Synthesis and Crystal Structure of a New Pr(Ⅲ)–K(Ⅰ) Heterometallic Oxalate Coordination Polymer

A new 3D heterometallic coordination polymer, namely [K2Pr2(C2O4)4·H2O]n(1), has been successfully synthesized under hydrothermal conditions. X-ray single-crystal diffraction determination reveals that 1 crystallizes in monoclinic system, space group P21/n with a = 12.060(4), b = 8.493(3), c = 15.776(5)(A), β = 93.235(3)°, V = 1613.4(9) 3, Z = 4, Mr = 730.12, Dc = 3.006 Mg/m3, μ = 6.581 mm-1, F(000) = 1368, the final R = 0.0283 and w R = 0.0866 for 2939 observed reflections with I 2σ(I). Complex 1 features an unusual 3D heterometallic coordination framework, in which oxalates exhibit three different coordination behaviours. Moreover, powder X-ray diffraction and thermal properties for 1 have also been investigated.     

Synthesis,Crystal Structure,and Topology Analysis of One Novel Interpenetrated 2D Cobalt Coordination Polymer, {[Co(HTCB)(4,4'-btb)]·H_2O}_n

One novel cobalt coordination polymer, {[Co(HTCB)(4,4'-btb)]·H2O}n(1, H3TCB= 1,3,5-tris(4-carboxyphenyl)benzene, 4,4'-btb = 4,4'-bis(1,2,4-triazol-3-yl)biphenyl), has been synthesized and characterized by elemental analysis, IR, powder X-ray diffraction(PXRD), and thermogravimetric(TG) analyses. X-ray diffraction analysis reveals that complex 1 is a 2D 2-fold interpenetrated {44,62}-sql [Co(HTCB)(4,4'-btb)] sheet based on the 1D [Co(HTCB)]n chains and1 D [Co(4,4'-btb)]n chains. The crystal of 1 crystallizes in triclinic, space group P 1 with a =9.529(12), b = 13.914(16), c = 14.906(17), V = 1903(4) 3, Z = 2, C45H34N6CoO7, Mr = 829.71,Dc = 1.448 g/cm3, F(000) = 858 and μ(MoKα) = 0.514 mm-1. The final R = 0.0655 and wR = 0.1136 for 6603 observed reflections with I 2σ(I) and R = 0.1136 and wR = 0.1747 for all data.     

Synthesis and Crystal Structure of a Cadmium（Ⅱ） Coordination Polymer：[Cd_2Cl_4（bpme）]_n·n（2H_2O）

A novel coordination polymer, [Cd2Cl4(bpme)]n·n(H2O) (1, bpme=2,5-bis(be-nzoimidazol-2-yl)pyrazine), has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction. The crystal of the complex belongs to the triclinic system, space group P , with a=7.0737(9), b=8.7886(11), c=9.4561(12) , α=105.3580(10), β=94.981(2), γ=96.879(2)°, V=558.46(12) 3, Mr=714.97, Z=1, F(000)=346, Dc=2.126 g/cm3, μ=2.412 mm-1, T=296(2) K, S=1.057, R=0.0533 and wR=0.1480. According to the structural analysis, the Cd(Ⅱ) ion adopts a slightly distorted six-coordinated octahedral geometry. The Cd(Ⅱ) atoms are bridged by four Cl atoms along the a direction, forming infinite straight chains which are further constructed to generate 2D network layer structures through the μ4-N bpme ligand in the b direction, and such 2D network layer structures finally form a novel three-dimensional infinite supramolecular framework through weak π-π stacking between two network layers and hydrogen bonds.     

Synthesis and Crystal Structure of a Novel Compound:[Nd_3(OH)_7(O_2CC_6H_4SO_3)(H_2O)]_n·nH_2O with a Pillar-layered Structure

A novel Nd(Ⅲ) compound,[Nd3(OH)7(O2CC6H4SO3)(H2O)]n·nH2O 1,has been synthesized by the hydrothermal reaction of Nd2O3 and 3-sulfobenzoic acid monosodium salt. It was characterized by IR spectroscopy,elemental analysis,thermogravimetric analysis and single-crystal X-ray diffraction. It crystallizes in monoclinic,space group P21/c with a = 13.024(3),b = 10.961(2),c = 12.792(3) ,β = 91.271(3)°,V = 1825.6(7) 3,Z = 4,Mr = 787.97,Dc = 2.867 g/cm3,μ = 8.584 mm-1,F(000) = 1460,S = 1.035,R = 0.0442 and wR = 0.1166 (I 2σ(I)). In this compound,the cross-linkage of Nd atoms by bridging hydroxy groups results in a Nd-O inorganic 200 layer,and such layers are linked by the 3-O3S-C6H4-CO2 dianions into a pillar-layered structure. The lattice water molecules are located in the cavity.     

