Browsing by Author "Brown, Loren C."

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    Crystal structure of the tetra-meth-yl(pheneth-yl)cyclo-penta-dienylmolybdenumtricarbonyl dimer.
    Brown, Loren C.; Marron, Danny; Smith, Casey; Merola, Joseph S. (International Union of Crystallography, 2018-07)
    The structure of the dimer bis-{tricarbon-yl[η5-tetra-meth-yl(pheneth-yl)cyclo-penta-dien-yl]molybdenum}(Mo-Mo), [Mo2(C17H21)2(CO)6], at 102 K has triclinic (P ) symmetry. The reaction between tetra-meth-yl(pheneth-yl)cyclo-penta-diene and molybdenum hexa-carbonyl in refluxing xylenes for 18 h led to a 56% yield of the dimer as a red solid. The asymmetric unit of the structure is the tetra-meth-yl(pheneth-yl)cyclo-penta-dienylmolybdenumtricarbonyl moiety and the entire dimeric mol-ecule is generated by inversion symmetry. The Mo-Mo bond length is 3.2773 (3) Å, a value slightly above the mean value for all [CpMo(CO)3]2 compounds listed in the CSD and slightly below the mean for [Cp*Mo(CO)3]2 complexes.
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    mer-Trichloridotris(tetrahydrothiophene-κS)-iridium(III): preparation and comparison with other mer trichloridotris(tetrahydrothiophene-κS)metal complexes
    Brown, Loren C.; DuChane, Christine M.; Merola, Joseph S. (International Union of Crystallography, 2016-08-09)
    The title complex, [IrCl₃(C₄H₈S)₃], was prepared according to a literature method. A suitable crystal was obtained by diffusion of pentane into a di­chloro­methane solution and analyzed by single-crystal X-ray diffraction at 100 K. The title complex is isotypic with mer-tri­chlorido­tris­(tetra­hydro­thio­phene-κS)rhodium(III). However, the orientation of the tetra­hydro­thio­phene rings is different from an earlier report of mer-tri­chlorido­tris­(tetra­hydro­thio­phene-κS)iridium(III) deposited in the Cambridge Structural Database. The IrS₃Cl₃ core shows a nearly octa­hedral structure with various bond angles within 1-2° of the perfect 90 or 180° expected for an octa­hedron. The structure of the title compound is compared with the previous iridium complex as well as the rhodium and other octa­hedral metal tris-tetra­hydro­thio­phene compounds previously structurally characterized. DFT calculations were performed, which indicate the mer isomer is significantly lower in energy than the fac isomer by 50.1 kJ mol⁻¹, thereby accounting for all compounds in the CSD being of the mer geometry. Powder X-ray diffraction of the bulk material showed that the preparation method yielded only the isomorph reported in this communication.