Bis(4-benzoyl-3-methyl-1-phenyl-4,5-dihydro-1H-pyrazol-5-olato-κ2 O,O′)(methanol-κO)dioxidouranium(VI) methanol monosolvate

In the title compound, [U(C17H13N2O2)2O2(CH3OH)]·CH3OH, the UVI ion is coordinated by seven O atoms in a distorted pentagonal–bipyramidal geometry with two 3-methyl-1-phenyl-4-benzoyl-4,5-dihydro-1H-pyrazol-5-olate groups with two O atoms in a bidentate chelating coordination mode and by three O atoms, one of which is from a methanol ligand. The crystal packing can be described by alternating layers of complex molecules along the a axis. The structure is stabilized by O—H⋯N and O—H⋯O hydrogen bonding and van der Waals interactions.

In the title compound, [U(C 17 H 13 N 2 O 2 ) 2 O 2 (CH 3 OH)]ÁCH 3 OH, the U VI ion is coordinated by seven O atoms in a distorted pentagonal-bipyramidal geometry with two 3-methyl-1-phenyl-4-benzoyl-4,5-dihydro-1H-pyrazol-5-olate groups with two O atoms in a bidentate chelating coordination mode and by three O atoms, one of which is from a methanol ligand. The crystal packing can be described by alternating layers of complex molecules along the a axis. The structure is stabilized by O-HÁ Á ÁN and O-HÁ Á ÁO hydrogen bonding and van der Waals interactions.

Comment
The ligands derived fromβ-diketone compounds such as those of 3-methyl-1-phenyl-4-benzoylpyrazol-5-one (H1MPBP) have been found to have good extractive ability for heavy metals traces and interesting biological activities (Okafor et al., 1981). Their metal complexes M II -(MPBP) 2 of copper(II) and zinc(II) are well known in the literature for their diverse therapeutic applications as anticarcinogenic, anti-inflammatory and analgesic activities (Caruso et al., 2000;Li et al., 1997;Zhou et al., 1999). Thus, we report here the synthesis of title compound and its crystal structure. The asymetric unit of structure of (I), and the atomic numbering used, is illustrated in Fig. 1.
The U VI ion is coordinated in a irregular octahedral geometry by two (3-Methyl-1-phenyl-4-benzoylpyrazol-5one)groups with two O atoms in bidentate chelating coordination and three O atoms, when one O atom is linked to methanol moiety. One molecule of methanol is cocrystalized with the title complexe. The bond lengths for co-ordination U(V) sphere is ranging from 1.760 (3) to 2.391 (3)Å for Cu-O distances ( Table 2). The crystal packing in the title structure can be described by alterning layers of complexe along the a axis (Fig. 2) Fig. 2) and a Van Der Waals interactions. These interactions link the molecules within the layers and also link the layers together and reinforcing the cohesion of the structure.

Experimental
106 mg (0.25 mmol) of dioxouranyl(II) acetate dihydrate (UO 2 (OAc) 2 ,2H 2 O) were dissolved in 15 ml of methanol. This solution was drop wisely added, under stirring, to a methanolic solution (10 ml) containing 139 mg of 3-methyl-1phenyl-4-benzoylpyrazol-5-one (0.5 mmol, H1MPBP). This mixture was refluxed during one night after which is abandoned for several weeks until the formation of suitable crystals. These crystals, recovered by filtration, were then washed several times with methanol and dried to yield 132 mg (60%) of the title compound.

Refinement
The remaining H atoms were localized on Fourier maps but introduced in calculated positions and treated as riding on their parent atoms (C and O) with C-H = 0.96 Å (methyl) or 0.93 Å (aromatic) and O-H = 0.82 Å with U iso (H) = 1.2U eq (C aromatic ) or U iso (H) = 1.5U eq (C methyl and O hydroxy ). In exept the H7o atom was located in difference Fourier maps and their coordinates were refined; the O-H7o distance was restrained to 0.82 (2)Å. The maxima and minima in the residual electron density are associated with atom U1. (Sheldrick, 2008); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg & Berndt, 2001); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figure 1
The asymmetric unit of (I) with the atom-labeling scheme. Displacement ellipsoids are drawn at the 50% probability level.

Figure 2
Altering layers of (I) viewed via b axis showing hydrogen bond interactions(O-H···N), in blue, as dashed lines.

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Acta Cryst. (2012). E68, m457-m458  Special details Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. Refinement. Refinement of F 2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F 2 , conventional R-factors R are based on F, with F set to zero for negative F 2 . The threshold expression of F 2 > 2sigma(F 2 ) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F 2 are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger.