配合物[Mn2(α-Furacrylic radical)4(phen)2(H2O)]·H2O的合成、晶体结构及热稳定性

One novel manganese(Ⅱ) complex [Mn2(α-Furacrylic radical)4(phen)2(H2O)]·H2O with α-furacrylic acid radical and 1,10-phenanthroline has been synthesized and characterized. Crystal data for this complex:monoclinic,space group C2/c,a=1.082 34(16)nm,b=2.445 8(4) nm,c=1.857 4(3) nm,β=104.353(2)°,V=4.763 5(12) nm3,Dc=1.471 g·cm-3,Z=4,F(000)=2 168. Final GooF=1.004,R1=0.039 7,wR2=0.108 7. The crystal structure shows that two neighboring manganese(Ⅱ) ions are linked together by two bridging α-furacrylic acid radicals and one bridging water molecule,forming a cage structure. The Mn(1)…Mn(1A) bond distance is 0.357 6 nm. Each manganese(Ⅱ) ion is coordinated with two nitrogen atoms of one 1,10-phenanthroline molecule and four oxygen atoms from three α-furacrylic acid radicals and one water molecule,forming distorted octahedral coordination geometry. Thermal stability of the complex was also discussed.     

Synthesis, Crystal Structure and Properties of a Dinuclear Cobalt（II） Complex [Co2（a-furacrylato）4（Phen）2（H2O）]·C2H5OH

A dinuclear cobalt(Ⅱ) complex [Co2(α-furacrylato)4(Phen)2(H2O)]·C2H5OH has been synthesized with α-furacrylic acid and 1,10-phenanthroline as the ligands, and its crystal structure was determined. The crystal is of monoclinic system, space group C2/c with a=1.07388(8), b=2.4300(2), c=1.86708(14)nm, β=104.3830(10)o, V=4.719.4(7) nm3 , Dc=1.503 g/cm3 , Z=2, F(000)=2196, GOOF=1.053, the final R=0.0343 and wR=0.0883. The crystal structure shows that two neighboring cobalt(Ⅱ) ions are linked by the bridging coordination of two α-furacrylic acid anions and one water molecule, and their end positions are respectively coordinated with two 1,10-phenanthroline molecules and two α-furacrylic acid anions, forming a dinuclear structure. Both cobalt(Ⅱ) ions adopt hexa-coordinated distorted octahedral geometry. The electrochemical and fluorescence properties of the title complex are also discussed.     

Hydrothermal Synthesis, Crystal Structure and Electrochemical Properties of Complex Mn2（phen）2（p-CBA）4（H2O）

One novel complex Mn2(phen)2(p-CBA)4(H2O) has been hydrothermally syn- thesized from p-chlorobenzoic acid (p-CBA), 1,10-phenanthroline (phen) and anhydrous man- ganese(Ⅱ) sulfate and then characterized. Crystal data for this complex: monoclinic, space group C2/c, with a = 2.3416(3), b = 1.5604(2), c =1.5605(2) nm, β = 121.048(2)o, V = 4.8849(12) nm3, Dc = 1.510 g/cm3, Mr = 555.26, Z = 8, μ = 0.798 mm-1, F(000) = 2256, GOOF = 1.032, the final R = 0.0393 and wR = 0.0816. The crystal structure shows that two neighboring manganese(Ⅱ ) ions are linked together by two bridge-chelating p-chlorobenzoic groups and one bridging water molecule, forming a cage structure with the Mn–Mn bond distance of 0.3512 nm. Each manganese(Ⅱ ) ion is coordinated by two nitrogen atoms of one 1,10-phenanthroline molecule and four oxygen atoms from three p-chlorobenzoic acid anions and one water molecule, giving a distorted octahedral coordination geometry. The cyclic voltammetric behavior of the complex was also investigated.     

