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Volume 69 
Part 5 
Pages m248-m249  
May 2013  

Received 26 March 2013
Accepted 2 April 2013
Online 10 April 2013

Key indicators
Single-crystal X-ray study
T = 173 K
Mean [sigma](N-C) = 0.002 Å
R = 0.018
wR = 0.042
Data-to-parameter ratio = 25.0
Details
Open access

trans-Dichloridotetrakis[(dimethylphosphoryl)methanaminium-[kappa]O]cobalt(II) tetrachloridocobaltate(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

The asymmetric unit of the title structure, [CoCl2(C3H11NOP)4][CoCl4]2, consists of one half of the trans-dichloridotetrakis[(dimethylphosphoryl)methanaminium]cobalt(II) tetracation lying on an inversion center and one tetrachloridocobaltate(II) dianion on a general position. Four O-coordinated cationic (dimethylphosphoryl)methanaminium (dpmaH+) ligands occupy the equatorial coordination sites, whereas the chloride ligands occupy axial positions of the roughly octahedral coordination polyhedron of the cobalt metal center. Intramolecular hydrogen bonds between the aminium groups and the O atom of the phosphoryl groups and additional hydrogen bonds between the aminium groups and the chloride ligands are present. Furthermore, four of the six H atoms not involved in intramolecular bonding of each cobalt(II) tetracation form weak hydrogen bonds to four adjacent tetrachloridocobaltate(II) counter-anions. By these intermolecular hydrogen bonds, one-dimensional polymeric strands are formed along the b-axis direction. The hydrogen bonding is analyzed using the graph-set method and the structural similarity with dpmaHCl is discussed.

Related literature

For related dpma compounds, see: Dodoff et al. (1990[Dodoff, N., Macicek, J., Angelova, O., Varbanov, S. G. & Spassovska, N. (1990). J. Coord. Chem. 22, 219-228.]); Borisov et al. (1994[Borisov, G., Varbanov, S. G., Venanzi, L. M., Albinati, A. & Demartin, F. (1994). Inorg. Chem. 33, 5430-5437.]); Trendafilova et al. (1997[Trendafilova, N., Georgieva, I., Bauer, G., Varbanov, S. G. & Dodoff, N. (1997). Spectrochim. Acta, A53, 819-828.]); Kochel (2009[Kochel, A. (2009). Inorg. Chim. Acta, 362, 1379-1382.]); Reiss & Jörgens (2012[Reiss, G. J. & Jörgens, S. (2012). Acta Cryst. E68, o2899-o2900.]); van Megen et al. (2013[Megen, M. van, Prömper, S. & Reiss, G. J. (2013). Acta Cryst. E69, m217.]). For a definition of the term tecton, see: Brunet et al. (1997[Brunet, P., Simard, M. & Wuest, J. D. (1997). J. Am. Chem. Soc. 119, 2737-2738.]). For related methylphosphinic acids and their derivatives, see: Reiss & Engel (2008[Reiss, G. J. & Engel, J. S. (2008). Acta Cryst. E64, o400.]); Meyer et al. (2010[Meyer, M. K., Graf, J. & Reiss, G. J. (2010). Z. Naturforsch. Teil B, 65, 1462-1466.]). For graph-set theory and its applications, see: Etter et al. (1990[Etter, M. C., MacDonald, J. C. & Bernstein, J. (1990). Acta Cryst. B46, 256-262.]); Bernstein et al. (1995[Bernstein, J., Davis, R. E., Shimoni, L. & Chang, N.-L. (1995). Angew. Chem. Int. Ed. 34, 1555-1573.]); Grell et al. (2002[Grell, J., Bernstein, J. & Tinhofer, G. (2002). Crystallogr. Rev. 8, 1-56.]). For related cobalt complexes, see: Kubíck et al. (2003[Kubíck, V., Vojtísk, P., Rudovský, J., Hermann, P. & Lukes, I. (2003). Dalton Trans. pp. 3927-3938.]); Girma et al. (2005[Girma, K. B., Lorenz, V., Blaurock, S. & Edelmann, F. T. (2005). Z. Anorg. Allg. Chem. 631, 1419-1422.]); Guzei et al. (2010[Guzei, I. A., Spencer, L. C., Ainooson, M. K. & Darkwa, J. (2010). Acta Cryst. C66, m89-m96.]).

