Hydrothermal Synthesis,Crystal Structure and Luminescent Property of a Cd(Ⅱ) Compound with(4,6)-Connected Topology

A new Cd(Ⅱ) coordination polymer, namely {Cd_2(L)(biimpy)(H_2O)}_n(1, H4 L = 3-(3?,5?-dicarboxylphenoxy)phthalic acid, biimpy = 2,6-bis(1-imdazoly)pyridine), has been successfully synthesized via the hydrothermal reactions of Cd(Ⅱ) ions, H_4L and biimpy. The crystal structure is of triclinic, space group P1 with a = 7.7874(5), b = 9.9716(5), c = 18.5278(6) ?, α = 91.327(4), β = 96.689(4), γ = 111.896(5)o, V = 1322.39(12) ?~3, C_(27)H_(17)Cd_2N_5O_(10), M_r = 796.26, Z = 2,D_c = 2.000 g/cm~3, F(000) = 780, μ = 1.679 mm~(-1), R = 0.0345 and wR = 0.0767 for 3890 observed reflections(I 2s(I)). Single-crystal X-ray structural analysis reveals that compound 1 features a three-dimensional(3D) framework based on two different dinuclear [Cd_2(COO)_2] building subunits, and topological analysis shows that it can be simplified into a binodal(4,6)-connected topological network with the point symbol of {3.4~2.5~2.6}{3~2.4~2.5~2.6~4.7~4.8}. Moreover, the thermal stability and luminescent property of compound 1 were also studied.     

Synthesis,Crystal Structure and Photoluminescent Property of a Novel Dy~(3+) Coordination Compound Containing Rare(H_2O)_(22) Clusters

A novel Dy~(3+) coordination compound,(H_2pipz)(H_3O)[Dy(pydc)_3]·11H_2O(1,pipz = piperazine and H_2pydc = pyridine-2,6-dicarboxylic acid),has been hydrothermally synthesized and characterized by X-ray single-crystal diffraction,elemental analysis. It is interesting that the packing structure of compound 1 contains 22-core water clusters. Compound 1 is extended into a threedimensional supramolecular structure via O···H···O hydrogen bonding interactions. Furthermore,the luminescent property of compound 1 was also investigated.     

A New Vanadium Phosphate Incorporating Copper-organonitrogen Ligand: Synthesis,Crystal Structure and Electrochemical Property

A new phosphovanadate metal-organic complex Cu(mbpy)(VO_2)(PO_4)(1, mbpy = 5,5?-dimethyl-2,2?-dipyridyl) has been hydrothermally synthesized and structurally characterized. Single-crystal structure analysis reveals that compound 1 crystallizes in the monoclinic space group P21/c with a = 7.6640(4), b = 18.8832(10), c = 10.1893(5) ?, β = 94.782(1)o, V = 1469.47(13) ?3, Z = 4, Mr = 425.69, Dc = 1.924 g/cm~3, F(000) = 852, μ(Mo Kα) = 2.224 mm-1, R = 0.0291 and w R = 0.0980. The crystal structure of 1 features a one-dimensional framework constructed by inorganic {Cu(VO_2)(PO_4)}∞ neutral chain and organic mbpy ligands. The electrochemical property of compound 1 modified carbon paste electrode has also been investigated.     

Synthesis,Crystal Structure and Gas Adsorption of a Two-fold Interpenetrated Three-dimensional Framework {[Cd(2-NO_2-BDC)(4,4?-DPA)]·(DMF)}_n