Synthesis and Crystal Structure of a Novel Bis（ethoxycarbonyl）glycoluril Macrocycle

A novel [2+4+2]-macrocyclic compound 3(C52H69N16O12, Mr = 1109.53) con- taining bis(ethoxycarbonyl)glycoluril groups was synthesized via the Mannich three-component reaction in one pot and its structure was characterized by single-crystal X-ray diffraction. It crystallizes in triclinic, space group P1 with a = 10.077(3), b = 10.642(3), c = 15.324(5) , α = 96.704(5), β = 102.304(5), γ = 104.546(5)°, Z = 2, V = 1528.7(8)3, Dc = 1.283 g/cm3, μ = 0.097 mm-1, F(000) = 628, R = 0.0818 and wR(I 2σ(I)) = 0.2346 for 3034 observed reflections.     

Synthesis and Crystal Structure of a 1-D Chain Coordination Complex {[Mn2（HCAM）3（H2bipy）]·5H2O}n

The 1-D chain coordination complex of {[Mn2（HCAM）3（H2bipy）]·5H2O}n （H3CAM = 4-hydroxypyridine-2,6-dicarboxylic acid, bipy = 4,4＇-bipyridine） has been synthesized by the reaction of 4-hydroxypyridine-2,6-dicarboxylic acid, 4,4＇-bipyridine and manganese carbonate under hydrothermal conditions, and its crystal structure was determined by X-ray diffraction method The crystal belongs to the monoclinic system, space group P21/n with a = 10.110（2）, b = 20.159（4）, c = 17.861（4）A,β = 99.67（3）°, V = 3.5884（12） nm3, Mr= 901.47, Z = 4, Dc= 1.669 g.cm^-3, μ= 0.798 mm^-1, F（000） = 1840, the final R = 0.0713 and ωR = 0.1853. The complex forms a 1-D chain bridged by HCAM, protonated 4,4-bipyridines link the 1-D chains to construct 2-D networks via N-H...O hydrogen bonds, and networks are further extended via π-π stacking and hydrogen bonds into 3-D supramolecular framework.     

Synthesis and Crystal Structure of a New(6,3)-Connected Ni(Ⅱ) Coordination Polymer

The coordination polymer [Ni(dpa)(bpp)]n(H2dpa = 2,4'-biphenyl-dicarboxylic acid,bpp = 1,3-di(4-pyridyl)propane) was hydrothermally prepared and characterized by single-crystal X-ray diffraction,FTIR spectra,elemental analysis and thermal analysis.The crystal is of triclinic system,space group P1 with a = 12.516(5),b = 12.943(5),c = 15.130(5) ,α = 94.331(5),β = 91.827(5),γ = 108.382(5)°,C54H44N4Ni2O8,Mr = 497.18,V = 2315.3(15) 3,Dc = 1.426 g/cm3,F(000) = 1032,μ = 0.875 cm-1,Z = 2,the final R = 0.0496 and wR = 0.1100 for 5365 reflections with Ⅰ 2σ(Ⅰ).X-ray diffraction analysis reveals that the carboxylate group of 2,4'-diphenic acids acting as bridging ligands adopts two coordination modes:bis-mondentate and bidentate chelating.The compound exhibits a two-dimensional(6,3)-connected architecture.     

