Showing papers by "Thomas A. Hamor published in 1992"
TL;DR: In this article, the molecular structure of [Mo(NO)(HB(Me2pz)3)(OCH2(CH20CH2)3CH20)] has been determined by X-ray diffraction methods.
Abstract: (n = 2-5; HB(Me,pz),- = hydrotris(3,5-dimethylpyrazoly1)borate) have been synthesized and characterized by spectroscopic methods. All contain the redox-active (MO(NO))~+ moiety incorporated in an unusually large chelate ring which forms a cyclic polyether structure. Cyclic voltammetric studies of these compounds reveal a reduction process at ca. -1.3 V (SCE) which is shifted to more anodic potentials in the presence of an equimolar concentration of sodium ions. At higher concentrations, decomposition is associated with the reduction process. In the case where n = 3, 1:l complexes with Li+, Na+, and K+ have been isolated. The molecular structure of [Mo(NO)(HB(Me2pz)3)(OCH2(CH20CH2)3CH20)] has been determined by X-ray diffraction methods. The compound crystallizes in the orthorhombic space group Pbca (No. 61) with eight molecules in a cell of dimensions a = 16.937 (3), b = 15.143 (4), and c = 22.034 (8) A. Full-matrix least-squares refinement gives final R, R, on Fof 0.051,0.079 for 3063 observed [F > 5u(F)] data, This structure confirms the presence of a 14-membered chelate ring (Md = 1.903 (4) and 1.910 (4) A; 0-Mo-0 = 101.0 (2)O) and a linear nitric oxide ligand (Mo-N-O = 177.9 (5)'; N-O = 1.190 (6) A). The cyclic polyether ring is extended away from the bulky HB(Me2pz), ligand.
14 citations
TL;DR: The rotameric conformations about the P-N bond of P-phenyl-P-(2,4,6-trimethylphenyl)phosphinamide have been obtained in six steps from dichlorophenylphosphine as discussed by the authors.
Abstract: The primary phosphinic amide P-phenyl-P-(2,4,6-trimethylphenyl)phosphinamide has been prepared in optically active form (75% enantiomeric excess) in six steps from dichlorophenylphosphine. The configuration of the intermediate N-(1-phenylethyl)-P-phenyl-P-(2,4,6-trimethylphenyl)phosphinamide has been established by an X-ray crystal structure determination of the minor diastereoisomer. This compound exhibits in the solid state two independent rotameric conformations about the P–N bond. Geometry optimisation by MNDO MO calculations refined these to the same rotamer having the nitrogen lone pair anticlinal to the P–O bond.
12 citations
TL;DR: In this paper, the type B meso-ionic heterocycle 3,5-diphenyl-1,2-dithiolium-4-olate (1) with aniline yields Nphenyl-(3-phenyl)-1-phenylimino-inden-2-yl)-amine (10) and 11-phenylonbenz[bindeno[2,1-e]-1,4-thiazine (12).
9 citations
TL;DR: In this paper, the crystal structure of the 1,2-phenylenediamide-bridged bimetallic complex [{Mo(NO)L(I)}2{1,2-(NH)2C6H4}] has been determined.
Abstract: Cyclic voltammetry of the 1,2-phenylenediamide-bridged bimetallic complex [{Mo(NO)L(Cl)}2{1,2-(NH)2C6H4}][L = HB(3,5-Me2C3HN2)3] has revealed two one-electron reduction processes separated by 770 mV, a value which is in accord with the presence of strongly interacting molybdenum centres but intermediate between those found for the corresponding complexes containing 1,4- and 1,3-disubstituted aryl bridging groups. The crystal structure of [{Mo(NO)L(I)}2{1,2-(NH)2C6H4}] has been determined. It contains Mo–N(arylamide) distances of 1.957(6)A and reveals a non-planar structure for the MoN(amide)–C–C–N(amide)Mo moiety which may account for the lower than expected Mo ⋯ Mo interaction detected electrochemically.
2 citations