CRYSTAL AND MOLECULAR-STRUCTURE OF (NI[(CH3)2C(OH)CH2COCH3]2))NI[NCS]4[P(CH2CH2CN)3]2 - BETA-HYDROXY KETONE CHELATE COMPLEX

The title compound has been synthesized and its crystal structure determined by single-crystal X-ray diffraction methods. The complex crystallizes in space group P$$, with [formula omitted] and y=104.37 (5)°. Full-matrix least-squares refinement of positional and thermal parameters for all atoms (three methyl H atoms fixed), with 3610 reflections (F > 3.92σ(F)) led to R=0.044 and Rw=0.064. Both cation and anion occupy crystallographic centers of symmetry. In the cation, the (3-hydroxy ketone ligand is (as expected) not planar: the hydroxyl oxygen atom and β-carbon atom lie+0.40 and-0.38 A out of a plane containing Ni and the other ligand atoms. The Ni-O distances to the carbonyl and hydroxyl oxygen atoms are 1.895 (3) and 1,927 (3) υ, respectively. The anion is trans octahedral; Ni-N-C angles show large distortions from linearity: 160.7 (3) and 163.9 (3)°. © 1979, American Chemical Society. All rights reserved.