The reaction of Cd(NO_3)_2·4H_2O with 4,4?-dipyridylacetylene(4,4?-DPA) and 2-nitroterephthalic acid(2-NO_2-H_2BDC) in DMF/H_2O mixed solvent has afforded a compound {[Cd(2-NO_2-BDC)(4,4?-DPA)]·(DMF)}_n(1). Compound 1 has been characterized by single-crystal X-ray diffraction, powder X-ray diffraction, thermogravimetry analysis, and IR spectrum. Compound 1 crystallizes in the monoclinic system, space group P21/n, with a = 12.1488(3), b = 14.6689(3), c = 13.1615(3) ?, β = 111.809(3)o, V = 2177.63(9) ?~3, Z = 4, C_(23)H_(18)N_4O_7 Cd, M_r = 574.81, D_c = 1.753 g/cm~3, μ = 8.523 mm~(-1), F(000) = 1152, the final R = 0.0411 and wR = 0.1064 for 3589 observed reflections with I 2s(I). In compound 1, the Cd(Ⅱ) ions are linked by the carboxylate groups of 2-NO_2-BDC ligands to give a two-dimensional layered structure based on the centrosymmetric dinuclear Cd_2(COO)_2 units, which are further connected by the 4,4?-DPA ligands to produce a three-dimensional framework with pcu topology. Careful examination revealed that compound 1 is a 2-fold interpenetrating framework. Furthermore, the gas adsorption properties of 1 for N_2 and CO_2 have also been investigated.     

A Zn(Ⅱ) Coordination Polymer Based on a Flexible Symmetric Multicarboxylate Ligand

A novel coordination polymer, namely [Zn_2(CAPA)(DMA)(H_2O)]_(2n)·n(H_2O)(1,H_4CAPA = 5-(bis(4-carboxybenzyl) amino) isophthalic acid, DMA = N,N-dimethylacetamide) has been synthesized through a solvothermal method and characterized by single-crystal X-ray diffraction, elemental analysis, infrared spectra, and thermogravimetric analyses. The crystal structure is of monoclinic, space group P21/n with a = 8.0585(5), b = 18.9733(10), c = 20.2044(14) ?, β = 101.144(7)o, V = 3030.9(3) ?~3, C_(56)H_(54)Zn_4N_4O_(21), M_r = 1378.58, Z = 2). The compound forms a three-dimensional(3D) supramolecular framework by linking adjacent layers via hydrogen bonds and π···π interactions. It is interesting that the crystal structure is much related to the flexibility and configuration of the ligand. In addition, the thermal stability and luminescence properties for the compound have also been investigated.     

Syntheses,Structures and Luminescent Properties of the Cadmium(Ⅱ) Complex with 3,3?-Thiodipropionic Acid

One new luminescent material of complex {[Cd(DPA)(H_2O)_2]·(H_2O)_2}_n(1) was synthesized by evaporation methods using 3,3?-thiodipropionic acid(DPA) and cadmium nitrate as the starting materials. Compound 1 crystallizes in the monoclinic system,space group P2_1/n with a = 7.5460(7),b = 13.372(3),c = 12.304(3) ?,β = 95.95(3)o,V = 1234.8(4) ?~3,D_c = 1.940 g/cm~3,C_6H_(16)O_8 SCd,M_r = 360.65,F(000) = 720,μ(Mo Ka) = 1.960 mm~(-1),Z = 4,R = 0.0460 and wR = 0.1185 for 1835 observed reflections(I 2σ(I)),and R = 0.0591,wR = 0.1245 for all data. The complex has been characterized by elemental analysis,FT-IR,TG,PXRD and X-ray single-crystal structure analysis and the fluorescence property has also been studied. As a result,complex 1 possesses a two-dimensional(2-D) structure through DPA ligands interconnecting Cd2+ ions. Complex 1 emits the intense fluorescence of 420 nm in the solid state at room temperature.     

A Zn(Ⅱ) Coordination Polymer with 4-Connected bbf Topology: Synthesis,Crystal Structure and Luminescent Property

A new Zn(Ⅱ) compound, namely {Zn(BTA)(pdc)_(0.5)}_n(1, HBTA = 1,2,3-benzotriazole, H_2pdc = terephthalic acid), has been hydrothermally synthesized and characterized by elemental analysis, infrared analysis, powder X-ray diffraction analysis and single-crystal X-ray structural analysis. The crystal structure is of monoclinic system, space group P21/c with a = 10.751(3), b = 9.792(3), c = 9.292(3) ?, β = 95.391(4)°, V = 973.9(5) ?3, C10H6N3O2 Zn, Mr = 265.57, Z = 4, Dc = 1.811 g/cm3, F(000) = 532, μ = 2.506 mm-1, R = 0.0221 and w R = 0.0605 for 2075 observed reflections(I 2s(I)). Single-crystal X-ray structural analysis reveals that compound 1 features a three-dimensional(3D) framework with 4-connected bbf topology. Moreover, the thermogravimetric(TG) analysis and photoluminescent property of 1 were also discussed.     

