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.     

Crystal Structure and Luminescent Properties of a 3D Cd(Ⅱ) Compound Constructed from Succinate and 3,6-Di(4-pyridyl)pyridazine

A three-dimensional(3D) coordination polymer,[Cd(SC)(DPPD)]_n(1,H_2SC = succinic acid and DPPD = 3,6-di(4-pyridyl)pyridazine),has been synthesized by the solvothermal reaction of Cd(NO_3)_2·4H_2O with H_2 SC and DPPD at 120 oC in DMF solvent. Compound 1 crystallizes in the monoclinic system,space group P2_1/c,with a = 10.7993(4),b = 11.7705(3),c = 13.5336(6) ?,V = 1678.89(11) ?~3,Z = 4,C18H14N4O_4 Cd,M_r = 462.73,D_c = 1.831 g/cm~3,μ = 1.335 mm~(-1),F(000) = 920.0,the final R = 0.0500 and wR = 0.1567 for 3714 observed reflections with I 2s(I). In compound 1,the Cd(Ⅱ) ions are linked by the SC~(2–) ligands to give a two-dimensional(2D) undulating sheet based on the centrosymmetric dinuclear Cd_2(COO)_2 units. The 2D sheets are further connected by the DPPD ligands to produce a 3D structure,which is a 6-connected(4~4·6·~(10)·8) topological network based on the dinuclear Cd_2(COO)_2 node. Compound 1 exhibits a photoluminescent emission with a maximum at 540 nm upon excitation at 460 nm.     

Two Preparation Methods-dominated Cd~(Ⅱ)-Based Coordination Polymers with Mixed Adenine Nucleobase and 5-Nitroisophathalate Ligands: Synthesis,Structure and Fluorescence

Two new CdⅡ-based coordination polymers(CPs) with mixed adenine(Hade) nucleobase and 5-nitroisophathalate(nip) ligands, {[Cd(Hade)_(0.5)(H_2O)_2(nip)]·H_2O}n 1 and {[Cd(Hade)(H_2O)_(1.25)(CH_3OH)0.75(nip)]·0.75 CH_3OH·0.5H_2 O}_n 2, were successfully obtained by varying the preparation methods and structurally characterized. Crystal data for 1: monoclinic, C2/c space group with a = 10.5546(6), b = 17.3496(6), c = 16.1198(9) ?, β = 104.2800(10)o, V = 2860.6(2) ?3, Dc = 2.058 g/cm~3, Mr = 443.13, Z = 8, F(000) = 1752, μ = 1.585 mm~(–1), the final R = 0.0394 and wR = 0.1109 for 2285 observed reflections with I 2σ(I). For 2: triclinic, P1 space group with a = 10.2032(7), b = 10.5098(8), c = 11.0223(8) ?, a = 65.7050(10)o, β = 74.5750(10)o, g = 61.5280(10)o, V = 943.38(12) ?~3, Dc = 1.888 g/cm3, Mr = 536.24, Z = 2, F(000) = 537, μ = 1.225 mm~(–1), the final R = 0.0225 and wR = 0.0702 for 3143 observed reflections with I 2σ(I). 1 presents a crisscrossed layer with mutually orthogonal {Cd(nip)} chains aggregated by neutral m-N(7),N(9)-Hade connector. By contrast, 2 displays a linear chain with CdⅡ ions extended by bis-bidentate chelating-nip2–connectors, which are further assembled into a broad ribbon by N-H···N hydrogen-bonding interactions. Additionally, the two solid-state samples with comparable thermal stability exhibit favorable luminescent emissions at room temperature, suggesting their potential applications as fluorescence materials.     

Synthesis and Crystal Structure of Salicylyl-4-phenyl Thiosemicarbazide Lead with a Two-dimensional Network

A two-dimensional lead complex, [Pb(C14N3O2H12S)(NO3)]n·nH2O, was prepared by the reaction of salicylyl-4-phenyl thiosemicarbazide and lead nitrate. The compound (C14H13N4O6PbS, Mr=572.53) crystallizes in the monoclinic space group P21/c with a=11.2984(2), b=15.6628(7), c=11.1118(2), β= 113.564(2)n, V=1802.43(10)3, Dc=2.110 g/cm3, Z=4, μ(MoKα)= 9.515 mm·1, F(000)=1084, the final R=0.0394 and wR=0.0701 for 2552 observed reflections with I > 2σ(I). The Pb(II) ion displays a distorted octahedron in which the hypothesized stereochemically active lone pair occupies the apex. The compound exhibits a two-dimensional network structure formed by the zigzag one-dimensional chains joined by two μ-O of two nitrate groups in overlapping. A large ring exists in the two-dimensional layers. The TGA of the title compound has been studied.     

