Bis(μ-pyridazine-3-carboxyl­ato-κ2O:O′)bis­[aqua­dioxido(pyridazine-3-carboxyl­ato-κ2N2,O)uranium(VI)] dihydrate

Leciejewicz, J.; Starosta, W.

doi:10.1107/S1600536808042219

Volume 65
Part 1
Page m94
January 2009

Received 6 November 2008
Accepted 11 December 2008
Online 17 December 2008

Key indicators
Single-crystal X-ray study
T = 293 K
Mean (C-C) = 0.013 Å
R = 0.043
wR = 0.127
Data-to-parameter ratio = 19.4
Details

Bis(-pyridazine-3-carboxylato-²O:O')bis[aquadioxido(pyridazine-3-carboxylato-²N²,O)uranium(VI)] dihydrate

Janusz Leciejewicz ^a ^* and Wojciech Starosta ^a

^aInstitute of Nuclear Chemistry and Technology, ul. Dorodna 16, 03-195 Warszawa, Poland
Correspondence e-mail: jlec@ichtj.waw.pl

The structure of the binuclear title complex, [U₂(C₅H₃N₂O₂)₄O₄(H₂O)₂]·2H₂O, is composed of centrosymmetric dimers in which each UO₂²⁺ ion is coordinated by two ligand molecules. One donates its N,O-bonding group and the other donates both carboxylate O atoms. Each of the latter bridges adjacent uranyl ions. The coordination environment of the metal center is a distorted pentagonal bipyramid. The dimers are interconnected by O-HO hydrogen bonds between coordinated and uncoordinated water molecules and carboxylate O atoms. An intramolecular O-HN interaction is also present.

Related literature

For the crystal structure of pyridazine-3-carboxylic acid hydrochloride, see: Gryz et al. (2003). For centrosymmetric dimeric molecules with a different bridging mode for the title ligand to calcium(II), see: Starosta & Leciejewicz (2007). For bond distances and angles in uranyl complexes with carboxylate ligands, see: Leciejewicz et al. (1995).

Experimental

Crystal data

[U₂(C₅H₃N₂O₂)₄O₄(H₂O)₂]·2H₂O
M_r = 1104.50
Monoclinic, C 2/c
a = 25.660 (5) Å
b = 6.8330 (14) Å
c = 16.673 (3) Å
= 96.73 (3)°
V = 2903.2 (10) Å³
Z = 4
Mo K radiation
= 11.23 mm^-1
T = 293 (2) K
0.19 × 0.12 × 0.07 mm

Data collection

Kuma KM-4 four-circle diffractometer
Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2008 $[Oxford Diffraction (2008). CrysAlis RED. Oxford Diffraction Ltd., Abingdon, England.]$ ) T_min = 0.234, T_max = 0.470
4406 measured reflections
4266 independent reflections
2746 reflections with I > 2(I)
R_int = 0.025
3 standard reflections every 200 reflections intensity decay: 1.0%

Refinement

R[F² > 2(F²)] = 0.043
wR(F²) = 0.127
S = 1.01
4266 reflections
220 parameters
5 restraints
H atoms treated by a mixture of independent and constrained refinement
_max = 2.83 e Å^-3
_min = -4.65 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
O4-H42O22ⁱ	0.81 (11)	2.23 (9)	2.933 (9)	146 (14)
O4-H41O22	0.83 (8)	1.98 (8)	2.803 (10)	175 (13)
O3-H31N11	0.82 (9)	1.94 (9)	2.754 (9)	170 (13)
O3-H32O4ⁱⁱ	0.82 (6)	1.90 (9)	2.707 (12)	170 (13)
Symmetry codes: (i) $[-x+{\script{1\over 2}}, -y+{\script{3\over 2}}, -z+1]$ ; (ii) $[x, -y+1, z-{\script{1\over 2}}]$ .

Data collection: KM-4 Software (Kuma, 1996 $[Kuma (1996). KM-4 Software. Kuma Diffraction Ltd. Wroclaw, Poland.]$ ); cell refinement: KM-4 Software; data reduction: DATAPROC (Kuma, 2001 $[Kuma (2001). DATAPROC. Kuma Diffraction Ltd. Wroclaw, Poland.]$ ); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL.

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: RK2117 ).

References

Gryz, M., Starosta, W., Ptasiewicz-Bak, H. & Leciejewicz, J. (2003). J. Coord. Chem. 56, 1505-1511.
Kuma (1996). KM-4 Software. Kuma Diffraction Ltd. Wroclaw, Poland.
Kuma (2001). DATAPROC. Kuma Diffraction Ltd. Wroclaw, Poland.
Leciejewicz, J., Alcock, N. W. & Kemp, T. J. (1995). Struct. Bonding (Berlin), 82, 43-85.
Oxford Diffraction (2008). CrysAlis RED. Oxford Diffraction Ltd., Abingdon, England.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
Starosta, W. & Leciejewicz, J. (2007). Acta Cryst. E63, m1662-m1663.

metal-organic compounds

Bis(-pyridazine-3-carboxylato-2O:O')bis[aquadioxido(pyridazine-3-carboxylato-2N2,O)uranium(VI)] dihydrate