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Title: Synthesis and crystal structure of Bi{sub 6.4}Pb{sub 0.6}P{sub 2}O{sub 15.2}

Bi{sub 6.4}Pb{sub 0.6}P{sub 2}O{sub 15.2} is a polymorph of structures with the general stoichiometry Bi{sub 6+x}M{sub 1-x}P{sub 2}O{sub 15+y}. However, unlike previously published structures that consist of layers formed by edge sharing OBi{sub 4} tetrahedra bridged by PO{sub 4} and TO{sub 6} (T=transition metal) tetrahedra and octahedra the title compound's structure is more complex. It is monoclinic, C2, a=19.4698(4) A, b=11.3692(3) A, c=16.3809(5) A, {beta}=101.167(1){sup o}, Z=10. Single-crystal X-ray diffraction data were refined by least squares on F{sup 2} converging to R{sub 1}=0.0387, wR{sub 2}=0.0836 for 7023 intensities. The crystal twins by mirror reflection across (001) as the twin plane and twin component 1 equals 0.74(1). Oxygen ions are in tetrahedral coordination to four metal ions and the O(BiPb){sub 4} units share corners to form layers that are part of the three-dimensional framework. Eight oxygen ions form a cube around the two crystallographically independent Pb ions. Pb-O bond lengths vary from 2.265(14) to 2.869(14) A. Pairs of such cubes share an edge to form a Pb{sub 3}O{sub 20} unit. The two oxygen ions from the unshared edges are part of irregular Bi polyhedra. Other oxygen ions of Bi polyhedra are part only of O(BiPb){sub 4} units, and some oxygen ionsmore » of the polyhedra are also part of PO{sub 4} tetrahedra. One, two, three and or four PO{sub 4} moieties are connected to the Bi polyhedra. Bi-O bond lengths {<=}3.1 A vary from 2.090(12) to 3.07(3) A. The articulations of Pb cubes, Bi polyhedra and PO{sub 4} tetrahedra link into the three-dimensional structure. - Graphical abstract: View of the structure of Bi{sub 6.4}Pb{sub 0.6}P{sub 2}O{sub 15.2} parallel to the b-axis.« less
Authors:
 [1] ;  [2] ;  [3]
  1. Department of Chemical Engineering and Texas Materials Institute, University of Texas at Austin, 1 University Station C0400, Austin, TX 78712 (United States)
  2. Department of Chemistry and Biochemistry, University of Texas at Austin, Austin, TX 78712 (United States)
  3. Department of Chemical Engineering and Texas Materials Institute, University of Texas at Austin, 1 University Station C0400, Austin, TX 78712 (United States), E-mail: steinfink@che.utexas.edu
Publication Date:
OSTI Identifier:
21049499
Resource Type:
Journal Article
Resource Relation:
Journal Name: Journal of Solid State Chemistry; Journal Volume: 180; Journal Issue: 10; Other Information: DOI: 10.1016/j.jssc.2007.07.021; PII: S0022-4596(07)00282-4; Copyright (c) 2007 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved; Country of input: International Atomic Energy Agency (IAEA)
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; BISMUTH COMPOUNDS; BOND LENGTHS; LAYERS; LEAD IONS; LEAD PHOSPHATES; MONOCLINIC LATTICES; MONOCRYSTALS; OXYGEN IONS; STOICHIOMETRY; SYNTHESIS; X-RAY DIFFRACTION