Tris{N-[bis(dimethylamino)phosphinoyl]-2,2,2-trichloroacetamido}(triphenylphosphine oxide)holmium(III)

In the title compound, [Ho(C6H12Cl3N3O2P)3(C18H15OP)], the HoIII ion is surrounded by six O atoms from the three bidentate N-[bis(dimethylamino)phosphinoyl]-2,2,2-trichloroacetamido ligands (L −) and by one O atom from the triphenylphosphine oxide ligand, with the formation of a distorted monocapped octahedron. In one ligand L −, the trichloromethyl group is rotationally disordered between two orientations in a 1:1 ratio, while two dimethylamino groups in another ligand L − are disordered between two conformations, each with the same 1:1 ratio.

In the title compound, [Ho(C 6 H 12 Cl 3 N 3 O 2 P) 3 (C 18 H 15 OP)], the Ho III ion is surrounded by six O atoms from the three bidentate N-[bis(dimethylamino)phosphinoyl]-2,2,2-trichloroacetamido ligands (L À ) and by one O atom from the triphenylphosphine oxide ligand, with the formation of a distorted monocapped octahedron. In one ligand L À , the trichloromethyl group is rotationally disordered between two orientations in a 1:1 ratio, while two dimethylamino groups in another ligand L À are disordered between two conformations, each with the same 1:1 ratio.

Experimental
Crystal data [Ho(C 6 H 12  supporting information   et al., 2006;Cao et al., 2005). The amide nitrogen atom of Lis deprotonated that leads to decrease

S2. Experimental
The synthesis of HL was carried out according to previously published procedure (Amirkhanov et al., 2010).

S3. Refinement
The H atoms were geometrically positioned (C-H 0.93-0.98Å), and refined as riding, with U iso (H) = 1.2-1.5 U eq of the parent atom. Atoms Cl4, Cl5, Cl6, C35, C36, C37 and C38 were treated as disordered between two positions each with occupancy factors fixed to 0.5. In the refinement, several constrains were applied: SIMU and ISOR for CL4A CL4B CL6A CL6B CL5A CL5B atoms; ISOR for disordered C atoms of one NMe 2 group; EADP instruction -for O6 C5 atoms. Also several ISOR and DFIX instructions were added.

Figure 1
Molecular structure of 1 with atom numbering scheme and 20% probability displacement ellipsoids. For each disordered atom, only one position (labelled with letter A) is shown. H atoms were omitted for clarity.

Tris{N-[bis(dimethylamino)phosphinoyl]-2,2,2-trichloroacetamido}(triphenylphosphine oxide)holmium(III)
Crystal data Special details Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 > 2σ(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.