ABSTRACT A new lanthanumm-ironm complex [La(DMSO)5(H2O)](μ-CN)2[Fe(CN)4]·H2O 1 (DMSO = dimethylsulfoxide) has been prepared by a facile approach, ball-milling method, and characterized by X-ray diffraction. The crystal belongs to monoclinic, space group P21/n with a = 9.7125(3), b = 21.5336(7), c = 14.3804(5)A, β = 93.242(3)°, C16H34FeLaN60O7S5, Mr= 777.55, V = 3002.8(2)A^3, Z = 4, Dc = 1.720 g/cm^3, S = 1.053, μ(MoKα) = 2.278 mm^-1, F(000) = 1564, R = 0.0490 and ωR = 0.1270. The crystal structure analysis of 1 reveals a slightly distorted squareantiprism eighffold-coordinated La(Ⅲ) ion and a 1-D zigzag chain structure extending through the Fe-CN-La-NC-Fe linkages. The [La(DMSO)5(H2O)](μ-CN)2[Fe(CN)4] species are held together via hydrogen bonds to form a three-dimensional framework.
Two new quaternary sulfides, KSmSiS4 (1) and KYbSiS4 (2), have been synthesized by high-temperature solid-state reaction. Single,crystal X-ray diffraction analyses indicate that both compounds crystallize in the space group P21/m, and the crystal data are as follows: a = 6.426(11), b = 6.582(11), c = 8.602(15)A, β= 107.90(13)°, Z = 2, V= 346.2(10) A^3, Dc = 3.317 g/cm^3, F(000) = 318,μ(MoKα) = 10.334 mm^-1, the final R = 0.0559 and wR = 0.1370 for 1; and α= 6.3244(10), b = 6.5552(10), c = 8.5701(15)A, β= 108.001(13)°, Z = 2, V = 337.91(9) A^3, De= 3.621 g/cm^3, F(000) = 334, μ(MoKα) = 15.737 mm^-1, the final R = 0.0422 and wR = 0.0960 for 2. The KLnSiS4 (Ln = Sm, Yb) structure consists of corrugated ∞^2 [LnSiS4]^- layers which are formed by edge-sharing LnS8 bicapped trigonal prisms and SiS4 tetrahedra. The K^+ cations are located in the cavities defined by S2 anions between the ∞^2[LnSiS4]^- layers. Band-gap analyses show that compounds 1 and 2 are semiconductors with optical band-gaps of 2.40 and 2.34 eV, respectively.
Two novel lanthanide-organic polymers [Er2(pdc)2(o-bdc)(H2O)2]·H2O(1,H2pdc = 2,6-pyridinedicarboxylic acid,o-H2bdc = 1,2-benzenedicarboxylic acid) and Er(Himdc)(mbdc)0.5(H2O)(2,H3imdc = 4,5-imidazoledicarboxylic acid,m-H2bdc = 1,3-benzenedicarboxylic acid) have been synthesized and characterized by elemental analysis,IR,thermogravimetric analysis and X-ray single-crystal diffraction studies.1 crystallizes in monoclinic,space group P21/c,while 2 in the orthorhombic space group Pbcn.Both compounds 1 and 2 display two-dimensional network structures. For 1, the tetranuclear parallelogram {Era} cluster as a building block is further assembled into a wonderful 2D grid, and the layers are interconnected via hydrogen bonds and π-π stacking interactions to yield a 3D supramolecular architecture; for 2, its configuration is a rare double-decker structure. These two complexes represent good examples for using mixcarboxylate-containing ligands to construct diverse 2D lanthanide coordination polymers.
One new sandwich-type tetra-nickel substituted polyoxotungsate,[Ni(trien)]4-[Ni4(H2O)2(HPW9O34)2]·4H2O(1,trien=triethylenetetramine),has been hydrothermally synthesized and characterized by IR,elemental analysis,TGA,and single-crystal X-ray diffraction analysis.Crystal data for 1:triclinic,space group P with a=13.279(3),b=13.816(3),c=14.494(4),α=95.403(1),β=113.173(4),γ=93.809(3)o,V=2418.0(10)3,Z=1 and Dc=3.861 g/cm3.X-ray crystallographic study shows that compound 1 is a relatively rare inorganic-organic hybrid polyoxo tungstate constructed from sandwich Ni-substituted polyoxo-anions and nickel complexes.
A new polar intermetallic compound, Eu3Sn5, has been synthesized by solid-state reaction of the corresponding pure elements in a stoicbiometric ratio in a welded tantalum tube at high temperature. Its crystal structure was established by single-crystal X-ray diffraction. EuaSn5 crystallizes in orthorhombic, space group Cmcm with a = 10.466(11), b = 8,445(8), c = 10.662(12)/k, V = 942.4(17)A^3, Z = 4, Mr = 1049.33, De= 7.396 g/cm^3, ,μ = 32.578 mm^-1, F(000) = 1756, the final R = 0.0236 and wR = 0.0472 for 535 observed reflections with I 〉 2σ(I). Its structure belongs to the modified Pu3Pd5 type. It is isostructural with SraSn5 and Ba3Sn5, featuring [Sn5] square pyramidal clusters described as “arachno” according to the Wade-Mingos electron counting rules. The europium cations are located at the voids between the square pyramidal clusters. Results of the extended Htickel band structure calculations indicate that Eu3Sn5 is metallic.
A new compound, (H3O)3{Na3(H2O)13(Cu(Gly)2)2(H2W12O42)}·11H2O (1), has been synthesized and structurally characterized, which represents the first example of a polyoxotungstate-surface being decorated with amino acid ligand. Two cis-{Cu(Gly)2}2+ engraft into the (H2W12O42)10- with Cu-O bond of 0.241 2(7) nm, and Na+ ions linked these (Cu(Gly)2)2(H2W12O42)6- clusters into a one-dimensional chain. CCDC: 278000.
Hai-Long Jiang, Jiang-Gao Mao* State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002