Solvothermal Synthesis,Crystal Structure and Characterizations of a Novel 2D Organic Decorated Manganese Thiostannate:MnSnS3(1,2-DACH)

A novel 1,2-diaminocyclohexane(1,2-DACH) decorated manganese thiostannate,namely MnSnS_3(1,2-DACH)(1),has been solvothermally synthesized by the reaction of Mn(CH_3COO)_2·4H_2O,Sn and S in the stoichiometric ratio in 1,2-DACH,which acted as an efficient structure-directing agent(SDA) and reactive solvent in the formation of the title compound. Single-crystal X-ray diffraction studies revealed that the title compound crystallizes in the monoclinic space group P2_1/c with a = 12.2458(7),b = 13.8588(7),c = 7.2292(4) ?,β = 99.460(6)°,V = 1210.20(12) ?~3,Z = 4,Dc = 2.108 g·cm~(-3),F(000) = 748,μ = 3.584 mm~(-1),R = 0.0348 and wR = 0.0823(I 2σ(I)). The structure features a neutral two-dimensional(2D) network constructed by the unsaturated [Mn(1,2-DACH)] complexes interconnecting [SnS_3]_n~(2n-) chains via sharing S. Thermal stability and optical property of compound 1 were characterized.     

Synthesis,Crystal Structure and Flame Retardance of 2-(3-Silatranylpropylamino)-4-phenyl-5,5-dimethyl-1,3,2-dioxaphosphorinane-2-oxide

The title compound, 2-(3-silatranylpropylamino)-4-dichlorophenyl-5,5-dimethyl-1,3,2-dioxaphosphorinane-2-oxide(2(C_(20)H_(33)N_2O_6Psi)·C_2H_6O·CH_4O, Mr = 991.20), has been synthesized by the nucleophilic substitution reaction of 2-chloro-4-phenyl-5,5-dimethyl-1,3,2-dioxaphosphorinane-2-oxide with γ-aminopropylsilatrane, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1 with a = 10.3783(15), b = 11.2402(17), c = 12.1675(18) ?, a = 70.653(4), b = 82.908(4), g = 85.690(4)°, V = 1328.1(3) ?3, Z = 1, Dc = 1.239 g/cm~3, μ = 0.19 mm~(-1), F(000) = 532, the final R = 0.0640 and wR = 0.2090 for 3615 observed reflections with I 2s(I). The cyclic dioxaphosphorinane ring in the molecule adopts a thermodynamically stable cis conformation, while the silatrane fragment forms a cage-like structure in which there exists an intramolecular Si?N donor-acceptor bond. In the crystal structure, centrosymmetrically related molecules are linked by pairs of N–H···O hydrogen bonds into dimers, generating rings with graph-set motif R22(8). Furthermore, a couple of O(7)–H(10)···O(3) hydrogen bonds were formed by O atom of P=O and H atom from hydroxyl in the solvent ethanol. Thermal property of the compound was also studied by means of thermogravimetry(TGA). The thermal analysis and preliminary fireproofing test show that the title compound has good flame retardance.     

