Solvothermal Synthesis,Crystal Structure and Electrochemical Property of Complex [Co(p-MBA)_2(2,2′-bipy)(H_2O)]·(H_2O)

One novel complex [Co(p-MBA)2(2,2′-bipy)(H2O)]·(H2O) has been synthesized by the reaction of p-methylbenzoic acid with 2,2′-bipyridine in the solvent mixture of water and methanol. It crystallizes in triclinic,space group P1 with a=0.70479(14),b=1.1211(2),c=1.6718(3) nm,α=103.806(3),β=90.795(3),γ=104.207(3)o,V=1.2399(4) nm3,Mr=512.41,Dc=1.373 g/cm3,Z=2,F(000)=532,μ=0.733 mm-1,R= 0.0432 and wR=0.0957. The crystal structural analysis shows that the cobalt atom is coordinated with three oxygen atoms from two p-methylbenzoic acids and one water molecule and two nitrogen atoms from one 2,2′-bipyridine,forming a distorted square-pyramidal coordination geometry. The cyclic voltammetry behavior of the complex is also reported.     

Syntheses and Crystal Structures of Two Cadmium(Ⅱ) Compounds Linked by N,N-Bis(3-pyridylmethyl)amine

Two cadmium(Ⅱ) compounds linked by a flexible dipyridyl ligand {[Cd2(Hbpma) Cl5(H2O)]·2H2O}n 1 and [Cd(Hbpma)Cl(H2O)2]2·2SO4·3H2O 2 (bpma = N,N-bis(3-pyridylmethyl)amine) have been synthesized and structurally characterized by single-crystal X-ray diffraction. Complex 1 crystallizes in triclinic, space group P with a = 9.5612(6), b = 11.3401(7), c = 11.5069(12), α = 112.8540(10), β = 106.5330(10), γ = 101.6680(10)°, V = 1030.77(14)3, C12H20Cd2Cl5N3O3, Mr = 656.36, Z = 2, Dc = 2.115 g/cm3, μ(MoKα) = 2.727 mm-1, F(000) = 636, S = 1.059, the final R = 0.0319 and wR = 0.0822 for 3443 observed reflections (I > 2σ(I)). For complex 2, it belongs to triclinic, space group P with a = 10.9487(4), b = 11.4197(4), c = 15.4288(5), α = 94.7470(10), β = 104.1000(10), γ = 104.42°, V = 1790.76(11)3, C24H42Cd2Cl2N6O15S2, Mr = 1014.46, Z = 2, Dc = 1.881 g/cm3, μ(MoKα) = 1.529 mm-1, F(000) = 1020, S = 1.050, the final R = 0.0178 and wR = 0.0451 for 6026 observed reflections (I > 2σ(I)). Complex 1 is found to have tetranuclear Cd(Ⅱ) clusters which are bridged by the protonated bpma ligands leading to one-dimensional coordination polymers, whereas complex 2 consists of binuclear Cd(Ⅱ) structures linked by the protonated bpma ligands. Both complexes are assembled into three-dimensional supramolecular structures through hydrogen bonding interactions.     

Synthesis and Crystal Structure of [Zn(FcCOO)2(2,2′-bipy)(H2O)]2·H2O

A novel complex [Zn(FcCOO)2(2,2′-bipy)(H2O)]2·H2O (Fc = (η5-C5H5)Fe(η5-C5H4), 2,2′-bipy = 2,2′-bipyridine) has been synthesized and characterized by elemental analysis, IR and X-ray diffraction. It crystallizes in monoclinic system, space group P21/c with a = 6.8187(4), b = 21.7155(13), c = 19.7411(12) (A), α = 90, β = 97.7420(10), γ = 90°, C64H58Fe4Zn2N4O11, Mr = 1413.28, V = 2896.4(3) (A)3, Dc = 1.620 g/cm3, Z = 2, F(000) = 1444, μ(MoKα) = 1.857 mm-1, R = 0.0523 and wR = 0.0982 for 3219 observed reflections (I ＞ 2σ(I)). Structural analysis shows that the zinc atom is coordinated with three oxygen atoms from two ferrocenemonocarboxylates and one water molecule together with two nitrogen atoms from 2,2′-bipyridine, giving a distorted square-pyramidal coordination geometry. The complex molecules are linked to form an infinite one-dimensional chain by both intermolecular hydrogen bonds and π-π stacking interactions of the bipyridine rings.     