Hydrothermal Synthesis,Crystal Structure and Thermal Stability Properties of the Complex [Cd_2(phen)_2(C_(14)H_(11)O_3)_4(CH_3CH_2OH)]·(CH_3OH)·(H_2O)

A dinuclear cadmium complex [Cd2(phen)2(C14H11O3)4(CH3CH2OH)]·(CH3OH)·(H2O) has been synthesized with benzilic acid and 1,10-phenanthroline by hydrothermal method.The crystal structure was determined by X-ray diffraction with crystal parameters as follows:triclinic system with space group P1,a = 1.21298(10),b = 1.32586(11),c = 2.4815(2) nm,α = 76.2630(10),β = 81.4500(10),γ = 69.1700(10)o,V = 3.6143(5) nm3,Dc = 1.438 g/cm3,Z = 1,F(000) = 1600,the final GOOF = 0.937,R = 0.0521 and wR = 0.1328.In the title complex,the dinuclear structure is defined by carboxyl oxygen atoms adopting a monodentate bridged coordination mode.The coordination environment of Cd(Ⅱ) ion is CdO4N2,giving a distorted octahedral coordination geometry.TG analysis shows that the title complex is stable under 140 ℃.     

Synthesis and Crystal Structure of a Cu(Ⅱ) Coordination Polymer: [Cu(L)(1,10-phen)]_n

A new complex [Cu(L)(1,10-phen)]n(1, L = N-3-pyridine sulfonyl amino acid) has been synthesized and characterized by IR, elemental analysis and X-ray diffraction analysis, and its crystal belongs to monoclinic, space group P21/c with a = 11.481(2), b = 18.094(4), c = 8.5198(17) , β = 102.26(3)°,V = 1729.5(6) 3, Z = 4, Dc = 1.759 g/cm3, F(000) = 932, μ = 1.422 mm-1, R = 0.0368 and wR = 0.0893. In 1, the Cu(Ⅱ) ion adopts a slightly distorted five-coordinated square pyramidal geometry. The L2- ligand adopts O of the carboxyl bridging adjacent Cu(Ⅱ) units to form an infinite chain structure along the c axis. Also, π-π stacking interactions between the adjacent chains expanded the 1-D structures into a 3-D supramolecular structure.     

Synthesis and Crystal Structure of a Novel Cobalt（Ⅱ） Coordination Polymer with 1,2,4,5-Benzenetetracarboxylate

A novel cobalt（II） coordination polymer,[Co（BTEC）1/2]n 1,has been synthesized with Co（NO3）2·6H2O and 1,2,4,5-benzenetetracarboxylic acid （H4BTEC） by the hydrothermal method,and characterized by elemental analysis,IR and single-crystal X-ray diffraction. Crystallographic data for 1： C5HO4Co,Mr = 183.99,monoclinic,space group C2/c,a = 16.619（6）,b = 7.416（3）,c = 8.040（3）A,β = 90.612（4）°,V = 990.8（6） A^3,Z = 8,Dc = 2.467 g/cm^3,μ = 3.390 mm^-1,F（000） = 720,R = 0.0307 and wR = 0.0847 for 912 observed reflections （I 〉 2σ（I））. X-ray crystal structural analysis revealed that each Co（II） adopts a tetrahedral coordination mode to link four separate BTEC ligands via uniform monodentate carboxylate groups and each BTEC ligand possesses an 8-connected geometry to connect eight Co（II） ions. Complex 1 exhibits a rare （4,8）-connected net with （45.6）2（410.614.84） topology.     

Urothermal Synthesis and Crystal Structure of a Zn（Ⅱ） Coordination Polymer with a 3-D Supramolecular Structure

A new metal-organic coordination polymer [Zn(hfipbb)(e-urea)]n(1,H2hfipbb = 4,4'-(hexafluoroisopropylidene)bis(benzoic acid),e-urea = ethylene urea) has been urothermally synthesized and characterized by elemental analysis and single-crystal X-ray diffraction.The title complex crystallizes in monoclinic,space group P21/c with a = 13.302(4),b = 10.981(3),c = 13.804(4) ,β = 93.587(5)°,V = 2012.3(10) 3,C20H14N2O5F6Zn,Mr = 541.72,Z = 4,Dc = 0.447 g/cm3, = 0.328 mm-1,F(000) = 272,R = 0.0340 and wR = 0.1107 for 4528 observed reflections(I >2σ(I)).In the structure of compound 1,two Zn(Ⅱ) ions are bridged by two carboxylate groups from two hfipbb ligands to form a dinuclear unit,and each dinuclear Zn(Ⅱ) unit is linked with its two adjacent dinuclear units through four hfipbb ligands into an infinite one-dimensional double-chain.The interesting structural feature of compound 1 is that the one-D double-chains are self-interconnected into a three-D supramolecular structure through hydrogen bonds between the coordinated e-urea molecules and carboxylate oxygen atoms(N1 and O2,N2 and O4).     

