Bis{μ-2-[(dimethyl­amino)­meth­yl]benzene­tellurolato}bis­[chlorido­palladium(II)] dichloro­methane hemisolvate

Butcher, R.J.; Chakravorty, T.; Singh, H.B.

doi:10.1107/S1600536812000104

Volume 68
Part 2
Pages m141-m142
February 2012

Received 22 December 2011
Accepted 3 January 2012
Online 11 January 2012

Key indicators
Single-crystal X-ray study
T = 100 K
Mean (C-C) = 0.012 Å
R = 0.039
wR = 0.102
Data-to-parameter ratio = 21.7
Details

Bis{-2-[(dimethylamino)methyl]benzenetellurolato}bis[chloridopalladium(II)] dichloromethane hemisolvate

Ray J. Butcher,^a ^* Tapash Chakravorty ^b and Harkesh B. Singh ^b

^aDepartment of Chemistry, Howard University, 525 College Street NW, Washington DC 20059, USA, and ^bDepartment of Chemistry, Indian Institute of Technology Bombay, Powai, Mumbai 400 076, India
Correspondence e-mail: rbutcher99@yahoo.com

The asymmetric unit of the title compound, [Pd₂(C₉H₁₂NTe)₂Cl₂]·0.5CH₂Cl₂, contains two half-molecules, each lying on a twofold rotation axis; each molecule is chiral and of the same enantiomer. This is only possible as the molecule has a hinged cis arrangement about the Pd²⁺ coordination spheres. For this hinged dimeric structure, the angles between the two coordination planes in each molecule are 21.59 (4) and 22.10 (4)°. This hinged cis arrangement also allows the two molecules to form pairs linked by secondary interactions between the Pd and Te atoms of an adjoining molecule, leading to a tetrameric overall structure. C-HCl interactions consolidate the crystal packing.

Related literature

For related structures of bridged dimers of palladium mediated by Se, see: Brown & Corrigan (2004); Chakraborty et al. (2011); Dey et al. (2006); Ford et al. (2004); Kaur et al. (2009); Morley et al. (2006); Nakata et al. (2009); Oilunkaniemi et al. (1999, 2001). For Se/Te-bridged Pd dimeric structures which exhibit either a hinged or cis arrangement of ligands about the bridging plane, see: Kaur et al. (2009); Oilunkaniemi et al. (2000); Chakravorty et al. (2012). For the synthesis of the title compound, see: Chakraborty et al. (2011).

Experimental

Crystal data

[Pd₂(C₉H₁₂NTe)₂Cl₂]·0.5CH₂Cl₂
M_r = 1699.51
Orthorhombic, P 2₁ 2₁ 2
a = 14.035 (2) Å
b = 14.842 (2) Å
c = 12.3188 (16) Å
V = 2566.0 (6) Å³
Z = 2
Mo K radiation
= 3.95 mm^-1
T = 100 K
0.32 × 0.26 × 0.18 mm

Data collection

Bruker APEXII CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) T_min = 0.615, T_max = 0.746
36521 measured reflections
5506 independent reflections
5148 reflections with I > 2(I)
R_int = 0.050

Refinement

R[F² > 2(F²)] = 0.039
wR(F²) = 0.102
S = 1.06
5506 reflections
254 parameters
H-atom parameters constrained
_max = 2.12 e Å^-3
_min = -0.90 e Å^-3
Absolute structure: Flack (1983), 2355 Friedel pairs
Flack parameter: 0.06 (4)

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
C1S-H1SACl1B	0.96	2.87	3.827 (9)	173
C5A-H5AACl1Aⁱ	0.95	2.91	3.778 (9)	152
C7A-H7AACl1Aⁱ	0.99	2.73	3.681 (9)	162
C9A-H9ACCl1A	0.98	2.70	3.313 (10)	121
C7B-H7BACl1Bⁱⁱ	0.99	2.77	3.746 (10)	169
C7B-H7BBCl1Sⁱⁱ	0.99	2.75	3.514 (10)	135
C9B-H9BBCl1B	0.98	2.67	3.300 (11)	123
Symmetry codes: (i) $[x+{\script{1\over 2}}, -y+{\script{1\over 2}}, -z+1]$ ; (ii) $[-x+{\script{1\over 2}}, y-{\script{1\over 2}}, -z+2]$ .

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Bruker, 2002); 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: JJ2116 ).

Acknowledgements

HBS acknowledges the DST, New Delhi, for financial support. TC acknowledges the CSIR, New Delhi, for a fellowship. RJB acknowledges the NSF-MRI program (grant No. CHE-0619278) for funds to purchase the diffractometer.

References

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metal-organic compounds