Solvothermal Synthesis, Crystal Structure and Electrochemical Property of Complex [Co(p-MBA)2(2,2'-bipy)(H2O)]·(H2O)

One novel complex [Co(p-MBA)2(2,2'-bipy)(H2O)]·(H2O) has been synthesized by the reaction of p-methylbenzoic acid with 2,2'-bipyridine in the solvent mixture of water and methanol. It crystallizes in triclinic, space group P-1 with a=0.70479(14), b=1.1211(2), c=1.6718(3) nm, α=103.806(3), β=90.795(3), γ=104.207(3)°, V=1.2399(4) nm3, Mr=512.41, Dc=1.373 g/cm3, Z=2, F(000)=532, μ=0.733 mm-1, R=0.0432 and wR=0.0957. The crystal structural analysis shows that the cobalt atom is coordinated with three oxygen atoms from two p-methylbenzoic acids and one water molecule and two nitrogen atoms from one 2,2'-bipyridine,forming a distorted square-pyramidal coordination geometry. The cyclic voltammetry behavior of the complex is also reported.     

Synthesis, Structure and Luminescent Properties of Polymeric Copper（Ⅰ） Halide Complexes Bearing Phosphine and N-donor Bridging Ligands

Three polymeric copper(I) halide complexes bearing phosphine and N-donor bridging ligands,[(PPh3)2Cu2(μ-Br)2(μ-4,4′-bipy)]∞ 1 (bipy=bipyridine),[(PPh3)2Cu2(μ-Br)2(μ-bpe)]∞ 2 (bpe=trans-1,2-bis(4-pyridyl)ethene) and [(PPh3)2Cu2(μ-Cl)2(μ-bpe)]∞ 3,were synthe-sized by the multilayer diffusion method,and the structures were refined by single-crystal X-ray diffraction. Complex 1 crystallizes in triclinic,space group P1 with a=9.122(3),b=9.322(3),c=13.201(4),α=106.440(4),β=105.965(5),γ=94.167(5)°,V=1021.3(6) 3,Mr=967.62,Z=1,Dc=1.573 g/cm3,F(000)=486,μ=3.111 mm-1,the final R=0.0383 and wR=0.0960 for 2792 observed reflections (I > 2σ(I)). Complex 2 crystallizes in triclinic,space group P1 with a=9.420(3),b=10.209(4),c=12.407(4),α=104.136(6),β=108.132(5),γ=95.338(6)°,V=1081.0(7) 3,Mr=496.83,Z=2,Dc=1.526 g/cm3,F(000)=500,μ=2.941 mm-1,the final R= 0.0445 and wR=0.1117 for 3251 observed reflections (I > 2σ(I)). Complex 3 crystallizes in triclinic,space group P1 with a=8.32(1),b=11.53(2),c=13.94(3),α=109.57(3),β=93.85(3),γ= 97.28(3)°,V=1242(4) 3,Mr=1074.59,Z=1,Dc=1.436 g/cm3,F(000)=548,μ=1.279 mm-1,the final R=0.0786 and wR=0.1586 for 2266 observed reflections (I > 2σ(I)). The complexes exhibit intensive solid-state photoluminescence tentatively assigned to an admixture of triplet intraligand (IL) and metal-to-ligand charge-transfer (MLCT) excited 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.     