Syntheses,Structures and Properties for Zn~Ⅱ Coordination Polymers Based on a Functional 4'-(3-Pyridyl)-3,2':6',3'-terpyridine Ligand

Two new Zn~Ⅱ coordination polymers,namely,[Zn L(o-bdc)]n(1) and [Zn L(mbdc)]_n·n H_2O(2)(L = 4?-(3-pyridyl)-3,2?:6?,3??-terpyridine,H_2(o-bdc) = benzene-1,2-dicarboxylic acid,H_2(m-bdc) = benzene-1,3-dicarboxylic acid),were synthesized by hydrothermal methods. The crystal structures have been determined by single-crystal X-ray diffraction. Compound 1 crystallizes in monoclinic C2/c space group,with a = 28.016(2),b = 11.3815(11),c = 19.8071(17) ?,β = 133.961(2)°,V = 4546.2(7) ?3,Z = 8,Mr = 539.83,Dc = 1.577 Mg/m~3,μ = 1.127 mm-1,F(000) = 2208,the final R = 0.0426 and w R = 0.0986 for 2875 observed reflections with I 2σ(I) and displays a 1D coordination chain. While compound 2 crystallizes in monoclinic C2/c space group,with a = 15.6003(14),b = 11.9152(11),c = 26.633(3) ?,β = 94.320(2)°,V = 4936.5(8) ?~3,Z = 4,M_r = 1115.67,Dc = 1.496 Mg/m~3,μ = 1.043 mm~(-1),F(000) = 2272,the final R = 0.0499 and w R = 0.1342 for 2659 observed reflections with I 2σ(I) and shows a classical 3D cds topological network with point symbol of {65.8}. Furthermore,thermal stability and luminescent properties of 1 and 2 have also been investigated.     

Synthesis, Crystal Structure and Luminescent Property of a Novel 1-D Cadmium(Ⅱ) Complex: [Cd2(C8H3NO6)2(H2O)4]n·2nH2O

A novel one-dimensional chain-like coordination polymer constructed from 3-nitrobenzene-1,2-dicarboxylic acid, [Cd2(C8H3NO6)2(H2O)4]n·2nH2O, has been synthesized and its structure was determined by X-ray crystallography method. The crystal belongs to monoclinic, space group P21/c with a = 6.1252(8), b = 20.706(3), c = 8.8067(11) (A), β = 95.608(2)°, V= 1111.6(2)(A)3, Mr =751.12, Dc = 2.244 g/cm3, F(000) = 736, μ = 2.011 mm-1, Z = 2, the final R = 0.0262 and wR = 0.0692for 2338 observed reflections with I ＞ 2σ(I). The structure of the title compound presents a 1-D chain-like structure constructed by dimer units, [Cd2(CsH3NO6)2(H2O)4]n, through two carboxylate oxygen atoms. The fluorescence of the tifle compound has been also discussed in this paper.     

Crystal Structures,Luminescent Properties and Hirshfeld Surface Analyses of Zn(Ⅱ) and Cd(Ⅱ) Compounds Based on 1-(2-Carboxyl-phenyl)-3-(pyridin-2-yl)pyrazole

