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Synthesis and crystal structure of M[Nb 6 Cl 15 ] (M = In, Tl): New Ternary Niobium Halides with Bridged [Nb 6 Cl 18 ] 4− Clusters
Author(s) -
Womelsdorf Hermann,
Meyer HansJürgen,
Lachgar Abdessadek
Publication year - 1997
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/zaac.199762301143
Subject(s) - orthorhombic crystal system , niobium , crystallography , crystal structure , chemistry , ternary operation , chloride , halide , inorganic chemistry , organic chemistry , computer science , programming language
Abstract New ternary niobium chlorides corresponding to the formula M[Nb 6 Cl 15 ] (M = In, T1) were synthesized from solid state reactions of NbCl 5 , niobium metal, and MCl 3 at 720°C. The crystal structure of In[Nb 6 Cl 15 ] was determined from single crystal X‐ray diffraction studies. The structure was refined in the orthorhombic symmetry (space group Pmma, Z = 4) with a = 1786.6(1) pm, b = 1345.52(8) pm, c = 929.34(8) pm, R F = 0.028 and R w = 0.037, GooF = 1.06 for all 1552 unique reflections. The lattice parameters of the isotypic Tl[Nb 6 Cl 15 ] compound were refined from X‐ray powder diffraction data: a = 1785.9(2) pm, b = 1347.2(2) pm, c = 930.2(1) pm. The structure of In[Nb 6 Cl 15 ] is made up of [Nb 6 Cl 18 ] 4− clusters linked to each other through terminal chloride ligands to form two sets of chains perpendicular to each other. The chains are linked through other terminal ligands to yield a three‐dimensional network. The In + or Tl + ions are located in a ten coordination site (distorted bicapped cubic geometry) made up of eight inner and two outer chloride ligands.