrosymmetric mononuclear Zr^IV compound, [ZrCl₄{P(O)(C₆H₅)₂P(C₆H₅)₂}₂]·C₆H₆, the central Zr^IV ion is coordinated by two O atoms from two symmetry-related (diphenylphosphino)diphenylphosphine ligands and four Cl atoms in a distorted octahedral geometry with the four Cl atoms in the equatorial positions. The molecule lies about a center of inversion and the benzene solvent molecule about another center of inversion. The P=O bond [1.528 (2) Å] is slightly longer than a typical P=O double bond (average 1.500 ).

Related literature

For general background to the structure and coordination mode of (diphenylphosphino)diphenylphosphine (DPDP), see: Ferguson et al. (1990); Kuramshin & Khramov (1983). For a Zr^IVcomplex with a DPDP ligand, see: Muratova et al. (1980). For comparison P-O bond distances, see: Berners-Price et al. (2009).

Experimental

Crystal data

[ZrCl₄(C₂₄H₂₀OP₂)₂]·C₆H₆
M_r = 1083.81
Triclinic, $[P \overline 1]$
a = 9.6073 (3) Å
b = 10.1521 (4) Å
c = 14.0204 (10) Å
= 79.027 (13)°
= 87.269 (13)°
= 73.096 (11)°
V = 1284.42 (11) Å³
Z = 1
Mo K radiation
= 0.59 mm^-1
T = 173 K
0.30 × 0.15 × 0.13 mm

Data collection

Rigaku Mercury diffractometer
Absorption correction: multi-scan (Jacobson, 1998) T_min = 0.900, T_max = 0.927
10324 measured reflections
5669 independent reflections
4497 reflections with I > 2(I)
R_int = 0.031

Refinement

R[F² > 2(F²)] = 0.045
wR(F²) = 0.151
S = 1.02
5669 reflections
296 parameters
H-atom parameters constrained
_max = 1.04 e Å^-3
_min = -0.81 e Å^-3

Table 1
Selected bond lengths (Å)

Zr1-Cl1	2.4450 (9)
Zr1-Cl2	2.4627 (7)
Zr1-O1	2.0820 (18)

Data collection: CrystalClear (Rigaku, 2007); cell refinement: CrystalClear; data reduction: CrystalStructure (Rigaku, 2007); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: CrystalStructure.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: NG2624 ).

Acknowledgements

We gratefully acknowledge the support of this work by a Grant-in-Aid for Scientific Research from the Ministry of Education, Science, Sports and Culture.

References

Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.
Berners-Price, S. J., Navarro, M. & Skelton, B. W. (2009). Acta Cryst. E65, o542.
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.
Ferguson, G., Myers, M. & Spalding, T. R. (1990). Acta Cryst. C46, 122-124.
Jacobson, R. (1998). Private communication to the Rigaku Corporation, Tokyo, Japan.
Kuramshin, I. Ya. & Khramov, A. S. (1983). Kazan. Gos. Univ. Kazan USSR. Deposited Doc. (VINITI 2649-83), p. 26. CAN 101:219102
Muratova, A. A., Sobanova, O. B., Yarkova, E. G., Khramov, A. S. & Pudovik, A. N. (1980). Zh. Obshch. Khim. 50, 275-280.
Rigaku (2007). CrystalClear and CrystalStructure. Rigaku Corporation, Tokyo, Japan.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.

metal-organic compounds