Hydrothermal Synthesis,Crystal Structure and Thermal Stability of a Binuclear Copper（Ⅱ） Complex with 3-（Pyridin-2-yl）-1,2,4-triazole

One novel binuclear copper(Ⅱ) complex [Cu 2 (Hpt) 2 (CO 3) 2 (H 2 O) 2 ]·H 2 O with copper carbonate and 3-(pyridin-2-yl)-1,2,4-triazole (Hpt) was hydrothermally synthesized and characterized by IR and X-ray diffraction analysis.The complex crystallizes in triclinic,space group P2 1 /n with a=0.6862(1),b=0.7805(1),c=1.1983(2) nm,α=72.03(2),β=107.72(3),γ=75.28(2)o,V=0.5884 nm 3,D c=2.105 g/cm 3,Z=1,F(000)=357,GOOF=1.041,the final R=0.01859 and wR=0.04348.The whole molecule is composed of two cooper ions,two Hpt molecules,two carbonate and three water molecules,forming a binuclear structure.The crystal structure shows that the cooper ion is coordinated with three nitrogen atoms from two Hpt molecules,two oxygen atoms from one carbonic acid and one water molecule,forming a distorted square pyramidal geometry.The TG analysis result shows that the title complex is stable under 131.0 ℃.     

[Ni(phen)2(3,5-DMBA)](m-MBA)2(H2O)2配合物的合成、晶体结构及电化学分析

The title complex of nickel (II) with 3,5-dimethylbenzoic acid, m-methylbenzoic acid and 1,10- phenanthroline was synthesized and characterized. Crystal data for this complex: triclinic, space group P1, a=1.198 5(2) nm, b=1.315 3(2) nm, c=1.531 8(3) nm, α=92.602(3)°, β=103.292(3)°, γ=114.849(3)°, V=2.104 7(6) nm³, D_c=1.361 g·cm^-3, Z=2, F(000)=902, final GooF=1.071, R₁=0.067 2, wR₂=0.155 5. The crystal structure shows that the nickel ion is coordinated with four nitrogen atoms of two 1,10-phenanthroline molecules and two oxygen atoms of one 3,5-dimethyl benzoic acid molecule, forming a distorted octahedral coordination geometry. The cyclic voltametric behavior of the complex was also investigated. CCDC: 286966.     

苯四甲酸桥连的镍配合物[Ni(btec)(H2O)4][Ni(imi)2(H2O)4]·2H2O的合成及结构

At room temperature, a coordination polymer [Ni(btec)(H2O)4][Ni(imi)2(H2O)4]·2H2O was synthesized by reaction of NiCl2·6H2O, 1,2,4,5-benzenetetracarboxylic dianhydridc and imidazole in a water/THF solution. The structure was determined by X-ray diffraction crystal structure analysis. It crystallizes in triclinic P1 space group with the crystal cell parameters of a=0.67542 (2) nm, b=1.000 14 (1) nm, c=1.09088 (3) nm, α=74.140(2)°, β= 74.388(1)°, y=73.239(2)°, and V=0.664 09(3) nm3, Z=1. The crystal structure shows that Ni1 atom is coordinated by four water and two imidazole molecules, while Ni2 is coordinated by four water molecules and two carboxyl oxygen atoms. The 1,2,4,5-benzenetetracarboxylate ions bridge Ni2 coordination centers to form one-dimensional chain structure. Moreover, the chains are further linked together by hydrogen bonds to form a two-dimensional network. CCDC: 295873.     

Synthesis,Crystal Structure and Thermal Stability of Complex [Cu（C_（14）H_（10）O_4）（C_（12）H_8N_2）_2]·2H_2O

The title complex has been synthesized with 2,2'-biphenyl dicarboxylic acid and 1,10-phenanthroline(phen)in the solvent mixture of water and methanol.It crystallizes(C38H28CuN4O6,Mr = 700.1)in triclinic,space group P1 with a = 1.0868(2),b = 1.2175(2),c = 1.6206(3)nm,α = 110.161(2),β = 102.605(3),γ = 93.667(2)o,V = 1941.6(6)nm3,Dc = 1.198 g/cm3,Z = 2,F(000)= 722,R = 0.0558 and wR = 0.1208.The crystal structure shows that the copper atom is coordinated with one oxygen atom from 2,2'-bphenyl dicarboxylic acid molecule and four nitrogen atoms from two 1,10-phenanthroline molecules,forming a distorted square-pyramidal coordination.The TG analysis shows that the title complex is stable under 160.0 ℃.     

