Synthesis, crystal structure and magnetic properties of novel copper compound Cu(phen)(m-CBA)_2

A novel compound Cu（phen）（m-CBA）2 was synthesized with m-chlorobenzoic acid（m-CBA）, 1,10-phenanthroline（phen） and Cu（OAc）2·H2O. It was characterized by IR, UV, elemental analyses and X-ray crystallography. It crystallizes in the monoclinic crystal system with C2/c space group, a=2.9699（4） nm, b=1.15452（2） nm, c=1.5335（2） nm, β=111.118（2）°, V=4.905 1（1） nm3, Z=8, F（000）=2 328, R1=0.072 8, wR2=0.223 4 [I2σ（I）]. Structure analysis shows that the copper center coordinates with two nitrogen atoms from one 1,10-phenanthroline molecule, two oxygen atoms from two m-chlorobenzoic acid molecules, giving a distorted squared planar coordination geometry. This novel compound shows paramagnetic interactions between copper centers.

Hydrothermal Synthesis,Crystal Structure and Fluorescence Spectrum Studies of a Supramolecular Compound {[2-(2-Pyridyl)benzimidazoleH_2]^(2+)·[SbCl_5]^(2-)}_2

A new supramolecular compound, { [2-（2-pyridyl）benzimidazoleH2]2＋.[SBC15]2-}2, was synthesized by the hydrothermal reaction of o-diaminobenzene, 2-pyridinecarboxylie acid and SbCl3 in 1：1 HC1 solution, and characterized by chemical analysis, elemental analysis, IR spectra, thermogravimetfic analysis and fluorescence spectra. The crystal structure was deter- mined by X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P211c, with a = 16.0397（13）, b = 14.3189（12）, c = 15.6370（13） A, β = 105.8980（10）°, V = 3454.0（5） A3, Z = 4, C24H22Cl10N6Sb2, Mr = 992.48, Dc = 1.909 g/cm3,/z = 2.366 mm-1, S = 1.010, F（000） = 1920, R = 0.0254 and wR = 0.0555. The coordination anion, [SbCl5]2- which is a distorted tetragonal pyramid, is composed by coordinating action with Sb3＋ ion and five adjacent chloride ions. Every four coordination anions of [SbCl5]2- form a biquaternion ring structure through the secondary bonding of Sb...Cl. Moreover, the compound adopts a three-dimensional network supramolecular structure because of the hydrogen bonds and π-π stacking between the rings and the 2-（2-pyridyl）benzimidazole divalent cations. The title compound also shows good fluorescent behaviors.

Synthesis and Crystal Structure of the Heteropolymate Compound Na_3H_2[Ce_3(H_2O)_(18)Bi_2W_(22)O_(76)]·23H_2O

A Bi(Ⅲ) contained heteropolymate compound Na3H2[Ce3(H2O)18Bi2W22O76] 23H2O 1 has been synthesized. It crystallizes in the triclinic system, space group P1 with a = 14.370(3), b = 17.113(3), c = 24.764(5) , = 74.33(3), = 77.20(3), ?= 65.29(3), V = 5285.3(18) 3, Z = 2, Mr = 6908.66, Dc = 4.341 g/cm3, F(000) = 6042, m(MoKa) = 28.543 mm-1, R = 0.0604 and wR = 0.1659 for 15788 reflections with I > 2(I). The structure analysis revealed that in the anionic framework of the title compound the [Bi2W22O76]14- anions are connected by Ce3+ and Na+ cations into a three dimensional network.

Synthesis, Crystal Structure and Quantum Chemical Study of the Ladder Organotin Compound {[(C_6H_5CH_2)2Sn]_2(O)(Cl_2)}_2

The title compound {[（C6H5CH2）2Sn]2（O）（Cl2）}2 has been synthesized by the reaction of bisbenzyltin dichloride with NaOH dilute solution, and its structure was determined by X-ray diffraction. The crystal belongs to monoclinic, space group C2/c, with a = 2.5081（17）, b = 1.0089（7）, c = 2.0909（14） nm, β = 94.267（8）°, V= 5.276（6） nm^3, Z = 4, De= 1.734 g/cm^3,μ（MoKa） = 21.55 cm^-1, F（000） = 2704, R = 0.0398 and Rw = 0.1024. According to structural analysis, the tin atom adopts a distorted five-coordinate trigonal bipyramidal geometry, and the ladder-like structure is shaped by one planar four-membered Sn2O2 ring together with two planar four-membered Sn2OCl rings.

