CRYSTAL AND MOLECULAR STRUCTURE OF DICYANOTRIS(PHENYLDIMETHYLPHOSPHINE)NICKEL(2) NI(CN)2(P(C6H5)(CH3)2)3

The crystal and molecular structure of dicyanotris(phenyldimethylphosphine)nickel(II), Ni(CN)2(P(C6H5) (CH3)2)3, has been determined from three-dimensional X-ray data collected by counter methods. The structure has been refined by least-squares techniques to a final R factor on F of 4.9%. The material crystallizes in space group Ci1-P1 of the triclinic system, with two molecules in a cell of dimensions a = 8.907 (8), b = 16.292 (15), c = 9.876 (9) Å, α = 97° 58 (1)′, β = 102° 40 (1)′, and y = 86° 40 (1)′. (Reduced cell: a = 8.907, b = 16.292, c = 17.842 Å, α = 146° 46Ȳ, β = 93° 55′, and 7 = 93° 20Ȳ.) The observed and calculated densities are 1.26 ± 0.01 and 1.260 g/cm3, respectively. The inner coordination about the Ni is trigonal bipyramidal with the two cyanides at the apices and the three phosphines in the basal plane. There is a slight but significant distortion toward a tetragonal-pyramidal geometry, which is discussed in relation to the far more distorted structure of Ni(CN)2(P(C6H6)(OC2H5)2)3. The Ni-P bond lengths are 2.261 (3), 2.223 (3), and 2.223 (3) Å, and the Ni-C distances are 1.84 (1) and 1.86 (1) Å. © 1969, American Chemical Society. All rights reserved.