[Scheme 1]

Experimental

Crystal data
  • [CoCl2(C3H11NOP)4][CoCl4]2

  • Mr = 963.68

  • Triclinic, [P \overline 1]

  • a = 7.7748 (3) Å

  • b = 11.1557 (5) Å

  • c = 12.1205 (5) Å

  • [alpha] = 110.738 (4)°

  • [beta] = 97.688 (4)°

  • [gamma] = 104.331 (5)°

  • V = 923.66 (8) Å3

  • Z = 1

  • Mo K[alpha] radiation

  • [mu] = 2.25 mm-1

  • T = 173 K

  • 0.76 × 0.33 × 0.08 mm

Data collection
  • Oxford Xcalibur diffractometer

  • Absorption correction: analytical [CrysAlis PRO (Oxford Diffraction, 2009[Oxford Diffraction (2009). CrysAlis PRO. Oxford Diffraction Ltd, Yarnton, England.]), based on expressions derived by Clark & Reid (1995[Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897.])] Tmin = 0.402, Tmax = 0.838

  • 15687 measured reflections

  • 4920 independent reflections

  • 4552 reflections with I > 2[sigma](I)

  • Rint = 0.020

Refinement
  • R[F2 > 2[sigma](F2)] = 0.018

  • wR(F2) = 0.042

  • S = 1.09

  • 4920 reflections

  • 197 parameters

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

  • [Delta][rho]max = 0.49 e Å-3

  • [Delta][rho]min = -0.38 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
N1-H11...Cl1 0.867 (19) 2.437 (19) 3.1879 (12) 145.3 (16)
N1-H11...Cl24i 0.867 (19) 2.730 (19) 3.2573 (13) 120.5 (15)
N1-H12...O2ii 0.88 (2) 2.16 (2) 2.9504 (16) 150.3 (17)
N1-H13...Cl23ii 0.87 (2) 2.38 (2) 3.2403 (12) 171.3 (17)
N2-H22...Cl1 0.920 (19) 2.250 (19) 3.1697 (13) 177.8 (15)
N2-H21...Cl21iii 0.924 (19) 2.288 (19) 3.2124 (12) 177.8 (16)
N2-H23...Cl22i 0.86 (2) 2.71 (2) 3.3612 (13) 134.0 (16)
N2-H23...Cl24i 0.86 (2) 2.70 (2) 3.2989 (12) 128.1 (16)
Symmetry codes: (i) x, y, z+1; (ii) -x, -y, -z+1; (iii) -x, -y+1, -z+1.

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: SHELXS97 (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: SJ5313 ).


Acknowledgements

Technical support by E. Hammes is gratefully acknowledged. Furthermore, I acknowledge support for the publication fee by the Deutsche Forschungsgemeinschaft (DFG) and the open access publication fund of the Heinrich-Heine-Universität Düsseldorf.

References

Bernstein, J., Davis, R. E., Shimoni, L. & Chang, N.-L. (1995). Angew. Chem. Int. Ed. 34, 1555-1573.  [CrossRef] [ChemPort] [ISI]
Borisov, G., Varbanov, S. G., Venanzi, L. M., Albinati, A. & Demartin, F. (1994). Inorg. Chem. 33, 5430-5437.  [CrossRef] [ChemPort] [ISI]
Brandenburg, K. (2012). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Brunet, P., Simard, M. & Wuest, J. D. (1997). J. Am. Chem. Soc. 119, 2737-2738.  [CrossRef] [ChemPort] [ISI]
Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897.  [CrossRef] [details]
Dodoff, N., Macicek, J., Angelova, O., Varbanov, S. G. & Spassovska, N. (1990). J. Coord. Chem. 22, 219-228.  [CrossRef] [ChemPort]
Etter, M. C., MacDonald, J. C. & Bernstein, J. (1990). Acta Cryst. B46, 256-262.  [CrossRef] [ISI] [details]
Girma, K. B., Lorenz, V., Blaurock, S. & Edelmann, F. T. (2005). Z. Anorg. Allg. Chem. 631, 1419-1422.  [CSD] [CrossRef] [ChemPort]
Grell, J., Bernstein, J. & Tinhofer, G. (2002). Crystallogr. Rev. 8, 1-56.  [CrossRef] [ChemPort]
Guzei, I. A., Spencer, L. C., Ainooson, M. K. & Darkwa, J. (2010). Acta Cryst. C66, m89-m96.  [CrossRef] [ChemPort] [details]
Kochel, A. (2009). Inorg. Chim. Acta, 362, 1379-1382.  [ISI] [CSD] [CrossRef] [ChemPort]
Kubíck, V., Vojtísk, P., Rudovský, J., Hermann, P. & Lukes, I. (2003). Dalton Trans. pp. 3927-3938.
Meyer, M. K., Graf, J. & Reiss, G. J. (2010). Z. Naturforsch. Teil B, 65, 1462-1466.  [ChemPort]
Megen, M. van, Prömper, S. & Reiss, G. J. (2013). Acta Cryst. E69, m217.  [CrossRef] [details]
Oxford Diffraction (2009). CrysAlis PRO. Oxford Diffraction Ltd, Yarnton, England.
Reiss, G. J. & Engel, J. S. (2008). Acta Cryst. E64, o400.  [CSD] [CrossRef] [details]
Reiss, G. J. & Jörgens, S. (2012). Acta Cryst. E68, o2899-o2900.  [CSD] [CrossRef] [ChemPort] [details]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [details]
Trendafilova, N., Georgieva, I., Bauer, G., Varbanov, S. G. & Dodoff, N. (1997). Spectrochim. Acta, A53, 819-828.
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.  [ISI] [CrossRef] [ChemPort] [details]


Acta Cryst (2013). E69, m248-m249   [ doi:10.1107/S1600536813008945 ]

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