Ab initio XRPD structure determination of organometallic compounds: The case of Pd(Phen)(C(O)N(Me)OC(O)), a model intermediate in the palladium-phenanthroline-catalyzed reductive carbonylation of aromatic nitro compounds

In the absence of suitable single crystals, the problem of determining the connectivity pattern of the title compound (and of its phenyl analogue), i.e. that of discriminating between two markedly different stereoisomers, has been solved by the powder diffraction technique. The structure of Pd(Phen)(C(O)N(Me)OC(O)) was solved by ab initio XRPD methods and refined by the Rietveld technique down to Rwp = 0.123, Rp = 0.087, and RF = 0.061 for 5000 data points (847 reflections) collected in the 8 < 2 θ < 108° range. The diffraction results have been cross-validated by steric energy computations within the field of the given crystal lattice.