A New Study of the Acid Rhodo Complex Salt [(NH3)5CrOHCr(NH3)5]Cl5.H2O Shows That the Crystals are Orthorhombic

Abstract

Diffraction data recorded at low temperature with Mo K\alpha from two different crystals have been used in the refinement of the structure of the acid rhodo complex salt, \mu-hydroxo-bis[pentaamminechromium(III)] chloride monohydrate [(NH3)5CrOHCr(NH3)5]Cl5.H2O. Several structural models in two different tetragonal space groups have been investigated before a satisfactory description of the structure was obtained. The compound crystallizes in the orthorhombic space group P212121, with a= 16.155 (3), b = 16.154 (3), c = 14.750 (7) Å and Z = 8. The apparent tetragonal symmetry arises due to rotation twinning of the crystals. The diffraction pattern is further complicated by tetragonal pseudo-symmetry of the chromium sites, which means that reflections with l = 2n + 1 are systematically weak. The two independent dimeric cations are involved in slightly different hydrogen-bond patterns. This observation and the relative orientation of the dimers in the crystal is in accordance with spectral and magnetic measurements.