Hydrothermal Synthesis and Crystal Structure of a One-dimensional Cadmium（Ⅱ） Complex

A metal-organic coordination polymer [Cd2(cbba)4(bix)2] n·nH2O (Hcbba=2-(4′-chlorine-benzoyl)-benzoic acid, bix=1,4-bis(imidazol-1-ylmethyl)-benzene) 1 has been hydrothermally synthesized and characterized by elemental analysis, IR, TG, fluorescence spectrum and single-crystal X-ray diffraction. Colorless crystals crystallize in the triclinic system, space group Pī with a=12.9891(15), b=15.3211(19), c=21.154(3), α=108.476(3), β=90.148(2), γ=105.429(3)°, V=3831.5(8)3 , C84H60Cd2Cl4N8O13 , Mr=1756.00, Dc=1.522g/cm3 , F(000)=1776, Z=2, μ(MoKα)=0.765 mm-1 , the final R=0.0724 and wR=0.1208 for 6916 observed reflections (I > 2σ(I)). The structure of 1 exhibits a one-dimensional infinite chain-like structure.     

Hydrothermal Synthesis and Crystal Structure of a New Nickel（II） Complex with 3,4-Pyridinedicarboxylic Acid and 1,4-Bis（imidazol-l-ylmethyl）-benzene Ligands

A metal-organic coordination polymer [Ni(PDB)(bix)(H2O)]n(H2PDB=3,4-pyri-dinedicarboxylic acid, bix=1,4-bis(imidazol-1-ylmethyl)-benzene) 1 has been hydrothermally synthesized and characterized by elemental analysis, IR, TG and single-crystal X-ray diffraction. Blue crystals crystallize in the triclinic system, space group P1 with a=9.1849(8), b=9.2065(9), c=12.9308(12) , α=103.3070(10), β=104.7160(10), γ=90.5900(10)o, V=1026.42(16)3 , C21H19N5NiO5 , Mr=480.12, Dc=1.553 g/cm3 , F(000)=496, Z=2, μ(MoKα)=0.991 mm1 , the final R=0.0325 and wR=0.0799 for 3561 observed reflections (I>2 (I)). The structure of 1 exhibits a two-dimensional network structure.     

Synthesis and Crystal Structure of a New Cadmium（Ⅱ） Complex with 3,4-Pyridinedicarboxylic Acid and 1,4-Bis（imidazol-1-ylmethyl）-butane Ligands

A metal-organic coordination polymer [Cd(PDB)(bimb)]n (H2PDB=3,4-pyridine- dicarboxylic acid, bimb=1,4-bis(imidazol-1-ylmethyl)-butane) 1 has been hydrothermally synthesi- zed and characterized by elemental analysis, IR, TG, fluorescence spectrum and single-crystal X-ray diffraction. Yellow crystals crystallize in the monoclinic system, space group Cc with a=19.001(5), b=7.948(2), c=13.392(4) , β=120.803(3)o, V=1737.0(8)3, C17H17CdN5O4, Mr=467.76, Dc=1.789 g/cm3, F(000)=936, Z=4, μ(MoKα)=1.293 mm-1, the final R=0.0266 and wR=0.0534 for 2707 observed reflections (I > 2?(I)). The structure of 1 exhibits a three-dimensional network structure.     

Synthesis and Crystal Structure of a New Nickel（II） Complex with 2,4-Pyridinedicarboxylic Acid and 1,4-Bis（imidazol-1-ylmethyl）-benzene） Ligands

A metal-organic coordination polymer [Ni(PDC)(bix)(H2O)]n (H2PDC = 2,4-pyri- dinedicarboxylic acid, bix = 1,4-bis(imidazol-1-ylmethyl)-benzene) 1 has been hydrothermally synthesized and characterized by elemental analysis, IR, TG and single-crystal X-ray diffraction. Blue crystals crystallize in the monoclinic system, space group C2/c with a = 25.1475(18), b = 13.1621(9), c = 14.2739(10), β = 118.4150(10)o, V = 4155.4(5) 3, C21H19N5NiO5, Mr = 480.12, Dc = 1.535 g/cm3, F(000) = 1984, Z = 8, μ(MoKα) = 0.979 mm-1, the final R = 0.0478 and wR = 0.1004 for 3727 observed reflections (I > 2σ(I)). The structure of 1 exhibits a one-dimensional chain-like structure.     