杂-双核配合物[CaCu(C3H2O4)2(H2O)4]n的合成、晶体结构及热稳定性

The title complex, [CaCu(C3H2O4)2(H2O)4]n, with a formula of C6H12CaCuO12 and Mr=379.78 has been sy-nthesized and characterized by single crystal X-ray diffraction structure analysis, elemental analysis, IR spectra and TG-DTG techniques. The results show that the crystal is Orthorhombic, space group Pbcn with a=0.669 21(5) nm, b=1.370 23(5) nm, c=1.322 39(10) nm, V=1.212 59(16) nm3, Dc=2.080 g·cm-3, μ=2.288 mm-1, F(000)=772 and Z=4. The final R=0.054 0 and wR=0.112 8 for 1 189 observed reflections with I>2σ(I). The structure of the title complex consists of CaO8 polyhedra and CuO6 elongated octahedra linked together by malonate ligands. The Ca(Ⅱ) cation, on a twofold axis, is coordinated by two water molecules and six malonate O atoms. The Cu(Ⅱ) cation, which lies in a centre of symmetry in an octahedral arrangement, is coordinated by four malonate O atoms and two water molecules. The structure comprises alternating layers along the [101] plane, with the shortest Cu…Cu distance of 0.762 46(6) nm. The whole 3D structure is maintained and stabilized by the presence of hydrogen bonds. Its thermo gravimetric analysis was determined by TG-DTG techniques. CCDC:663184.     

配合物[Cu(PTA)(phen)2]·(PTA)·(H2O)4的合成、晶体结构及电化学性质

The title complex has been synthesized by using terephthalic acid (PTA), 1,10-phenanthroline (phen) and copper monohydrate. It crystallizes in monoclinic space group C2/c with a=2.959 0(2) nm, b=1.466 4(10) nm, c=1.764 3(12) nm, β=105.593(11)°, V=7.372(9) nm³, Dc=1.489 g·cm^-3, Z=8, F(000)=3 416, R₁=0.043 6, wR₂= 0.151 9. The crystal structure shows that the copper atom is coordinated with four nitrogen atoms from two phens and one oxygen atom from one terephthalic acid, forming a distorted square-pyramid coordination geometry. The cyclic voltametric behavior of the complex is also reported. CCDC: 277047.     

配合物[Co(phen)2(m-chlorobenzoic acid)2·(H2O)]·(H2O)2的水热合成、晶体结构电化学分析

The title complex has been synthesized with m-chlorobenzoic acid, 1,10-phenanthroline and cobalt perchlorate anhydrous in the solvent mixture of water and methanol. Crystal data for this complex: triclinic, space group P1, a=0.870 7(3) nm, b=1.284 4(4) nm, c=1.692 9(5) nm; α=75.430(5)°, β=77.562(5)°, γ=86.346(5)°, V=1.789 4(9) nm³, D_c=1.456 g·cm^-3, Z=2, F(000)=806. Final GooF=1.065, R₁=0.068 4, wR₂=0.127 5. The crystal stru-cture shows that the Cobaly ion is coordinated with four nitrogen atoms from two 1,10-phenanthroline molecules and two oxygen atoms from one m-chlorobenzoic acid molecule and one water molecule respectively, forming a distorted octahedral coordination geometry. The cyclic voltametric behavior of the complex is also reported. CCDC: 619087.     

The synthesis and crystal structure of heteronuclear complex of lanthanide with sulfo-salicylic acid [Na3YLa2(C7H3SO6)4.26H2O]n

The titled complex has been synthesized by the reaction of sodium sulfo-salicylate with lanthanum and yttrium perchlorate. The crystal structure has been determined by single crystal X-ray diffractometry. The crystal is monoclinic with space group C2/c. The unit cell parameters are as follows: a=16.289(8), b=18.323(8), c=22.044(8) A, β=106.34(2)°, V=6314(6) A3, Z=4 and Dc=1.764 g/cm3. The structure was solved by direct method. The least-square refinement based on 3776 observed reflections [F > 6σ(F)] converged to a final R=8.6% and F(000) is 3548. Yttrium ion with eight-coordinate is located in central of the molecule, the two lanthanum ions with ten-coordinate are located at the two sides of yttrium ion. There are two positions for Na in the molecule, one is in the C2 axis with six coordinate, the other one is in a general position with five-coordinate.     

