Synthesis and Structure of Dibenzoyl-bissemicarbazone Neodymium(Ⅲ) Perchlorate

A new Schiff base Dibenzoyl-bissemicarbazone C15H16N6O2(L) and its complex with neodymium(Ⅲ ) perchlorate [NdL2(H2O)2](ClO4)3 were synthesized. The crystal and molecular structure of the title complex were determined by single crystal X-ray diffraction. The crystal is monoclinic and conforms to space group P. with cell constants a=10. 893(2) A, b= 12. 118(3) A , c=22. 494(5) A , β=89. 86(3)% V = 2969.19A3. The final standard deviation R=0. 0919. In the complex Nd is coordinated by four nitrogen and six oxygen atoms, of which four nitrogen and four oxygen atoms are provided by two neutral ligands L, and the other two oxygen atoms are provided by two water molecules, forming a ten-coordinated complex cation, which the perchlorate groups exist in the outer sphere. The coordination polyhedron takes a bicapped anti-square prism arrangement. That the average bond length of Nd-N is 2. 735 A indicates that the coordination of N in groups to Nd( Ⅲ ) is very weak.     

Synthesis and Crystal Sturcture of a New Praseodymium（Ⅲ）polym煳x：[

A novel polymeric Pr2Cu3 complex of iminodiacetic acid (H2L1=NH{CH2COOH}2) [Pr2Cu3(L1)6]n , 1, has been synthesized and structurally characterized. The title complex Pr2Cu3O24N6C24H30 (Mr=1258.97) crystallized in trigonal space group Pc1 (No. 165) with a = 13.424(4), c=14.752(6)(); V=2303(1)()3; F(000)=1226; λ(MoKα)=35.2 cm-1; Dc=1.820 g.cm-3; Z=2. The final R and Rw are 0.072 and 0.081 respectively for 1412 reflections with I>3σ(I). In crystal 1, the Pr3+ ion is nine-coordinated by 6 O atoms from three bidentate chelating carboxylate groups and 3 O atoms from three anti-anti bridging carboxylic groups of six L1 ligands; the Cu2+ ion is six-coordinated by 4 O and 2 N atoms from two pentadentate L1 ligands. Each pair of Pr(Ⅲ) atoms is bridged by three L1 ligands, each of which also chelates with one copper(Ⅱ) ion, thus forming a Pr2Cu3 cluster unit. Such cluster units are cross-linked by flexible L1 ligands into a three-dimensional coordination framework.     

Synthesis, Crystal Structure, and Cytotoxic Property of Di（μ1”,1”-azide）bis（4-nitro-2-（3＇-dimethylaminon-propylimino）methylenephenolate）dizinc（Ⅱ）

The title azide-bridged dinuclear Schiff base zinc(Ⅱ) complex [Zn2(C12H16N3O3)2-(μ1,1-N3)2] was prepared and characterized by elemental analysis, IR spectrum, and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group F21/n with a = 8.736(2), b = 14.850(3), c = 11.775(2) (A), β = 102.42(3)°, V= 1491.8(5) (A)3, Z= 2, Dc = 1.593 g/cm3, Mr = 715.36, λ(MoKα) = 0.71073 (A), μ = 1.669 mm-1, F(000) = 736, the final R = 0.0338 and wR = 0.0789. A total of 3411 unique reflections were collected, of which 2777 with Ⅰ＞2σ(Ⅰ) were observed. The molecule of the complex is located on a crystallographic inversion centre. Each Zn atom in the complex is five-coordinated by one Schiff base ligand and two bridging azide groups, forming a trigonal bipyramidal configuration. The Zn…Zn distance is 3.328(2) (A). In the crystal structure, molecules are linked through intermolecular C-H…N hydrogen bonds, forming layers parallel to the bc plane. The complex shows low cytotoxic property to both normal and carcinoma cells.     

