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Volume 68 
Part 11 
Pages m1390-m1391  
November 2012  

Received 12 October 2012
Accepted 15 October 2012
Online 20 October 2012

Key indicators
Single-crystal X-ray study
T = 100 K
Mean [sigma](C-C) = 0.011 Å
Disorder in solvent or counterion
R = 0.052
wR = 0.147
Data-to-parameter ratio = 10.0
Details
Open access

cis-(2,2'-Bipyridine-[kappa]2N,N')bis(isonicotinamide-[kappa]N1)palladium(II) bis(hexafluoridophosphate)

aDepartment of Chemistry, University of the Incarnate Word, San Antonio, TX 78209, USA,bDepartment of Chemistry & Biochemistry, University of Oklahoma, Norman, OK 73019, USA,cDepartment of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia, and dChemistry Department, Faculty of Science, King Abdulaziz University, PO Box 80203 Jeddah, Saudi Arabia
Correspondence e-mail: edward.tiekink@um.edu.my

In the title salt, [Pd(C10H8N2)(C6H6NO)2](PF6)2, the PdII atom is in a slightly distorted square-planar coordination environment by N atoms derived from two 4-pyridinecarboxamide ligands, in a cis disposition, and a chelating 2,2'-bipyridine molecule. The monodentate ligands are nearly orthogonal to each other [dihedral angle = 85.7 (5)°] and to the PdN4 plane [dihedral angles = 79.3 (3) and 78.7 (3)°]. The amide O atoms lie to opposite sides of the PdN4 plane. The most notable feature of the crystal packing is a linear supramolecular chain orientated approximately along [310] and formed via 16-membered {...HNCO}4 motifs. These are connected into a three-dimensional network by amide-H...O, F interactions. Both PF6- anions are disordered over two positions of equal occupancy in respect of the F atoms.

Related literature

For the synthesis of compounds with supramolecular structures involving carboxamides as ligands, see: Sun et al. (2011[Sun, D., Wei, Z., Yang, C., Wang, D., Zhang, N., Huang, R. & Zheng, L. (2011). CrystEngComm, 13, 1591-1601.]); Moncol et al. (2007[Moncol, J., Mudra, M., Lonnecke, P., Hewitt, M., Valko, M., Morris, H., Svorec, J., Melnik, M., Mazur, M. & Koman, M. (2007). Inorg. Chim. Acta, 360, 3213-3225.]). For related palladium(II) complexes with isonicotinamide, see: Galstyan et al. (2011[Galstyan, A., Sanz Miguel, P. J. & Lippert, B. (2011). Inorg. Chim. Acta, 374, 453-460.]); Fujimura et al. (2004[Fujimura, T., Seino, H., Hidai, M. & Mizobe, Y. (2004). J. Organomet. Chem. 689, 738-743.]); Qin et al. (2001[Qin, Z., Jennings, M. C. & Puddephatt, R. J. (2001). Inorg. Chem. 40, 6220-6228.]). For hydration of palladium-coordinated nitriles, see: Sanchez et al. (2000[Sanchez, G., Serrano, J. L., Ramirez de Arellano, M. C., Perez, J. & Lopez, G. (2000). Polyhedron, 19, 1395-1406.]).

[Scheme 1]

Experimental

Crystal data
  • [Pd(C10H8N2)(C6H6NO2)2](PF6)2

  • Mr = 796.78

  • Monoclinic, C 2/c

  • a = 22.5920 (14) Å

  • b = 13.8299 (8) Å

  • c = 17.9092 (12) Å

  • [beta] = 95.269 (8)°

  • V = 5572.0 (6) Å3

  • Z = 8

  • Cu K[alpha] radiation

  • [mu] = 7.55 mm-1

  • T = 100 K

  • 0.46 × 0.16 × 0.15 mm

Data collection
  • Bruker APEX CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 2007[Sheldrick, G. M. (2007). SADABS. University of Göttingen, Germany.]) Tmin = 0.126, Tmax = 0.401