Synthesis, Crystal Structure and Photoluminescent Property of a Three-dimensional Zinc（Ⅱ） Coordination Polymer: [Zn1.5（PDB）（bix）0.5（μ2-OH）]2n

A new metal-organic coordination polymer [Zn1.5(PDB)(bix)0.5(μ2-OH)]2n 1 (H2PDB = pyridine-3,4-dicarboxylic acid, bix = 1,4-bis(imidazol-1-ylmethyl)-benzene) has been hydrothermally synthesized and structurally characterized by elemental analysis, IR, TG and single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group P2/c with a = 7.411(2), b = 7.848(3), c = 25.048(8), V = 1451.8(8)3, C28H22N6O10Zn3, Mr = 798.63, Dc = 1.827 g/cm3, μ(MoKα) = 2.529 mm-1, F(000) = 804, Z = 2, the final R = 0.0440 and wR = 0.1035 for 1952 observed reflections (I > 2σ(I)). It exhibits a three-dimensional framework structure. Moreover, its luminescent property has been investigated in the solid state.     

Hydrothermal Synthesis, Crystal Structure and Magnetic Properties of a Novel Zero-dimensional Manganese（Ⅱ） Complex with 2,2′-Diphenic Acid and 1,10-Phenanthroline Ligands

A novel metal-organic coordination polymer [Mn3(2,2′-dipha)3(phen)6]n·3nH2O (2,2′-dipha = 2,2′-diphenic acid, phen = 1,10-phenanthroline) 1 has been hydrothermally synthe- sized and structurally characterized by single-crystal X-ray diffraction, elemental analyses, IR spectroscopy, and magnetic susceptibility measurements. The crystal crystallizes in triclinic, space group P1 with a = 16.921(5), b = 18.307(5), c = 18.450(5) , α = 113.369(5), β = 108.529(5), γ = 102.984(5)o, V = 4553(2) 3, C114H72Mn3N12O14.25, Mr = 2002.66, Dc = 1.461 g/cm3, μ(MoKα) = 0.488 mm1, the final F(000) = 2058, Z = 2, R = 0.0491 and wR = 0.0980 for 9087 observed reflections (I > 2σ(I)). In the crystal structure, the manganese atom is six-coordinated with two carboxylate oxygen atoms from different carboxylate groups of the same dipha and four nitrogen atoms from two different phen ligands, showing a slightly distorted octahedral geometry. Fur- thermore, it exhibits a zero-dimensional structure with dipha-Mn-phen- as building units. Variable- temperature magnetic measure shows an overall anti-ferromagnetic behavior for compound 1.     

Synthesis, Structure and Luminescent Properties of a New Terbium（Ⅲ） Complex with 5-Bromoisophthalic Acid

The self-assembly of 5-bromoisophthalic acid (H2BIPA) with Tb(NO3)3·6H2O under hydrothermal conditions gives rise to a 3D coordination polymer, [Tb2(BIPA)3(CH3CH2OH)]n (1), which was characterized by elemental analysis, IR and single-crystal X-ray diffraction. The crystal is of monoclinic system, space group P21/c with a = 19.2591(17), b = 8.2537(7), c = 18.5663(17), β = 104.4720(10)°, V = 2857.6(4)3, C26H15Br3O13Tb2, Mr = 1092.95, Dc = 2.540 g/cm3, F(000) = 2040, μ = 9.173 mm-1 and Z = 4. The final R = 0.0324 and wR = 0.0767 for 5299 observed reflections (I > 2σ(I)). Complex 1 displays an unusual three-dimensional (4,6)-connected network with (48.66.8)2(44.62)2(42.84) topology, which is different from [Tb(HBDC)(BDC)(H2O)4]·3.3H2O (BDC = isophthalate) because the -Br substituent of isophthalate results in different electronic effect and steric hindrance to change the coordination modes of carboxylate groups in the assembly process. Moreover, luminescent properties of 1 have also been investigated in the solid state.     