Synthesis,Crystal Structure,Magnetic Property and DFT Study of a Novel 2D Polymer [Cu(pdc)(bpy)]·H_2O

A new copper complex [Cu(pdc)(bpy)]·H2 O(1, H2 pdc = 3,5-pyridinedicarboxylic acid, bpy = 2,2-bipyridine) has been solvothermally synthesized and characterized by single-crystal X-ray diffraction, elemental analysis, IR spectroscopy, UV-vis spectroscopy and magnetic measure- ments. Complex 1 crystallizes in monoclinic system, space group P21 /c, a = 10.893(2), b = 7.3641(15), c = 1.9921(4), β = 92.16(3), V = 1596.9(6)3, Dc = 1.676 g/cm3, Mr = 402.84, Z = 4, F(000) = 820, μ = 1.404 mm-1, the final R = 0.0237 and wR = 0.0693. The Cu(II) ion is five-coordinated by two O atoms from two pdc ligands, one N atom from another pdc ligand and two N atoms from the bpy ligand. The pdc anion, which acts as a tridentate ligand, links three Cu ions, forming(3,3)-connected two-dimensional(2D) sheets. We also studied the electronic structure and orbital energies of complex 1 by DFT methods, and the results are consistent with UV-vis spectrum.     

Three-dimensional 3d-4d Heterometallic Coordination Polymer——Synthesis,Structure,Magnetic and Luminescent Properties

A new three-dimensional 3d-4d heterometallic coordination polymer,[Cd2Mn(H2O)4(BTC)2]·2H2O(BTC=1,3,5-benzenetricarboxylate) was prepared under hydrothermal conditions and characterized by single crystal X-ray diffraction.This compound crystallized in the monoclinic space group C2/c,with cell parameters a=1.9452(4) nm,b=0.7094(2) nm,c=1.8064(4) nm,β=118.02(3)°,V=2.2004(8) nm3 and Z=4.Its structure contains trinuclear mixed metal clusters,which are further connected by BTC to form a three-dimensional framework.The compound exhibits intense photoluminescence at room temperature.Magnetic studies of the compound show a dominant antiferromagnetic exchange between the Mn(Ⅱ) ions.     

Synthesis,Crystal Structure and Water-induced Reversible Crystal-to-amorphous Transformation Property of [{Ni(IBG)(4,4'-bipy)(H_2O)_2}·3H_2O]_n

A novel NiII complex [{Ni(IBG)(4,4'-bipy)(H2O)2}·3H2O]n 1 (H2IBG = isophthaloylbisglycine and 4,4'-bipy = 4,4'-bipyridine) has been synthesized and characterized by singlecrystal X-ray diffraction, elemental analysis, IR spectra and thermogravimetric analysis. It crystallizes in monoclinic, space group P2/c with a = 15.5420(7), b = 22.4344(1), c = 8.3455(5), β = 101.538(3)o, V = 2670.1(7)3, Z = 4, C22H32N4NiO13, Mr = 619.23, Dc = 1.443 g/cm3, F(000) = 1296.0, μ(MoKα) = 0.750 mm-1, the final R = 0.0570 and wR = 0.1445 for 2296 observed reflections with I 2σ(I). In the structure, the NiII metal center is coordinated in an octahedral environment arranged by two water molecules, two carboxylate oxygen atoms and two nitrogen atoms from two 4,4'-bipy ligands. Thermal decomposition and powder X-ray diffraction results indicate that the transformation from the crystal form, [{Ni(IBG)(4,4'-bipy)(H2O)2}·3H2O]n, to the amorphous powder, Ni(IBG)(4,4'-bipy)(H2O)2, is reversible, so the latter form may be utilized as an absorbing agent for water and water vapor.     

