trans-Dibromobis(cyclohexylamine)platinum(II)

Abstract

Introduction. The title compound was prepared by a modification of Dhara's (1970) method involving the reaction of K2[PtC14] (0.97 g) with KI (1.6 g) in water (10 ml). Cyclohexylamine (0.49 g) was added dropwise to the resulting solution and the yellow precipitate of [Pt(C6HIINH2)2I 2] was filtered off and dried. The yellow powder (0.66 g) was stirred with aqueous silver nitrate (0.34 g, 50 ml) for a week. AgI was removed by filtration and KBr solution (0.14 g, 25 ml)was added dropwise to the filtrate. A pale-yellow powder precipitated and was separated by filtration. This powder was dissolved in acetone and crystals of the title compound were obtained by slow evaporation of this solution. Composition: calculated, C, 26.1; H, 4.7; N, 5.1%; found, C, 26.3; H, 4.7; N, 5.0%. The crystals were long needles, the needle axis being a. A crystal, which was homogeneous under the polarizing microscope, was cut and ground into a cylinder of dimensions r = 0.07, l = 0.25 mm. Photographs showed the systematic absences of P21/c. The cell was determined by the least-squares fit of 15 well centred reflections (17 ° < 20 < 25 ° ) on a Syntex P21 diffractometer at 296 K and the density was determined by flotation in aqueous zinc bromide solutions, yielding Z = 2. The intensities of 1885 independent reflections up to 20 = 55 ° (hk + l) were measured with Mo Ka radiation at 296 K. The computer-controlled Syntex P21 diffractometer was operated in a 20(counter)-0(crystal) scan mode with a crystal monochromator. After removal of systematically absent reflections and of those for which I < ix(I), 1306 were considered observed [I > 3.0tr(I)] and were used for the structure determination; 191 were considered unobserved and were given no weight in the structure

Formation of Palladium Bis(amine) Complexes from Reaction of Amine with Palladium Tris(o-tolyl)phosphine Mono(amine) Complexes

“…Comparison of the intensity of these triplets to the intensity of the single tert -butyl resonance at δ 1.27 established the 2:1 ratio of benzylamine ligands to tert -butyl groups, while the equivalence of the benzylamine ligands is consistent with their trans orientation. Palladium bis(amine) complexes of the form Pd(amine) 2 X 2 (X = halide, acetate) typically possess trans amine ligands, and although cis palladium(II) bis(amine) complexes can be generated under certain conditions, cis to trans isomerization is typically facile . Addition of D 2 O to a solution of 16 in C 6 D 6 resulted in rapid deuterium exchange of the amino protons of the benzylamine ligands, as indicated by the disappearance of the δ 2.4 resonance and loss of coupling to the benzylic resonance at δ 3.81 in the 1 H NMR spectrum.…”

Conformational isomerism of trans-[Pt(NH2C6H11)2I2] and the classical Wernerian chemistry of [Pt(NH2C6H11)4]X2 (X=Cl, Br, I)

“…Crystal structures were previously reported for compounds 2 and 4 [24, 25]. We collected a new data set for an identical polymorph of 4 at low temperature and obtained a higher resolution structure.…”

“…The full molecule is therefore present in the anti conformation. This structure is isomorphous with one previously reported in the literature [25]. In this previous study, the collection was carried out at room temperature and the hydrogen atoms were not included in the model.…”