Synthesis,Crystal Structure and Antitumor Activity of Mixed Ligand Coordination Compound of Copper with Norfloxacin and 1,10-Phen,[Cu(NFLX)(phen)(H2O)]NO3·3H2O

The mixed ligand coordination compound of copper with norfloxacin (NFLX) and 1, 10-phen has been synthesized and characterized by means of X-ray single crystal diffraction. The structure features of the coordination compound are described. Antibacterial activities of the coordination compound have been tested against different microorganisms. The antitumor activities of the coordination compound on leukemia HL-60 cell line and liver cancer BEL-7402 cell line have been measured, respectively. The results indicated that the coordination compound has strong inhibitory effect on HL-60 and BEL-7402 cell lines.

Syntheses and Crystal Structures of Two Novel Spiro Compounds Containing 1,5-Dioxaspiro[5.5]undecane-2,4-dione

Two novel spiro compounds,3-benzylidene-1,5-dioxaspiro[5.5]undecane-2,4-dione 1 and 3-（2-fluorobenzylidene）-1,5-dioxaspiro[5.5]undecane-2,4-dione 2,have been synthesized and characterized by X-ray single-crystal diffraction,IR and elemental analysis.Compound 1 belongs to the monoclinic system,space group P21/n with a=12.326（3）,b=5.6420（11）,c=20.089（4）,β= 101.79（3）o,C16H16O4,Mr= 272.29,V=1367.7（5）3,Z=4,Dc=1.322g/cm3,F（000）=576,μ（MoKa）=0.095 mm-1,the final R=0.0420 and wR=0.1159.Compound 2 is of monoclinic system,space group P21/n with a=12.283（3）,b=5.6367（11）,c=20.055（4）,β=102.00（3）o,C16H15FO4,Mr=290.28,V=1358.2（5）3,Z=4,Dc=1.420 g/cm3,F（000）=608,μ（MoKa）=0.110 mm-1,the final R=0.0353 and wR=0.0860.

Syntheses,Crystal Structures and Antibacterial Activities of 5-Chloro-3-methyl-1-phenyl-1H-pyrazole-4-carboxylic Acid and Its Copper(Ⅱ) Compound

The title compounds 5-chloro-3-methyl-1-phenyl-1H-pyrazole-4-carboxylic acid（C11H9Cl N2O2, HL）（1） and [Cu（L）2（H2O）]（2） were prepared and structurally characterized by elemental analysis, IR and single-crystal X-ray diffraction. Compound 1（C11H9Cl N2O2） crystallizes in the monoclinic system, space group P21/n with a = 7.249（3）, b = 20.515（10）, c = 7.249（3）,β= 96.30°, V = 1071.6（9） ？3, Z = 4, Mr = 236.65, Dc = 1.467 g/cm3, F（000） = 488, GOOF = 1.029, μ= 0.341 mm-1, the final R = 0.0736 and w R = 0.1966 for 1500 observed reflections with I 〉 2σ（I）. Compound 2（C22H18Cl2Cu N4O5） crystallizes in the monoclinic system, space group P21/c with a = 7.2931（6）, b = 24.548（2）, c = 13.2726（11）, β= 99.4040（10）°, V = 2344.2（3） ？3, Z = 4, Mr = 552.84, Dc = 1.566 g/cm3, F（000） = 1124, GOOF = 1.050, μ= 1.201 mm-1, the final R = 0.0376 and w R = 0.1000 for 3626 observed reflections with I 〉 2σ（I）. 1 and 2 are connected through hydrogen bonding interactions to generate 2D and 3D supramolecular structures, respectively. Moreover, the preliminary antibacterial activities of 1 and 2 against the gram positive bacteria（S. aureus, C. albicans and B. subtilis） and gram negative bacteria（E. coli and P. aeruginosa） have been tested by using the microdilution method, and the results indicate that 2 is more active than 1 against the tested bacteria.

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 ℃ 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） A,V = 1678.89（11） A^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.

