{1,3-Bis[(diphenyl­phosphanyl-κP)­oxy]prop-2-yl-κC2}iodido(trimethyl­phosphane)cobalt(II)

Xu, G.; Li, X.

doi:10.1107/S1600536810013747

Volume 66
Part 5
Page m545
May 2010

Received 19 March 2010
Accepted 14 April 2010
Online 21 April 2010

Key indicators
Single-crystal X-ray study
T = 293 K
Mean (C-C) = 0.003 Å
R = 0.024
wR = 0.061
Data-to-parameter ratio = 17.5
Details

{1,3-Bis[(diphenylphosphanyl-P)oxy]prop-2-yl-C²}iodido(trimethylphosphane)cobalt(II)

Guoqiang Xu ^a and Xiaoyan Li ^a ^*

^aSchool of Chemistry and Chemical Engineering, Shandong University, Jinan 250100, People's Republic of China
Correspondence e-mail: xli63@sdu.edu.cn

The title compound, [Co(C₂₇H₂₅O₂P₂)I(C₃H₉P)], was synthesized by the addition of 1-iodobutane to a solution of the parent cobalt complex {1,3-bis[(diphenylphosphanyl)oxy]prop-2-yl}bis(trimethylphosphane)cobalt(II). Two five-membered cobaltocycles with considerable ring bending (sum of internal angles = 516.4 and 517.7°) are formed through two P atoms of the PPh₂ groups and a metallated Csp³ atom. The Co^II atom is centered in a trigonal-bipyramidal configuration.

Related literature

For general background to transition metal complexes with PCP pincer ligands and their preparation, see: Boom & Milstein (2003); Pandarus et al. (2008); Xu et al. (2009); Zheng et al. (2009). For Co-Csp³ bond lengths, see: Klein et al. (2003).

Experimental

Crystal data

[Co(C₂₇H₂₅O₂P₂)I(C₃H₉P)]
M_r = 705.31
Orthorhombic, P b c a
a = 15.161 (3) Å
b = 18.194 (4) Å
c = 21.410 (4) Å
V = 5906 (2) Å³
Z = 8
Mo K radiation
= 1.82 mm^-1
T = 293 K
0.20 × 0.15 × 0.10 mm

Data collection

Bruker SMART CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 2004) T_min = 0.713, T_max = 0.876
35496 measured reflections
6237 independent reflections
5551 reflections with I > 2(I)
R_int = 0.071

Refinement

R[F² > 2(F²)] = 0.024
wR(F²) = 0.061
S = 1.04
6237 reflections
357 parameters
H atoms treated by a mixture of independent and constrained refinement
_max = 0.57 e Å^-3
_min = -0.54 e Å^-3

Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); 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); software used to prepare material for publication: SHELXTL.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: ZQ2034 ).

Acknowledgements

We gratefully acknowledge support by NSF China (No. 20872080/20772072).

References

Boom, M. & Milstein, D. (2003). Chem. Rev. 103, 1759-1792.
Bruker (1997). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Klein, H.-F., Beck, R., Flörke, U. & Haupt, H.-J. (2003). Eur. J. Inorg. Chem. pp. 853-862.
Pandarus, V., Castonguay, A. & Zargarian, D. (2008). Dalton Trans. pp. 4756-4761.
Sheldrick, G. M. (2004). SADABS. University of Göttingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Xu, G., Sun, H. & Li, X. (2009). Organometallics, 28, 6090-6095.
Zheng, T., Sun, H., Chen, Y., Li, X., Dürr, S., Radius, U. & Harms, K. (2009). Organometallics, 28, 5771-5776.

metal-organic compounds

{1,3-Bis[(diphenylphosphanyl-P)oxy]prop-2-yl-C2}iodido(trimethylphosphane)cobalt(II)