Two compounds,[Zn_2(Hcppp)_2(cppp)_2(H_2O)_2]·2 NO_3·6 H_2O(1) and [Cd(Hcppp)_2Cl_2]· 3H_2O(2)(Hcppp = 1-(2-carboxyl-phenyl)-3-(pyridin-2-yl)pyrazole),are synthesized and characterized by IR,TGA and X-ray single-crystal/powder diffraction.Compound 1 crystallizes in monoclinic system,space group P2_1/c with a = 9.894(2),b = 15.856(3),c = 20.430(4) ?,β = 101.70(3)°,V = 3138.5(11) ?~3,Z = 2,M_r = 1457.94,D_c = 1.543 g/cm~3,F(000) = 1504,R = 0.0278 and wR = 0.0749 for 6157 observed reflections(I 2σ(I)).Compound 2 crystallizes in triclinic system,space group P1 with a = 9.1424(4),b = 11.6427(5),c = 16.1345(7) ?,α = 102.6430(10)°,β = 95.4530(10)°,γ = 104.0060(10)°,V = 1605.94(12) ?~3,Z = 2,M_r = 767.88,D_c = 1.588 g/cm~3,F(000) = 776,R = 0.0307 and wR = 0.0764 for 6275 observed reflections(I 2σ(I)).Compound 1 exhibits a binuclear structure while compound 2 shows a mononuclear structure.In compound 1,two cppp-ligands display the μ_2-kN,N′:k O and two Hcppp ligands show the μ_1-kN,N′ coordination modes.However,two Hcppp ligands connect one Cd(Ⅱ) cation and exhibit the μ_1-kN,N′ binding mode in compound 2.The compounds are both studied using Hirshfeld surface analyses and 2D fingerprint plots.The luminescent properties are also discussed.     

Syntheses, Crystal Structures and Characterization of Two New Cadmium（II） Arsonates

Two cadmium arsonate coordination polymers, Cd(HL1)2 (1, H2L1 = 4-aminophenylarsonatic acid) and Cd(H2L2)2·2H2O (2, H3L2 = 2-(4-arsonphenylamino)acetic acid), have been synthesized and characterized by IR and single-crystal X-ray diffraction. Crystal data for 1: triclinic, space group P1 with a = 5.7559(12), b = 7.0903(14), c = 8.9925(18), α = 89.04(3), β = 80.79(3), γ = 85.09(3)o, Dc = 2.496 g·cm-3, μ = 6.095 mm-1, F(000) = 260, Z = 1, the final R = 0.0574 and wR = 0.1376 for 1489 observed reflections with I > 2σ(I). And those for 2: monoclinic, space group P21/c with a = 4.7595(10), b = 9.925(2), c = 22.609(5), β = 91.81(3)°, Dc = 2.167 g·cm-3, μ = 4.168 mm-1, F(000) = 684, Z = 2, the final R = 0.0335 and wR = 0.0815 for 2340 observed reflections with I > 2σ(I). The structure of 1 shows a two-dimensional layer consisting of inorganic chains of {CdN2(AsO3)2} along the a axis linking with the phenyl groups. These layers are further linked through strong interlayer hydrogen bonding interaction to form a three-dimensional hydrogen bond supramolecular architecture. Compound 2 has inorganic chains of {CdO2(AsO3)2} similar to 1, which connect with four adjacent inorganic chains forming a three-dimensional framework.     

Two Cobalt(Ⅱ) Coordination Polymers Based on Tetrazylphosphonate and Tetrazylphosphonic Acid Ligands

Two cobalt coordination polymers with the same 2D structure have been hydrothermally synthesized based on two bifunctional ligands with tetrazole and phosphonate(phosphonic acid) groups,namely,diethyl 4-(2H-1,2,3,4-tetrazol-5-yl) benzylphosphonate(C_2H_5-L1) and 4-(2H-1,2,3,4-tetrazol-5-yl)benzylphosphonic acid(H_2L2). The structures of the two complexes are characterized by elemental analysis,IR,TGA and X-ray single-crystal/powder diffraction. The pink block crystals of complex [Co(L1)(H_2O)]·H_2O(1) belong to the monoclinic system,space group C2/m with a = 20.8390(11),b = 7.2695(3),c = 10.0156(6) ?,β = 109.773(7)o,V = 1427.80(13) ?~3,Z = 4,D_c = 1.680 mg/cm~(-3),M_r = 361.16,F(000) = 740,R = 0.0316 and wR = 0.0826 for 1702 observed reflections(I 2σ(I)). The purple block crystals of complex [Co(L2)(H_2O)]·2H_2O(2) also belong to the monoclinic system,space group C2/c with a = 25.5382(16),b = 7.3844(3),c = 15.1925(11) ?,β = 124.238(9)o,V = 2368.6(2) ?~3,Z = 8,D_c = 1.969 mg/cm~(-3),M_r = 351.12,F(000) = 1432,R = 0.0475,wR = 0.1617 for 2088 observed reflections(I 2σ(I)). Both the nitrogen atoms of tetrazole group and oxygen atoms of phosphonate(phosphonic acid) groups in the ligands coordinated with the metal cobalt. The magnetic property of complex 1 is also 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.     