Crystal Structure and Magnetic Properties of a Dinuclear Terbium Compound Tb_2(μ_2-anthc)_4(anthc)_2(1,10-phen)_2

A dinuclear Tb（Ⅲ） compound, Tb_2（μ_2-anthc）_4（anthc）_2（1,10-phen）_2（1, Hanthc = 9-anthracenecarboxylic acid and 1,10-phen = 1,10-phenanthroline）, was synthesized under solvothermal condition and structurally characterized by single-crystal X-ray diffraction. Compound 1 crystallizes in the triclinic system, space group P1, with a = 12.5061（12）, b = 13.3168（10）, c = 15.0079（12） ？, α = 110.620（7）, β = 102.941（7）, γ = 107.036（7）o, V = 2081.8（3） ？~3, Z = 1, C_（114）H_（70）N_4O_（12）Tb_2, M_r = 2005.58, D_c = 1.600 g/cm^3, μ = 1.759 mm^（-1）, F（000） = 1008, the final R = 0.0294 and w R = 0.0608 for 8900 observed reflections with I 〉 2s（I）. In compound 1, two Tb（Ⅲ） ions are linked by four carboxylate groups of the bridging anthc– ligands to give a dinuclear Tb_2（μ_2-anthc）_4 unit wherein each Tb（III） ion is further capped by a terminal anthc– ligand and a 1,10-phen ligand in a chelating fashion. Detailed direct-current and alternating-current susceptibility measurements showed no slow magnetism relaxation phenomenon was observed for 1.

Synthesis, Crystal Structure, Luminescence Property and DFT Calculations of a New Coordination Compound Containing 8-Aminoquinoline Ligand

A new luminescent compound, Zn（8-aminoql）2（SCN）2 （1, 8-aminoql = 8-amino quinoline）, has been synthesized and its structure was characterized by IR, elemental analysis and X-ray single-crystal diffraction. Compound 1 belongs to the orthorhombic system, space group Pbca with a = 8.503（2）, b = 14.427（4）, c = 31.922（8）A, V= 3916.0（18） A3, Z = 8, C20H16N6S2Zn, Mr = 469.88, Dc = 1.594 Mg/m3, μ = 1.488 mm-1, F（000） = 1920, T = 296（2） K, the final R = 0.0293 and wR = 0.0645 for all 2763 observed reflections （1 〉 2a（/））. Compound 1 displays a 3D supramolecular architecture formed by N-H--S hydrogen bonds and π...π aromatic packing interactions. Photoluminescence studies reveal that it displays obvious fluorescent emission band （λex = 320 nm） at 533 nm in the solid state at room temperature. The emission bands possess a broad asymmetric feature, which can be assigned to ligand-to-ligand charge transfer transitions based on DFT calculations.

Synthesis and Crystal Structure of the Mixed-quadriligand Bismuth Complex [Bi(S_2CNEt_2)_2(NO_3)]·[1,10-Phen]

The mixed-quadriligand bismuth complex [Bi(S2CNEt2)2(NO3)]?[1,10-Phen] has been synthesized, and its crystal structure was determined by X-ray single-crystal diffraction. The crystal belongs to monoclinic, space group P21/n with a = 10.074(17), b = 15.05(2), c = 18.99(3) ?, β = 98.85(3)o, V = 2845(8) ?3, Z = 4, F(000) = 1464, Dc = 1.746 g/cm3, μ = 6.523 mm-1, R = 0.0333 and wR = 0.0703. In this complex, the bismuth atom is eight-coordinated in a capped distorted pentagonal bipyramidal geometry.

Two [Ni(dmit)_2]^- Compounds Showing Layered and Chain Alignments: Crystal Structures and Magnetic Properties

Two metal-dithiolene compounds with a formula of[4-ClBz-l-APy][Ni（dmit）2]（1）and[4-NO2Bz-l-APy][Ni（dmit）2]（2,4-ClBz-1-APy = 1-N-（4＇-chlorobenzyl）pyridinium,4-NO2Bz-1-APy = l-N-（4＇-nitrobenzyl）pyridinium,dmit^（2-）= 1,3-dithiole-2-thione-4,5-dithiolate） were synthesized and characterized.Two compounds crystallize in triclinic space group P1 and P1,respectively,but with different cell parameters and packing structures.The[Ni（dmit）2]^- anions and cations of 1 form mixed column stacks along the a axis and alternately layered alignments in the crystal of 2,which are parallel to the crystallographic（110） plane.Two compounds show a similar magnetic behavior,the magnetic exchange natures are mainly antiferromagnetic,and the magnetic susceptibility data can be fitted to the simple Curie-Weiss law.For 1 and 2,the fitted Curie constants are much less than the spin-only value expected for an S =1/2 system,and the fitted Weiss constants marking magnetic interaction are also very smaller.This fact implies that the weak CurrieWeiss-type paramagnetism is not the intrinsic characteristics of two compounds.

