Crystal and Molecular Structure of (Ni((CH3)2C(OH)CH2COCH3)2) (Ni(NCS)4(P(CH2CH2CN)3)2): A Beta-Hydroxyketone Chelate Complex.

摘要

The title compound has been synthesized and its crystal structure determined by single-crystal X-ray diffraction methods. The complex crystallizes in space group P1, with a = 12.773(4), b = 11.421(3), c = 8.864(3) A; alpha = 106.37(5), beta = 78.56(5), gamma = 104.37(5) degrees. Full-matrix least-squares refinement of positional and thermal parameters for all atoms (3 methyl H atoms fixed), with 3610 reflections (F > 3.92 sigma(F)) led to R = 0.044 and R(W) = 0.064. Both cation and anion occupy crystallographic centers of symmetry. In the cation, the beta-hydroxyketone ligand is (as expected) not planar: the hydroxyl oxygen atom and beta 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) A, respectively. The anion is trans-octahedral; Ni-N-C angles show large distortions from linearity: 160.7(3) and 163.9(3) degrees. (Author)