Synthesis and Crystal Structure of Di-μ1,1-azido-bis（（azido）[N-ethyl-N＇-（1-pyridin-2-ylmethylidene）ethane-1,2-diamino]cadmium（Ⅱ））

The dinuclear Schiff base cadmium（Ⅱ） complex [Cd2（C10H15N3）2（N3）2 （μ1,1-N3）2] was prepared and characterized by elemental analysis, IR spectrum, and single-crystal X-ray dif- fraction. The crystal belongs to the monoclinic system, space group P21/n with a = 10.819（2）, b = 11.058（2）, c = 12.766（3）A, β = 102.456（2）°, V = 1491.3（7）A^3, Z = 2, Dc = 1.665 g/cm^3, Mr = 747.42, λ（MoKα） = 0.71073 （A）, μ = 1.470 mm^-1, F（000） = 744, R = 0.0307 and wR = 0.0584. A total of 3420 unique reflections were collected, of which 2575 with Ⅰ 〉 2σ（Ⅰ） were observed. There is a crystallographic inversion centre at the midpoint of the two metal atoms in the complex. Each CdⅡ atom in the complex is in a distorted octahedral coordination. The molecules in the crystal are linked through the intermolecular hydrogen bonds of N-H…N and C-H…N, forming a three- dimensional network.     

Synthesis and Characterization of a New Symmetric Dinucleating Ligand and Its Dizinc(Ⅱ)Complex with Alkoxo and Carboxylate Bridges

<正>A novel dinuclear zinc(Ⅱ)complex[Zn_2L(μ-OAc)](PF_6)_2(CH_3OH)has been synthesized from a new symmetrical compartmental ligand HL in which the pendant arms,bearing pyridyl groups,are bridged by 1,3-diaminopropan-2-ol.X-ray crystal structure shows that the two zinc atoms reside within the adjacent ligand compartments and are bridged by the endogenous alkoxo-O from ligand and one exogenous carboxylate from acetate with a syn-syn mode.The coordination geometry of two zinc atoms is a distorted trigonal bipyramid with the pyridyl-N atoms and bridging alkoxo-O atom providing the equatorial donor set.Such coordination geometry observed in this complex is similar to that found in the dinuclear unit of phospholipase C.     

Synthesis and Crystal Structure of catena-Poly[[[2,4-dibromo-6-[（3-dimethylaminopropylimino）-methyl]phenolato]copper（II）]-μ-azido]

A novel end-to-end azido-bridged polynuclear Schiff-base copper（II） complex, [Cu（C12H15Br2N2O）（N3）]n, was prepared and characterized by elemental analysis, IR spectra, and single-crystal X-ray diffraction. The crystal belongs to the orthorhombic system, space group Pbcn with a = 24.588（5）, b = 10.377（2）, c = 13.022（3） A, V= 3322.6（12） A^3, Z = 8, Dc = 1.874 g/cm^3, Mr = 468.65, λ（MoKa） = 0.71073 A,μ = 6.130 mm^-1, F（000） = 1832, R = 0.0637 and wR = 0.1176. The Cu atom in the complex is five-coordinated in a square pyramidal geometry by three donor atoms of the Schiff-base ligand, and two N atoms from two bridging azide ligands. The [2,4-dibromo-6-[（3-dimethylaminopropylimino）methyl]phenolato]copper（II） units are linked by the bridging azide ligands, giving zigzag polymeric chains with backbones of the [--Cu-N-N-N--Cu]n type running along the b axis.     

以Schiff碱N-丁酰基水杨酰肼为配体的三核镍(Ⅱ)配合物的合成与结构

The trinuclear nickel (Ⅱ) complex Ni3(C11H11N2O3)2(C5H5N)4 was prepared by the reaction of Ni(OAc)2 @ 4H2Owith N-butylsalicylhydrazide Schiff base ligand and characterized by X-ray crystallography. The crystal belongs totriclinic, Mr=930.91, space group P1 with cell parameters a =9. 8489(2)A, b = 12. 3110(2) A, c = 18. 4035(3) A, α=71.353(2)°, β=76.638(2)°, γ=84.815(2)°, V=2056.72(6)A3, Z=2, Dc=1.503g@cm-3,μ(MoKα) = 1. 417mm-1, F(000) = 964, R = 0. 0317, wR = 0. 0868. A total of 5393 independent reflectionswere collected, of which 4448 reflections with I ≥ 2 σ(I) were observed. There are two centrosymmetrical trin-angle of 180°. The interatomic distances between the nickel atoms on the two sides are 9. 2030(8) A and 9. 1876(9) A for the two molecules, respectively. The central nickel atom adopts an axially elongated octahedral geometrywhereas the nickel atoms on the two sides have square-planar coordination environment. CCDC: 194083.     