Synthesis and Crystal Structure of a Coordination Polymer {[Co(phth)(phen)(H_2O)]·(C_2H_5OH)}_n

1 INTRODUCTION Metal-organic coordination polymer has particu- lar and special structure characters with some caves, holes and channels[1], and can be used in selected catalysis, molecular recognition, reversible exchan- ge of host-guest molecules (ions), super purity sepa- ration, biological conductor[2～5], etc. In the past ten years, polymers with bridging ligand have been widely investigated[6, 7]. The development of supra- molecular architectures of inorganic-organic hybrid molecules …     

Synthesis, Crystal Structure and Thermal Stability of the Coordination Polymer [Co（2-mpac）_2（py）·4H_2O）]_n

A new coordination polymer with the formula of [Co(2-mpac)2(py)·4H2O)]n (1, 2-mpac = 5-methyl-2-pyrazinecarboxylic acid, py = pyrazine) has been synthesized through hydrothermal synthesis and structurally characterized by X-ray single-crystal diffraction method. 1 exhibits a 3D supramolecular network. Crystal data: monoclinic, space group C2/m, a = 15.907(9), b = 7.104(3), c = 9.793(5), β = 95.232(8)o, V = 1102.0(10)3, Z = 2, S = 0.995, the final R = 0.0509, wR = 0.1626 for 1002 observed reflections with (I > 2σ(I)) and R = 0.0530, wR = 0.1667 for all data. In addition, elemental analysis, IR and thermalgravimetric analysis are presented.     

Synthesis and Crystal Structure of a Novel Ca(Ⅱ) Coordination Polymer Containing Dipyridine Dicarboxylic Ligand

The novel alkaline metal complex Ca(BPDCH)2(1, BPDCH2 = 2,2'-bipyridine-5,5'-dicarboxylic acid) has been synthesized by the hydrothermal reaction of Ca(NO3)2·4H2O with 2,2'-bipyridine-5,5'-dicarboxylic acid. The molecular and crystal structures of complex 1 have firstly been characterized by FTIR, elemental analysis, and X-ray single-crystal diffraction. The 3D MOF structure of complex 1 was interpreted by the versatile binding modes-the intermolecular hydrogen bonds and π-π stacking interactions of 2,2'-bipyridine-5,5'-dicarboxylic acid ligand. The analysis results show complex 1 belongs to a coordination polymer with 3D MOF structure. The results of thermogravimetric analysis and solubility demonstrate complex 1 is a thermostable compound and does not dissolve in water and traditional organic solvents.     

Synthesis,Crystal Structure,Thermal Behavior and Photoluminescence of a Novel Two-dimensional Cd(Ⅱ) Coordination Polymer

A new coordination polymer, [Cd2(bptc)(L)2(H2O)2]·5H2O(1, L = 2-(2-chloro-6-fluorophenyl)-1H-imidazo[4,5-f][1,10]phenanthroline and H4 bptc = 3,3',4,4'-biphenyltetracarboxylic acid), has been synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/n with a = 18.868(4), b = 7.2111(14), c = 19.464(4), β = 95.75(3)°, C54H31Cd2Cl2F2N8O15, Mr = 1365.57, V = 2635.0(9)3, Z = 2, Dc = 1.721 g/cm3, S = 1.034, μ(MoKα) = 0.995 mm–1, F(000) = 1358, R = 0.0501 and wR = 0.1076. In 1, each bptc anion bridges four Cd(II) atoms to form 2D layer structures, which are further extended by π-π stacking interactions into a 3D supramolecular architecture. The thermal behavior and luminescent properties of the compound have also been studied.     

Synthesis,Crystal Structure and Luminescence of a New Zn(Ⅱ) Dimer: [Zn(bpdc)(L)]_2·4H_2O

A new dimeric compound, [Zn(bpdc)(L)]2·4H2O(1, L = 11-fluoro-dipyrido[3,2-a:2',3'-c]phenazine and bpdc = 1,1'-biphenyl-2,2'-dicarboxylate), has been synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic, space group C2/c with a = 23.671(5), b = 22.547(5), c = 13.741(3), β = 123.47(3)o, V = 6118(2) 3, Z = 4, C66H44Cl2F2N8O12Zn2, Mr = 1380.73, Dc = 1.499 g/cm3, F(000) = 2816, μ(MoKa) = 0.949 mm-1, R = 0.0572 and wR = 0.1620. In 1, Zn1 and the symmetry formed Zn1 ions are connected by four bridging bidentate carboxylate groups from two independent bpdc anions to yield a binuclear unit with the Zn···Zn separation by bpdc anions of 4.168. Two L ligands are located on both sides of the dimer in chelating bidentate modes. The lateral L ligands from neighboring dimers are paired through strong π-π interactions to result in a fascinating 1D ladder-like supramolecular array. In addition, neighboring supramolecular ladders are packed each other to yield a 3D supramolecular architecture with a 1D channel.