Hydrothermal Synthesis,Crystal Structure and Fluorescence Spectrum Studies of a Novel Supramolecular Compound {[2-(2-Pyridyl)benzimidazoleH_2]_2·[BiCl_6]·Cl}

A novel supramolecular compound,{[2-（2-pyridyl）benzimidazoleH2]2·[BiCl6]·Cl},was synthesized by the hydrothermal reaction of o-phenylenediamine and α-pyridinecarboxylic acid with BiCl3 in 6.0 mol·L-1 HCl solution,and characterized by elemental analysis,IR,X-ray single-crystal diffraction and photoluminescence spectroscopy.The crystal （C24H22N6Cl7Bi,Mr= 851.61） belongs to the triclinic system,space group P1 with a =7.2887（18）,b =9.548（2）,c= 12.469（3）,α=85.306（4）,β=82.814（4）,γ=71.349（4）°,Z=1,V=814.9（3）3,Dc=1.735 g/cm3,μ（MoKα）=6.007 mm-1,F（000）=410,R=0.0307 and wR=0.0787.The bismuth ion and six chlorine ions construct a distorted octahedral configuration.The three-dimensional supramolecular network is built from electrostatic attractions,hydrogen bonds and π-π interaction between the BiCl6 anion,Cl anion and [2-（2-pyridyl）benzimidazoleH2] cation.The photoluminescence spectroscopy study shows that the title compound has a blue fluorescent emission at 450 nm in the solid state.

Synthesis and Crystal Structure of Dicopper(II) Compound Containing Oxalate and Reduced Imino Nitroxide Radicals

A new dicopper(II) compound with oxalate and reduced imino nitroxide radicals [Cu2(m-C2O4)(Him2-py)2(H2O)2](NO3)2 (Him2-py=1-hydroxy-2-(2-pyridyl)-4,4,5,5-tetramethyli- midazoline) has been synthesized and its crystal structure was determined by X-ray diffraction method. The complex crystallizes in monoclinic, space group P21/n with a = 9.913(4), b = 19.057(8), c = 10.169(4) ? b = 114.292(7), V = 1751(1) 3, C26H38Cu2N8O14, Mr = 813.72, Dc = 1.543 g/cm3, m(MoKa) = 1.290 mm-1, F(000) = 840, Z = 2, the final R = 0.0398 and wR = 0.0986 for 1878 observed reflections (I>2s(I)). The imino nitroxide 2-(2-pyridyl)-4,4,5,5-tetramethyl- imidazoline-1-oxyl (im2-py) is reduced in the reaction to yield Him2-py which consists of oxalato-bridged centrosymmetric [Cu2(m-C2O4)(Him2-py)2(H2O)2]2+ ions and noncoordinated NO3- anions. Each copper(II) ion is in a distorted tetragonal pyramid environment: two nitrogen atoms from Him2-py and two oxygen atoms from the oxalate group are in the basal plane, and one water molecule at the axial position.

A Dinuclear Dysprosium-2-quinolinecarboxylate-1,10-Phenanthroline Compound:Crystal Structure and Magnetism

A dinuclear dysprosium（III） compound,[Dy2（μ2-OH）2（QLC）4（1,10-phen）2]·4H2O（1）（QLC-= 2-quinolinecarboxylate and 1,10-phen = 1,10-phenanthroline）,was synthesized and structurally and magnetically characterized.Compound 1 crystallizes in triclinic system,space group P1 with a = 10.9439（3）,b = 11.2823（3）,c = 12.2323（4） ？,α = 107.446（3）,β = 91.700（3）,γ = 91.511（2）°,V = 1439.25（8） A3,Z = 1,C（64）H（50）N8O（14）Dy2,Mr = 1480.12,Dc = 1.708 g/cm3,μ = 2.653 mm-1 and F（000） = 734.The final R = 0.0366 and w R = 0.0736 for 5816 observed reflections with I 〉 2σ（I）.Compound 1 contains the mononuclear [Dy（QLC）2（1,10-phen）] subunit formed from one 1,10-phen and two QLC-ligands chelating Dy（III） ion.Two mononuclear [Dy（QLC）2（1,10-phen）] subunits are bridged by a pair of μ2-OH groups to give a centrosymmetric dinuclear [Dy2（μ2-OH）2（QLC）4（1,10-phen）2] with each Dy（III） ion being eight-coordinated.Detailed susceptibility measurements revealed that compound 1 does not show slow magnetic relaxation under zero direct-current field but exhibits field-induced slow magnetic relaxation under 2 kOe applied field.