Synthesis,Structure and Magnetic Property of a New Three-dimensional Copper(Ⅱ) Coordination Polymer Constructed from 5-Tert-butyl Isophthalic Acid and N-donor Ligand

A new 3D copper(Ⅱ) coordination polymer, {[Cu_2(tbip)_2(1,3,5-tib)]×2H_2O}n(1, H_2 tbip = 5-tert-butyl isophthalic acid, 1,3,5-tib = 1,3,5-tris(1-imidazolyl)benzene), has been synthesized by hydrothermal reaction of Cu(OAc)_2·4H_2O, H_2 tbip and 1,3,5-tib. It has been structurally characterized by element analysis, IR and magnetic measurement. X-ray single-crystal analysis was carried out for 1, which crystallizes in the triclinic system, space group P1 with a = 7.822(3), b = 15.854(6), c = 17.553(6) ?, a = 113.033(4), β = 90.694(4), g = 101.006(4)°, V = 1957.3(12) ?~3, Z = 1, D_c = 1.493 g/cm~3, M_r = 1759.70, F(000) = 908, R = 0.0721 and w R = 0.1978 with I 2s(I). The single-crystal X-ray diffraction studies reveal that compound 1 exhibits 2D [Cu(tbip)] layers which are further pillared by 1,3,5-tib ancillary ligand with terminal tridentate coordination mode to generate the final 3D structure. Magnetic susceptibility data for 1 have been measured in the range of 2~300 K. There are antiferromagnetic interactions between copper ions of the compound.     

A New Cd(Ⅱ) Coordination Polymer Constructed by 3-(2-Pyridyl)pyrazole and 5-Nitroisophthalic Acid:Synthesis,Crystal Structure and Theoretical Calculations

A new coordination polymer, [Cd_2(NIPH)(L)_2(H_2O)]n(1, HL = 3-(2-pyridyl)pyrazole and H_2NIPH = 5-nitroisophthalic acid), has been synthesized. The structure of complex 1 has been characterized by X-ray single-crystal diffraction, elemental analysis, IR spectrum analysis, thermogravimetric analysis and fluorescence spectrum analysis. Complex 1 belongs to the triclinic system, space group P1 with a = 8.9539(6), b = 11.6252(8), c = 12.2472(8) ?, α = 80.011(2), β = 80.3850(10), γ = 86.773(2)°, V = 1237.37(14) ?~3, Z = 2, D_c = 1.987 g/cm~3, μ = 1.780 mm~(-1), M_r = 740.25, F(000) = 724, the final R = 0.0295 and wR = 0.1015 with I 2σ(I). Two H_2NIPH as monodentate and bidentate ligands and two L ligands link four Cd(Ⅱ) ions to form a tetranuclear subunit. Each pair of the tetranuclear subunits is bridged by NIPH ligands to yield a one-dimensional double-chain structure. Furthermore, the 1D chains are linked into a 3D supramolecular framework with hydrogen bonds and π-π interactions. In addition, we analyzed Natural Bond Orbital(NBO) in using the PBE0/LANL2DZ method built in Gaussian 03 Program. The calculation results indicated the obvious covalent interaction between the coordinated atoms and Cd(Ⅱ) ion.     

An 8-Connected Chiral Lanthanide Metal-organic Framework Constructed from Naturally Camphoric Acid:Crystal Structure,Vibrational Circular Dichroism Spectroscopy and Second-order Nonlinear Optical Effect

A chiral lanthanide metal-organic framework based on enantiopure camphoric acid(D-H_2cam), [Nd_3(D-cam)8(H_2O)_4Cl]_n(1), has been synthesized and characterized by single-crystal X-ray structural analysis, elemental analysis, IR, thermal gravimetric, and X-ray powder diffraction. Crystal data for the title compound are as follows: orthorhombic system, space group P212121 with a = 13.8287(7), b = 14.0715(7), c = 25.7403(12) ?, V = 5008.8(4) ?3, M_r = 1333.08, Z = 4, F(000) = 2644, D_c = 1.768 g/cm3, μ(MoKα) = 3.189 mm-1, the final R = 0.0351 and w R = 0.0814(I 2σ(I)). Compound 1 displays an 8-connected bcu topology 3D framework and hydrogen-bonding interactions stabilize the solid-state structure. The vibrational circular dichroism(VCD) spectrum and second-order nonlinear optical effect of compound 1 have been studied in the solid state.     