Construction of a Set of Cadmium（Ⅱ） Coordination Polymers with Atza and 2,2′-Bipy or 1,10-Phen Ligands （Atza=5-Aminotetrazole-1-acetato Anion）

Reactions of CdX2(X=NO3-, ClO4-) with Hatza (atza=5-aminotetrazole-1-acetato anion) and 2,2′-bipyridine (2,2′-bipy) or 1,10-phenanthroline (1,10-phen) in a methanol/aqueous solution produced a set of new Cd(Ⅱ) coordination polymers, {[Cd(atza)(H2O)(2,2′-bipy)]ClO4}n (1), {[Cd(atza)(H2O)(1,10-phen)]ClO4 }n (2), {[Cd(atza)(H2O)(2,2′-bipy)]NO3}n (3) and {[Cd(atza)2 (1,10-phen)]·0.5H2O}n (4). Single-crystal X-ray diffraction analysis reveals that each Cd(Ⅱ) ion has a distorted octahedral coordination geometry in 1-4, and the Cd(Ⅱ) ion centers are connected through the tridentate atza bridging ligands to form a 2D layer (1-3) or ID chain (4) structure. The fluorescent properties of 2 and 4 are also discussed.     

Synthesis, Crystal Structure and Fluorescene of a One-dimensional Compound {CdI_2(2,2′-bipy)}_n

The title compound, {CdI2(2,2′-bipy)}n, was prepared by the hydrothermal reac- tion of CdI2 and 2,2′-bipy in an aqueous solution, and its crystal structure was determined by X-ray single-crystal analysis. Crystallographic data for 1: C10H8N2CdI2, monoclinic system, space group C2/c, a = 16.927(1), b = 10.0925(7), c = 7.7422(3) , β = 106.0629(4)°, V = 1271.00(14) 3, Z = 4, F(000) = 944, μ = 6.546 mm-1, Dc = 2.730 g/cm3, Mr = 522.38, the final R = 0.0309 and wR = 0.0805 for 1310 observed reflections (I > 2σ(I)). X-ray crystal structure analysis shows that the Cd atom is coordinated by four iodines and two N atoms from one 2,2′-bipy to form an 1-D chain-like structure through bridging iodines. The fluorescene of the title compound was also discussed.     

Hydrothermal Synthesis and Crystal Structure of a New One-dimensional Nickel(Ⅱ) Complex with 2-Pyridinecarboxyic Acid and 4,4′-Bipyridine Ligands

A new metal-organic coordination polymer [Ni[(2-pya)2(4,4′-bipy)]n·6nH2O (2-pya = 2-pyridinecarboxylic acid, 4,4′-bipy = 4,4′-pyridine) 1 has been hydrothermally synthesized and structurally characterized by elemental analysis, IR spectrum, TG and single-crystal X-ray diffraction. The complex crystallizes in tetragonal, space group I41/a with a = b = 22.5642(19), c = 10.7118(18), V = 5453.8(11) 3, C22H28N4NiO10, Mr = 567.19, Dc = 1.382 g/cm3, μ(MoKα) = 0.769 mm-1, F(000) = 2368, Z = 8, the final R = 0.0572 and wR = 0.1254 for 1401 observed reflections (I > 2σ(I)). It exhibits a one-dimensional chain-like structure by mixed ligands of 2-pyridinedicarboxylic acid and 4,4′-pyridine.     

Synthesis and Crystal Structure of a Manganese(Ⅱ) Complex with 2-(4'-Chlorine-benzoyl)-benzoic Acid and 1,10-Phenanthroline

A new metal-organic complex Mn2(cbba)4(phen)2 (Hcbba = 2-(4'-chlorine-benzoyl)-benzoic acid, phen = 1,10-phenanthroline) 1 has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction, elemental analyses and IR spectroscopy. The compound crystallizes in orthorhombic, space group Pbcn with a = 12.154(5), b = 18.166(7), c =31.197(13) (A°), V = 6887(5) (A°)3, C80H48C14Mn2N4O12, Mr= 1508.90, Dc = 1.455 g/cm3, μ(MoKa) =0.591 mm-1, F(000) = 3080, Z = 4, the final R = 0.0408 and wR = 0.0873 for 4033 observed reflections (I > 2σ(I)). In the crystal structure, the manganese atom is six-coordinated with four carboxylate oxygen atoms from three different cbba ligands and two nitrogen atoms from phen ligands, showing a distorted octahedral geometry. Furthermore, it exhibits a 3D supramolecular network through π-π interactions.     