Synthesis and Crystal Structure of a New Cadmium（Ⅱ） Coordination Polymer with Ethylenediaminetetraacetic Acid

A new cadmium(Ⅱ) coordination polymer,namely,[KCd2(edta)I]n(1,H4edta = ethylenediaminetetraacetic acid),has been prepared and structurally characterized by single-crystal X-ray diffraction.Crystallographic data for 1:C10H12Cd2IKN2O8,Mr = 679.02,monoclinic,space group P21/n,a = 9.870(5),b = 8.989(4),c = 19.082(10) ,β = 104.581(10)o,V = 1638.5(13) 3,Z = 4,Dc = 2.753 g/cm3,μ = 4.776 mm-1,F(000) = 1272,the final R = 0.0473 and wR = 0.1311 for 2846 observed reflections with I > 2σ(I).Polymer 1 features a 2-D layered structure,in which each edta4-ligand chelates/bridges five adjacent six-/seven-coordinated Cd(Ⅱ) centers with all ten donors(eight oxygen and two nitrogen) involved with coordination.Additional iodide I-ions as counterions are bound to the Cd(Ⅱ) centers in a terminal mode and the potassium K+ ions are located in the layers and surrounded by O and I atoms from neighboring environment.The thermal stability of 1 has been discussed.     

Synthesis and Crystal Structure of a Cobalt（Ⅱ） Coordination Polymer with Benzene-1,3,5-triacetate and 1,4-Di（1H-imidazol-1-yl）benzene

A novel coordination polymer, [Co3 (bta)2(dib)2]·4H2O (1, H3bta=benzene-1,3,5-triacetic acid, and dib=1,4-di(1H-imidazol-1-yl)benzene), has been hydrothermally prepared and characterized by IR spectroscopy, elemental analysis and single-crystal X-ray diffraction. The crystal is of triclinic system, space group Pī, with a=9.141(2), b=9.667(2), c=13.855(2), α=100.83(3), β=90.81(3), γ=100.94(3)°, V=1179.0(4)3 , C48H46N8O16Co3 , Mr=1167.72, Dc=1.645 g/cm 3 , F(000)=599, μ=1.127 mm-1 and Z=1. The final R=0.0634 and wR=0.1703 for 4291 observed reflections (I > 2σ(I)). In the title complex, the bta ligand acts as a four-dentate bridging ligand to link up cobalt atoms into a lamellar framework, which are further interlinked by the dib ligands to generate a binodal (3,8)-connected tfz-d net.     

Synthesis and Crystal Structure of 4,5-Bis（2-chloroethylthio）phthalonitrile

A novel phthalonitrile compound,[C12H10Cl2N2S2],has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction.The crystal belongs to the monoclinic system,space group P21/n with a = 10.6417(8),b = 7.5737(6),c = 18.2758(14),β = 105.2480(10)°,Mr = 317.24,V = 1421.12(19)3,Z = 4,Dc = 1.483 g/cm3,F(000) = 648,μ = 0.733 mm-1,R = 0.0173 and wR = 0.2183.In the structure,the C atoms of the aromatic ring,the two cyanide groups and the two S atoms are almost coplanar(maximum deviation from the mean plane = 0.049(7) ).Two potential weak intermolecular interactions of C-H…N and one type of π…π stacking interaction with a centroid-centroid separation of 3.751(8) stabilize the crystal structure.     

Hydrothermal Synthesis and Crystal Structure of a One-dimensional Copper（Ⅱ） Complex

A metal-organic coordination polymer [Cu(cbba)2(bix)]n(Hcbba = 2-(4'-chlorine-benzoyl)-benzoic acid,bix = 1,4-bis(imidazol-1-ylmethyl)-benzene) 1 has been hydrothermally synthesized and characterized by elemental analysis,IR,TG,UV and single-crystal X-ray diffraction.Blue crystals crystallize in the monoclinic system,space group C2/c with a = 26.127(3),b = 10.6143(14),c = 14.5676(19) ,β = 111.289(2),V = 3764.3(8) 3,C42H30Cl2CuN4O6,Mr = 821.14,Dc = 1.449 g/cm3,F(000) = 1684,Z = 4,μ(MoKα) = 0.777 mm 1,the final R = 0.0528 and wR = 0.1200 for 2241 observed reflections(I > 2(I)).The structure of 1 exhibits a one-dimensional chain-like structure.     

