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 luminescent Cd(Ⅱ) coordination polymer, [Cd(L)2(H2O)]n 1 (HL = xan-thene-9-carboxylic acid), was synthesized hydrothermally and characterized by satisfactory elemental analysis, FT-IR spectra and single-crystal X-ray diffraction. The crystal is of orthorhombic system, space group P212121 with a = 6.4548(4), b = 13.0876(12), c = 27.466(2), V = 2320.3(3)3, C28H20CdO7, Mr = 580.84, Z = 4, Dc = 1.663 g/cm3, F(000) = 1168, μ = 0.990 mm-1, Flack parameter = 0.00(2), the final R = 0.0296 and wR = 0.0691 for 5301 observed reflections (I 2σ(I)). 1 features a one-dimensional (1D) carboxylate oxygen-bridged inorganic chain, which is further connected by intermolecular hydrogen bonds into a three-dimensional (3D) framework. Moreover, compound 1 exhibits strong photoluminescence in the solid state at room temperature.
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.
One novel 1-D copper(Ⅱ)-organic compound,namely {[Cu2(PP)2(CBPC)]2·7H2O}n(1,H2CBPC=1-[(2'-carboxybiphenyl-4-yl)methyl]-2-propylimidazole-4-carboxylic acid,HPP=3-(2-pyridyl)pyrazole),was synthesized under hydrothermal conditions.X-ray diffraction analyses reveal that the two Cu(Ⅱ) ions in the distorted dimer [Cu2(PP)2] of 1 are linked by the carboxylate oxygen atoms on the phenyl and imidazole rings,respectively,forming one interesting snake-like chain.Single-crystal X-ray analyses reveal that it crystallizes in monoclinic,space group C2/c with a=30.656(8),b=12.715(3),c=22.405(5),β=122.758(3)°,V=7344(3)3,Z=4,Mr=1681.65,Dc=1.521 g/cm3,F(000)=3464,μ=1.221 mm-1,the final R=0.0453 and wR=0.1023 for 4617 observed reflections with Ⅰ 〉2σ(Ⅰ).
The solvothermal reaction of CuI with 5-amino-2-benzimidazolethiol in acetonitrile condition affords complex [Cuz(5-amino-2-benzimidazolethiol)2]2 which has been characterized by elemental analysis, infrared spectrum and single-crystal X-ray diffraction analysis. Crystal data for C28H24N12S4Cu4: monoclinic, space group C2/c with a = 15.970(5), b = 12.365(4), c = 16.293(5) A, fl = 91.977(6)°, V = 3215.5(18), Z = 4, Mr= 910.99, Dc= 1.882 g/cm3 , F(000) = 1824, p = 2.913 mm-1, λ(MoKa) = 0.71073A, T= 293(2) K, the final R = 0.0527 and wR = 0.1342. X-ray diffraction analysis revealed that the title complex exhibits a l D channel constructed from tetranuclear-copper(I) motifs connected by hydrogen bonds and shows strong photoluminescence in the solid state at room temperature.
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.
The title complex, [Cd(MeHbibzim)(1,4-bdc)]n (1, MelToibzim = 1-methyl-2,2'- bibenzimidazole, 1,4-bdc = terephthalate), was synthesized with hydrothermal reactions. The compound crystallizes in monoclinic, space group C2/c with a = 9.822(4), b = 18.510(7), c = 22.372(9) A, β = 98.359(6)°, C23H16CdN4O4, Mr = 524.81, V= 4024(3) A3, Z = 8, Dc. = 1.733 g/cm3, μ(MoKa) = 1.126 mm-1, F(000) = 2096, the final R = 0.0597 and wR = 0.1374 for 3906 observed reflections (1 〉 2σ(I)). X-ray diffraction analysis reveals that the Cd atom is coordinated by two nitrogen atoms from the chelating MeHbibzim and three carboxyl oxygen atoms from three terephthalate ligands, thus forming a distorted square pyramidal coordination sphere, [CdN2O3]. Every two Cd atoms are linked together via two carboxyl groups into a dinuclear unit with Cd...Cd separation of 3.806(4) A. The dinuclear building units are linked by terephthalate ligands into two-dimensional layers, which are further aggregated into a 3D framework via hydrogen bonding interactions.
