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Volume 69 
Part 1 
Pages m56-m57  
January 2013  

Received 19 November 2012
Accepted 10 December 2012
Online 15 December 2012

Key indicators
Single-crystal X-ray study
T = 100 K
Mean [sigma](C-C) = 0.003 Å
R = 0.035
wR = 0.087
Data-to-parameter ratio = 18.5
Details
Open access

Redetermination of cis-bis(ethylenediamine-[kappa]2N,N')bis(nitrito-[kappa]N)cobalt(III) (ethylenediamine-[kappa]2N,N')tetrakis(nitrito-[kappa]N)cobaltate(III) monohydrate

aLaboratório de Materiais Inorgânicos, Universidade Federal de Santa Maria, 97105-900 Santa Maria, RS, Brazil
Correspondence e-mail: rburrow@ewald.base.ufsm.br

The structure of the title compound, [Co(NO2)2(NH2CH2CH2NH2)2][Co(NO2)4(NH2CH2CH2NH2)]·H2O, was redetermined with a modern CCD-equipped diffractometer. In comparison with the original determination based on photographic data [Kushi et al. (1976[Kushi, Y., Kuramoto, M., Yamamoto, S. & Yoneda, H. (1976). Inorg. Nucl. Chem. Lett. 12, 629-633.]). Inorg. Nucl. Chem. Lett. 12, 629-633], the current study allows the location of reliable postions for the H atoms and thus leads to better understanding of the interionic and intermolecular interactions. The crystal structure consists of an octahedrally coordinated cationic CoIII complex ion, an octahedrally coordinated anionic CoIII complex ion and a lattice water molecule. The complex cation, complex anion and lattice water molecule are connected by an intricate network of O-H...O and N-H...O hydrogen bonds, forming a three-dimensional structure.

Related literature

For background to CoIII complexes, see: Angelici (1969[Angelici, R. J. (1969). Synthesis and Technique in Inorganic Chemistry, Philadelphia: W. B. Saunders.]); Bernal (1985[Bernal, I. (1985). Inorg. Chim. Acta, 96, 99-110.]); Bernal & Kauffman (1987[Bernal, I. & Kauffman, G. B. (1987). J. Chem. Educ. 64, 604-610.]); Murmann (1955[Murmann, R. K. (1955). J. Am. Chem. Soc. 77, 5190-5190.]). For a previous report of the crystal structure of the title compound, see: Kushi et al. (1976[Kushi, Y., Kuramoto, M., Yamamoto, S. & Yoneda, H. (1976). Inorg. Nucl. Chem. Lett. 12, 629-633.]). For synthetic details, see: Bailor & Rollinson (1946[Bailor, J. C. & Rollinson, L. L. (1946). Inorg. Synth. 2, 222-225.]); Sharrock (1980[Sharrock, P. (1980). J. Chem. Educ. 57, 778-778.]). For a description of the Cambridge Structural Database, see: Allen (2002[Allen, F. H. (2002). Acta Cryst. B58, 380-388.]).

[Scheme 1]

Experimental

Crystal data
  • [Co(NO2)2(C2H8N2)2][Co(NO2)4(C2H8N2)]·H2O

  • Mr = 592.25

  • Monoclinic, P 21 /n

  • a = 14.7580 (5) Å

  • b = 6.7060 (2) Å

  • c = 20.6845 (7) Å

  • [beta] = 96.969 (2)°

  • V = 2031.96 (11) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 1.73 mm-1

  • T = 100 K

  • 0.40 × 0.15 × 0.05 mm

Data collection
  • Bruker X8 Kappa APEXII diffractometer

  • Absorption correction: numerical (SADABS; Bruker, 2012[Bruker (2012). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.692, Tmax = 0.925

  • 63576 measured reflections

  • 6280 independent reflections

  • 4801 reflections with I > 2[sigma](I)