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 and Characterization of a Two-dimensional Cadmium(Ⅱ) Metal Organic Framework with Fes Topology

A new Cd(Ⅱ) coordination polymer, {[Cd(Hnbta)(L)]·H2O}n(L = 1,4-bis(5,6-dimethylbenzimidazol-1-yl)butane), H3nbta= 5-nitrobenzene-1,2,3-tricarboxylic acid), has been hydro-thermally synthesized and characterized by elemental analyses, IR, XRPD, and single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group P21/n with a = 17.3056(13), b = 11.0114(9), c = 17.7484(14) A, β = 117.3640(10)o, V = 3003.7(4) A3, Z = 4, C31H31CdN5O9, Mr = 730.01, Dc = 1.614 g/cm3, μ = 0.792 mm-1 and F(000) = 1488. The cadmium(Ⅱ) ions are bridged by Hnbta2- to generate a two-dimensional metal organic framework with fes topology. In addition, the thermal stability and fluorescence properties of the complex were also studied.     

Synthesis,Crystal Structure and Luminescent/magnetic Properties of Two Metal-organic Frameworks Based on Multi-N/O-donor Mixed Ligands

Two new complexes, namely [Cd_2(L)(pycy)(Cl)]·2 H_2 O(1) and [Cu(HL)(H_2 btac)]·2 H_2 O, have been synthesized by the reaction of the corresponding metal salts with mixed ligands including 1-(1 H-imidazol-4-yl)-4-(4 H-tetrazol-5-yl)benzene(HL), 2,6-pyridinedicarboxylic acid(H2 pycy) and 1,2,4,5-benzenetetracarboxylic acid(H4 btac), and characterized by single-crystal X-ray diffraction, IR spectroscopy, elemental analysis and powder X-ray diffraction(PXRD). Complex 1 crystallizes in triclinic, space group P■ with a = 9.8938(7), b = 10.1662(7), c = 12.4520(8) ?, α = 92.7070(10), β = 108.1310(10), γ = 105.3230(10)°, V = 1136.44(13) ?3, Z = 2, C17 H12 N7 O6 Cl Cd2, Mr = 670.59, Dc = 1.960 g/cm3, μ = 2.037 mm-1, S = 1.062, F(000) = 648, the final R = 0.0532 and w R = 0.1651 for 12156 observed reflections(I 2σ(I)). Complex 2 crystallizes in triclinic, space group P■ with a = 7.3058(8), b = 7.4890(8), c = 10.8937(12) ?, α = 71.3810(10), β = 84.134(2), γ = 65.745(2)°, V = 514.68(10) ?3, Z = 1, C_(20) H_(16) Cu N6 O10, M_r = 563.94, D_c = 1.819 g/cm~3, μ = 1.139 mm-1, S = 1.187, F(000) = 287, the final R = 0.0314 and w R = 0.0807 for 3564 observed reflections(I 2σ(I)). Single-crystal X-ray structural analysis reveals that complex 1 features a trinodal(3,3,4)-connected two-dimensional(2 D) net layer with Schl?fli symbol(4·6·8)(4·6~2·8~3)(6~2·8) while 2 has a 2 D network with 4~4 sql topology. Moreover, the photoluminescent property of 1 and magnetic property of 2 were also discussed.     

Synthesis and Crystal Structure of N-[(3aR,4R,4aR,5aS,6S,6aS)-1,3-Dioxooctahydro-4,6-ethenocyclopropa[f]isoindol-2(1H)yl]-4-(trifiuoromethyl)phenylmethanimine Monohydrate

The crystal structure of the title compound (C19H17F3N2O4,Mr=394.35) was determined by single-crystal X-ray diffraction.The crystal belongs to monoclinic,space group C2/c with a=28.383(6),b=10.355(2),c=12.799(3)(A),β=111.74(3)°,V=3493.8(12)(A)3,Z=8,De=1.499 g/cm3,λ(MoKα)=0.71073,F(000)=1632,μ= 0.127 mm-1,R=0.0412 and wR=0.1019.In the title compound,there exist three intennolecular hydrogen interactions (O(4)...O(1),O(4)...O(3) and O(4)...N(1)) between water.The neighboring molecules are linked to each other generating a two-dimensional network structure via the three intermolecular hydrogen bonds and π-π interactions shaped by phen-phen with centroid distance of 4.049 (A).     

