Two new organic-inorganic hybrid mono-transition-metal-substituted polyoxometalates [Ni（2,2′-bipy）3]3[Ni（H2O）SiW11O39]·11H2O 1 and [Cu（dien）（H2O）][Cu（dien）（H2O）2]2- [CuSiW11O39]·5.5H2O 2 （2,2′-bipy = 2,2′-bipyridine, dien = diethylenetriamine） have been hydrothermally synthesized and characterized by single-crystal X-ray diffraction, elemental analysis, magnetic properties, and IR spectrum. Crystal data for 1： monoclinic, space group P21/n, a = 17.492（3）, b = 33.481（5）, c = 20.493（3）A^°, β = 101.894（3）°, Dc = 2.563 mg/A^°^3, F（000） = 8440, μ = 11.454 mm^-1 and Z = 4; and those for 2：monoclinic, space group P21/n, a = 11.114（3）, b = 22.803（7）, c = 22.468（7） A^°, β = 97.896（6）°, Dc = 4.036 mg/A^°^3, F（000） = 6140, μ = 23.942 mm^-1 and Z = 4. The study on the magnetic susceptibility of 2 demonstrates the presence of ferromagnetic interaction.
Two new quaternary sulfides,La3Sn0.25GeS71 and Sm3 Sn0.25GeS72,have been synthesized by a facile solid-state reaction,and their crystal structures were determined by singlecrystal X-ray diffraction analysis.The two compounds crystallize in the P6 3 space group,and the crystal data are as follows-La3Sn0.25GeS7：a=10.3335（7）,c=5.8455（7）,Z=2;Sm3Sn0.25GeS7：a=9.999（3）,c=5.787（2）,Z=2.Single-crystal analysis indicated that the two compounds consist of three types of building blocks：LnS 8 anti-tetragonal prism,SnS 6 octahedron,and GeS 4 tetrahedron.
A new borate [H2EG][B7O10（OH）3] （1） based on [B14O20（OH）6]4- polyborate anions has been solvothermally synthesized in the presence of H2EG as a template （EG = ethylene glycol）. The structure was determined by single-crystal X-ray diffraction and further characterized by FFIR, elemental analysis and thermogravimetric analysis. Compound 1 crystallizes in the triclinic system, space group Pi, with a = 8.5095（4）, b = 8.8694（4）, c = 10.0756（4） A, a = 95.094（2）, β = 96.936（2）, γ = 116.844（2）°, V = 664.66（5） A3. The structure of 1 consists of [B14O20（OH）6]4- moiety, which could be regarded as the largest isolated polyborate anion so far. The anions are interlinked via hydrogen bonding to form a 3D supramolecular network, whereas the diprotonated [H2EG]2＋ are filled in the free space of inorganic borate network and interact with the inorganic framework by extensive hydrogen bonds. It is noteworthy that the EG acts not only as a solvent, but also as a template.
Two new hybrid polyoxotungstates, [Co（2,2＇-bipy）3][a-H5PW11CoO40]-3H2O 1 and [Fe（2,2＇-bipy）3]2[a-HBW12O40]-2.5H2O 2 （2,2＇-bipy = 2,2＇-dipyridyl）, have been hydrothermally synthesized and characterized by IR, TGA and single-crystal X-ray structural analyses. The results of X-ray crystallography analyses exhibit that 1 consists of one a-Keggin anion [a-H5PW11CoO40]2- and one isolated [Co（2,2＇-bipy）3]2＋ complex, while 2 is constructed from one a-Keggin anion [a- HBW12O40]4- and two isolated [Fe（2,2＇-bipy）3]2＋ cations. The data for 1： orthorhombic system, space group Pbcn, a = 16.062（6）, b = 27.278（10）, c = 16.951（6）A, V = 7427（5）A3 and Z = 4; and those for 2： triclinic system, space group P1, a = 13.787（3）, b = 17.857（5）, c = 18.918（5）A, a = 88.009（12）, β = 72.768（10）, γ = 74.935（10）°, V = 4291（2）A3 and Z = 2.
The special role of magnesium atom in the polar intermetallics has been extensively investigated in recent yea...
Xiao-Wu Lei, Jiang-Gao Mao* State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002, PR China
The title compound,[Cu4I4（C4H8N4）4],has been synthesized and characterized by single-crystal X-ray diffraction analysis.It crystallizes in monoclinic,space group Pbca,with a=18.1851（10）,b=9.3697（5）,c=19.8034（10）A,V=3374.3（3）A^3,C16H32Cu4I4N16,Mr=1210.34,Z=4,Dc=2.383 g/cm^3,μ=6.183 mm^-1,F（000）=2272,S=1.032,the final R=0.0309 and wR=0.1180 for 3854 observer reflections（I〉2σ（I））.The structure of the title compound consists of tetranuclear copper cluster units bridged by the halogen atoms with the 3,5-dimethyl-4-aminotriazole ligands coordinated to the metal ions through the triazole nitrogen atoms.The luminescent property of 1 was also studied.