Crystal Structure and Properties of a Copper(Ⅱ) Complex Containing p-Toluenesulfonate and Imidazole Ligands

A novel supramolecular mixed ligand complex of formula [Cu(PTS)2(Him)2(H2O)2] (C20H26CuN4O8S2,PTS=p-toluenesulfonate,Him=imidazole) has been synthesized in aqueous solution and characterized by elemental analysis,IR and single-crystal X-ray diffraction.The compound crystallizes in the monoclinic system,space group P21/n,Z=2,a=5.650(2),b=14.671(3),c=14.638(3),β=100.10(3)°,V=1194.60(4)3,Dc=1.607 g/cm3,μ(MoKα)=1.143 mm-1,F(000)=598,R=0.0615 and wR=0.1503 for 1752 observed reflections with I 2σ(I).The copper(II) ion in the complex adopts a slightly distorted octahedral coordination geometry and is six-coordinated with N2O4 donor set consisting of two nitrogen atoms and four oxygen atoms provided by the ligands of two imidazole molecules,two water molecules and two p-toluenesulfonate ions.The sulfonate group of the PTS ligand remains weak-coordinated and forms a number of hydrogen bonds with water molecules and imidazole ligands.X-ray structural analysis reveals that the coordination molecules are connected to form a 3-D supramolecular framework by electrostatic interaction,weak van der Waals forces,hydrogen bonding and π-π interaction.The thermal behaviour of the title complex was investigated by using DSC and TG-DTG techniques.     

N,N′-苄基-1,2二胺合铜的合成和晶体结构及与DNA的相互作用(英文)

A ligand,(N,N′-dibenzylethane-1,2-diamine)(L),and its complex with copper acetate was synthesized and characterized by some spectral analyses.The copper ! ion is six-coordinated and exhibites octahedral coordination geometry,the coordination atoms are four nitrogen atoms from two(L) ligands and two carboxyl oxygen atoms from two acetic acid groups,respectively.After studying the interaction of the complex with calf thymus DNA through UV and fluorescence spectra,we can find that there is a strong binding and a large affinity berween the complex and calf thymus DNA.CCDC: 649416.     

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.     

七配位K[InⅢ(Hdtpa)]·3.5H2O配合物的合成及结构测定

In this paper, the title complex K[InⅢ (Hdtpa)] · 3.5H2O(dtpa=diethylenetriaminepentaacetic acid) was synthesized and its crystal structure was determined by single-crystal X-ray structure analysis.The crystal belongs to monoclinic system, P21/c(No. 14) space group with a= 0. 978 1 (2) nm,b=0. 733 8(1) nm, c＝2. 962 9(6) nm, β=91.81(3)°, V=0. 212 6(1) nm3, Z=4, M=606.31, Dx=1.895 g · cm-3, μ=1. 382 1 mm-1, F(000)=1 228, R=0. 035 and Rw=0. 041 for 2 802 unique reflections. The complex anion [InⅢ (Hdtpa)]- has a pseudo-monocapped trigonal prismatic sevencoordination structure in which the seven coordinate atoms, three N and four O atoms, are all from a ligand dtpa. In addition, it can be seen that the complex anion [InⅢ (Hdtpa)]－ can furnish a free carboxyl group(-CH2COOH) being used for molecular embellishment to form the target diagnosis- and treat-drug of anticancer.     

Synthesis and crystal structure of dinuclear nickel (Ⅱ) complex

The crystal structure of Ni(Ⅱ) complex with 3-hydroxyl-1, 5-diazacycloheptane-N, N'-diacetate was determined by X-ray diffraction method. Crystal data for Ni2 (C9H14N2O5)2·2H2O: monoclinic, space group P21/n, a = 1.1717(5), b = 0.9794(3), c = 1.2971(2) nm, β= 96.62(3), V= 1.4786(7) nm3, Dc = 1.377 g/cm3, Z = 2,μ=13.321 cm-1 (Mo-Kα), F(000)=640. The final R and Rw are 0.075 and 0.089 respectively. The Ni(Ⅱ) ion forms 2:2 complex with ligand. Two ligands are bridged by two Ni(Ⅱ) atoms which are bridged by two O atoms. Every Ni(Ⅱ) is coordinated by two N atoms and four 0 atoms. The coordination polyhedron of the Ni(Ⅱ) ion is a distorted octahedron.     