A Novel Cd(Ⅱ)-MOF Constructed from an Organosillicon Tetracarboxylic Acid Ligand

A silicon-based tetracarboxylate connector has been prepared and employed in the construction of new metal-organic framework(MOF) material. A novel Cd(Ⅱ) coordination compound, namely, [Cd_4(H_2O)(L)(DMA)_2]_n(1, H_4L = 5,5?-(diphenylsilanediyl) diisophthalic acid, DMA = N,N-dimethylacetamide) has been successfully synthesized based on the ligand. X-ray single-crystal structure analysis reveals that polymer 1 crystallizes in monoclinic, space group P1 with a = 10.3335(11), b = 14.1557(15), c = 22.004(2) ?, α = 72.308(2), β = 88.105(2), γ = 88.363(3)o, V = 3064.2(6) ?~3, Cd_4Si_2C_(64)N_2O_(19)H_(52), Mr = 1659, Dc = 1.790 g/cm~3, μ(Mo Kα) = 1.486 mm~(-1), F(000) = 1630, Z = 2, the final R = 0.0660 and w R = 0.1302 for 12069 observed reflections(I 2σ(I)). Its structure has been further characterized by elemental analysis, thermogravimetric analyses and IR spectroscopy. Additionally, luminescent property of the title compound has been explored, and shows intense photoluminescent property in the solid state at room temperature.     

Synthesis, Crystal Structure and Photoluminescence of a 2D Two-fold Interpenetrating Cd(Ⅱ) Coordination Polymer Based on a Flexible Reduced Schiff Base Ligand

<正>By the reaction of cadmium chloride with a reduced Schiff base ligand (H_2L = N-(4- carboxybenzyl)-glycine), a novel Cd(II) compound [Cd(HL)_2]·4H_2O (1) has been obtained. Single-crystal X-ray diffraction analysis reveals that it crystallizes in orthorhombic, space group Pbcn with a = 13.9788(8), b = 24.4204(14), c = 13.9580(8), V = 4764.8(5)~3, Z = 8, M_r = 600.84, D_c = 1.675 g/cm~3, μ = 0.983 mm~(-1), F(000) = 2448, S = 1.084, R = 0.0806 and wR = 0.1705 (I > 2σ(I)). It displays a 2D two-fold interpenetrating structure. The Cd(II) ions are six-coordinated. The cross-linkage of Cd(II) ions by the bridge of HL anions results in a [Cd(HL)_2] layer. Every two [Cd(HL)_2]_n layers are penetrated with each other, resulting in a two-fold interpenetrating double-layer structure by π-π stacking interactions and hydrogen bonds. Such double-layers are further linked by hydrogen bonds into a supramolecular structure. Photoluminescent investigation shows that compound 1 displays strong emission in the purple region.     

Syntheses and Structures of a New Tetrazylphosphonate Ligand and the Coordination Polymer Based on Zn~(Ⅱ)

A novel tetrazylphosphonate ligand, namely ethyl 4-(2-ethyl-2H-1,2,3,4-tetrazol-5-yl) benzylphosphonate(Et-L), was designed and successfully achieved from p-cyano benzyl chloride, based on which a zinc coordination polymer(1) with a 2D layer structure has been hydrothermally synthesized and structurally characterized by elemental analysis, IR, TGA and X-ray single-crystal diffraction. The colorless block crystals of H_2L·H_2O were also obtained under the same hydrothermal conditions, which belongs to monoclinic system, space group P2_1/c with a = 13.3141(7), b = 5.1650(3), c = 21.9839(18) ?, β = 115.307(5)°, V = 1366.69(15) ?~3, Z = 4, D_c = 1.391 mg/cm~(-3), Mr = 349.58, F(000) = 600, R = 0.0748 and wR = 0.1917 for 2392 observed reflections(I 2σ(I)). The colorless block crystals of complex 1([Zn(L)(H_2O)]_n) also belong to monoclinic system, space group P2_1/c with a = 22.7464(10), b = 6.0430(3), c = 9.7704(4) ?, β = 92.525(4)°, V = 1341.70(10) ?~3, Z = 4, D_c = 1.731 mg/cm_(-3), M_r = 349.58, F(000) = 712, R = 0.0596 and wR = 0.1688 for 2357 observed reflections(I 2σ(I)). Only the oxygen atoms of phosphonic group are coordinated with the metal zinc probably because the hydrogen atom of tetrazole has been substituted by ethyl group. Photoluminescence properties of the complex are also investigated.     

