Proton ENDOR spectroscopy of bis(2,2,6,6-tetramethylheptane-3,5-dionato)copper(II) and crystal structure of bis(2,2,6,6-tetramethylheptane-3,5-dionato)palladium(II)

Abstract

The proton electron nuclear double resonance spectroscopy of a single crystal of bis( 2,2,6,6tetramethylheptane-3,5-dionato)copper( 11) in the palladium analogue has been studied. Tensors could be determined for the y-proton and t w o nearest But protons as well as six protons on the nearest-neighbour palladium complex. The assignment of most of these was enabled by the comparison with theoretically calculated tensors. This calculation procedure has been described previously: it uses the molecular orbital coefficients as obtained from an extended Huckel calculation and includes all t w o -and three-centre contributions. The remaining experimental curves could not be fitted t o calculated tensors. The structure of the palladium analogue, C, H, O, Pd, was determined by X-ray crystallography at 140 K: monoclinic, space group P2,/n, a = 1 1.245(3), b = 12.008(8), c = 9.851 (3) A, p = 11 0.1 7(3)", and Z = 2 (Mo-K, radiation, graphite crystal monochromator). Final conventional R = 0.029, R' = 0.044 for 1 654 unique reflections and 186 variables.

Synthesis and characterization of fluorinated β-ketoiminate and imino-alcoholate Pd complexes: precursors for palladium chemical vapor deposition

“…1 for which the basal plane shows an essentially planar arrangement. 14 The crystal structure of 2c is shown in Fig. 3 and the corresponding bond distances and angles are presented in Table 3.…”