氢键构筑的二维网状结构镍配合物[Ni(en)2(dpas)2]的合成、晶体结构及电化学性质

A new 2D Hydrogen-bonded network complex [Ni(en)2(dpas)2] (Nadpas=sodium diphenylamine sulphonic acid salt,en=ethanediamine) has been synthesized in aqueous solution,and characterized by elemental analysis,IR. The crystal structure was determined by single-crystal X-ray diffraction. The complex crystallizes in space group P21/c,with cell parameters a=0.605 6(5)nm,b=1.448 1(5) nm,c=1.711 9(5)nm,β=93.257(5)°,and V=1.498 9(14) nm3,Dc=1.497 g·cm-3,Z=2,F (000)=708,R=0.027 7,wR=0.072 5. The crystal structure shows that the nickel atom is coordinated with four nitrogen atoms from the two en and two oxygen atoms from two dpas to form a mononuclear complex. Furthermore,the adjacent complex units are extended into a 2D supramolecular network through hydrogen bonds.     

草酸根桥联的双核铜(Ⅱ)配合物[Cu2(phen)2(H2O)2(μ2-C2O4)](NO3)2的合成及晶体结构

A new binuclear copper(Ⅱ) complex, [Cu₂(phen)₂(H₂O)₂(μ₂-C₂O₄)](NO₃)₂, has been synthesized and characterized by elemental analysis, IR and UV-Vis spectrum. Its crystal structure was determined by single crystal X-ray diffraction techniques. Crystal data: monoclinic, space group P2₁/c, a=0.712 21(8) nm, b=1.170 93(14) nm, c=1.783 7(2) nm, β=111.828(2)°, and V=1.380 8(3) nm³, D_c=1.769 Mg·m^-3, Z=2, F(000)=744, R₁=0.025 4, wR₂=0.069 5, Gof=1.077, Δρ=328～-455 e·nm^-3. The complex is packed by one centrosymmetry binuclear copper(Ⅱ) unit, oxalate dianion and NO₃^- anion. In the molecule structure of the title complex, two Cu(Ⅱ) ions are bridged by oxalate dianion and each Cu(Ⅱ) ions coordinates with two nitrogen atoms from 1,10-phenanthroline ligand and one oxygen atom from water to form a five-coordinate distorted square-pyramidal configuration. The hydrogen bonds are observed between coordinated water molecules and NO₃^- anions. The analysis of the crystal structure indicates that the complex has a two-dimensional stacking network structure, which is formed by intramolecular hydrogen bonds, intermolecular hydrogen bonds and stacking effect of aromatic ring. CCDC: 255345.     

Hydrothermal Synthesis and Crystal Structure of Complex Mn2（phen）2（p-MBA）4（H2O）

A novel Mn（Ⅱ） complex Mn2（phen）2（p-MBA）4（H2O） has been hydrothermally synthesized by the reaction of p-methyl benzoic acid （p-MBA） with 1,10-phenanthroline （phen）. Crystal data for this complex： monoclinic, space group C2/c, a= 2.3328（3）, b =1.5549（2）, c = 1.5557（2） nm, β = 121.726（2）°, V= 4.7997（11） nm^3, Mr = 1028.85, Dc = 1.424 g/cm^3, Z = 4, F（000） = 2128, μ（MoKa） = 0.590mm^-1, GOOF = 1.060, R = 0.0333 and wR = 0.0767. In the crystal, each Mn（Ⅱ） ion is coordinated by two nitrogen atoms from one o-phenanthroline molecule, three oxygen atoms from three p-methyl benzoic acids and one oxygen atom from one water molecule, giving a six-coordinate distorted octahedral coordination geometry. Two neighboring Mn（Ⅱ） ions are bridged by two p-methyl benzoic acid groups and one water molecule, and their end positions are respectively coordinated by one 1,10-phenanthroline and one p-methyl benzoic acid molecule, giving a binuclear cage structure, of which the Mn（Ⅱ）…Mn（Ⅱ） distance is 0.3502 nm.     