Synthesis and Crystal Structure of a New Dinuclear Manganese(Ⅱ) Manganese(Ⅲ) Complex of a Macrocyclic Ligand

A mixed-valence dinuclear manganese complex, [MnⅡMnⅢL](ClO4)·1/2MeOH, where L is a macrocyclic ligand derived from the cyclocondensation of sodium 2,6-diformyl-4-methylphenolate with N,N-bis(2-aminoethyl)-2-hydroxybenzyl amine, was obtained and its structure was determined by X-ray diffraction. The orange crystal is a monoclinic system with space group P21/c and lattice parameters a=1.1617(4), b=1.4005(3), c=1.4641(3) nm, β=113.03(2)°, and Z=2. The crystal structure shows that each pendant-arm is bonded in a bidentate fashion to the adjacent metal atom and that both the arms are on the same side of the macrocycle. The two Mn atoms are bridged by two μ2-phenoxy oxygen atoms of the tetra-imine macrocycle, and each Mn atom, locating in a trigonal prismatic coordination environment(N3O3), is six-coordinated by the two imine nitrogen atoms, one tertiary nitrogen atom and a pendant phenol moiety apart from the two oxygen atoms.     

N，N′-苄基-1，2二胺合铜的合成和晶体结构及与DNA的相互作用

A ligand， (N，N′-dibenzylethane-1，2-diamine) (L)， and its complex with copper acetate was synthesized and characterized by some spectral analyses. The copper(Ⅱ) ion is six-coordinated and exhibites octahedral coordination geometry， the coordination atoms are four nitrogen atoms from two(L) ligands and two carboxyl oxygen atoms from two acetic acid groups， respectively. After studying the interaction of the complex with calf thymus DNA through UV and fluorescence spectra， we can find that there is a strong binding and a large affinity berween the complex and calf thymus DNA. CCDC: 649416.     

Synthesis, Structure and Magnetic Properties of a Linear Trinuclear Mn（II） Complex with a Multifunctional Group Ligand

By use of a new ligand containing both salicylic acid moiety and salicylaldehyde Schiff base moiety, 5-(2-hydroxybenzylideneamino)-2-hydroxybenzoic acid (H3L), a linear trinuclear Mn(II) complex was prepared. This complex crystallizes in triclinic, space group P1 with a = 12.0196(7), b = 13.7440(13), c = 15.7554(14) , α = 111.529(3), β = 96.691(2), γ = 94.802(2)o, C96H100Mn3N6O32, Mr = 2014.64, V = 2382.0(3) 3, Z = 1, μ = 0.478, Dc = 1.404 g/cm3, F(000) = 1049, R = 0.0554 and wR = 0.1610 for 8973 observed reflections (I 2σ(I)). The complex consists of a trinuclear cluster and two solvate ethanol molecules. Three linearly disposed Mn atoms, with an inversion center on the central one, are bridged by six carboxylate groups from six bulky mono-anionic ligands (H2L–), and the octahedral coordination spheres for each of the metal centers are thus formed, with the aid of additional ligation of two small molecules (ethanol and water) to both ends. The magnetic properties of the title complex are also included in this paper.     

One—dimensional Zigzag Chain Coordination Polymer [Zn（μ—phth）（imi）2]∞ Bridged by o—Phthalato

The reaction of zinc carbonate with o-phthalic acid and imidazole in an aqueous-alcohol solution led to the formation of colorless crystals of [Znμ-phthimi2]∞. Single-crystal X-ray analysis has revealed that the complex crystallizes in a monoclinic system, space group Pn with a = 8.394(2), b = 9.976(3), c = 9.959(3)A, β = 104.409(4)°, V = 807.6(4)A3, Z = 2, C14H12N4O4Zn, Mr = 365.6(5), Dc = 1.504 g/cm3, μ = 1.544 mm-1, F000 = 372, the final R = 0.0466 and wR = 0.1171 for 1834 reflections with I>2σ(I). The complex displays a zigzag infinite chain structure in which each zinc(Ⅱ)center is coordinated by two oxygen atoms and two nitrogen atoms to generate a ZnN2O2 distorted tetrahedral geometry. The neighboring zinc atoms are bridged by the o-phthalate ligand. Each chain is linked by hydrogen bonds with its neighbors to form a three-dimensional coordination polymer.     

N-乙基-1，10-菲罗啉-2-甲胺镍(Ⅱ)配合物的合成、晶体结构及性质研究(英)

A novel ligand N-ethyl-1,10-phenanthroline-2-methanamine and its Ni(Ⅱ) complex have been synthesized. The crystal structure of the complex has been determined by X-ray diffraction method. The Ni(Ⅱ) is five-coordinated by three nitrogen atoms from the ligand and two Cl^- anions in a distorted trigonal bipyramidal environment: the N(2), Cl(1) and Cl(2) in equatorial plane; the N(1) and N(3) in axial positions. The UV-spectra and IR-spectra of the ligand and its Ni(Ⅱ) complex were recorded and discussed. The thermodynamic properties of the ligand with various bivalent metals were studied by potentiometric titrations and the order of the stability constants is in agreement with the Irving-Williams order in coordination chemistry. CCDC: 221750.     

