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Volume 68 
Part 11 
Pages m1347-m1348  
November 2012  

Received 18 September 2012
Accepted 4 October 2012
Online 13 October 2012

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Key indicators
Single-crystal X-ray study
T = 200 K
Mean [sigma](C-C) = 0.004 Å
R = 0.030
wR = 0.081
Data-to-parameter ratio = 12.2
Details
Open access

Bis(2,2'-bipyrimidine-[kappa]2N1,N1')palladium(II) bis(tetrafluoroborate) acetonitrile monosolvate

Adam Duong,a James D. Wuesta and Thierry Marisa*

aDépartement de Chimie, Université de Montréal, 2900 Boulevard Édouard-Montpetit, Montréal, Québec, Canada H3C 3J7
Correspondence e-mail: thierry.maris@umontreal.ca

The reaction of [Pd(MeCN)4](BF4)2 with 2,2'-bipyrimidine (bpm) in MeCN-CHCl3 afforded the title compound, [Pd(C8H6N4)2](BF4)2·C2H3N. The asymmetric unit contains two half complexes, with the PdII atoms both lying on a twofold axis. Each metal atom adopts a tetrahedrally distorted square-planar geometry. In the crystal, [Pd(bpm)2] dications are linked by C-H...N hydrogen bonds, forming chains parallel to the b axis. The chains are further linked by C-H...F and C-H...N interactions involving the tetrafluoroborate anions and acetonitrile molecules. In this way, each chain interacts with six surrounding chains to generate the observed three-dimensional structure.

Related literature

Similar Pd(bpm)2 complexes are unknown, but the subject of related dicationic adducts of PdII with 2,2'-bipyridyl (bpy) has been reviewed by Constable (1989[Constable, E. C. (1989). Adv. Inorg. Chem. 34, 1-63.]) and McKenzie (1971[McKenzie, E. D. (1971). Coord. Chem. Rev. 6, 187-216.]), and the structures of representative analogues have been reported by Chieh (1972[Chieh, P. C. (1972). J. Chem. Soc. Dalton Trans. pp. 1643-1646.]), Duong et al. (2011[Duong, A., Maris, T. & Wuest, J. D. (2011). Inorg. Chem. 50, 5605-5618.]), Gao et al. (2010[Gao, E. J., Zhang, Y. X., Zhu, M. C., Liu, H. Y., Huang, Y., Zhang, M., Su, M., Guo, M. J., Guan, F., Gao, X. N. & Wang, M. L. (2010). Russ. J. Coord. Chem. 36, 853-858.]), Geremia et al. (1992[Geremia, S., Randaccio, L., Mestroni, G. & Milani, B. (1992). J. Chem. Soc. Dalton Trans. pp. 2117-2118.]), Hinamoto et al. (1972[Hinamoto, M., Ooi, S. & Kuroya, H. (1972). J. Chem. Soc. Chem. Commun. pp. 356-357.]), Maeda et al. (1986[Maeda, S., Nishida, Y., Okawa, H. & Kida, S. (1986). Bull. Chem. Soc. Jpn, 59, 2013-2014.]), Milani et al. (1997[Milani, B., Anzilutti, A., Vicentini, L., Sessanta o Santi, A., Zangrando, E., Geremia, S. & Mestroni, G. (1997). Organometallics, 16, 5064-5075.]), Stoccoro et al. (2002[Stoccoro, S., Alesso, G., Cinellu, M. A., Minghetti, G., Zucca, A., Bastero, A., Claver, C. & Manassero, M. (2002). J. Organomet. Chem. 664, 77-84.]), Wehman et al. (1994[Wehman, P., Dol, G. C., Moorman, E. R., Kamer, P. C. J., van Leeuwen, P. W. N. M., Fraanje, J. & Goubitz, K. (1994). Organometallics, 13, 4856-4869.]) and Yue et al. (2008[Yue, C.-Y., Jiang, F.-L., Yuan, D.-Q., Chen, L., Wu, M.-Y. & Hong, M.-C. (2008). Chin. J. Struct. Chem. 27, 467-470.]).

[Scheme 1]

Experimental

Crystal data

  • [Pd(C8H6N4)2](BF4)2·C2H3N

  • Mr = 637.41

  • Monoclinic, C 2/c

  • a = 18.0686 (4) Å

  • b = 18.1126 (4) Å

  • c = 14.8351 (3) Å

  • [beta] = 108.613 (1)°

  • V = 4601.13 (17) Å3

  • Z = 8

  • Cu K[alpha] radiation

  • [mu] = 7.38 mm-1

  • T = 200 K

  • 0.20 × 0.11 × 0.10 mm
Data collection

  • Bruker SMART 6000 diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 2004[Sheldrick, G. M. (2004). SADABS. University of Göttingen, Germany.]) Tmin = 0.311, Tmax = 0.478

  • 31076 measured reflections

  • 4246 independent reflections

  • 4006 reflections with I > 2[sigma](I)