A new 3-D porous Gd-Cu heterometallic polymer [Gd2Cu3(bpy)2(ip)6]·6H2O (1) (bpy = 2,2'-bipyridine, H2ip = isophthalic acid) has been hydrothermally synthesized and structurally characterized. Compound 1 crystallizes in the triclinic space group P1and displays a 3-D non-interpenetrated α-Po network with 1-D channels filled transversely by the hexa-nuclear chain-like (H2O)6. The EPR and thermal stability of 1 were investigated.
Two new polyoxomolybdate compounds,namely CuII2（HL）3]2[Mo8O26]·（H2O）4（1） and [NiII（HL）3]2（Mo8O26）·（H2O）3（2）（HL = 3-（2-pyridyl）pyrazole）,were designed and synthesized under hydrothermal conditions.X-ray diffraction analyses reveal that compound 1 consists of one β-Mo8O264-cluster and a Cu2 dimer which is built from two Cu（II） ions linked by three 3-（2-pyridyl）pyrazole ligands.Compound 2 is generated by two kinds of polyoxomolybdate clusters of α-[Mo8O26]4-and β-[Mo8O26]4-.In complexes 1 and 2,the multi-dimensional frameworks are con-structed with the help of hydrogen-bonding links between the terminaloxygen atoms of [Mo8O26]4-,water molecules,and 3-（2-pyridyl）pyrazole ligands.Crystal data of 1：C24H25Cu2Mo4N9O15,Mr = 1190.37,monoclinic,space group P21/c,a = 10.850（2）,b = 18.510（4）,c = 17.230（3） ,β = 100.57（3）°,V = 3401.6（12） 3,Z = 4,Dc = 2.324 g/cm3,F（000） = 2312,μ = 2.742 mm-1,R = 0.0302 and wR = 0.0775（Ⅰ 〉 2σ（Ⅰ））;Crystal data for 2：C48H48Mo8N18Ni2O29,Mr = 2225.98,monoclinic,space group P21/n,a = 20.799（2）,b = 14.7970（13）,c = 23.141（2） ,β = 91.6180（10）°,V = 7119.0（11） 3,Z = 4,Dc = 2.077 g/cm3,F（000） = 4344,μ = 1.968 mm-1,R = 0.0309 and wR = 0.0696（Ⅰ〉 2σ（Ⅰ））.
A novel compound, {[Y（HPIDC）（OX）1/2（H2O）]·2H2O}n （1, H3PIDC = 2-（pyridin-4- yl）-1H-imidazole-4,5-dicarboxylic acid, H2OX = oxalic acid）, has been synthesized under hydrothermal conditions and characterized by thermal analysis （TGA）, powder X-ray diffraction （PXRD）, and single-crystal X-ray diffraction. Complex 1 crystallizes in monoclinic space group P21/c with a = 8.342（8）, b = 14.61（1）, c = 11.487（1）, β = 90.78（9）°, V = 1400.4（2）3, Z = 4, C11H11N3O9Y, Mr = 418.14, Dc = 1.983 g/cm3, F（000） = 836, Rint = 0.0509, T = 293（2） K, μ = 4.240 mm-1, the final R = 0.0477 and wR = 0.1125 for 2770 observed reflections with I 2σ（I）. Compound 1 exhibits a 3D framework and generates the 1D open channels filled with free water molecules. The structure of 1 can be rationalized as a diamondoid network when the atom yttrium is regarded as a 4-connected node linking four surrounding yttrium atoms. The luminescent property of compound 1 is also investigated.
A new wave-like infinite chain coordination polymer [Cu3（CN）3（PPh3）4]n（1,PPh3=triphenylphosphine） has been synthesized by solution reaction and characterized by X-ray single-crystal structure diffraction analysis.The complex crystallizes in space group P1 with a=13.343（6）,b=13.429（7）,c=20.694（10）A,α=103.163（4）,β=96.704（5）,γ=101.981（6）o,V=3479（3）A^3,Z=2,C75H60Cu3N3P4,Mr=1317.76,Dc=1.258 g/cm^3,F（000）=1356,μ=1.043 mm^-1,the final R=0.0680 and wR=0.1305 for 9232 observed reflections with I〉2σ（I）.The infinite chain is linked by C-H…π H bonding interactions to form a 2-D supramolecular network.Luminescent study reveals that the complex has green-light emission.