Three novel inorganic-organic hybrid materials, [Cu(imi)2(H2O)(MoO4)]n 1, [Cuz(imi)3(MoO4)E]n.nH2O 2 and [Cu3(imi)2(OH)2(MoO4)2]n 3 (imi = imidazole), were synthesized and characterized by X-ray single-crystal structure determination. 1 crystallizes in orthorhombic, space group Pca21 with a = 13.382(4), b = 8.527(2), c = 9.622(3)A, V = 1098.0(5) A^3 Z = 4, C6H10CuMoN4O5, Mr = 377.66, Dc = 2.285 g/cm^3, F(000) = 740,μ(MoKa) = 3.095 mm^-1, the final R = 0.0256 and wR = 0.0722 for 1896 observed reflections with I 〉 2σ(I). 2 crystallizes in monoclinic, space group P2t/c with a= 11.170(2), b = 7.8244(15), c = 22.631(4)A, β = 115.790(7)°, V = 1780.9(6)A^3 Z = 4, C9H14Cu2Mo2N6O9, Mr = 669.24, Dc= 2.496 g/cm^3, F(000)=1295,μ(MoKa) = 3.792 mm^-1, the final R = 0.0225 and wR = 0.0615 for 3838 observed reflections with I 〉 2σ(I). 3 crystallizes in monoclinic, space group P21/c with a = 5.5599(19), b = 23.771(8), c = 7.3044(18)A , β = 129.356(16)°, V = 746.5(4)A^3, Z = 2, C6H10Cu3Mo2N4O10, Mr = 680.71, Dc = 3.029 g/cm^3, F(000) = 650,μ(MoKa) = 5.900 mm^-1, the final R = 0.0215 and wR = 0.0524 for 1620 observed reflections with I 〉 2σ(I).
The title compound, [Cu2(DMPz)2PMo12O40]·HDMPz (1, DMPz = 2,5-dimethyl pyrazine), has been synthesized and characterized by single-crystal X-ray diffraction analysis. It crystallizes in triclinic, space group P1 with a = 11.075(2), b = 11.551(2), c = 11.886(2) A.α = 106.352(2), β = 109.862(3), γ = 109.504(1)°, V = 1206.8(3) A3, C18H26CU2Mo12N6O40P, Mr = 2275.78, Z = 1, Dc = 3.131 g/cm3, μ = 4.011 mm^-1, F(000) = 1073, S = 1.066, the final R = 0.0389 and wR = 0.1056 for 3739 observed reflections with I 〉 2σ(I). The structural analysis indicates that the title compound is composed of Keggin clusters [PMo12O40]3- connected by one-dimensional [CB(DMPz)]2n^2n+ chains to form a two-dimensional grid layer with holes occupied by monoprotonated DMPz molecules. In the solid of the title compound, the 2D grid layers are stacked together in an ABAB packing mode.
The reactions of SbCl3 and HgCl2 with 2-(3-pyridyl)benzimidazole (PyBIm) in solution acidified with HCl have been investigated. The PyBIm ligands are protonated into 2-(3-pyridinio)benzimidazolium (H2PyBIm) cations and the corresponding metal ions are bonded with chloride atoms into coordination anions, forming two new coordination compounds, namely, (H2PyBIm)(SbCl5) 1 and (H2PyBIm)2(Hg2Cl8) 2. Both compounds were characterized by X-ray crystallography. Crystal data for 1: triclinic, space group P1^- with a = 5.7030(7), b = 9.0625(11), c = 16.5929(18) A, α = 91.808(7)°, β = 93.234(6), γ = 99.216(7)°, C12H11N3SbCl5, Mr = 496.24, V = 844.44(17) A^3, Z = 2, Dc = 1.952 g/cm^3, μ(MoKα) = 2.419 mm^-1, F(000) = 480, the final R = 0.0496 and wR = 0.1382 for 3433 observed reflections (I 〉 2σ(I)). Crystal data for 2: monoclinic, space group P21/c with a = 7.8061(5), b = 15.8127(9), c = 12.2435(9) , β = 91.955(4)o, C24H22N6Hg2Cl8, Mr = 1079.26, V = 1510.40(17) 3, Z = 2, Dc = 2.373 g/cm3, μ(MoKα) = 10.889 mm-1, F(000) = 1008, the final R = 0.0293 and wR = 0.0562 for 2854 observed reflections (I 〉 2σ(I)). X-ray diffraction analysis reveals that the antimony(III) is five-coordinated, exhibiting a slightly distorted square-pyramidal coordination geometry; while in 2, a dimeric [Hg2Cl8]^4-anion consists of two trigonal bipyramids sharing two common edges. The organic cations and coordination anions are connected into a one-dimensional belt and a two-dimensional sheet through N-H···Cl hydrogen bonding interactions in compounds 1 and 2, respectively; both are further aggregated into 3D frameworks by strong π-π contacts.