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Volume 69 
Part 9 
Page m524  
September 2013  

Received 11 August 2013
Accepted 26 August 2013
Online 31 August 2013

Key indicators
Single-crystal X-ray study
T = 150 K
Mean [sigma](C-C) = 0.005 Å
Disorder in main residue
R = 0.033
wR = 0.068
Data-to-parameter ratio = 16.5
Details
Open access

Bis[O,O'-bis(4-tert-butylphenyl) dithiophosphato-[kappa]2S,S']bis(pyridine-[kappa]N)lead(II)

aInstitute of Functionalized Materials, Sichuan University of Science and Engineering, Zigong 643000, People's Republic of China, and bCollege of Chemistry and Pharmaceutical Engineering, Sichuan University of Science and Engineering, Zigong 643000, People's Republic of China
Correspondence e-mail: zxlsuse@sina.com

In the title compound, [Pb(C20H26O2PS2)2(C5H5N)2], the PbII ion is coordinated by two S,S'-bidentate anions and two pyridine molecules. The PbN2S4 coordination geometry approximates to a pentagonal bipyramid with one equatorial site vacant. The N atoms occupy the axial sites. One of the pyridine molecules is disordered over two sets of sites in a 0.907 (7):0.093 (7) ratio and one of the tert-butyl groups is disordered over two sets of sites in a 0.534 (6):0.466 (6) ratio. An intramolecular C-H...O interaction occurs in one of the ligands. In the crystal, pairs of short Pb...S contacts [3.4018 (11) Å] generate a centrosymmetric dimeric assembly with the distant S atom lying in the region of the vacant coordination site of the metal atom. No directional packing interactions occur.

Related literature

For the preparation of the ligand, see: Li & Xie (1997[Li, J.-S. & Xie, B. (1997). Acta Chim. Sin. 55, 892-896.]). For van der Waals radii, see: Bondi (1964[Bondi, A. (1964). J. Phys. Chem. 68, 441-451.]).

[Scheme 1]

Experimental

Crystal data
  • [Pb(C20H26O2PS2)2(C5H5N)2]

  • Mr = 1152.39

  • Triclinic, [P \overline 1]

  • a = 12.4260 (3) Å

  • b = 12.9136 (3) Å

  • c = 17.9749 (4) Å

  • [alpha] = 89.7528 (18)°

  • [beta] = 79.4467 (19)°

  • [gamma] = 71.298 (2)°

  • V = 2681.22 (10) Å3

  • Z = 2

  • Mo K[alpha] radiation

  • [mu] = 3.40 mm-1

  • T = 150 K

  • 0.25 × 0.20 × 0.20 mm

Data collection
  • Bruker APEXII diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2008[Bruker (2008). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.483, Tmax = 0.549

  • 22556 measured reflections

  • 10953 independent reflections

  • 9252 reflections with I > 2[sigma](I)

  • Rint = 0.031

Refinement
  • R[F2 > 2[sigma](F2)] = 0.033

  • wR(F2) = 0.068

  • S = 1.02

  • 10953 reflections

  • 663 parameters

  • 572 restraints

  • H-atom parameters constrained

  • [Delta][rho]max = 0.80 e Å-3

  • [Delta][rho]min = -0.69 e Å-3

Table 1
Selected bond lengths (Å)

Pb1-N1 2.711 (3)
Pb1-N2 2.732 (18)
Pb1-S3 2.8090 (9)
Pb1-S1 2.9009 (9)
Pb1-S4 3.0577 (9)
Pb1-S2 3.0742 (9)

Table 2
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
C12-H12...O1 0.95 2.45 3.083 (5) 124

Data collection: APEX2 (Bruker, 2008[Bruker (2008). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2008[Bruker (2008). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL.


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HB7129 ).


Acknowledgements

The authors acknowledge financial assistance from Sichuan University of Science and Engineering, the Institute of Functionalized Materials (grant No. 2009xjkPL004) and the Education Committee of Sichuan Province (No. 13ZB0134)

References

Bondi, A. (1964). J. Phys. Chem. 68, 441-451.  [CrossRef] [ChemPort] [ISI]
Bruker (2008). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Li, J.-S. & Xie, B. (1997). Acta Chim. Sin. 55, 892-896.  [ChemPort]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [details]


Acta Cryst (2013). E69, m524  [ doi:10.1107/S1600536813023945 ]

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