cis-(2,2′-Bipyridine-κ2N,N′)bis­(isonicotinamide-κN1)palladium(II) bis­(hexa­fluoridophosphate)

Adrian, R.A.; Quintela, B.; Powell, D.R.; Ng, S.W.; Tiekink, E.R.T.

doi:10.1107/S1600536812043036

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 (C-C) = 0.011 Å
Disorder in solvent or counterion
R = 0.052
wR = 0.147
Data-to-parameter ratio = 10.0
Details

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

Rafael A. Adrian,^a ⁺ Brayan Quintela,^a Douglas R. Powell,^b Seik Weng Ng ^c,^d and Edward R. T. Tiekink ^c ^*

^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 Pd^II 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-HO, 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); Moncol et al. (2007). For related palladium(II) complexes with isonicotinamide, see: Galstyan et al. (2011); Fujimura et al. (2004); Qin et al. (2001). For hydration of palladium-coordinated nitriles, see: Sanchez et al. (2000).

Experimental

Crystal data

[Pd(C₁₀H₈N₂)(C₆H₆NO₂)₂](PF₆)₂
M_r = 796.78
Monoclinic, C 2/c
a = 22.5920 (14) Å
b = 13.8299 (8) Å
c = 17.9092 (12) Å
= 95.269 (8)°
V = 5572.0 (6) Å³
Z = 8
Cu K radiation
= 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) T_min = 0.126, T_max = 0.401
30116 measured reflections
5182 independent reflections
3944 reflections with I > 2(I)
R_int = 0.072

Refinement

R[F² > 2(F²)] = 0.052
wR(F²) = 0.147
S = 1.01
5182 reflections
520 parameters
144 restraints
H-atom parameters constrained
_max = 0.67 e Å^-3
_min = -0.78 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
N2-H1NO2ⁱ	0.88	2.29	3.031 (11)	142
N2-H1NO2ⁱⁱ	0.88	2.37	3.032 (11)	132
N2-H2NF9ⁱⁱⁱ	0.88	2.24	3.037 (15)	151
N2-H2NF11'ⁱⁱⁱ	0.88	2.38	3.220 (14)	159
N4-H3NF7'^iv	0.88	2.52	3.175 (19)	132
N4-H3NF8^iv	0.88	2.55	3.10 (2)	121
N4-H4NO1^v	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); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; 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) and DIAMOND (Brandenburg, 2006); software used to prepare material for publication: publCIF (Westrip, 2010).

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

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Fujimura, T., Seino, H., Hidai, M. & Mizobe, Y. (2004). J. Organomet. Chem. 689, 738-743.
Galstyan, A., Sanz Miguel, P. J. & Lippert, B. (2011). Inorg. Chim. Acta, 374, 453-460.
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