(μ1-Methano­lato-κ1O)-μ1-methoxo-κ1O-(μ2-2-amino-1-methyl-5H-imidazol-4-one-κ2N:N′)-hexa­carbonyl­dirhenium(I)

Schutte, M.; Visser, H.G.; Roodt, A.

doi:10.1107/S1600536812041700

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 (C-C) = 0.009 Å
R = 0.030
wR = 0.078
Data-to-parameter ratio = 18.1
Details

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

M. Schutte,^a ^* H. G. Visser ^a and A. Roodt ^a

^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 Re^I 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 Re^I 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 Rh^I 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-HO and three C-HO, 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). For similar Re^I methoxy-bridged structures, see: Franklin et al. (2008); Klausmeyer & Beckles (2006). For structures of creatinine, see: Bell et al. (1995); du Pré & Mendel (1955). For structures with creatinine as a monodentate ligand, see: Canty et al. (1979); Mitewa et al. (2002); Matos Beja et al. (1991); Panfil et al. (1995). For a tetranuclear Re^I complex, see: Schutte et al. (2012a). For similar Re^I structures, see: Schutte et al. (2011, 2012b,c).

Experimental

Crystal data

[Re₂(CH₃O)₂(CO)₆(C₄H₆N₃O)]
M_r = 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 radiation
= 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) T_min = 0.174, T_max = 0.371
46753 measured reflections
4276 independent reflections
3920 reflections with I > 2(I)
R_int = 0.050

Refinement

R[F² > 2(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
_max = 2.32 e Å^-3
_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-HA	D-H	HA	DA	D-HA
N3-H3O31ⁱ	0.92 (8)	2.17 (8)	3.061 (6)	162 (7)
C2-H2BO13ⁱⁱ	0.96	2.54	3.453 (9)	159
C2-H2CO23ⁱⁱ	0.96	2.61	3.504 (9)	154
C34-H34AO31ⁱ	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); cell refinement: SAINT-Plus (Bruker, 2008); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg & Putz, 2005); software used to prepare material for publication: WinGX (Farrugia, 1999).

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

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