Syntheses and Crystal Structures of Two Complexes with 3-（3-Pyridyl）acrylic Acid

1 INTRODUCTION A recent feature in the development and progress of chemical research is the concern for molecular assemblies, ensembles, and all of structural aggre- gates[1]. The self-assembly of transition metal ions and N-containing organic ligands has been proven a popular approach for the construction of supramo- lecular architecture[2～7]. 3-(3-Pyridyl)acrylic acid is an excellent ligand, not only due to its prolific coor- dination sites but also to its potential hydrogen bon- ding…     

铜配合物[Cu(2,2''''-bipy)(pydco)(H2O)]·4H2O的合成与晶体结构

配合物[Cu(2,2’-bipy)(pydco)(H2O)].4H2O(2,2’-bipy=2,2’联吡啶,pydco=氮氧化-2,6-二甲酸吡啶)的结构由X-射线测定,配合物属三斜晶系,P墿空间群,晶胞参数:a=0.68120(14),b=1.1850(2),c=1.2554(3)nm,α=86.06(3),β=81.60(3),γ=86.16(3)°,V=0.99854(4)nm3,Z=2。2,2’联吡啶提供两个配位原子(N1,N2),氮氧化-2,6-二甲酸吡啶提供两个配位氧原子以及一个配位水提供一个氧原子参与了配位,中心Cu(II)离子是一个畸变的四角锥结构。有趣的是,配合物的结晶水组成了一条条的水带,配合物分子正是由这些水带中的氢键连接在一起的。     

Synthesis, Crystal Structure and Fluorescene of a One-dimensional Compound {CdI2（2,2＇-bipy）}n

The title compound, {CdI2(2,2'-bipy)}n, was prepared by the hydrothermal reaction of CdI2 and 2,2'-bipy in an aqueous solution, and its crystal structure was determined by X-ray single-crystal analysis. Crystallographic data for 1: C10H8N2CdI2, monoclinic system, space group C2/c, a = 16.927(1), b = 10.0925(7), c = 7.7422(3) (A), β = 106.0629(4)°, V = 1271.00(14)(A)3, Z = 4, F(000) = 944, μ = 6.546 mm-1, Dc= 2.730 g/cm3, Mr = 522.38, the final R = 0.0309 and wR = 0.0805 for 1310 observed reflections (I＞2σ(Ⅰ)). X-ray crystal structure analysis shows that the Cd atom is coordinated by four iodines and two N atoms from one 2,2'-bipy to form an 1-D chain-like structure through bridging iodines. The fluorescene of the title compound was also discussed.     

Hydrothermal Synthesis, Crystal Structure and Fluorescent Property of a Keggin Polyoxometalate [CuI(2,2''-bipy)2]3[PWⅥ12O40]

A Keggin-type tungstohosphate compound [CuI(2,2'-bipy)2]3[PWVI12O40] 1 (bipy = bipyridine) was prepared by the hydrothermal method for the first time. Single-crystal X-ray diffraction revealed that 1 (C60H48Cu3N12O40PW12) crystallizes in the monoclinic system, space group P21/c with a = 16.9837(10), b = 17.9732(13) c = 27.8701(13)(A), β = 96.1039(10)°, V = 8459.2(9)(A)3, Mr = 4004.89, Z = 4, Dc = 3.145 g/cm3, μ = 17.089 mm-1, F(000) = 7208, S = 1.005, the final R = 0.0469 and wR = 0.0827 for 10807 observed reflections (I > 2σ(I)). Compound 1 consists of one discrete normal Keggin polyanion [PWVI12O40]3- and three isolated coordinated cat- ions [CuI(2,2'-bipy)2]+. Significantly, there exist three crystallographically independent asymmetric reduced copper (I) centers in 1. Furthermore, the compound shows strong photoluminescence property in solid state at room temperature.     

