[1,2-Bis­(diisopropyl­phosphan­yl)ethane-κ2P,P′]dichloridonickel(II)–9H-carbazole (1/2)

Cañavera-Buelvas, F.; Flores-Alamo, M.; García, J.J.

doi:10.1107/S1600536811010555

Volume 67
Part 4
Page m501
April 2011

Received 4 March 2011
Accepted 21 March 2011
Online 26 March 2011

Key indicators
Single-crystal X-ray study
T = 122 K
Mean (C-C) = 0.002 Å
R = 0.026
wR = 0.065
Data-to-parameter ratio = 16.5
Details

[1,2-Bis(diisopropylphosphanyl)ethane-²P,P']dichloridonickel(II)-9H-carbazole (1/2)

Farah Cañavera-Buelvas,^a Marcos Flores-Alamo ^a and Juventino J. García ^a ^*

^aFacultad de Química, Universidad Nacional Autónoma de México, México DF 04510, Mexico
Correspondence e-mail: juvent@servidor.unam.mx

In the title compound, [NiCl₂(C₁₄H₃₂P₂)]·2C₁₂H₉N, the neutral [Ni(dppe)Cl₂] complex [dppe is 1,2-bis(diisopropylphosphanyl)ethane] consists of a tetracoordinated Ni²⁺ cation and has a crystallographic twofold axis passing through the metal atom and the mid-point of the CH₂-CH₂ bond of the dppe ligand. The metal atom shows slight tetrahedral distortion from an ideal square-planar coordination geometry, as reflected in the dihedral angle between NiCl₂ and NiP₂ planes of 15.32 (2)°. The 9H-carbazole ring system is essentially planar (r.m.s. deviation = 0.022 Å). In the crystal packing, there are two symmetry-related 9H-carbazole molecules between two adjacent Ni^II complexes, with an angle between the carbazole mean planes of ca 77°.

Related literature

For the use of nickel complexes of the type [Ni(dppe)Cl₂] as starting materials and precursors in metal-mediated and catalytic systems, respectively, see: Vicic & Jones (1997); Arévalo & García (2010). For details of tetrahedral distortion and motifs, see: Angulo et al. (2003); Dahlenburg & Kurth (2001); Etter et al. (1990).

Experimental

Crystal data

[NiCl₂(C₁₄H₃₂P₂)]·2C₁₂H₉N
M_r = 726.35
Monoclinic, C 2/c
a = 22.5830 (5) Å
b = 8.4374 (2) Å
c = 18.9630 (5) Å
= 101.544 (2)°
V = 3540.15 (15) Å³
Z = 4
Mo K radiation
= 0.82 mm^-1
T = 122 K
0.42 × 0.16 × 0.02 mm

Data collection

Oxford Diffraction Xcalibur Atlas Gemini diffractometer
Absorption correction: analytical [CrysAlis PRO (Oxford Diffraction, 2009 $[Oxford Diffraction (2009). CrysAlis PRO, CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Yarnton, England.]$ ); based on expressions derived by Clark & Reid (1995)] T_min = 0.851, T_max = 0.987
12792 measured reflections
3484 independent reflections
2908 reflections with I > 2(I)
R_int = 0.027

Refinement

R[F² > 2(F²)] = 0.026
wR(F²) = 0.065
S = 1.05
3484 reflections
211 parameters
H atoms treated by a mixture of independent and constrained refinement
_max = 0.62 e Å^-3
_min = -0.26 e Å^-3

Table 1
Selected geometric parameters (Å, °)

Ni1-Cl1	2.2221 (4)
Ni1-P1	2.1581 (5)

P1ⁱ-Ni1-P1	88.61 (3)
P1ⁱ-Ni1-Cl1ⁱ	168.757 (16)
P1ⁱ-Ni1-Cl1	89.797 (16)
Cl1ⁱ-Ni1-Cl1	93.87 (2)
Symmetry code: (i) $[-x, y, -z+{\script{1\over 2}}]$ .

Data collection: CrysAlis CCD (Oxford Diffraction, 2009 $[Oxford Diffraction (2009). CrysAlis PRO, CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Yarnton, England.]$ ); cell refinement: CrysAlis RED (Oxford Diffraction, 2009 $[Oxford Diffraction (2009). CrysAlis PRO, CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Yarnton, England.]$ ); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: BH2344 ).

Acknowledgements

We thank PAPIIT-DGAPA-UNAM (IN-201010) and CONACYT (080606) for their financial support of this work and DGAPA-UNAM for a postdoctoral grant to FCB. We also thank Dr A. Arévalo for technical assistance.

References

Angulo, I. M., Bouwman, E., van Gorkum, R., Lok, S. M., Lutz, M. & Spek, A. L. (2003). J. Mol. Catal. A Chem. 202, 97-106.
Arévalo, A. & García, J. J. (2010). Eur. J. Inorg. Chem. pp. 4063-4074.
Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897.
Dahlenburg, L. & Kurth, V. (2001). Inorg. Chim. Acta, 319, 176-182.
Etter, M. C., MacDonald, J. C. & Bernstein, J. (1990). Acta Cryst. B46, 256-262.
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.
Oxford Diffraction (2009). CrysAlis PRO, CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Yarnton, England.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Vicic, D. A. & Jones, W. D. (1997). J. Am. Chem. Soc. 119, 10855-10856.

metal-organic compounds

[1,2-Bis(diisopropylphosphanyl)ethane-2P,P']dichloridonickel(II)-9H-carbazole (1/2)