1-Diphenyl­phosphino-1′-(diphenyl­phosphinoyl)cobaltocenium hexa­fluorido­phosphate

Xiang-Hua Wu; Rui Guo; Shan Jin; Guang-Ao Yu; Sheng-Hua Liu

doi:10.1107/S1600536808027992

. 2008 Sep 6;64(Pt 10):m1247. doi: 10.1107/S1600536808027992

1-Diphenylphosphino-1′-(diphenylphosphinoyl)cobaltocenium hexafluoridophosphate

Xiang-Hua Wu ^a, Rui Guo ^a, Shan Jin ^a,^*, Guang-Ao Yu ^a, Sheng-Hua Liu ^a

PMCID: PMC2959285 PMID: 21201004

Abstract

The title compound, [Co(C₁₇H₁₄OP)(C₁₇H₁₄P)]PF₆, was obtained unintentionally as the product of an attempted synthesis of [1,1′-bis(oxodiphenylphosphoranyl)cobaltocenium] hexafluoridophosphate. The O atom of the oxo group is disordered over two positions with site occupancies of 0.65:0.35. The crystal structure contains weak intermolecular C—H⋯F hydrogen bonds, connecting the components of the structure into chains parallel to [010].

Related literature

For related literature, see: Song (2004 ▶).

Experimental

Crystal data

[Co(C₁₇H₁₄OP)(C₁₇H₁₄P)]PF₆
M _r = 718.40
Monoclinic,
a = 12.0364 (14) Å
b = 10.7014 (13) Å
c = 24.973 (3) Å
β = 103.94°
V = 3121.9 (6) Å³
Z = 4
Mo Kα radiation
μ = 0.77 mm⁻¹
T = 293 (2) K
0.30 × 0.20 × 0.10 mm

Data collection

Bruker SMART CCD diffractometer
Absorption correction: none
33887 measured reflections
7444 independent reflections
3990 reflections with I > 2σ(I)
R _int = 0.093

Refinement

R[F ² > 2σ(F ²)] = 0.053
wR(F ²) = 0.101
S = 0.85
7444 reflections
416 parameters
H-atom parameters constrained
Δρ_max = 0.40 e Å⁻³
Δρ_min = −0.50 e Å⁻³

Data collection: SMART (Bruker, 2001 ▶); cell refinement: SAINT (Bruker, 2001 ▶); 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 Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808027992/lh2674sup1.cif

e-64-m1247-sup1.cif^{(37KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808027992/lh2674Isup2.hkl

e-64-m1247-Isup2.hkl^{(364.2KB, hkl)}

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Table 1. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C4—H4⋯F6ⁱ	0.98	2.49	3.450 (4)	167
C18—H18⋯F5	0.98	2.43	3.327 (4)	152

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Symmetry code: (i) Inline graphic .

Acknowledgments

The authors acknowledge financial support from the National Natural Science Foundation of China (grant Nos. 20572029 and 20772039).

supplementary crystallographic information

Comment

The molecular structure of the title compound consists of a [(η5-Ph₂POC₅H₄)(η5-Ph₂PC₅H₄)Co]⁺ cation and a PF6^- anion, (I) (Fig. 1), which essentially identical to the isomorphous complex [(η5Ph₂POC₅H₄)₂Co]⁺(PF6)^- (II) (Song, 2004). The two substituted Cp rings are staggered and essentially parallel with a dihedral angle of 0.2 (3)° for (II) and 0.2 (9)° for (I). The distance between the Co atom and the centroid of Cp ring is 1.635 (9) Å for (II) and 1.644 (1) Å for (I). In both structures, the two Ph₂P substituents are trans to each other with respect to the Co metal center. However, both P atoms are double bonded to two O atoms in (II) while in (I) the single O atom of the oxo group is disordered with an approximate ratio of occupancies of 0.65:0.35. The crystal structure contains weak intermolecular C—H···F hydrogen bonds, connecting the components of the structure into one-dimensional chains.

Experimental

The title compound was obtained unintentionally as a side-product of synthesis of [1,1'-bis(oxodiphenylphosphoranyl) cobaltocenium] hexafluorophosphate (Song, 2004). Crystals appropriate for data collection were obtained by slow evaporation from dichloromethane and hexane solution at romm temperature.