A new layered bismuth tellurium oxychloride, Bi(3)Te(4)O(10)Cl(5) has been synthesized by a solid-state reaction under vacuum using Bi(2)O(3), TeO(2), and TeCl(4) as reagents. The structure of Bi(3)Te(4)O(10)Cl(5) has been determined by single-crystal X-ray diffraction. Bi(3)Te(4)O(10)Cl(5) contains two different lone pair cations, Bi(3+) and Te(4+) that are in asymmetric coordination environments. Bi(3)Te(4)O(10)Cl(5) has a novel two-dimensional layered structure consisting of distorted BiO(4)Cl(2) octahedra, BiO(4)Cl(3) polyhedra, TeO(4) polyhedra, and isolated Cl(-) ions. Complete structural analysis, infrared spectrum, thermogravimetric analysis, and dipole moment calculations are presented. Crystal data: Bi(3)Te(4)O(10)Cl(5), monoclinic, space group C2/m (No. 12), a = 15.372(3) A, b = 4.1004(7) A, c = 13.301(2) A, beta = 98.336(5) degrees, V = 829.5(2) A(3), and Z = 2.

A new highly symmetric layered lead chloride material, Cs(2)PbCl(2)(NO(3))(2) has been synthesized by a hydrothermal reaction method using Pb(NO(3))(2), CsCl, and water at 240 degrees C. The structure has been determined by single-crystal X-ray diffraction. Cs(2)PbCl(2)(NO(3))(2) has a novel two-dimensional layered structure containing PbO(4)Cl(4) polyhedra and NO(3) trigonal planes. Cs(2)PbCl(2)(NO(3))(2) is a novel variant on the layered perovskite theme, of which the structure is closely related to the n = 1 layered perovskite families. Detailed structural analysis, Infrared and UV-vis diffuse reflectance spectra, thermogravimetric analysis, and ion-exchange reactions of Cs(2)PbCl(2)(NO(3))(2) are reported. Crystal data: Cs(2)PbCl(2)(NO(3))(2), tetragonal, space group I4(1)/amd (No. 141), a = b = 5.6905(6) A, c = 32.946(5) A, V = 1066.9(2) A(3), and Z = 4.

Two new metal antimony oxychlorides, Sb(2)ZnO(3)Cl(2) and Sb(16)Cd(8)O(25)Cl(14), have been synthesized by solid-state reactions using Sb(2)O(3) and ZnCl(2) (or CdCl(2)) as reagents. The structures of Sb(2)ZnO(3)Cl(2) and Sb(16)Cd(8)O(25)Cl(14) have been determined by single-crystal X-ray diffraction. Both of the reported materials contain Sb(3+) cations that are in an asymmetric coordination environment attributable to their stereoactive lone pair. Sb(2)ZnO(3)Cl(2) has a novel two-dimensional layered structure consisting of distorted ZnO(2)Cl(2) tetrahedra and SbO(3) polyhedra. Sb(16)Cd(8)O(25)Cl(14) exhibits a one-dimensional structure consisting of Sb(3+)-Cd(2+)-oxide rods, Cd(2+)-chloride double chains, and isolated Cl(-) ions. Complete separation of the halophile and chalcophile moieties is observed from the reported materials. Detailed structural analysis, IR spectra, thermogravimetric analysis, ion-exchange reactions, and dipole moment calculations are presented. Crystal data: Sb(2)ZnO(3)Cl(2), orthorhombic, space group Pnma (No. 62), a = 17.124(4) A, b = 5.5598(12) A, c = 6.4823(14) A, V = 617.2(2) A(3), and Z = 4; Sb(16)Cd(8)O(25)Cl(14), monoclinic, space group I2/m (No. 12), a = 14.251(3) A, b = 3.9895(8) A, c = 21.145(4) A, beta = 97.35(3) degrees, V = 1192.3(4) A(3), and Z = 8.

Supporting Information. X-ray crystallographic file in CIF format, experimental and calculated powder XRD patterns, pore size distribution plot, powder XRD patterns showing the crystallization process, crystallographic description, and wire models for CAUMOF-8. This material is available free of charge via the Internet at http://pubs.acs.org.

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