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.
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 Cu2(5-amino-2-benzimidazolethiol)22 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), β = 91.977(6)°, V = 3215.5(18), Z = 4, Mr = 910.99, Dc = 1.882 g/cm3 , F(000) = 1824, μ = 2.913 mm-1 , λ(MoKα) = 0.71073 , T = 293(2) K, the final R = 0.0527 and wR = 0.1342. X-ray diffraction analysis revealed that the title complex exhibits a 1D channel constructed from tetranuclear-copper(Ⅰ) motifs connected by hydrogen bonds and shows strong photoluminescence in the solid state at room temperature.
The title complex, Cd(MeHbibzim)(1,4-bdc)n (1, MeHbibzim = 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), β = 98.359(6)°, C23H16CdN4O4 , Mr = 524.81, V = 4024(3)3 , Z = 8, Dc = 1.733 g/cm3 , μ(MoKα) = 1.126 mm-1 , F(000) = 2096, the final R = 0.0597 and wR = 0.1374 for 3906 observed reflections (Ⅰ > 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). 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.
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) , α = 91.808(7), β = 93.234(6), γ = 99.216(7)o, C12H11N3SbCl5, Mr = 496.24, V = 844.44(17) 3, Z = 2, Dc = 1.952 g/cm3, 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.
