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Volume 68 
Part 11 
Pages m1359-m1360  
November 2012  

Received 27 September 2012
Accepted 5 October 2012
Online 13 October 2012

Key indicators
Single-crystal X-ray study
T = 100 K
Mean [sigma](C-C) = 0.009 Å
R = 0.030
wR = 0.078
Data-to-parameter ratio = 18.1
Details
Open access

([mu]1-Methanolato-[kappa]1O)-[mu]1-methoxo-[kappa]1O-([mu]2-2-amino-1-methyl-5H-imidazol-4-one-[kappa]2N:N')-hexacarbonyldirhenium(I)

aDepartment of Chemistry, University of the Free State, PO Box 339, Bloemfontein, 9301, South Africa
Correspondence e-mail: schuttem@ufs.ac.za

In the title compound, [Re2(CH3O)2(CO)6(C4H6N3O)], the two ReI atoms are linked by a methoxo and methanolato bridge, as well as by a creatinine ligand that coordinates in a bidentate fashion. Three fac-carbonyl ligands occupy the rest of the slightly distorted octahedral geometry around each ReI atom. The bridging methanolato and methoxo ligands are bent out of the Re2O2 plane by 49.2 (4) and 47.8 (3)° respectively. This is normally associated with a methanolato-bridging-type coordination rather that the more planar methoxo-type bridging. Furthermore, the creatinine bridging molecule is very slightly distorted from the Re2N2C plane, indicating that the pyrazolo N atom bonded to the RhI atom is not protonated. Charge balance can thus only be attained if one assumes a positional disorder for the methanolato/methoxo H atom. All attempts to locate disordered protons around these O atoms were unsuccessful. Four hydrogen bonds, one N-H...O and three C-H...O, are observed in the structure. The molecules pack in a head-to-head and tail-to-tail fashion when viewed along the c axis, in alternating columns.

Related literature

For the synthesis of the starting material, see: Alberto et al. (1996[Alberto, R., Schibli, R. & Schubiger, P. A. (1996). Polyhedron, 15, 1079-1089.]). For similar ReI methoxy-bridged structures, see: Franklin et al. (2008[Franklin, B. R., Herrick, R. S., Ziegler, C. J., Cetin, A., Barone, N. & Condon, L. R. (2008). Inorg. Chem. 47, 5902-5909.]); Klausmeyer & Beckles (2006[Klausmeyer, K. K. & Beckles, F. R. (2006). Acta Cryst. E62, m2417-m2418.]). For structures of creatinine, see: Bell et al. (1995[Bell, T. W., Hou, Z., Luo, Y., Drew, M. G. B., Chapoteau, E., Czech, B. P. & Kumar, A. (1995). Science, 269, 671-674.]); du Pré & Mendel (1955[Pré, S. du & Mendel, H. (1955). Acta Cryst. 8, 311-313.]). For structures with creatinine as a monodentate ligand, see: Canty et al. (1979[Canty, A. J., Chaichit, N. & Gatehouse, B. M. (1979). Acta Cryst. B35, 592-596.]); Mitewa et al. (2002[Mitewa, M., Todorov, T., Gencheva, G., Angelova, O. & Bakalova, T. N. (2002). J. Coord. Chem. 55, 1367-1372.]); Matos Beja et al. (1991[Matos Beja, A., Carvalho Paixão, J. A., Martin Gil, J. & Aragon Salgado, M. (1991). Acta Cryst. C47, 2333-2336.]); Panfil et al. (1995[Panfil, A., Fiol, J. J. & Sabat, M. (1995). J. Inorg. Biochem. 60, 109-122.]). For a tetranuclear ReI complex, see: Schutte et al. (2012a[Schutte, M., Brink, A., Visser, H. G. & Roodt, A. (2012a). Acta Cryst. E68, m1208-m1209.]). For similar ReI structures, see: Schutte et al. (2011[Schutte, M., Kemp, G., Visser, H. G. & Roodt, A. (2011). Inorg Chem. 50, 12486-12498.], 2012b[Schutte, M., Muller, T. J., Visser, H. G. & Roodt, A. (2012b). Acta Cryst. E68, m741-m742.],c[Schutte, M., Visser, H. G. & Roodt, A. (2012c). Acta Cryst. E68, o914.]).

[Scheme 1]

Experimental

Crystal data
  • [Re2(CH3O)2(CO)6(C4H6N3O)]

  • Mr = 714.67

  • Orthorhombic, P b c n

  • a = 24.066 (2) Å

  • b = 10.0715 (8) Å

  • c = 14.5969 (11) Å

  • V = 3538.1 (5) Å3

  • Z = 8

  • Mo K[alpha] radiation

  • [mu] = 13.73 mm-1

  • T = 100 K

  • 0.25 × 0.15 × 0.10 mm

Data collection
  • Bruker APEXII CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2008[Bruker (2008). APEX2, SAINT-Plus and SADABS. Bruker AXS Inc, Madison, Wisconsin, USA.]) Tmin = 0.174, Tmax = 0.371

  • 46753 measured reflections

  • 4276 independent reflections

  • 3920 reflections with I > 2[sigma](I)