Hydrothermal Synthesis and Crystal Structure of a Cobalt(Ⅱ) Coordination Polymer: [Co(C2O4)(bix)]n (bix=1,4-Bis(imidazol-1-ylmethyl)-benzene)

<正>A new two-dimensional cobalt coordination polymer has been prepared and fully characterized by elemental analysis, IR, TG and single-crystal X-ray diffraction. The compound [Co(C_2O_4)(bix)]_n 1 crystallizes in the monoclinic system, space group C2/c, with a = 11.549(3), b = 15.700(3), c = 9.260(2), β = 102.984(3)°, V = 1636.0(6)~3, C_(16)H_(14)CoN_4O_4, M_r = 383.23, D_c = 1.556 g/cm~3, μ(MoKα) = 1.078 mm~(-1), F(000) = 780, Z = 4, the final R = 0.0455 and wR = 0.1286 for 1483 observed reflections (I > 2σ(I)). Of the compound, the Co center is octahedrally coordinated with oxalate acting as a tetra-dentate ligand coordinated to the cobalt atom and each bix serving as a bridging ligand by employing two N-donors to coordinate with the Co center. An infinite {Co_2(C_2O_4)_2}_∞ chain is formed along the a axis. Furthermore, the 1D chains are held together via bix ligands to generate a two-dimensional network structure with 1D coronal-like channels (ca. 5.691 × 15.700).     

Hydrothermal Synthesis and Crystal Structure of a 2D Zinc（Ⅱ） Coordination Polymer with 5-Hydroxynicotinic Acid

The title compound,[Zn(5-hydroxynicotinate) 2 2H 2 O] n,has been synthesized by reacting zinc sulfate vitriol with 5-hydroxynicotinic acid under hydrothermal conditions,and its structure was determined by X-ray crystallography with the following data:monoclinic,space group C2/c,C 12 H 12 N 2 O 8 Zn,M r=377.61,a=10.223(3),b=10.319(3),c=13.613(4),β=105.922(6)°,Z=4,V=1380.9(8)3,F(000)=768,D c=1.816 g/cm 3,μ(MoKα)=1.826 mm-1,the final R=0.0401 and wR=0.1380 for 1157 observed reflections (I > 2σ(I)).In the structure of the title compound,the Zn II ion located in an inversion center lies in a distorted tetrahedral environment at a N 2 O 2 coordination mode,and the 5-hydroxynicotinic acid ligand links symmetry-related Zn II ions at a μ 2-N,O bridging way forming a two-dimensional covalent structure.In the crystal,solvent water molecules form intermolecular O-H O hydrogen bonds and pyridine rings of adjacent layers form π-π stacking (3.346),which connect adjacent two-dimensional sheets into a three-dimensional supramolecular network.     

Hydrothermal Synthesis and Crystal Structure of a Novel Polyoxometalate K(C_4N_2H_(12))_4(C_4N_2H_(11))_(2-)[Mo_8~ⅤMo_4~ⅥCdP_8O_(54)(OH)_8]F·6H_2O

The title compound 1 has been synthesized by the reaction of H_2MoO_4, CdCl_2, H_3PO_4, KF, piperazine hexahydrate and water in aqueous solution under mild hydrothermal conditions. Single-crystal X-ray analysis reveals that the title compound crystallizes in the triclinic system, space group P(-1) with a = 14.049(3), b = 15.972(3), c = 20.043(4) (A), α = 85.82(3), β = 81.28(3),γ = 67.15(3)°, V= 4095.9(14) (A)~3, M_r = 3204.62, Z=2,D_c = 2.598 g/cm~3,μ = 2.360 mm~(-1), F(000) = 3124, the final R = 0.0314, wR = 0.0826 and S = 0.989 for 18592 observed reflections with I > 2σ(I). The crystal packing is stabilized by N-H…O and O-H…O intra- and intermolecular hydrogen bonds to form an infinite 3D network.