Cu(Ⅱ)-牛磺酸缩水杨醛席夫碱-邻菲咯林三元配合物的合成、晶体结构及性质

The title complex was synthesized by reaction of taurine salicylic schiff base(TSSB), O-phenanthroline(phen) and cupric acetate in water-ethanol solution. The crystal structure was determined by X-ray diffraction method and the chemical formula weight of the complex is 498.00. The crystal structure of the title complex belongs to orthorhombic system with space group Pbcn and cell parameters: a=3.107 2(4) nm, b=1.289 09(18) nm, c= 1.034 78(14) nm; and V=4.144 7(10) nm³, Z=8, D_c=1.596 g·cm^-3, μ=1.197 mm^-1, F(000)=2 048. The compound is an one-dimensional chain complex of infinite length which are connected with hydrogen bonds. The Cu(Ⅱ) was coordinated by two oxygen atoms and three nitrogen while the o atoms of Ac- groups did not participate in the coordination. The Cu(Ⅱ) formed a distorted tetragonal pyramid and the capacities of coordination to Cu(Ⅱ) of atoms was discussed. Besides, the TG-IR of the complex was analyzed. The kinetics of the thermal decomposition reaction of the complex was studied under a non isothermal condition by TG-IR. TG and DTG curves indicate that the complex decomposed in three stages: (?) The kinetic parameters were obtained from the analysis of TG,DTG cures by OZAWA-Flynn-Wall method, and the activation energy and the value of A of the three stages are 74.98 kJ·mol^-1, 286.65 kJ·mol^-1, 87.55 kJ·mol^-1; 9.66×10⁸ s^-1,1.82×10²⁸ s^-1, 3.09×10³s^-1, respectively.     

配合物[Tb(p-ClBA)_3(phen)]_2的结构和性能(英文)

Terbium p-chlorobenzoate complex with 1,10-phenanthroline, [Tb( p-ClBA)_3phen]_2 (1) has been obtained in the ethanol solution, where p-ClBA=p-chlorobenzoate and phen=1,10-phenanthroline. It crystallizes in the triclinic system, space group P1, a=1.008 1(2) nm, b=1.185 7(2) nm, c=1.431 1(3) nm, α=110.826(4)°, β=96.436(4)°, γ=101.737(4)°, Z=2. The two Tb(Ⅲ) ions are linked by four carboxylate groups through their bidentate bridging modes, forming a dimeric unit with crystallographic inversion center. Each terbium ion has an eight-coordinate geometry with four of the coordination sites occupied by four oxygen atoms from the four bridging carboxylates, respectively, two oxygen atoms from bidentate carboxylate, and the remaining positions occupied by two nitrogen atoms from a 1,10-phenanthroline molecule. The Tb(Ⅲ) ion adopt a distorted square antiprism coordination geometry. The excitation and luminescence data observed at room temperature show that the title complex emits very intensive green fluorescence under ultraviolet light. The result of thermal analysis indicates the complex [Tb(p-ClBA)_3phen]_2 is quite stable to heat. CCDC: 221921.     

Synthesis and Structure Study of Molybdenum Complex Mo[o-NHCOCH_3-m-NO_2C_6H_3COOH]_2_O2Cl_2·PhCl

The crystal and molecular structures of molybdenum complex, Mo [ o- NHCOCH3- m-NO2C6H3COOH]2O2Cl2.PhCl are reported. The crystal belongs to space group Cc of monoclinic system with unit cell parameters:α= 11. 214 (3) A .b= 19. 544 (4 ) A . c = 14. 091 (6) A .β=94.06(3)°,V'=3080.3 A3 and Z=4. The structure was refined to R=0. 061.The coordination number for the Mo atom Is six. The coordination polyhedron formed by four O atoms and two Cl atoms around the Mo atom is a distorted octahedron. Four O atoms and one Mo atom construct a plane. Two benzyl planes in coordinate groups and the benzyl plane of solvent are almost parallel. The quantum-chemical calculations were carried out. There are hydrogen bonds in the Complex. The EHMO calculations and the existence of hydrogen bonds prove that the O atoms are stronger coordinated atoms in the carbonyls than in the carboxyls.