Abstract
The crystal structure of tetraphenylarsonium nitridotetrachloroosmate(VI), (Ph4 As)[OsNCl4 ], has been determined from three-dimensional X-ray diffractometer data. The crystals are tetragonal with unit-cell dimensionsa = 12.667(3),c = 7.820(2) Å, space groupP4/n andZ = 2. Full-matrix least-squares refinement, using 1189 independent reflections, has reachedR = 0.037.
Two discrete ionic species are present in the structure. The [OsNCl4]− anion has 4mm (C 4v) point symmetry, and the osmium atom has a square-pyramidal coordination with Os-N and Os-Cl bond lengths of 1.604 and 2.310 Å respectively. Because of the strongly π-donating nature of the terminal nitrido ligand the basal plane is depressed to 0.58 Å below the osmium atom, such that the N-Os-Cl angles are 104.5 °. The tetrahedral tetraphenylarsonium cation has ¯4(S 4) crystallographic symmetry with As-C distances of 1.912 Å and two independent C-As-C angles of 105.1 and 111.7 °.
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Phillips, F.L., Skapski, A.C. Crystal structure of tetraphenylarsonium nitridotetrachloroosmate(VI): a complex of five-coordinate osmium. Journal of Crystal and Molecular Structure 5, 83–92 (1975). https://doi.org/10.1007/BF01387002
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DOI: https://doi.org/10.1007/BF01387002