Synthesis,Crystal Structure and Characterization of a Nickel Complex Based on Phenoxyimine Ligand and Catalysis of the Vinyl Polymerization of Norbornene

The title complex N,O-bis{2-[[(2-benzhydryl-4,6-dimethylphenyl)imino]-methyl]-phenol}-nickel(II)(C_(56)H_(48)N_2NiO_2) has been synthesized by the reaction of 2-[[(2-benzhydryl-4,6-dimethylphenyl)mino]-methyl]-phenol with Ni(CH_3COO)_2·4 H_2O, and characterized by elemental analysis and IR spectrum. The spatial structure of the complex has been confirmed by single-crystal X-ray diffraction analysis. The compound belongs to the monoclinic system, space group C2/c with a = 39.035(8), b = 13.276(3), c = 17.679(4) ?, β = 98.06(3)°, V = 9071(3) ?~3, C_(56)H_(48)N_2NiO_2, M_r = 839.67, Z = 8, D_c = 1.230 Mg/m~3, μ = 0.472 mm~(-1), F(000) = 3536, T = 293(2) K, the final R = 0.0675 and w R = 0.1345(I 2s(I)). The compound showed excellent catalytic activity up to 1.268 × 10~7 g of PNB(mol of Ni)~(-1)h~(-1) for the addition polymerization of norbornene by using methylaluminoxane(MAO) as a cocatalyst.     

Synthesis,Structure, Photoluminescence and Photocatalytic Properties of a New Cd(Ⅱ) Metal-organic Framework Based on 1,4-Di(2,6-dimethyl-3,5-dicarboxypyridyl)benzene

A new 3D coordination polymer, [Cd_2(L)(bpb)_2]_n(1, H_4L = 1,4-di(2,6-dimethyl-3,5-dicarboxypyridyl) benzene, bpb = 1,4-bis(4-pyridyl) benzene, has been hydrothermally synthesized and characterized by single-crystal X-ray diffraction analysis, elemental analysis, TGA, IR spectroscopy and UV-Vis spectrum. Complex 1 crystallizes in orthorhombic, space group C2221, with a = 10.9393(12), b = 20.900(3), c = 20.027(2) ?, β = 90°, V = 4578.9(9) ?~3, Dc = 41.668 Mg/cm~3, M_r = 1149.74, F(000) = 2312.0, μ = 0.996 mm~(–1), Z = 4, the final R = 0.0316 and wR = 0.0786 for 4271 observed reflections with I 2σ(I). Structural analysis shows that 1 possesses a 3D network based on the 2D layer bridged by L~4-ligands, while the 2D layers are composed of the adjacent 1D chains joined by L~4-ligand. The photoluminescent investigation indicates that one broad emission band with the maximum of 445 nm can be observed in 1. Moreover, compound 1 has high photocatalytic degradation effects on methylene blue under UV irradiation.     

Synthesis,Crystal Structure and Luminescent Property of a New Copper(Ⅰ) Iodide Complex Based on 3,5-Dimethyl-4-amino-triazole

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(I2σ(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.     

Synthesis,Structure and Electric Property of a 3D Supramolecular Co~Ⅱ Coordination Complex

The title compound, [Co(C_(16)H_(10)N_2S_4)_2(H_2O)_4](C_(14)H_9N_2O_4)2(1,C_(16)H_(10)N_2S_4=4-pyridine-tetrathiafulvalene-4-pyridine and C14 H9 N2 O4 = 4-(4-carboxyphenyl)diazenyl)benzoate),has been successfully synthesized under hydrothermal conditions. The structure was determined by elemental analyses and single-crystal X-ray diffraction analysis. Moreover, the conductivity property of compound 1 was investigated. Compound 1 crystallizes in triclinic system, space group P1 with a = 6.4006(3), b = 7.1818(4), c = 33.0932(14) ?, α = 89.261(4), β = 86.530(3), γ = 66.642(4)°, V =1393.90(12) ?3, Z = 1, C60 H46 N8 O12 S8 Co, M3 r = 1386.46, Dc = 1.652 g/cm, μ = 0.684 mm-1 and F(000) = 713. The final R = 0.0411 and wR = 0.0810 for 3936 observed reflections with I 2σ(I).Compound 1 contains one-half of the complex cation with the CoI I ion located on an inversion center,and one 4-(4-carboxyphenyl)diazenyl)benzoate counter anion. The Co atom has a N2 O4 octahedral coordination. Complex 1 forms a three-dimensional supramolecular network and a semiconducting behavior is observed with srt= 0.04 S·cm-1.     