Synthesis and Crystal Structure of 2-Nitro-9,9-bis（methylpropionate）fluorine

The title compound of 2-nitro-9,9-bis(methylpropionate)fluorine (C21H21NO6 , Mr=383.39) was synthesized for the first time. Complete assignments were achieved by 1H NMR, IR, EI-MS, elemental analysis and single-crystal X-ray diffraction technique. The crystal belongs to monoclinic, space group P21/c with a=11.4581(15), b=10.3624(14), c=16.573(2) , β=96.629(2) o , V=1954.6(5) 3 , Z=4, Dc=1.303 g/cm 3 , μ=0.096 mm -1 , F(000) = 808, R =0.0493 and wR=0.1499 for 3107 observed reflections with I > 2σ(I). X-ray analysis reveals that three fused rings of the fluorene system are almost coplanar and the two ester groups are nearly perpendicular to the fused-ring system. Weak C-H O hydrogen bonding connects the molecules into centrosymmetric dimmers.     

Synthesis and Crystal Structure of 3-（4-Bromobenzyloxy）-6-morpholinopyridazine

The title compound 3-(4-bromobenzyloxy)-6-morpholinopyridazine(C15H16BrN3O2) was synthesized,and its crystal structure was studied.It crystallizes in the triclinic system,space group P with a = 8.3408(17),b = 8.8620(18),c = 10.832(2) ,α = 108.09(3),β = 91.28(3),γ = 100.90(3)°,Dc = 1.562 g/cm3,Z = 2,λ = 0.71073 ,μ(MoKα) = 2.769 mm-1,Mr = 350.22,V = 744.5(3) 3,F(000) = 356,the final R = 0.0522 and wR = 0.1366 for 2016 observed reflections with I > 2σ(I).In the crystal structure,the morpholine ring adopts a chair conformation with O(2) and N(3) atoms at the flap positions-0.656(7) and 0.622(6)  out of the mean plane formed by the other four C atoms,respectively.These molecules generate centro-symmetric dimers through intermolecular π-π interaction.     

Synthesis and Crystal Structure of a New μ-Oxamide Trimeric Hetero-tetranuclear Complex

1 INTRODUCTION The study of spin exchange interaction between metal centers through extended bridges is an active subject in the field of coordination chemistry[1～3]. Polynuclear complexes with extended ligand bri- dges are currently of considerable interest[4～6]. One of the best strategies to design and synthesize poly- nuclear species is ‘complex as ligand’ approach[4, 7]. The oxamide group is proved to be an interesting multiatomic bridge, linking metals in polynuclear complexes[8…     

A Fe(Ⅱ) Coordination Polymer Based on 1,10-Phenanthroline Derivative and Oxalic Acid:Synthesis,Structure,and Properties

A Fe-based coordination polymer,[Fe(C₂O_4)_0.5(4-NCP)]_n·2nH₂O (1,4-HNCP=2-(4-carboxyphenyl)-1H-imidazo(4,5-f)-(1,10)phenanthroline,H₂C₂O₄=oxalic acid),was hydrothermally synthesized and characterized by infrared spectrum,elemental analysis,single-crystal X-ray diffraction,power X-ray diffraction,and UV-vis absorption spectrum.Structural analyses reveal that polymer 1 possesses a (4,4)-connected 2D network.In addition,1 shows photocatalytic activity toward the degradation of rhodamine B (RhB) in the presence of H₂O₂ under visible light illumination.     

