L. Solujic et al., SYNTHESIS AND CHARACTERIZATION OF DIASTEREOMERIC NICKEL(II) COMPLEXESOF BI(1-PHENYL-3,4-DIMETHYL-2,5-DIHYDRO-1H-PHOSPHOLE), Inorganic chemistry, 33(25), 1994, pp. 5654-5658
The reaction of -3,4-dimethyl-2,5-dihydro-1H-phosphole)]nickel(II) wit
h silver tetrafluoroborate in dichloromethane/acetonitrile solution le
ads to the formation of the meso (1) and racemic (2) diastereomers of
-3,4-dimethyl-2,5-dihydro-1H-phosphole)]nickel(II) tetrafluoroborate a
nd a single diastereomer of -3,4-dimethyl-2,5-dihydro-1H-phosphole)]ni
ckel(II) tetrafluoroborate (3). These compounds were separated by frac
tional crystallization and characterized by elemental analysis, physic
al properties, H-1, H-1{P-31}, C-13{H-1}, and P-31{H-1} NMR spectrosco
py, electronic spectroscopy, and cyclic voltammetry. The structures of
complexes 1 and 2 were determined by X-ray crystallography. Complex 1
crystallizes in the monoclinic space group C2/c with a = 18.443(5) An
gstrom, b = 14.139(2) Angstrom 18.535(3) Angstrom, beta = 104.19(2)deg
rees, and Z = 4. Complex 2 crystallizes in the monoclinic space group
P2 with a = 17.108(4) Angstrom, b = 9.512(3) Angstrom, c = 14.78(3) An
gstrom, beta = 90.59(2)degrees, and Z = 2. Refinements converged to R(
F) = 0.084 and 0.051 for 3572 and 2068 independent observed (I greater
than or equal to 3 sigma(I)) reflections, respectively.