Abstract
Abstract The new polychalcogenide Cs4Nb2S11 was prepared from the melt. Cs4Nb7S11 is orthorhombic, oP68, s.g. Pca21 (No.29), Z = 4 with a = 13.775(9) Å, b = 8.043(9) A , c = 18.306(5) Å. The crystal structure was determined from diffractometer data and refined to a conventional R of 0.052 (1104 Fo’s, 154 variables). It is characterized by asymmetric discrete binuclear moieties [Nb2S11]4- which are separated by the alkali cations. Each Nb atom is side-on coordinated by two S2 2- groups, one bridging and one terminal sulfide ligand. Nb-S bond lengths are 2.15(1) Å to 2.22(1) Å (terminal) and 2.44(1 )Å to 2.51(1) Å (others). A further longer Nb-S bond (2.86(1)A and 2.90(1)A, resp.) expands the coordination of the two crystallographically independent transition metal atoms to distorted pentagonal bipyramidal configurations. The Nb-Nb-distance is 3.517(3) Å. The anionic groups are arranged in hexagonal close packed slabs running parallel to (001). The atomic arrangement corresponds to that of K4Ta2S11
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