Mixed-metal molybdenum(II)–rhodium(II) trifluoroacetates, [Mo2-xRhx(O2CCF3)4], have been prepared by codeposition from the gas phase of individual volatile building units, Mo2(O2CCF3)4 and Rh2(O2CCF3)4. The composition of the bimetallic complexes isolated in the crystalline form can be modified by varying temperature and ratio of starting materials. This is an interesting system for which single crystal X-ray study fails to provide an unambiguous evidence of whether the products consist of starting homometallic or newly formed heterometallic paddle-wheel units. Both metal atoms occupy the same crystallographic position while the M–M and M–O distances are averaged in respect to the parent homometallic compounds. The results of mass-spectroscopic and magnetic measurements clearly indicate that the bimetallic carboxylates contain a statistical mixture of homometallic dimolybdenum and dirhodium units. The products can be considered as a result of co-crystallization of isomorphous dinuclear molecules.
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