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Volume 69 
Part 11 
Pages m614-m615  
November 2013  

Received 6 October 2013
Accepted 12 October 2013
Online 19 October 2013

Key indicators
Single-crystal X-ray study
T = 290 K
Mean [sigma](N-C) = 0.002 Å
R = 0.022
wR = 0.051
Data-to-parameter ratio = 38.2
Details
Open access

Bis[(di­methyl­phosphor­yl)methan­amin­ium] tetra­chlorido­palladate(II)

aInstitut für Anorganische Chemie und Strukturchemie, Lehrstuhl II: Material- und Strukturforschung, Heinrich-Heine-Universität Düsseldorf, Universitätsstrasse 1, D-40225 Düsseldorf, Germany
Correspondence e-mail: reissg@hhu.de

In the crystal structure of the title compound, (C3H11NOP)2[PdCl4], (di­methyl­phosphor­yl)methanaminium (dpmaH+) cations are connected head-to-tail by strong N-H...O hydrogen bonds, forming inversion-related cyclic dimers. The square-planar [PdCl4]2- counter-dianion is located about a center of inversion. The dications and the [PdCl4]2- dianions are connected by medium-strong N-H...Cl hydrogen bonds, forming zigzag chains parallel to [001]. Somewhat weaker N-H...Cl hydrogen bonds connect the chains into a three-dimensional network.

Related literature

For transition metal complexes built by the neutral dpma ligand, see: Kochel (2009[Kochel, A. (2009). Inorg. Chim. Acta, 362, 1379-1382.]). For simple dpmaH+ salts, see: Reiss & Jörgens (2012[Reiss, G. J. & Jörgens, S. (2012). Acta Cryst. E68, o2899-o2900.]); Buhl et al. (2013[Buhl, D., Gün, H., Jablonka, A. & Reiss, G. J. (2013). Crystals, 3, 350-362.]); Lambertz et al. (2013[Lambertz, C., Luppa, A. & Reiss, G. J. (2013). Z. Kristallogr. New Cryst. Struct. 228, 227-228.]); Reiss (2013a[Reiss, G. J. (2013a). Acta Cryst. E69, o1253-o1254.]). For dpmaH+ metal complexes, see: Reiss (2013b[Reiss, G. J. (2013b). Acta Cryst. E69, m248-m249.],c[Reiss, G. J. (2013c). Acta Cryst. E69, m250-m251.],d[Reiss, G. J. (2013d). Z. Kristallogr. New Cryst. Struct. 228, 431-433.]). For some structures and applications of tetra­chlorido­palladate(II) salts, see: Willett & Willett (1977[Willett, R. D. & Willett, J. J. (1977). Acta Cryst. B33, 1639-1641.]); Hardacre et al. (2001[Hardacre, C., Holbrey, J. D., McCormac, P. B., McMath, S. E. J., Nieuwenhuyzen, M. & Seddon, K. R. (2001). J. Mater. Chem. 11, 346-350.]); Lee et al. (2004[Lee, C. K., Peng, H. H. & Lin, I. J. B. (2004). Chem. Mater. 16, 530-536.]); Song et al. (2012[Song, H., Yan, N., Fei, Z., Kilpin, K. J., Scopelliti, R., Li, X. & Dyson, P. J. (2012). Catal. Today, 183, 172-177.]); Vranec et al. (2012[Vranec, P., Potocnák, I. & Repovský, P. (2012). Acta Cryst. C68, m370-m376.]); Serpell et al. (2013[Serpell, C. J., Cookson, J., Thompson, A. L., Brown, C. M. & Beer, P. D. (2013). Dalton Trans. 42, 1385-1393.]). For graph-set analysis, see: Grell et al. (2002[Grell, J., Bernstein, J. & Tinhofer, G. (2002). Crystallogr. Rev. 8, 1-56.]).

[Scheme 1]

Experimental

Crystal data
  • (C3H11NOP)2[PdCl4]

  • Mr = 464.39

  • Monoclinic, P 21 /n

  • a = 9.3600 (3) Å

  • b = 7.81198 (19) Å

  • c = 11.9892 (3) Å

  • [beta] = 110.110 (3)°

  • V = 823.21 (4) Å3

  • Z = 2

  • Mo K[alpha] radiation

  • [mu] = 1.96 mm-1

  • T = 290 K

  • 0.18 × 0.12 × 0.11 mm

Data collection
  • Oxford Diffraction Xcalibur CCD diffractometer

  • Absorption correction: analytical [using a multifaceted crystal model (Clark & Reid, 1995[Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897.])] Tmin = 0.764, Tmax = 0.850

  • 26379 measured reflections

  • 3595 independent reflections

  • 3077 reflections with I > 2[sigma](I)