  • 30116 measured reflections

  • 5182 independent reflections

  • 3944 reflections with I > 2[sigma](I)

  • Rint = 0.072

Refinement
  • R[F2 > 2[sigma](F2)] = 0.052

  • wR(F2) = 0.147

  • S = 1.01

  • 5182 reflections

  • 520 parameters

  • 144 restraints

  • H-atom parameters constrained

  • [Delta][rho]max = 0.67 e Å-3

  • [Delta][rho]min = -0.78 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
N2-H1N...O2i 0.88 2.29 3.031 (11) 142
N2-H1N...O2ii 0.88 2.37 3.032 (11) 132
N2-H2N...F9iii 0.88 2.24 3.037 (15) 151
N2-H2N...F11'iii 0.88 2.38 3.220 (14) 159
N4-H3N...F7'iv 0.88 2.52 3.175 (19) 132
N4-H3N...F8iv 0.88 2.55 3.10 (2) 121
N4-H4N...O1v 0.88 1.97 2.836 (11) 168
Symmetry codes: (i) [x-{\script{1\over 2}}, y-{\script{1\over 2}}, z]; (ii) [-x+{\script{3\over 2}}, y-{\script{1\over 2}}, -z+{\script{3\over 2}}]; (iii) [x, -y+1, z+{\script{1\over 2}}]; (iv) [x+{\script{1\over 2}}, y-{\script{1\over 2}}, z]; (v) [-x+{\script{3\over 2}}, -y+{\script{1\over 2}}, -z+1].

Data collection: SMART (Bruker, 1998[Bruker (1998). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 1998[Bruker (1998). SMART and SAINT. 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: ORTEP-3 for Windows (Farrugia, 2012[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]) and DIAMOND (Brandenburg, 2006[Brandenburg, K. (2006). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: publCIF (Westrip, 2010[Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.]).


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: SU2513 ).


Acknowledgements

The authors appreciate the support of the Chemistry Department at the University of the Incarnate Word. The authors thank the National Science Foundation (grant CHE-0130835) and the University of Oklahoma for funds to purchase the X-ray instrument and computers. We also thank the Ministry of Higher Education (Malaysia) for funding structural studies through the High-Impact Research scheme (UM.C/HIR-MOHE/SC/12).

References

Brandenburg, K. (2006). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Bruker (1998). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.  [ISI] [CrossRef] [ChemPort] [details]
Fujimura, T., Seino, H., Hidai, M. & Mizobe, Y. (2004). J. Organomet. Chem. 689, 738-743.  [CSD] [CrossRef] [ChemPort]
Galstyan, A., Sanz Miguel, P. J. & Lippert, B. (2011). Inorg. Chim. Acta, 374, 453-460.  [ISI] [CSD] [CrossRef] [ChemPort]
Moncol, J., Mudra, M., Lonnecke, P., Hewitt, M., Valko, M., Morris, H., Svorec, J., Melnik, M., Mazur, M. & Koman, M. (2007). Inorg. Chim. Acta, 360, 3213-3225.  [ISI] [CSD] [CrossRef] [ChemPort]
Qin, Z., Jennings, M. C. & Puddephatt, R. J. (2001). Inorg. Chem. 40, 6220-6228.  [ISI] [CSD] [CrossRef] [PubMed] [ChemPort]
Sanchez, G., Serrano, J. L., Ramirez de Arellano, M. C., Perez, J. & Lopez, G. (2000). Polyhedron, 19, 1395-1406.  [ISI] [CrossRef] [ChemPort]
Sheldrick, G. M. (2007). SADABS. University of Göttingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Sun, D., Wei, Z., Yang, C., Wang, D., Zhang, N., Huang, R. & Zheng, L. (2011). CrystEngComm, 13, 1591-1601.  [ISI] [CSD] [CrossRef] [ChemPort]
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.  [ISI] [CrossRef] [ChemPort] [details]


Acta Cryst (2012). E68, m1390-m1391   [ doi:10.1107/S1600536812043036 ]

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