Two new organic-inorganic hybrid mono-transition-metal-substituted polyoxometalates Ni(2,2'-bipy)33Ni(H2O)SiW11O39·11H2O 1 and Cu(dien)(H2O)Cu(dien)(H2O)22-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) , β = 101.894(3)o, Dc = 2.563 mg/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) , β = 97.896(6)o, Dc = 4.036 mg/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 FTIR,elemental analysis and thermogravimetric analysis.Compound 1 crystallizes in the triclinic system,space group P,with a = 8.5095(4),b = 8.8694(4),c = 10.0756(4) ,α = 95.094(2),β = 96.936(2),γ = 116.844(2)°,V = 664.66(5) 3.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][α-H5PW11CoO40]·3H2O 1 and [Fe(2,2′-bipy)3]2[α-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 α-Keggin anion [α-H5PW11CoO40]2- and one isolated [Co(2,2′-bipy)3]2+ complex,while 2 is constructed from one α-Keggin anion [α-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) ,V = 7427(5) 3 and Z = 4;and those for 2:triclinic system,space group P,a = 13.787(3),b = 17.857(5),c = 18.918(5) ,α = 88.009(12),β = 72.768(10),γ = 74.935(10)o,V = 4291(2) 3 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),V=3374.3(3)3,C16H32Cu4I4N16,Mr=1210.34,Z=4,Dc=2.383 g/cm3,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),α=103.163(4),β=96.704(5),γ=101.981(6)o,V=3479(3)3,Z=2,C75H60Cu3N3P4,Mr=1317.76,Dc=1.258 g/cm3,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.
