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Starting from vanadium which was not free of oxide, VCl 4  was prepared; its reaction with PPh 4 Cl in the presence of K 2 S 5  in dichloromethane yielded PPh 4 [VOCl 3 OH]. From V 2 S 5 , PPh 4 Cl and S 2 Cl 2  in acetonitrile, sulfur crystallized first, then PPh 4 [VOCl 4 ], and then (PPh 4 ) 2 [VOCl 4 ]·4CH 3 CN. Upon standing with the mother liquor at -18°C, the latter was converted to (PPh 4 ) 2 [VOCl 4 ]·2CH 3 CN. According to its X-ray crystal structure determination, PPh 4 [VOCl 3 OH] (space group Pbca, a = 1105.5, b = 1920.8, c = 2242.8 pm, Z - 8) has nearly square-pyramidal anions that are associated to chains by 0-H⋯C1 bridges. PPh 4 [VOCl 4 ] is isotypic with AsPh 4 [VOCl 4 ] and has strictly square-pyramidal anions (space group P4/n, a = 1254.0, c = 765.0 pm, Z = 2). In (PPh 2 ) 2 [VOCl 4 ]·4CH 3 CN (space group P1̄, a = 1281.3, b = 1276.6, c = 1841.5 pm, α = 84.11°, β= 83.96, γ = 64.31°, Z = 2) the square pyramid of the VOCl 4  2-  ion is distorted towards a trigonal-bipyramidal shape (C 2v  symmetry) having trans-ClVCl angles of 145.88° and 156.87° and O=V-Cl angles of 107° and 101.6°. In (PPh 4 ) 2 [VOCl 4 ]·2CH 3 CN (space group P1, a = 1017.1, b = 1029.3, c = 2416.0, α = 77.74°, ß = 79.99°, γ = 78.94°, Z = 2), the VOCl 4  2-  structure is even closer to trigonal-bipyramidal, with trans-ClVCl angles of 133.25° and 165.80° and 0=V-Cl angles of 113.3° and 97°.

zeitschrift für naturforschung b

Die Oxochlorovanadate PPh 4 [VOCl 3 OH], PPh 4 [VOCl 4 ], (PPh 4  ) 2  [VOCl 4  ]·2CH 3 CN und (PPh 4 ) 2 [VOCl 4 ]·CH 3 CN mit auffälligen Abweichungen von der quadratisch-pyramidalen Anionenstruktur / The Oxochlorovanadates PPh 4 [VOCl 3 OH], PPh 4 [VOCl 4 ], (PPh 4  ) 2  [VOCl 4  ]·2CH 3 CN and (PPh 4 ) 2 [VOCl 4 ]·CH 3 CN with Remarkable Deviations from the Square-Pyramidal Anion Structure