  • Rint = 0.050

Refinement
  • R[F2 > 2[sigma](F2)] = 0.030

  • wR(F2) = 0.078

  • S = 1.16

  • 4269 reflections

  • 236 parameters

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

  • [Delta][rho]max = 2.32 e Å-3

  • [Delta][rho]min = -2.30 e Å-3

Table 1
Selected bond lengths (Å)

Re1-C11 1.886 (6)
Re1-C13 1.908 (7)
Re1-C12 1.918 (8)
Re1-O2 2.149 (4)
Re1-N3 2.150 (5)
Re1-O1 2.153 (4)
Re2-C21 1.849 (5)
Re2-C22 1.935 (6)
Re2-C23 1.949 (6)
Re2-O2 2.065 (4)
Re2-O1 2.073 (4)
Re2-N1 2.136 (5)

Table 2
Hydrogen-bond geometry (Å, °)

D-H...A D-H H...A D...A D-H...A
N3-H3...O31i 0.92 (8) 2.17 (8) 3.061 (6) 162 (7)
C2-H2B...O13ii 0.96 2.54 3.453 (9) 159
C2-H2C...O23ii 0.96 2.61 3.504 (9) 154
C34-H34A...O31i 0.96 2.44 3.332 (7) 155
Symmetry codes: (i) [x, -y+2, z+{\script{1\over 2}}]; (ii) [-x+{\script{1\over 2}}, y+{\script{1\over 2}}, z].

Data collection: APEX2 (Bruker, 2008[Bruker (2008). APEX2, SAINT-Plus and SADABS. Bruker AXS Inc, Madison, Wisconsin, USA.]); cell refinement: SAINT-Plus (Bruker, 2008[Bruker (2008). APEX2, SAINT-Plus and SADABS. Bruker AXS Inc, Madison, Wisconsin, USA.]); data reduction: SAINT-Plus; 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 & Putz, 2005[Brandenburg, K. & Putz, H. (2005). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: WinGX (Farrugia, 1999[Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.]).


Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: TK5155 ).


Acknowledgements

Leo Kirsten is thanked for the data collection. The University of the Free State, the Department of Chemistry, the NRF and Sasol Ltd are gratefully acknowledged for funding.

References

Alberto, R., Schibli, R. & Schubiger, P. A. (1996). Polyhedron, 15, 1079-1089.  [CrossRef] [ChemPort] [ISI]
Bell, T. W., Hou, Z., Luo, Y., Drew, M. G. B., Chapoteau, E., Czech, B. P. & Kumar, A. (1995). Science, 269, 671-674.  [CrossRef] [ChemPort] [PubMed] [ISI]
Brandenburg, K. & Putz, H. (2005). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Bruker (2008). APEX2, SAINT-Plus and SADABS. Bruker AXS Inc, Madison, Wisconsin, USA.
Canty, A. J., Chaichit, N. & Gatehouse, B. M. (1979). Acta Cryst. B35, 592-596.  [CrossRef] [details] [ISI]
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.  [CrossRef] [ChemPort] [details]
Franklin, B. R., Herrick, R. S., Ziegler, C. J., Cetin, A., Barone, N. & Condon, L. R. (2008). Inorg. Chem. 47, 5902-5909.  [ISI] [CSD] [CrossRef] [PubMed] [ChemPort]
Klausmeyer, K. K. & Beckles, F. R. (2006). Acta Cryst. E62, m2417-m2418.  [CSD] [CrossRef] [details]
Matos Beja, A., Carvalho Paixão, J. A., Martin Gil, J. & Aragon Salgado, M. (1991). Acta Cryst. C47, 2333-2336.  [CrossRef] [details]
Mitewa, M., Todorov, T., Gencheva, G., Angelova, O. & Bakalova, T. N. (2002). J. Coord. Chem. 55, 1367-1372.  [ISI] [CSD] [CrossRef] [ChemPort]
Panfil, A., Fiol, J. J. & Sabat, M. (1995). J. Inorg. Biochem. 60, 109-122.  [CrossRef] [ChemPort] [ISI]
Pré, S. du & Mendel, H. (1955). Acta Cryst. 8, 311-313.  [CrossRef] [details]
Schutte, M., Brink, A., Visser, H. G. & Roodt, A. (2012a). Acta Cryst. E68, m1208-m1209.  [CSD] [CrossRef] [ChemPort] [details]
Schutte, M., Kemp, G., Visser, H. G. & Roodt, A. (2011). Inorg Chem. 50, 12486-12498.  [CSD] [CrossRef] [ChemPort] [PubMed]
Schutte, M., Muller, T. J., Visser, H. G. & Roodt, A. (2012b). Acta Cryst. E68, m741-m742.  [CSD] [CrossRef] [details]
Schutte, M., Visser, H. G. & Roodt, A. (2012c). Acta Cryst. E68, o914.  [CSD] [CrossRef] [details]
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.  [CrossRef] [details]


Acta Cryst (2012). E68, m1359-m1360   [ doi:10.1107/S1600536812041700 ]

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