Synthesis, Crystal Structure and Electrochemical Properties of a One-dimensional Chain Coordination Polymer [Mn（phen）（2,4,6-TMBA）2（H2O）]n

A one-dimensional chain-like coordination polymer [Mn(phen)(2,4,6-TMBA)2(H2O)]n has been synthesized from 2,4,6-trimethylbenzoic acid, 1,10-phenanthroline and anhydrous manga- nese(Ⅱ ) sulfate and then characterized. Crystal data for this complex: tetragonal, space group I41, a = 2.05643(16), b = 2.05643(16), c = 1.3939(2) nm, V = 5.8946(11) nm3, Mr = 579.54, Z = 8, Dc = 1.306 g/cm3, μ(MoKα) = 0.490 mm-1, F(000) = 2424, S = 0.985, the final R = 0.0411 and wR = 0.0950. The Flack factor is -0.01(2). The crystal structure shows that two neighboring man- ganese(Ⅱ ) ions are linked together by one bridge-chelating 2,4,6-trimethylbenzoic group, forming a one-dimensional chain structure. The manganese(Ⅱ ) ion is coordinated with two nitrogen atoms of one 1,10-phenanthroline, three oxygen atoms from three 2,4,6-trimethylbenzoic acids and one water oxygen atom, giving a distorted octahedral coordination geometry. The cyclic voltametric behavior of the complex was also investigated.     

Synthesis and Crystal Structure of 3,3＇-（4-Dimethylaminobenzylidene）- bis-（4-hydroxycoumarin）

The title compound 3,3'-(4-dimethylaminobenzylidene)-bis-(4-hydroxycoumarin) 3 was synthesized by the reaction of 4-hydroxycoumarin with 4-dimethylaminobenzaldehyde, and its chemical structure was determined by X-ray single-crystal diffraction. It crystallizes in monoclinic, space group P21/n with a = 11.698(2), b = 10.882(2), c = 16.594(3) , β = 90.69(3)o, V = 2112.1(7) 3, Z = 4, F(000) = 952, Dc = 1.432 Mg/m3, Mr = 455.45, μ = 0.102 mm-1, λ = 0.71073 , the final R = 0.0779 and wR = 0.2143 for 3031 observed reflections with I > 2σ(I).     

Two-dimensional Grid-type Zinc（Ⅱ） Coordination Polymer Constructed by a New Aromatic Carboxylate Ligand

A new aromatic carboxylate ligand,namely 5-(pyrrolidin-1-yl)-1,3-benzenedicar-boxylic acid(H2pybdc),was synthesized and characterized by FT-IR and single-crystal X-ray diffraction analysis.It crystallizes in triclinic system,P1 space group with a = 10.05(5) ,b = 11.53(5),c = 12.92(6) ,α = 112.11(6)°,β = 92.79(7)°,γ = 102.98(7)°,V = 1337.113,Z = 4,Mr = 253.25,Dc = 1.258 g.cm-3,μ = 0.099 mm-1,F(000) = 536,the final R = 0.0822 and wR = 0.2575 for 1893 observed reflections(I >2σ(I)).Based on it,a two-dimensional grid-type Zn(Ⅱ) coordina-tion polymer of {[Zn(pybdc)(bpy)(H2O)].2H2O.0.5CH3OH}n(1) was solvothermally synthesized,which crystallizes in triclinic,space group P1 with a = 10.218(5) ?,b = 11.176(5) ,c =11.350(5) ,α = 95.855(5)°,β = 94.248(5)°,γ = 101.421(5)°,V = 1257.9(2) 3,Z = 2,Mr = 524.84,Dc = 1.386 g.cm-3,μ = 1.024 mm-1,F(000) = 546,the final R = 0.0635 and wR = 0.1879 for 3913 observed reflections(I >2σ(I)).     

Synthesis and Crystal Structure of Bis（barbiturato） triwater Complex of Copper（Ⅱ）

1 INTRODUCTION A variety of transition metal complexes with barbiturates have been prepared owing to their important roles in clinical detection and identi- fication of drug[1～5]. They have the general formula of M(Ⅱ)(barb)2L2, where M is a transition metal (Co, Cr, Zn, Cu etc), barb the anion of a substituted barbituratic acid and L an organic base, usually pyridine. In these complexes, the donor atom in the barbiturate anion is a deprotonated nitrogen atom and, the coordination …