Aqua­tricarbon­yl(4-carboxy­pyridine-2-carboxyl­ato-κ2N,O2)rhenium(I)

Schutte, M.; Visser, H.G.

doi:10.1107/S160053680802761X

Volume 64
Part 10
Pages m1226-m1227
October 2008

Received 25 July 2008
Accepted 28 August 2008
Online 6 September 2008

Key indicators
Single-crystal X-ray study
T = 100 K
Mean (C-C) = 0.007 Å
R = 0.027
wR = 0.065
Data-to-parameter ratio = 15.7
Details

Aquatricarbonyl(4-carboxypyridine-2-carboxylato-²N,O²)rhenium(I)

Marietjie Schutte ^a and Hendrik G. Visser ^a ^*

^aDepartment of Chemistry, University of the Free State, PO Box 339, Bloemfontein 9300, South Africa
Correspondence e-mail: visserhg.sci@ufs.ac.za

There are two molecules with similar bond dimensions in the asymmetric unit of the title complex, [Re(C₇H₄NO₄)(CO)₃(H₂O)]. The metal centre is coordinated facially by three carbonyl groups, is chelated by a 4-carboxypyridine-2-carboxylate ligand and is also coordinated by a water molecule. O-HO hydrogen bonds give rise to a three-dimensional network.

Related literature

For the monoclinic polymorph of the title compound, see: Mundwiler et al. (2004). For related structures, see: Kemp (2006); Roodt et al. (2003); Schutte et al. (2007); Wang et al. (2003); Alvarez et al. (2007). For the synthesis of the precursor, see: Alberto et al. (1996);

Experimental

Crystal data

[Re(C₇H₄NO₄)(CO)₃(H₂O)]
M_r = 454.37
Triclinic, $[P \overline 1]$
a = 9.5024 (11) Å
b = 12.4254 (16) Å
c = 12.4889 (16) Å
= 101.799 (4)°
= 107.943 (4)°
= 111.346 (4)°
V = 1220.4 (3) Å³
Z = 4
Mo K radiation
= 10.00 mm^-1
T = 100 (2) K
0.27 × 0.17 × 0.05 mm

Data collection

Bruker APEXII diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2004) T_min = 0.140, T_max = 0.605
15096 measured reflections
5848 independent reflections
4869 reflections with I > 2(I)
R_int = 0.037

Refinement

R[F² > 2(F²)] = 0.026
wR(F²) = 0.065
S = 1.05
5848 reflections
373 parameters
7 restraints
H atoms treated by a mixture of independent and constrained refinement
_max = 1.21 e Å^-3
_min = -1.80 e Å^-3

Table 1
Selected geometric parameters (Å, °)

N1-Re1	2.180 (4)
O5-Re1	2.153 (3)
O15-Re2	2.148 (3)
N2-Re2	2.166 (4)
C11-Re2	1.892 (5)
C12-Re2	1.947 (5)
C2-Re1	1.906 (5)
C3-Re1	1.885 (6)
C13-Re2	1.883 (5)
O14-Re2	2.153 (3)
O4-Re1	2.170 (3)
Re1-C1	1.915 (5)

C11-Re2-C12	89.52 (19)
C11-Re2-O15	170.52 (16)
C12-Re2-O15	98.45 (16)
C11-Re2-O14	95.63 (16)
C12-Re2-O14	96.35 (17)
O15-Re2-O14	78.48 (12)
O15-Re2-N2	74.98 (12)
C2-Re1-O5	98.77 (15)
C1-Re1-O4	95.49 (17)
O5-Re1-O4	80.73 (12)
O5-Re1-N1	74.77 (12)

Table 2
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O7-H7O15ⁱ	0.82	1.81	2.595 (4)	160
O4-H4BO16ⁱⁱ	0.85 (5)	2.51 (5)	2.920 (5)	111 (4)
O4-H4BO8ⁱⁱⁱ	0.85 (5)	2.01 (3)	2.780 (5)	150 (5)
O4-H4BO16ⁱⁱ	0.85 (5)	2.51 (5)	2.920 (5)	111 (4)
O14-H14BO6	0.85 (5)	1.84 (2)	2.671 (5)	169 (5)
O14-H14AO18ⁱⁱⁱ	0.840 (18)	1.87 (2)	2.674 (4)	161 (5)
Symmetry codes: (i) x+1, y, z+1; (ii) x, y, z+1; (iii) x-1, y, z.

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT-Plus (Bruker, 2004); 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 (Brandenberg & Putz, 2005) and ORTEP-3 (Farrugia, 1999); software used to prepare material for publication: SHELXL97.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: NG2479 ).

Acknowledgements

The University of the Free State and Professor A. Roodt are gratefully aknowledged for financial support. Dr A.J. Muller is kindly acknowledged for the data collection.

References

Alberto, R., Schibli, R. & Schubiger, P. A. (1996). Polyhedron, 15, 1079-1083.
Alvarez, C. M., Garcia-Rodriguez, R. & Miguel, D. (2007). Dalton Trans. pp. 3546-3554.
Brandenberg, K. & Putz, H. (2005). DIAMOND. Crystal Impact GbR, Bonn, Germany.
Bruker (2004). SAINT-Plus (including XPREP) and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Bruker (2005). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.
Kemp, G. (2006). PhD thesis, University of Johannesburg, South Africa.
Mundwiler, S., Kundig, M., Ortner, K. & Alberto, R. (2004). Dalton Trans. pp. 1320-1328.
Roodt, A., Otto, S. & Steyl, G. (2003). Coord. Chem. Rev. 245, 121-129.
Schutte, M., Visser, H. G. & Steyl, G. (2007). Acta Cryst. E63, m3195-m3196.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Wang, W., Spingler, B. & Alberto, R. (2003). Inorg. Chim. Acta, 355, 386-391.