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Materials Science Forum, Vol.378-3, 798-801, 2001
Structure determination of two organometallic complexes from powder data using grid-search techniques
The structures of the organometallic complexes [Re(PPh3)(2)(CO)(2)(DBQ)](+).PF6- (DBQ = 3,5-di-tert.butyl-benzoquinone) and [Fe(teec)(6)](2+).2BF(4)(-) (teec = 1-(2-chloroethyl)-tetrazole) -from now on Re- and Fe-complex respectively- have been determined from Guinier-camera powder data, using the grid-search techniques performed by the program MRIA [1,2]. Both structures were solved in two stages. In both cases, first the organometallic moieties were located, then they were kept fixed and the PF6- and BF4- respectively were searched for. After the determination of the position of the whole molecule, torsion-angle variations were applied to determine more accurately the position of the rings and some other smaller fragments. Rietveld Refinement (RR) on basis of Guinier data turned out to be unstable and high-resolution data were considered necessary. For the second compound synchrotron data were collected at the ESRF. The RR with this data is in progress and gives better results. Some crystal data and the R-factors in the several stages are listed in Table 1. It is remarkable how the torsion-angle search improves the starting model used for the refinement.