A Copper（Ⅱ）-cadmium（Ⅱ） Heterometallic Hexanuclear Complex：[Cd_4Cu_2（pdc）_4（H_2O）_（14）]（H_3pdc=3,5-Pyrazoledicarboxylic Acid）

The title complex 1,[Cd 4 Cu 2 (pdc) 4 (H 2 O) 14 ] (H 3 pdc=3,5-pyrazoledicarboxylic acid),has been solvothermally synthesized and structurally characterized by single-crystal X-ray diffraction.Complex 1 crystallizes in triclinic,space group P1 with a=0.67235(10),b=1.27935(18),c=1.28569(17) nm,α=112.633(2),β=102.971(3),γ=97.089(2)o,V=0.9673(2) nm 3,C 20 H 32 Cd 4 Cu 2 N 8 O 30,M r=1441.22,D c=2.474 g/cm 3,μ(MoKα)=3.356 mm 1,F(000)=698,S=1.003,Z=1,the final R=0.0471 and wR=0.0748 for I > 2σ(Ⅰ).In 1,two deprotonated 3,5-pyrazoledicarboxylic acids (pdc 3),one copper(Ⅱ) ion and one cadmium(Ⅱ) ion firstly form a pyrazole-bridged Cu II Cd II dinuclear unit,two of which related by an inversion center are connected by another two cadmium(Ⅱ) ions through chelating carboxylate groups to construct the copper(Ⅱ)-cadmium(Ⅱ) heterometallic hexanuclear complexes.Plenty of hydrogen bond interactions existing in the system further lead to a three-dimensional (3D) supramolecular framework.     

Synthesis, Crystal Structure and Luminescent Property of [Zn(C12H9O3)2(C10H8N2)]n·nH2O

Under hydrothermal condition, the reaction of 2-naphthoxyacetic acid with ZnCl2 and 4,4'-bipyridine (4,4'-bipy)has afforded a new Zn(Ⅱ) compound,[Zn(C12H9O3)2(C10H8N2)]n·nH2O1, which was structurally characterized by single-crystal X-ray diffraction analysis. The crystal is of monoclinic, space group P21/c with a = 7.7335(2), b = 19.3834(4), c = 20.1707(4) (A), β =104.9830(10)°, V = 2920.82(11) A3, C34H28ZnN2O7, Mr = 641.95, Z = 4, Dc = 1.460 g/cm3, μ = 0.895 mm-1, F(000) = 1328, R = 0.0406 and wR = 0.0876 for 4417 observed reflections (Ⅰ>2σ(Ⅰ)). Complex 1 consists of one-dimensional zigzag chains deriving from Zn(C12H9O3)2 units linked by 4,4'-bipy ligands, and lattice water molecules decorate between the chains. Non-covalent interactions, such as hydrogen-bonding and aromatic π-π interactions, lead to the formation of a 3D network structure. The thermogravimetric analysis (TGA) and luminescent property for 1 have also been studied in this paper.     

Hydrothermal Synthesis and Crystal Structure of a Cadmium（Ⅱ） Polymer with a Two-dimensional Network Structure： [ Cd（pzdc）（2,2＇-bipy） ]n·nH2O

A metal-organic coordination compound formulated as [Cd（pzdc）（2,2＇-bipy）]n·nH2O 1 （Hzpzdc = pyrazine-2,3-dicarboxylic acid, 2,2＇-bipy = 2,2＇-bipyridine） has been hydrothermally synthesized and structurally characterized by elemental analysis, IR, TG fluorescence spectrum and single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group P2 1/c with a = 10.8081（13）, b = 14.4328（17）, c = 10.2530（12） A, β = 98.504（2）°, V= 1581.8（3） ]A3, C16H14CdN4O5, Mr= 454.71, Dc = 1.909 g/cm^3, μ（MoKa） = 1.420 mm^-1, F（000） = 904, Z = 4, the final R = 0.0230 and wR = 0.0554 for 2901 observed reflections （I 〉 2σ（I））. It exhibits an interesting two-dimensional network structure and shows yellow photoluminescent property at room temperature.     

