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Volume 69 
Part 6 
Pages m337-m338  
June 2013  

Received 10 March 2013
Accepted 14 May 2013
Online 22 May 2013

Key indicators
Single-crystal X-ray study
T = 173 K
Mean [sigma](C-C) = 0.004 Å
H completeness 91%
Disorder in main residue
R = 0.029
wR = 0.073
Data-to-parameter ratio = 12.1
Details
Open access

Di-[mu]-azido-diazidodi-[mu]-oxalato-dihistaminetetracopper(II) 0.9-hydrate

aDepartment of Chemistry and Environmental Science, Grenfell Campus, Memorial University of Newfoundland, Corner Brook, Newfoundland, A2H 6P9, Canada, and bDepartment of Chemistry, University of Florida, Gainesville, FL 32611-7200, USA
Correspondence e-mail: cliu@grenfell.mun.ca

The title compound, [Cu4(C2O4)2(N3)4(C5H9N3)2]·0.9H2O, contains a tetranuclear CuII-based molecule composed of two oxalate-bridged CuII dimers linked through end-on azide ions and related by an inversion center. The tetranuclear unit contains two crystallographically independent CuII ions. One CuII ion coordinates to two N atoms of a histamine molecule, two O atoms of a bridging oxalate ligand, and an N atom of an end-on bridging azide ligand, leading to an elongated square-pyramidal coordination geometry in which the azide ion occupies the axial position. The other CuII ion, which has a square-planar coordination geometry, is coordinated by two O atoms of a bridging oxalate ligand and two N atoms of two different azide ligands, one which is bridging. In the crystal, a two-dimensional network parallel to (010) is formed by N-H...N and N-H...O hydrogen bonds. A partially occupied solvent water molecule refined to an occupancy of 0.447 (5). Two of the azide ligands were refined as disordered over two sets of sites with refined occupancies in the ratios 0.517 (8):0.483 (8) and 0.553 (5):0.447 (5).

Related literature

For background to bridging oxalate and azide ligands, see: Coronado et al. (2003[Coronado, E., Giménez, M. C., Gómez-Garcia, C. J. & Romero, F. M. (2003). Polyhedron, 22, 3115-3122.]); Ribas et al. (1999[Ribas, J., Escuer, A., Monfort, M., Vicente, R., Cortes, R., Lezama, L. & Rojo, T. (1999). Coord. Chem. Rev. 193-195, 1027-1068.]); Pardo et al. (2010[Pardo, E., Train, C., Lescouezec, R., Boubekeru, K., Ruiz, E., Lloret, F. & Verdaguer, M. (2010). Dalton Trans. 39, 4951-4958.]); Sun et al. (1997[Sun, X. R., Miao, M. M., Cheng, P., Liao, D. Z., Jiang, Z. H. & Wang, G. L. (1997). Transition Met. Chem. 22, 302-303.]).

[Scheme 1]

Experimental

Crystal data
  • [Cu4(C2O4)2(N3)4(C5H9N3)2]·0.9H2O

  • Mr = 838.62

  • Triclinic, [P \overline 1]

  • a = 7.7003 (10) Å

  • b = 8.2841 (11) Å

  • c = 11.8677 (15) Å

  • [alpha] = 106.005 (2)°

  • [beta] = 91.715 (2)°

  • [gamma] = 115.010 (2)°

  • V = 650.07 (15) Å3

  • Z = 1

  • Mo K[alpha] radiation

  • [mu] = 3.31 mm-1

  • T = 173 K

  • 0.12 × 0.11 × 0.04 mm

Data collection
  • Bruker SMART CCD area-detector diffractometer

  • Absorption correction: integration [based on measured indexed crystal faces (SHELXTL; Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.])] Tmin = 0.654, Tmax = 0.877

  • 5770 measured reflections

  • 2885 independent reflections

  • 2442 reflections with I > 2[sigma](I)

  • Rint = 0.041

Refinement
  • R[F2 > 2[sigma](F2)] = 0.029

  • wR(F2) = 0.073

  • S = 1.03

  • 2885 reflections

  • 238 parameters

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

  • [Delta][rho]max = 0.60 e Å-3

  • [Delta][rho]min = -0.56 e Å-3

Table 1
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
N9-H9...O5i 0.80 (4) 2.18 (4) 2.861 (6) 143 (3)
N9-H9...N6'i 0.80 (4) 2.59 (4) 3.171 (6) 130 (3)
N9-H9...N3'ii 0.80 (4) 2.60 (4) 3.145 (7) 127 (3)
N9-H9...N6iii 0.80 (4) 2.38 (4) 3.108 (6) 151 (3)
Symmetry codes: (i) -x, -y+1, -z; (ii) -x+1, -y+1, -z; (iii) x, y-1, z-1.

Data collection: APEX2 (Bruker, 2008[Bruker (2008). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2008[Bruker (2008). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: LH5597 ).


Acknowledgements

CL wishes to thank the Vice President (Grenfell Campus) Research Fund 208384 47333 2000 from Grenfell Campus, Memorial University of Newfoundland, for supporting this work. KAA wishes to acknowledge the National Science Foundation and the University of Florida for funding the purchase of the X-ray equipment.

References

Bruker (2008). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Coronado, E., Giménez, M. C., Gómez-Garcia, C. J. & Romero, F. M. (2003). Polyhedron, 22, 3115-3122.  [ISI] [CSD] [CrossRef] [ChemPort]
Pardo, E., Train, C., Lescouezec, R., Boubekeru, K., Ruiz, E., Lloret, F. & Verdaguer, M. (2010). Dalton Trans. 39, 4951-4958.  [CSD] [CrossRef] [ChemPort] [PubMed]
Ribas, J., Escuer, A., Monfort, M., Vicente, R., Cortes, R., Lezama, L. & Rojo, T. (1999). Coord. Chem. Rev. 193-195, 1027-1068.  [ISI] [CrossRef] [ChemPort]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [ChemPort] [details]
Sun, X. R., Miao, M. M., Cheng, P., Liao, D. Z., Jiang, Z. H. & Wang, G. L. (1997). Transition Met. Chem. 22, 302-303.  [CrossRef] [ChemPort] [ISI]


Acta Cryst (2013). E69, m337-m338   [ doi:10.1107/S1600536813013329 ]

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