The crystal and molecular structure of lead hexa-antipyrine perchlorate

Vijayan, M. ; Viswamitra, M. A. (1966) The crystal and molecular structure of lead hexa-antipyrine perchlorate Acta Crystallographica, 21 . pp. 522-532. ISSN 0365-110X

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Lead hexa-antipyrine perchlorate is isomorphous with a series of metal hexa-antipyrine perchlorates, M(C11H12ON2)6(CIO4) 2, where M = Mg2+, Ca2+ or Zn2+ and crystallizes in a hexagonal unit having dimensions a = 14.33 (±0.03), c = 9.75 (±0.03) Å and space group P3̅ (C⅔t). The solution of the structure in the c-axis projection was facilitated by the heavy-atom method using (hki0) reflexions. A knowledge of the z coordinates obtained previously from a study of the magnesium compound was utilized to work out the complete structure and the refinement was done three-dimentional least-squares method to an agreement index of 0.079 for 736 observed reflexions. In structure, each Pb2+ ion is surrounded by six antipyrine oxygen atoms in a slightly distorted octahedral form with Pb-O(6) = 2.446 (±0.016) Å. The five-membered pyrazolone ring is planar and is inclined at an angle of 68° to the phenyl ring. The tetrahedral ClO4 ions occupy viods provided by the adjacent antipyrine groups. The two non-equivalent Cl-O bonds, Corrected for effects of thrmal oscillation, have lengths 1.453 (I) and 1.457 Å(3) respectively.

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