二苯乙醇酸铜配合物的合成、晶体结构、电化学和荧光性质

以二苯乙醇酸为配体合成了1个新的化合物[Cu(2,2′-bipy)(BAA)][Cu(2,2′-bipy)(BAA)(H2O)]2.(H2O)3(BAA=二苯乙醇酸阴离子,2,2′-bipy=2,2′-联吡啶)。该化合物晶体属三斜晶系,空间群P1,晶胞参数:a=1.121 7(5)nm,b=1.360 2(6)nm,c=2.335 2(10)nm,α=99.260(6)°,β=101.223(8)°,γ=94.805(8)°,V=3.425(3)nm3,Dc=1.385 g.cm-3,Z=6,μ(Mo Kα)=0.992 mm-1,F(000)=1 474,最终偏离因子R1=0.0561,wR2=0.1128。在标题化合物的不对称单元中有3个单核铜(Ⅱ)配合物,且3个中心铜(Ⅱ)离子的配位数不完全相同,如Cu(1)离子的配位数是4,而Cu(2)和Cu(3)离子的配位数都是5。本文还测定了标题化合物的电化学性能和荧光性能,结果表明:在电化学过程中配合物的电子转移是准可逆的,电子转移数为2个;配合物在478 nm的光激发下可发射荧光。     

Synthesis,Crystal Structure and Fluorescence Property of a New Trinuclear Nickel(Ⅱ) Complex Bridged by 2,6-Pyridine Dicarboxylic Acid

A new trinuclear nickel complex,[Ni3(pdc)3(2,2'-bipy)3(H2O)2]·2H2O(H2pdc = pyridine 2,6-dicarboxylic acid,2,2'-bipy = 2,2'-bipyridine) has been hydrothermally synthesized and characterized by IR,elemental analysis and X-ray diffraction methods.Crystal data for this complex:monoclinic,space group P21/n,a = 21.206(4),b = 10.002(2),c = 28.066(6),β = 108.18(3)°,C51H41N9Ni3O16,Mr = 1212.06,V = 5.656(2) nm3,Dc = 1.423 g·cm-3,μ(MoKα) = 1.062 mm-1,Z = 4,F(000) = 2488,GOOF = 1.034,the final R = 0.0543 and wR = 0.1237 for 6149 observed reflections with Ⅰ 2σ(Ⅰ).In the complex,three nickel(Ⅱ) ions are bridged by the pyridine 2,6-dicarboxylic acid groups,and all nickel(Ⅱ) ions are seven-coordinated by nitrogen atoms of 2,2'-bipyridine and pyridine 2,6-dicarboxylic acid and oxygen atoms from pyridine 2,6-dicarboxylic and water to adopt a severely distorted pentagonal bipyramidal geometry.The emission and excitation peaks of the complex in ethanol solutions are located at 336 and 316 nm,respectively.     

一维链状配位聚合物[Cd{5-(NO2)sal}2(2,2'-bipy)]n的合成与晶体结构

A coordination polymer of [Cd{5-(NO2)sal}2(2,2'-bipy)]n (5-(NO2)sal=5-nitrosalicylate, 2,2'-bipy=2,2'-bipyridine) was synthesized by hydrothermal reaction and characterized by elemental analysis, IR and X-raydiffraction single crystal structure analysis. The title complex crystallizes in monoelinic with space group C2/c, a=2.730 8(16) nm, b=1.272 3(5) nm, c=0.674 5(3) nm,β=96.73(2)°, V=2.327(2) nm3, Z=4, R=0.022 2, wR=0.057.The 5-nitrosalicylate anions doubly bridge the Cd(Ⅱ) atoms to form one-dimensional polymeric chain with therepeated eight-membered ring units (Cd-O-C-O)2. The crystal structure is stabilized by intra- and interchainhydrogen bonds interactions.