μ-Azido-κ2N1:N1-μ-chlorido-bis­[(2-chloro-3-dimethyl­amino-1-phenyl­prop-1-en-1-yl-κ2C1,N)palladium(II)] chloro­form monosolvate

Mafud, A.C.; Oliviera, M.A.R.; Gambardella, M.T.P.

doi:10.1107/S1600536812047927

Volume 69
Part 1
Page m15
January 2013

Received 11 November 2012
Accepted 21 November 2012
Online 8 December 2012

Key indicators
Single-crystal X-ray study
T = 293 K
Mean (C-C) = 0.017 Å
R = 0.063
wR = 0.170
Data-to-parameter ratio = 22.1
Details

-Azido-²N¹:N¹--chlorido-bis[(2-chloro-3-dimethylamino-1-phenylprop-1-en-1-yl-²C¹,N)palladium(II)] chloroform monosolvate

Ana C. Mafud,^a ^* Milene A. R. Oliviera ^b and Maria T. P. Gambardella ^b

^aInstituto de Fisica de Sao Carlos, Av. do Trabalhador Saocarlense, 400 Sao Carlos, SP, Brazil, and ^bInstituto de Quimica de Sao Carlos, Av. do Trabalhador Saocarlense, 400 Sao Carlos, SP, Brazil
Correspondence e-mail: mafud@usp.br

In the binuclear title complex, [Pd₂(C₁₁H₁₃ClN)₂Cl(N₃)]·CHCl₃, each Pd^II atom has a slightly distorted square-planar geometry being coordinated by a C and an N atom of the 2-chloro-3-dimethylamino-1-phenylpropyl ligand, a bridging Cl atom and an N atom of a bridging end-on azide group. There is a short intramolecular C-HCl contact in the complex molecule. In the crystal, the chloroform solvent molecule is linked to the complex via a C-H [pi] interaction.

Related literature

For the crystal structures of similar compounds, see: Moro et al. (2004); Caires et al. (2006).

Experimental

Crystal data

[Pd₂(C₁₁H₁₃ClN)₂Cl(N₃)]·CHCl₃
M_r = 799
Monoclinic, P 2₁ /c
a = 15.416 (3) Å
b = 11.474 (3) Å
c = 17.094 (4) Å
= 97.14 (2)°
V = 3000.2 (12) Å³
Z = 4
Mo K radiation
= 1.76 mm^-1
T = 293 K
0.2 × 0.1 × 0.1 mm

Data collection

Enraf-Nonius TurboCAD4 diffractometer
Absorption correction: scan (North et al., 1968) T_min = 0.691, T_max = 0.832
7536 measured reflections
7278 independent reflections
2686 reflections with I > 2(I)
R_int = 0.066
3 standard reflections every 120 min intensity decay: 1%

Refinement

R[F² > 2(F²)] = 0.063
wR(F²) = 0.170
S = 0.93
7278 reflections
329 parameters
H-atom parameters constrained
_max = 0.75 e Å^-3
_min = -0.60 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

Cg1 is the centroid of the C1A-C6A ring.

D-HA	D-H	HA	DA	D-HA
C11A-H11BCl1	0.96	2.74	3.299 (11)	118
C12-H12Cg1ⁱ	0.98	2.77	3.713 (13)	163
Symmetry code: (i) -x+2, -y, -z+1.

Data collection: CAD-4 EXPRESS (Enraf-Nonius, 1994); cell refinement: CAD-4 EXPRESS; data reduction: XCAD4 (Harms & Wocadlo, 1995); 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, 2012); software used to prepare material for publication: WinGX (Farrugia, 2012).

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: SU2528 ).

Acknowledgements

We are extremely grateful to the late Professor Antonio Carlos Favero Caires for suppling us with the sample used, and to the CNPq National Council for Technological and Scientific Development for supporting this study.

References

Caires, A. C. F., Mauro, A. E., Moro, A. C., de Oliveira Legendre, A. & Ananias, S. R. (2006). Quím. Nova, 29, 750-754.
Enraf-Nonius (1994). CAD-4 EXPRESS. Enraf-Nonius, Delft, The Netherlands.
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.
Harms, K. & Wocadlo, S. (1995). XCAD4. University of Marburg, Germany.
Moro, A. C., Mauro, A. E. & Ananias, S. R. (2004). Eclet. Quím. 29, 57-61.
North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.

metal-organic compounds

-Azido-2N1:N1--chlorido-bis[(2-chloro-3-dimethylamino-1-phenylprop-1-en-1-yl-2C1,N)palladium(II)] chloroform monosolvate