Bulk material vs. single crystal: powder diffraction to the rescue

Abstract

The crystal structure of bulk microcrystalline material obtained by interaction of two rigid building blocks, namely dirhodium(II) tetra(trifluoroacetate), [Rh₂(O₂CCF₃)₄], and bis(4’-pyridyl)diphenylsilane, (C₆H₅)₂Si(C₅H₄N)₂, has been solved ab initio using X-ray powder diffraction data. The title product of the 1 ∶ 1 composition, [Rh₂(O₂CCF₃)₄·(µ₂-(C₆H₅)₂Si(C₅H₄N)₂)], is a one-dimensional zigzag polymer built on axial Rh⋯N interactions averaged at 2.16 Å. Its structural characterization complements the previously reported product of the 2 ∶ 1 composition obtained from the same reaction, namely {[Rh₂(O₂CCF₃)₄]₂·(µ₄-(C₆H₅)₂Si(C₅H₄N)₂)}. The latter has a 2D layered network revealed by the single crystal diffraction study. A combination of powder and single crystal X-ray techniques is shown to be methodologically important and complementary for understanding of product assembling in the system.