  • Rint = 0.073

Refinement
  • R[F2 > 2[sigma](F2)] = 0.035

  • wR(F2) = 0.087

  • S = 1.07

  • 6280 reflections

  • 340 parameters

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

  • [Delta][rho]max = 0.72 e Å-3

  • [Delta][rho]min = -0.84 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
N11-H11A...O11i 0.83 (3) 2.26 (3) 3.048 (2) 158 (2)
N11-H11B...O23ii 0.79 (3) 2.23 (3) 2.991 (2) 163 (2)
N11-H11B...O13iii 0.79 (3) 2.57 (2) 2.966 (2) 113 (2)
N12-H12A...O24iv 0.86 (3) 2.22 (3) 3.060 (2) 164 (2)
N12-H12B...O12v 0.80 (3) 2.38 (3) 3.030 (2) 139 (2)
N13-H13A...O22vi 0.84 (3) 2.42 (3) 3.186 (2) 152 (2)
N13-H13B...O13iii 0.87 (3) 2.47 (3) 3.206 (2) 143 (2)
N14-H14A...O27ii 0.94 (3) 2.12 (3) 3.038 (2) 164 (2)
N14-H14B...O24iv 0.85 (2) 2.42 (2) 3.060 (2) 132 (2)
N21-H21A...O28vii 0.82 (3) 2.56 (3) 3.185 (2) 134 (2)
N22-H22A...O27viii 0.83 (2) 2.18 (3) 2.981 (2) 164 (2)
N22-H22B...O1 0.89 (2) 2.16 (3) 2.967 (2) 151 (2)
O1-H1A...O26iv 0.84 (3) 2.19 (3) 2.953 (2) 152 (3)
O1-H1A...O24iv 0.84 (3) 2.53 (3) 3.081 (2) 124 (2)
O1-H1B...O25viii 0.82 (3) 2.07 (3) 2.866 (2) 162 (3)
Symmetry codes: (i) [-x+{\script{3\over 2}}, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]; (ii) -x+1, -y, -z; (iii) x, y-1, z; (iv) -x+1, -y+1, -z; (v) [-x+{\script{3\over 2}}, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]; (vi) x+1, y, z; (vii) [-x+{\script{1\over 2}}, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]; (viii) x, y+1, z.

Data collection: APEX2 (Bruker, 2012[Bruker (2012). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2012[Bruker (2012). APEX2, SAINT and SADABS. 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: DIAMOND (Brandenburg, 2009[Brandenburg, K. (2009). 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: WM2706 ).


Acknowledgements

Financial support from the Conselho Nacional de Desenvolvimento Científico (CNPq, Brazil; grants 485245/2007-8 and 479747/2009-1), the Fundação de Amparo à Pesquisa (FAPERGS, Rio Grande do Sul; grant 10/1645-9) is gratefully acknowledged, as are fellowships from CNPq (JRMV & RAB; grant 308731/2009-3) and the Coordenação de Aperfeiçoamento de Pessoas de Nível Superior (CAPES, Brazil; JRMV). The diffractometer was funded by a CT-INFRA grant from the Financiadora de Estrutos e Projetos (FINEP, Brazil).

References

Allen, F. H. (2002). Acta Cryst. B58, 380-388.  [ISI] [CrossRef] [details]
Angelici, R. J. (1969). Synthesis and Technique in Inorganic Chemistry, Philadelphia: W. B. Saunders.
Bailor, J. C. & Rollinson, L. L. (1946). Inorg. Synth. 2, 222-225.
Bernal, I. (1985). Inorg. Chim. Acta, 96, 99-110.  [CrossRef] [ChemPort] [ISI]
Bernal, I. & Kauffman, G. B. (1987). J. Chem. Educ. 64, 604-610.  [CrossRef] [ChemPort]
Brandenburg, K. (2009). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Bruker (2012). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Kushi, Y., Kuramoto, M., Yamamoto, S. & Yoneda, H. (1976). Inorg. Nucl. Chem. Lett. 12, 629-633.  [CrossRef] [ChemPort]
Murmann, R. K. (1955). J. Am. Chem. Soc. 77, 5190-5190.  [CrossRef] [ChemPort] [ISI]
Sharrock, P. (1980). J. Chem. Educ. 57, 778-778.  [CrossRef] [ChemPort]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.  [ISI] [CrossRef] [ChemPort] [details]


Acta Cryst (2013). E69, m56-m57   [ doi:10.1107/S1600536812050325 ]

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