Abstract
The crystal structures of the mixed transition-metal nitrosylpentacyanoferrate trihydrates have been determined from three-dimensional single-crystal X-ray diffraction data. These polynuclear cyanides crystallize in the monoclinic space group P 2 1/ n ( Z = 4) with lattice parameters of a = 7.385(1), b = 14.905(3), c = 10.810(2) Å, β = 91.54(2)°; and a = 7.4109(3), b = 14.9430(9), c = 10.8423(6) Å, β = 91.570(4)° for 1:1 (Cd/Mn) and 1:1 (Cd/Zn)[Fe(CN) 5NO · 3H 2O, respectively. The final least-squares full-matrix refinements, based on 1978 and 2026 unique reflections, yielded reliability factors equal to 0.048 and 0.044, respectively. The mixed cation centers are six-coordinated, with five cyanide ligands and one water molecule in an octahedral arrangement. The Fe atoms also display octahedral symmetry with five cyanide ligands and one nitrosyl group. The distorted octahedral metal centers, which are geometrically arranged in a staggered fashion, are united by cyanide bridging. Two of the three water molecules which are uncoordinated occupy channels in the crystal lattice and are held in position by hydrogen bonding to the coordinated water molecule, O(1). Important bond distances and angles are presented and appropriately discussed. Conoscopic, infrared, thermogravimetic, and crystallographic results are reported.
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