  • Rint = 0.035

Refinement
  • R[F2 > 2[sigma](F2)] = 0.022

  • wR(F2) = 0.051

  • S = 1.09

  • 3595 reflections

  • 94 parameters

  • H atoms treated by a mixture of independent and constrained refinement

  • [Delta][rho]max = 0.46 e Å-3

  • [Delta][rho]min = -0.57 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
N1-H12...Cl1 0.88 (2) 2.40 (2) 3.2220 (15) 155 (2)
N1-H11...O1i 0.86 (2) 1.89 (2) 2.7425 (17) 172 (2)
N1-H13...Cl1ii 0.84 (2) 2.73 (2) 3.3752 (15) 135.1 (18)
N1-H13...Cl2ii 0.84 (2) 2.82 (2) 3.5241 (16) 143.4 (18)
Symmetry codes: (i) -x, -y, -z+1; (ii) [-x+{\script{1\over 2}}, y-{\script{1\over 2}}, -z+{\script{1\over 2}}].

Data collection: CrysAlis PRO (Oxford Diffraction, 2009[Oxford Diffraction (2009). CrysAlis PRO. Oxford Diffraction Ltd, Yarnton, England.]); cell refinement: CrysAlis PRO); data reduction: CrysAlis PRO); program(s) used to solve structure: SHELXS2013 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL2013 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: DIAMOND (Brandenburg, 2012[Brandenburg, K. (2012). 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: WM2775 ).


Acknowledgements

This publication was funded by the German Research Foundation (DFG) and the Heinrich-Heine-Universität Düsseldorf under the funding programme Open Access Publishing.

References

Brandenburg, K. (2012). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Buhl, D., Gün, H., Jablonka, A. & Reiss, G. J. (2013). Crystals, 3, 350-362.  [CrossRef] [ChemPort]
Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897.  [CrossRef] [IUCr Journals]
Grell, J., Bernstein, J. & Tinhofer, G. (2002). Crystallogr. Rev. 8, 1-56.  [CrossRef] [ChemPort]
Hardacre, C., Holbrey, J. D., McCormac, P. B., McMath, S. E. J., Nieuwenhuyzen, M. & Seddon, K. R. (2001). J. Mater. Chem. 11, 346-350.  [Web of Science] [CrossRef] [ChemPort]
Kochel, A. (2009). Inorg. Chim. Acta, 362, 1379-1382.  [Web of Science] [CSD] [CrossRef] [ChemPort]
Lambertz, C., Luppa, A. & Reiss, G. J. (2013). Z. Kristallogr. New Cryst. Struct. 228, 227-228.  [ChemPort]
Lee, C. K., Peng, H. H. & Lin, I. J. B. (2004). Chem. Mater. 16, 530-536.  [Web of Science] [CSD] [CrossRef] [ChemPort]
Oxford Diffraction (2009). CrysAlis PRO. Oxford Diffraction Ltd, Yarnton, England.
Reiss, G. J. (2013a). Acta Cryst. E69, o1253-o1254.  [CSD] [CrossRef] [ChemPort] [IUCr Journals]
Reiss, G. J. (2013b). Acta Cryst. E69, m248-m249.  [CSD] [CrossRef] [ChemPort] [IUCr Journals]
Reiss, G. J. (2013c). Acta Cryst. E69, m250-m251.  [CSD] [CrossRef] [ChemPort] [IUCr Journals]
Reiss, G. J. (2013d). Z. Kristallogr. New Cryst. Struct. 228, 431-433.
Reiss, G. J. & Jörgens, S. (2012). Acta Cryst. E68, o2899-o2900.  [CSD] [CrossRef] [ChemPort] [IUCr Journals]
Serpell, C. J., Cookson, J., Thompson, A. L., Brown, C. M. & Beer, P. D. (2013). Dalton Trans. 42, 1385-1393.  [CSD] [CrossRef] [ChemPort] [PubMed]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [IUCr Journals]
Song, H., Yan, N., Fei, Z., Kilpin, K. J., Scopelliti, R., Li, X. & Dyson, P. J. (2012). Catal. Today, 183, 172-177.  [Web of Science] [CSD] [CrossRef] [ChemPort]
Vranec, P., Potocnák, I. & Repovský, P. (2012). Acta Cryst. C68, m370-m376.  [CSD] [CrossRef] [ChemPort] [IUCr Journals]
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.  [Web of Science] [CrossRef] [ChemPort] [IUCr Journals]
Willett, R. D. & Willett, J. J. (1977). Acta Cryst. B33, 1639-1641.  [CSD] [CrossRef] [IUCr Journals]


Acta Cryst (2013). E69, m614-m615   [ doi:10.1107/S1600536813028067 ]

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