  • Rint = 0.031
Refinement

  • R[F2 > 2[sigma](F2)] = 0.030

  • wR(F2) = 0.081

  • S = 1.03

  • 4246 reflections

  • 347 parameters

  • H-atom parameters constrained

  • [Delta][rho]max = 1.07 e Å-3

  • [Delta][rho]min = -0.75 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
C1-H1...N11i 0.95 2.62 3.460 (4) 148
C6-H6...N15ii 0.95 2.45 3.237 (4) 140
C14-H14...N16iii 0.95 2.40 3.228 (4) 146
C2-H2...F7iii 0.95 2.38 3.282 (3) 159
C3-H3...F2iv 0.95 2.44 3.240 (3) 142
C8-H8...F3v 0.95 2.45 3.270 (4) 145
C13-H13...F6vi 0.95 2.37 2.982 (3) 122
C15-H15...F8iv 0.95 2.52 3.408 (4) 155
C18-H18B...F5vii 0.98 2.55 3.373 (5) 142
Symmetry codes: (i) [x+{\script{1\over 2}}, y+{\script{1\over 2}}, z]; (ii) [-x+{\script{1\over 2}}, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]; (iii) [-x+{\script{1\over 2}}, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]; (iv) [x, -y+1, z-{\script{1\over 2}}]; (v) [-x+{\script{1\over 2}}, -y+{\script{1\over 2}}, -z]; (vi) [-x, y, -z+{\script{1\over 2}}]; (vii) [-x+{\script{1\over 2}}, -y+{\script{1\over 2}}, -z+1].

Data collection: SMART (Bruker, 2003[Bruker (2003). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2003[Bruker (2003). 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: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]) and Materials Studio (Accelrys, 2002[Accelrys (2002). Materials Studio. Accelrys Inc., San Diego, California, USA.]); software used to prepare material for publication: UdMX (Maris, 2004[Maris, T. (2004). UdMX. Université de Montréal, Montréal, Québec, Canada.]) and 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: RZ5009 ).

Acknowledgements

We are grateful to the Natural Sciences and Engineering Research Council of Canada, the Ministère de l'Éducation du Québec, the Canada Foundation for Innovation, the Canada Research Chairs Program, and the Université de Montréal for financial support.

References

Accelrys (2002). Materials Studio. Accelrys Inc., San Diego, California, USA.
Bruker (2003). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Chieh, P. C. (1972). J. Chem. Soc. Dalton Trans. pp. 1643-1646.  [CrossRef]
Constable, E. C. (1989). Adv. Inorg. Chem. 34, 1-63.  [CrossRef] [ChemPort]
Duong, A., Maris, T. & Wuest, J. D. (2011). Inorg. Chem. 50, 5605-5618.  [ISI] [CSD] [CrossRef] [ChemPort] [PubMed]
Gao, E. J., Zhang, Y. X., Zhu, M. C., Liu, H. Y., Huang, Y., Zhang, M., Su, M., Guo, M. J., Guan, F., Gao, X. N. & Wang, M. L. (2010). Russ. J. Coord. Chem. 36, 853-858.  [CrossRef] [ChemPort]
Geremia, S., Randaccio, L., Mestroni, G. & Milani, B. (1992). J. Chem. Soc. Dalton Trans. pp. 2117-2118.  [CrossRef]
Hinamoto, M., Ooi, S. & Kuroya, H. (1972). J. Chem. Soc. Chem. Commun. pp. 356-357.  [CrossRef] [ISI]
Maeda, S., Nishida, Y., Okawa, H. & Kida, S. (1986). Bull. Chem. Soc. Jpn, 59, 2013-2014.  [CrossRef] [ChemPort] [ISI]
Maris, T. (2004). UdMX. Université de Montréal, Montréal, Québec, Canada.
McKenzie, E. D. (1971). Coord. Chem. Rev. 6, 187-216.  [CrossRef] [ChemPort] [ISI]
Milani, B., Anzilutti, A., Vicentini, L., Sessanta o Santi, A., Zangrando, E., Geremia, S. & Mestroni, G. (1997). Organometallics, 16, 5064-5075.
Sheldrick, G. M. (2004). SADABS. University of Göttingen, Germany.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Stoccoro, S., Alesso, G., Cinellu, M. A., Minghetti, G., Zucca, A., Bastero, A., Claver, C. & Manassero, M. (2002). J. Organomet. Chem. 664, 77-84.  [CSD] [CrossRef] [ChemPort]
Wehman, P., Dol, G. C., Moorman, E. R., Kamer, P. C. J., van Leeuwen, P. W. N. M., Fraanje, J. & Goubitz, K. (1994). Organometallics, 13, 4856-4869.  [CrossRef] [ChemPort]
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.  [ISI] [CrossRef] [ChemPort] [details]
Yue, C.-Y., Jiang, F.-L., Yuan, D.-Q., Chen, L., Wu, M.-Y. & Hong, M.-C. (2008). Chin. J. Struct. Chem. 27, 467-470.  [ChemPort]

Acta Cryst (2012). E68, m1347-m1348   [ doi:10.1107/S1600536812041591 ]

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