Hydrothermal Synthesis and Crystal Structure of a Zinc(Ⅱ) Polymer with a Two-dimensional Layer Structure: [Zn(pzdc)(phen)] n·nH_2O

A metal-organic coordination compound formulated as [Zn(pzdc)(phen)] n·nH_2O 1 (H_2pzdc=pyrazine-2,3-dicarboxylic acid,phen=1,10-phenanthroline) has been hydrothermally synthesized and structurally characterized by elemental analysis,IR,fluorescence spectrum and single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system,space group P2_(1/n) with α=11.607(2),b=11.719(2),c=13.140(3)(A),β=110.707(3)°,V=1671.9(6)(A)~3,C_(18)H_(12)ZnN_4O_5,Mr=429.69,D_c=1.707 g/cm~3,μ(MoKα)=1.511 mm~(-1),F(000)=872,Z=4,the final R=0.0356 and wR=0.0853 for 2713 observed reflections (Ⅰ> 2σ(Ⅰ). It exhibits an interesting two-dimensional layer structure and shows yellow photoluminescent property at room temperature.     

Synthesis,Structures, and Fluorescence Property of a Novel Heterometallic Complex Constructed by Imidazole

A novel heterometallic complex constructed by imidazole ligand, CoZn(C_3N_2H_3)_4(1), has been synthesized under hydrothermal conditions. Compound 1 was characterized by IR spectra, thermal analysis, powder X-ray diffraction and single-crystal X-ray diffraction. Single-crystal X-ray diffraction studies reveals that compound 1 is in the tetragonal system, space group I4_1cd with a = 23.4371(5), b = 23.4371(5), c = 12.4430(7) ?, V = 6834.9(4) ?~3, Z = 16, C_(12)H_(12)CoN_8Zn, M_r = 392.60, D_c = 1.526 g/cm~3, F(000) = 3152, μ = 2.381 mm~(–1), R = 0.0323 and w R = 0.0789. The CoZn(C_3N_2H_3)_4 is one-dimensional heterometallic molecular chains, which are further extended into a 3D open framework. Moreover, the solid-state fluorescence property of the complex has also been investigated at room temperature.     

A Carboxylate-bridged Co(Ⅱ) Layer Complex: Synthesis,Structure and Magnetic Property

A 2D coordination polymer, [Co(NPA)(H_2 O)_2]_n(1, H_2 NPA = 3-nitrophthalic acid), has been synthesized by solvothermal method and characterized by single-crystal X-ray diffraction analysis, FT-IR spectroscopy, elemental analysis, thermogravimetric analysis and powder X-ray diffraction. Complex 1 crystallizes in orthorhombic space group Pbca with a = 7.2261(2), b = 14.6450(5), c = 19.6671(7) ?, V = 2081.31(11) ?~3, Z = 8, C_8 H_7 CoNO_8, M_r = 304.08, D_c = 1.941 mg/m~3, μ = 1.686 mm~(-1), S = 1.054, F(000) = 1224, the final R = 0.0248 and wR = 0.0603 for 1834 observed reflections(I 2σ(I)). The crystal structural analysis demonstrates that the Co(Ⅱ) ions in 1 are linked by single and double μ_2-1,3-bridging carboxylate bridges, forming a 2D layer structure. Moreover, magnetic property of 1 was also discussed.