Synthesis, Crystal Structure and Thermal Stability of a Saturated Dimeric Ce(Ⅲ)-chelated Complex Based on Benzoate and 1,10-Phenanthroline Ligands

The title complex, [Ce(BA)3phen]2 (BA = benzoate, phen = 1,10-phenanthroline),was prepared by the reaction of Ce(NO3)3·6H2O, benzoic acid and 1,10-phenanthroline. The complex was characterized by single-crystal X-ray diffraction, elemental analysis, IR spectra and TG-DTG techniques. The results show that the crystal is of triclinic, space group P(1) with a =10.912(2), b = 11.962(3), c = 12.474(3)(A), a = 104.889(3), β = 93.523(3), γ = 113.332(3)°,C66H46Ce2N4O12, Mr = 1366.90, V= 1420.2(6) (A)3, Z = 1, Dc = 1.598 g/cm3,μ = 1.652 mm-1, S =1.024 and F(000) = 682. The final R = 0.0391 and wR = 0.0947 for 4878 observed reflections with I ＞ 2σ(1). The structure of the title complex consists of two Ce(C6H5COO)3(C12H8N2) units,forming a binuclear molecule. Each Ce(Ⅲ) is coordinated by two O atoms of one bidentate chelating carboxylate group, five O atoms of two bidentate bridging and two tridentate chelating-bridging carboxylate groups, and two N atoms of one 1,10-phenanthroline molecule to complete a distorted monocapped square antiprism geometry. Its thermogravimetric analysis was determined by TG-DTG techniques.     

Synthesis,Crystal Structure and Electrochemical Property of a Dinuclear Manganese（Ⅱ） Complex [Mn_2（C_（12）H_8N_2）_4（C_8H_5O_4）_2]（C_8H_4O_4）·H_2O

One dinuclear manganese(II)complex [Mn2(C12H8N2)4(C8H5O4)2](C8H4O4)·H2O has been synthesized with o-phthalic acid and 1,10-phenanthroline.The crystal structure was determined by X-ray diffraction.The crystal belongs to the triclinic system,space group P1 with a = 1.17767(3),b = 1.22292(2),c = 1.35860(3)nm,α = 110.5300(10),β = 97.6140(10),γ = 93.7300(10)o,V = 1.80307(7)nm3,Dc = 1.404 g/cm3,Z = 2,F(000)= 784,the final GOOF = 1.047,R = 0.0398 and wR = 0.1038.The crystal structure of the title complex consists of one [Mn2(C12H8N2)4(C8H5O4)2]2+ cation,one uncoordinate o-phthalate anion(C8H4O4)2-and one uncoordinate water molecule.In [Mn2(C12H8N2)4(C8H5O4)2]2+,the central Mn(II)ion is coordinated by four nitrogen atoms and two oxygen atoms to give a distorted octahedral coordination geometry.The electrochemical property of the title complex was also studied.     

Synthesis,Crystal Structure and Thermal Stability Properties of a Binuclear Copper(Ⅱ) Coordination Polymer {[Cu_2(4,4'-bipy)_2(o-ABA)_4(H_2O)_2][(H_2O)_2]}_n

One-dimensional chain copper(Ⅱ) coordination polymer has been synthesized and characterized in the solvent mixture of water and alcohol with o-acetamidobenzoic acid,4,4'-bipyridine and copper perchlorate.It is of tetragonal,space group P41212 with a=1.57756(10),b= 1.57756(10),c=2.1438(3)nm,V=5.3352(8) nm3,Dc=1.524 g/cm3,Z=4,F(000)=2536,R= 0.0479 and wR=0.0979.The crystal structure shows two coordination modes.The copper(1) is coordinated with two nitrogen atoms of one 4,4'-bipyridine molecule and two oxygen atoms from two o-acetamidobenzoic acid molecules,forming a distorted tetrahedral coordination geometry;the copper(2) is coordinated with two nitrogen atoms of one 4,4'-bipyridine molecule,four oxygen atoms from two o-acetamidobenzoic acid molecules and two water molecules,generating a distorted octahedral coordination geometry.The result of TG analysis shows that the title complex is stable below 180.0 ℃.     

