111548-87-9Relevant academic research and scientific papers
Dimorphs of ethane>dichloronickel(II)
Busby, Richard,Hursthouse, Michael B.,Jarrett, Penelope S.,Lehmann, Christian W.,Malik, K. M. Abdul,Phillips, Coral
, p. 3767 - 3770 (1993)
The two known forms, A and B, of dichloronickel(II), , were synthesized and identified by IR spectroscopy.The spectra showed that form A had a lower symmetry than form B.The forms were also found to differ by solid-state 31P NMR spectroscopy and powder X-ray diffraction, but the solution properties were identical.The IR spectrum of the dichloromethane solvate of was the same as that of form B but with a strong additional band due to CH2Cl2.The X-ray diffraction pattern from this sample matched that calculated for a previously published crystal structure of *CH2Cl2, thus identifying the form used in that work.Crystals of form A obtained from acetone were used for a single-crystal X-ray structure determination.Comparison of the molecular structures showed that both forms have the same chelate-ring conformation (δ) but differ in the orientations of the phenyl rings.There is a non-crystallographic two-fold axis in form B which is absent from A, explaining the additional bands present in the IR spectrum of the latter.Solid-state 31P NMR was better than IR spectroscopy at distinguishing the two forms from each other and from mixtures.
Diphosphine complexes of nickel: Analogies in molecular structures and variety in crystalline arrangement
Bomfim, Jo?o A.S.,De Souza, Fabio P.,Filgueiras, Carlos A.L.,De Sousa, Alexsandro G.,Gambardella, Maria Teresa P.
, p. 1567 - 1573 (2008/10/08)
This work comprised the preparation of six complexes of Ni(II) and their study by spectroscopy and X-ray diffraction. These complexes are: [Ni(dppe)Cl2]CH2Cl2 (I), [Ni(dppen)Cl2] (II), [Ni(dppm)Br2]CH2Cl2 (III), [Ni(dppe)(NCS)2] (IV), [Ni(dppen)I2] (V), [Ni(dppp)Cl2]CH2Cl2 (VI), where dppe = 1,2-bis(diphenylphosphine)ethane, dppen = cis-1,2-bis(diphenylphosphine)ethene, dppm = bis(diphenylphosphine)methane, dppp = 1,3-bis(diphenylphosphine)propane. The structures of complexes II-VI are unknown in the literature. Although the molecular structures of the six complexes present many similarities, their crystalline arrangements vary considerably. This is a feature not presented hitherto in previous work involving complexes of this type. In addition, a systematic spectroscopic study was undertaken on all six complexes.
Reaction of [Ni(Ph2PCH2CH2PPh2)2] with DCl: Controlling the formation of HD and D2
Davies, Sian C.,Henderson, Richard A.,Hughes, David L.,Oglieve, Kay E.
, p. 425 - 431 (2007/10/03)
The reaction between anhydrous DCl and [Ni(Ph2PCH2CH2PPh2)2] in dichloromethane produced mixtures of HD and D2. The relative amounts of the dihydrogen isotopomers produced depends on the concentration of acid. Mechanistic investigations showed that the reaction involves initial formation of [NiD(Ph2PCH2CH2PPh2)2]. This deuteriation labilises the nickel to phosphine dissociation. At low concentrations of acid, phosphine chelate ring opening produces [NiCl2(Ph2PCH2CH2PPh2)] (confirmed by X-ray crystallography) and free Ph2PCH2CH2PPh2 together with HD (65 ± 5) and D2 (35 ± 5%). The hydrogen atom of HD originates from a phosphine ligand. At high concentrations of acid the rate of attack of DO at [NiD(Ph2PCH2CH2PPh2 2)2]+ becomes faster than phosphine chelate ring opening and results in the formation of [Ni(Ph2PCH2CH2PPh2) 2]Cl2 and predominantly D2. Experimentally, the highest concentration of DC1 that can be used without appreciable decomposition of the complex is 0. 2 mol dm 3. At this concentration of acid the dihydrogen isotopomer distribution is HD (35 ± 5) and D2 (65 ± 5%); however, analysis of the product distribution indicates that at much higher acid concentrations D2 could be the exclusive isotopomer.