Crystal Structure and Magnetic Properties of a Two-dimensional Compound{(Me2NH2)4[Co(SIP)2]·2(DMF)·3(H2O)}n

-

Syntheses,Crystal Structures and Fluorescence Properties of Two Mononuclear Copper(Ⅱ) Compounds

Two new compounds,1（[Cu（IDB_）2]Cl_2·2CH_3CH_2OH·2H_2O（IDB = N,N-di（2-benzimidazolylmethyl）imine]） and 2（[Cu（EDTB）]·2[C_6H_4（OH）COO]·6H_2O（EDTB = N,N,N＇,N＇-tetrakis-[（2-benzimidazolyl）methyl]-1,2-ethanediamine]）,have been synthesized and their crystal structures were determined by single-crystal X-ray diffraction. Crystal 1 belongs to the triclinic system,space group P1 with a = 9.565（2）,b = 9.863（2）,c = 10.252（3） ？,α = 81.915,β = 88.330,γ = 87.347°,V = 956.28（40） ？3,Z = 1,F（000） = 427,D_c = 1.419 g/cm3,Mr = 817.27 and μ（MoKα） = 0.764 mm^（-1）. The final R indices（I 〉 2σ（I））： R = 0.0505,wR = 0.1417; R indices（all data）： R = 0.0591,wR = 0.1525. Crystal 2 is of triclinic system,space group P1 with a = 11.487（3）,b = 13.396（4）,c = 17.977（5） ？,α = 73.899（5）,β = 86.629（5）,γ = 65.018（4）°,V = 2403.8（12） ？3,Z = 2,F（000） = 1072,D3c = 1.417 g/cm,Mr = 1025.54,μ（MoKα） = 0.528 mm^（-1）. The final R indices（I 〉 2σ（I））： R = 0.0769,w R = 0.163 2; R indices（all data）： R = 0.0769,wR = 0.1632. The two compounds exhibit mononuclear structures. The copper（Ⅱ） atom of crystal 1 is six-coordinated by four nitrogen atoms of benzimidazole groups and two amine nitrogen atoms from the ligand IDB to adopt a distorted octahedral coordination geometry. The copper（Ⅱ） atom of crystal 2 is six-coordinated by four nitrogen atoms of benzimidazole groups and two amine nitrogen atoms from the ligand EDTB to show a distorted octahedral coordination geometry. Particularly,the two compounds exhibit fluorescent properties at room temperature in ethanol.

Solvothermal Synthesis,Crystal Structure and Luminescent Property of a Two-dimensional Lead(Ⅱ) Compound：[Pb(bmzbc)2]n

A two-dimensional coordination polymer, [Pb（bmzbc）2]n（1）（Hbmzbc =4-benzimidazole-1-yl-benzoic acid）, has been synthesized by the solvothermal reaction of Pb（NO3）2 with Hbmzbc at 120 ℃ in ethanol solvent. 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 orthorhombic system, space group Pccn, with a = 12.5801（7）, b = 20.0795（11）, c = 9.1830（6） ？, V = 2319.6（2） A^3, Z = 4, C（28）H（18）N4O4Pb, Mr = 681.65, Dc = 1.952 g/cm^3, μ = 7.319 mm^-1, F（000） = 1312, the final R = 0.0336 and wR = 0.0965 for 1699 observed reflection with I 〉 2σ（I）. In 1, the bmzbc^– ligands bridge the Pb（Ⅱ） ions to generate a 2-D sheet with（4, 4） topology. The complex exhibits turquoise photoluminescent emission with a maximum at 480 nm upon excitation at 300 nm.

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.

Synthesis and Crystal Structure of Novel Dimer of Bismuth(Ⅲ) Complex with Dithiotetrahydropyrrolocarbamate: [Bi(S_2CNC_4H_8)_2(NO_3)]_2

A novel dimer of the bismuth(Ⅲ) complex with dithiotetrahydropyrrolocarbamate, [Bi(S_2CNC_4H_8)_2·(NO_3)]_2, was synthesized and the crystal structure was determined by X-ray single crystal diffraction. The crystal belongs to a monoclinic system with space group P2_1/n, a=0.64718(13) nm, b=2.6738(6) nm, c=1.0423(2) nm, β=106.384(3)°, Z=4, V=1.730(3) nm^3, D_c=2.163 g/cm^3, μ=10.682 mm^(-1), F(000)=1072, R=0.0329, wR=0.0659. The structure shows a distorted pentagonal bipyramidal configuration with the seven-coordinated central Bi atom. In the crystal, the molecular packing in the unit cell reveals that the two adjacent molecules are symmetrically linked each other in the dimer by virtue of a couple of Bi-S interaction.