Synthesis, Crystal Structure and Thermal Stability of a Saturated Dimeric Ce(III)-chelated Complex Based on Benzoate and 1,10-Phenanthroline Ligands

The title complex, [Ce(BA)3phen]2 (BA = benzoate, phen = 1,10-phenanthroline), was prepared by the reaction of Ce(NO3)3·6H2O, benzoic acid and 1,10-phenanthroline. The complex was characterized by single-crystal X-ray diffraction, elemental analysis, IR spectra and TG-DTG techniques. The results show that the crystal is of triclinic, space group P1 with a = 10.912(2), b = 11.962(3), c = 12.474(3) , α = 104.889(3), β = 93.523(3), γ = 113.332(3)o, C66H46Ce2N4O12, Mr = 1366.90, V = 1420.2(6) 3, Z = 1, Dc = 1.598 g/cm3, μ = 1.652 mm-1, S = 1.024 and F(000) = 682. The final R = 0.0391 and wR = 0.0947 for 4878 observed reflections with I > 2σ(I). The structure of the title complex consists of two Ce(C6H5COO)3(C12H8N2) units, forming a binuclear molecule. Each Ce(III) is coordinated by two O atoms of one bidentate chelating carboxylate group, five O atoms of two bidentate bridging and two tridentate chelating-bridging carboxylate groups, and two N atoms of one 1,10-phenanthroline molecule to complete a distorted monocapped square antiprism geometry. Its thermogravimetric analysis was determined by TG-DTG techniques.     

三维超分子化合物[Ag4(L)4](PMBS)4·2H2O的合成、晶体结构和荧光性质

The title compound,[Ag4(L)4](PMBS)4·2H2O (1),where L=2,5-bis (4-pyridyl)-3,4-diaza-2A-hexadiene,PMBS =p-methylbenzenesulfonate was synthesized and its crystal structure was determined by X-ray diffraction structure analysis.The crystal is of triclinic,space group P1 with a=0.820 3(2) nm,b=1.3227(3) nm,c=2.0610(3) nm,α=76.155(2)°,β=78.651 (4)°,γ=89.993(3)°,V=2.126 2(8) nm3,Z=2,Dc= 1.644 g·cm-3,F(000)= 1068,R=0.052 4,wR=0.113 6.The Ag atoms are linear coordinated by two N atoms of two L ligands,while the p-methylben-zenesulfonate molecules are included in the lattice and connected to [Ag(L)]n by hydrogen bonding interactions to form a three-dimensional supramoleculur structure.CCDC:727587.     

Hydrothermal Synthesis and Crystal Structure of Complex Mn2(phen)2(p-MBA)4(H2O)

A novel Mn(Ⅱ)complex Mn2(phen)2(p-MBA)4(H2O)has been hydrothermally synthesized by the reaction of P-methyl benzoic acid(p-MBA)with 1,10-phenanthroline(phen).Crystal data for this complex:monoclinic,space group C2/c,a=2.3328(3),b=1.5549(2),c=1.5557(2)nm,β=121.726(2)°,V=4.7997(11)nm3,Mr=1028.85,Dc=1.424 g/cm3,Z=4,F(000)=2128,μ(MoKa)=0.590mm-1,GOOF=1.060,R=0.0333 and wR=0.0767.In the crystal,each Mn(Ⅱ)ion is coordinated by two nitrogen atoms from one o-phenanthroline molecule.three oxygen atoms from three P-methyl benzoic acids and one oxygen atom from one water molecule,giving a six-coordinate distorted octahedral coordination geometry.Two neighboring Mn(Ⅱ)ions are bridged by two P-methyl benzoic acid groups and one water molecule,and their end positions are respectively coordinated by one 1,10-phenanthroline and one p-methyl benzoic acid molecule,giving a binuclear cage structure,of which the Mn(Ⅱ)…Mn(Ⅱ)distance is 0.3502 nm.