[Journal logo]

Volume 69 
Part 4 
Pages m179-m180  
April 2013  

Received 28 January 2013
Accepted 20 February 2013
Online 2 March 2013

Key indicators
Single-crystal X-ray study
T = 296 K
Mean [sigma](C-C) = 0.004 Å
R = 0.031
wR = 0.076
Data-to-parameter ratio = 21.7
Details
Open access

Bromido(1,4,7,10,13-pentaazacyclohexadecane)cobalt(III) dibromide dihydrate

aDepartment of Chemistry, Faculty of Science, Fukuoka University, Nanakuma, Jonan-ku, Fukuoka 814-0180, Japan
Correspondence e-mail: kurisaki@fukuoka-u.ac.jp

The title salt, [CoBr(C11H27N5)]Br2·2H2O, contains a complex cation with mirror symmetry and two Br- counter-anions that are likewise located on the mirror plane. The central CoIII atom of the complex cation has one Br- ion in an axial position, one N atom of the pentadentate macrocyclic ligand in the other axial position and four N atoms of the ligand in equatorial positions, defining a distorted octahedral coordination geometry. The macrocyclic ligand is coordinated to the CoIII atom within a 5, 6, 5 arrangement of chelate rings in the equatorial plane of the four N atoms. Due to symmetry, the configuration of the chiral N atoms is 1RS, 4SR, 10RS, 13SR. In the crystal, N-H...Br, O-H...Br and N-H...O hydrogen bonds between the complex cation, anions and lattice water molecules generate a three-dimensional network.

Related literature

For background to metal complexes with azamacrocycles, see: Mewis & Archida (2010[Mewis, R. E. & Archida, S. J. (2010). Coord. Chem. Rev. 254, 1686-1712.]). For related structures, see: Curtis et al. (1987a[Curtis, N. F., Osvath, P. & Weatherburn, D. C. (1987a). Aust. J. Chem. 40, 811-827.],b[Curtis, N. F., Gainsford, G. J., Osvath, P. & Weatherburn, D. C. (1987b). Aust. J. Chem. 40, 829-839.]); Eigenbrot et al. (1988[Eigenbrot, C., Osvath, P., Lappin, A. G., Curtis, N. F. & Weatherburn, D. C. (1988). Acta Cryst. C44, 2085-2087.]); Tahirov et al. (1993[Tahirov, T. H., Lu, T.-H., Chen, B.-H., Lai, C.-Y. & Chung, C.-S. (1993). Acta Cryst. C49, 1910-1912.]); Bombieri et al. (1982[Bombieri, G., Forsellini, E., Delpra, A., Cooksey, C. J., Humanes, M. & Tobe, M. L. (1982). Inorg. Chim. Acta, 61, 43-49.]). For the synthesis of the macrocyclic ligand, see: Richman & Atkins (1974[Richman, J. E. & Atkins, T. J. (1974). J. Am. Chem. Soc. 96, 2268-2270.]).

[Scheme 1]

Experimental

Crystal data
  • [CoBr(C11H27N5)]Br2·2H2O

  • Mr = 564.07

  • Orthorhombic, P n m a

  • a = 13.139 (3) Å

  • b = 9.6674 (18) Å

  • c = 15.393 (3) Å

  • V = 1955.2 (7) Å3

  • Z = 4

  • Mo K[alpha] radiation

  • [mu] = 7.02 mm-1

  • T = 296 K

  • 0.40 × 0.22 × 0.14 mm

Data collection
  • Rigaku Saturn724+ diffractometer

  • Absorption correction: numerical (NUMABS; Rigaku, 1999[Rigaku (1999). NUMABS. Rigaku Corporation, Tokyo, Japan.]) Tmin = 0.189, Tmax = 0.501

  • 28744 measured reflections

  • 2370 independent reflections

  • 1964 reflections with I > 2[sigma](I)

  • Rint = 0.075

Refinement
  • R[F2 > 2[sigma](F2)] = 0.031

  • wR(F2) = 0.076

  • S = 1.02

  • 2370 reflections

  • 109 parameters

  • 4 restraints

  • H-atom parameters constrained

  • [Delta][rho]max = 0.89 e Å-3

  • [Delta][rho]min = -0.88 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
N1-H1...Br2 0.91 2.5 3.303 (3) 147
N2-H2...Br3 0.91 2.57 3.415 (2) 155
N3-H3...OWi 0.91 2.24 3.060 (4) 150
OW-HW2...Br2 0.87 2.64 3.491 (3) 168
OW-HW1...Br3ii 0.82 2.67 3.489 (3) 170
Symmetry codes: (i) [x+{\script{1\over 2}}, y, -z+{\script{1\over 2}}]; (ii) [-x+{\script{3\over 2}}, -y, z-{\script{1\over 2}}].

Data collection: CrystalClear (Rigaku, 2008[Rigaku (2008). CrystalClear. Rigaku Corporation, Tokyo, Japan.]); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SIR92 (Altomare et al., 1993[Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993). J. Appl. Cryst. 26, 343-350.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]); software used to prepare material for publication: WinGX (Farrugia, 2012[Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.]).


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: WM2723 ).


Acknowledgements

This work was partially supported by Grants-in-Aid for Scientific Research (C) 22550088 and (B) 23300319 from the Japan Society for the Promotion of Science.

References

Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993). J. Appl. Cryst. 26, 343-350.  [CrossRef] [ISI] [details]
Bombieri, G., Forsellini, E., Delpra, A., Cooksey, C. J., Humanes, M. & Tobe, M. L. (1982). Inorg. Chim. Acta, 61, 43-49.  [CrossRef] [ChemPort] [ISI]
Curtis, N. F., Gainsford, G. J., Osvath, P. & Weatherburn, D. C. (1987b). Aust. J. Chem. 40, 829-839.  [CrossRef]
Curtis, N. F., Osvath, P. & Weatherburn, D. C. (1987a). Aust. J. Chem. 40, 811-827.  [CrossRef] [ChemPort]
Eigenbrot, C., Osvath, P., Lappin, A. G., Curtis, N. F. & Weatherburn, D. C. (1988). Acta Cryst. C44, 2085-2087.  [CrossRef] [details]
Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.  [ISI] [CrossRef] [ChemPort] [details]
Mewis, R. E. & Archida, S. J. (2010). Coord. Chem. Rev. 254, 1686-1712.  [ISI] [CrossRef] [ChemPort]
Richman, J. E. & Atkins, T. J. (1974). J. Am. Chem. Soc. 96, 2268-2270.  [CrossRef] [ChemPort] [ISI]
Rigaku (1999). NUMABS. Rigaku Corporation, Tokyo, Japan.
Rigaku (2008). CrystalClear. Rigaku Corporation, Tokyo, Japan.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]
Tahirov, T. H., Lu, T.-H., Chen, B.-H., Lai, C.-Y. & Chung, C.-S. (1993). Acta Cryst. C49, 1910-1912.  [CrossRef] [details]


Acta Cryst (2013). E69, m179-m180   [ doi:10.1107/S1600536813004947 ]

This is an open-access article distributed under the terms of the Creative Commons Attribution Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.