Synthesis and Crystal Structure of a Novel Hetero-bimetallic Complex with a Three-dimensional Network Structure: Bis(malonato)tetra(aqua)calcum(Ⅱ)cobalt(Ⅱ)

The title complex [CaCo(C3H2O4)2(H2O)4]n with a formula of C6H12CaCoO12 and Mr = 375.17 has been synthesized and structurally characterized by X-ray diffraction. The crystal is of monoclinic, space group C2/c with a = 14.195(9), b = 7.708(5), c = 13.441(8) (A),β = 119.575(9)°,V = 1279.0(14)(A)3, Dc = 1.948 g/cm3, μ = 1.803 mm-1, F(000) = 764 and Z = 4. The final R =0.0245 and wR = 0.0652 for 1344 observed reflections with I ＞ 2o(I). The structure of the title complex consists of CaO8 polyhedra and CoO6 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 Co(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 Co-Co distance of 6.961(5) (A). The whole 3D structure is maintained and stabilized by the presence of hydrogen bonds.     

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.     

Synthesis and Crystal Structure of Co(DMSO)2(H2O)2(SCN)2 with One-dimensional Hydrogen-bonded Structure (DMSO = Dimethylsulfoxide)

1 INTRODUCTION The development of supramolecular complexes has recently attracted considerable attention due to the fundamental interest in self-assembly processes of transition-metal complexes, supramolecular che- mistry and crystal engineering[1]. The ultimate goal is to gain control in order to direct their function[2]. Self-assembly through coordination and nonco- valent interactions such as hydrogen bonds, aromatic π···π stacking, steric repulsion and Van der Waals forces leads …     

Synthesis,Crystal Structure and Characterization of Polynuclear Potassium(I), Copper(II) and Cobalt(II) Complex with Acetylacetonethylenediamine

The title complex [K{Cu(acen)}₃]₂[Co(NCS)₄]·1/4CH₃OH (acen = acetylacetonethylenediamine anion) has been prepared and characterized. Single-crystal x-ray analysis reveals that the complex crystallizes in space group P I with a = 11.442(2), b = 15.098(3), c = 28.500(4) Å, α = 82.77(1), β = 83.58(1), γ = 85.07(1)°. The crystal consists of the complex [K{Cu(acen)}₃]⁺ cations, [Co(NCS)₄]^2? anions and methanol molecules. Three [Cu(acen)] molecules function as bridging ligands through phenolic O atoms to one K⁺ to give the tetranuclear [K{Cu(acen)}₃]⁺ cation. Each copper(II) atom in the cation is in a square-planar geometry, being coordinated by two oxygen atoms and two nitrogen atoms from a quadridentate acen ligand. The cobalt(II) atom is coordinated by four nitrogen atoms of thiocyanate ligands, forming a deformed tetrahedral environment. The IR and UV-Vis spectra have also been investigated.     

Synthesis and Molecular Structure of Bis(ethylenediamine)acetatonickel(II)hexafluoridophosphate Complex [Ni(en)2(CH3CO2)]PF6. An Unexpected Acetylacetonato Cleavage Reaction

The title complex was synthesized by an unusual reaction between [Ni(acac)₂(H₂O)₂] and ethylenediamine in water solution. The crystal structure of 1 shows the nickel(II) core in a tetragonally distorted octahedral environment coordinated to two ethylenediamine molecules and one acetate ligand. This is the first example of a mononuclear bis(ethylenediamine)nickel(II) complex, where the oxygen atoms of the auxiliary ligand are in cis configuration. The compound exhibits an extensive association between the complex cation and the respective anion through classical N–H ··· O and N–H ··· F intermolecular hydrogen bonds, which generate a supramolecular 3D arrangement in the solid state.     

Synthesis and Crystal Structure of Copper(II) Complex with N-Acetoxyl-picolinamide

1 INTRODUCTION The picoloylhydrazide compounds are close to thebiologic environment and can react with microele-ments in organism so as to have antitubercular andantineoplastic activities. However, owing to the exis-tence of amino group, this kind of compounds aretoxic to some extent[1]. In order to decrease theirtoxicity, hydrazone or hydrazide compounds synthe-sized by the condensation reaction of amino and car-bonyl groups have been well studied in recentyears[1～7]. Herein we report t…     

CRYSTAL STRUCTURE OF [Ni((C)_6H_(11)O)_2PS_2)·(C_4H_9NH_2)_4]-(C_6H_(11)O)_2PS_2

<正> [Ni((C6H11O)2PS2)·(C4H9NH2)4](C6H11O)2PS2,Mr-=938. 05, triclinic,P1,a=13. 513(6),b=16. 040 (7), c= 12. 891(6) A , α= 95. 66 (4),β= 90. 23(4),γ= 75. 46(3)°,V = 2691 A3,Z=2,Dc= 1. 16 g·cm3.μ=6. 07cm-1,MoKa radiation, λ=0. 71069 A ,F(000) = 1020,R=0. 100 for 4595 reflections with I≥3σ(I). The title compound molecule consists of a complex cation [Ni((C6H11O)2PS2)(C4H9-NH2)4]+ and a complex anion (C6H11O)2PS2- . The Ni (Ⅱ) atom in the cation is octahedrally coordinated by four nitrogen atoms from four w-butylamine ligands and two sulfur atoms from one (C6H11O)2PS2 group.     

CRYSTAL STRUCTRURE OF POTASSIUM BIS- (11-MOLYBDOSILICA-TO)DYSPROSATE(Ⅲ)

<正> Crystal of the title complex K10H3[Dy(SiMo11O39)2]·29H2O(Mr= 4331.85) is monoclinic with space group P21/n,a= 17. 256(1) ,b = 26. 817(1) ,c = 21.797(1) A,β= 104. 39(1)°, V = 9770. 2 (A3), Z= 4, F (000) = 8140, and Dc= 2. 94g/cm3. The Dy3+ is coordinated by eight oxygen atoms from two tetradentate (SiMo11O39)8- ligands,forming a square antiprism. The cation K+ is coordinated by oxygen atoms from heteropoly ligands (SiMo11O39)8- and water molecules, the number of atoms that are coordinated to the potassium atoms can be divided into four groups:six,seven, eight and nine.     

Monomeric and polymeric dinuclear complexes of Co(II) or Ni(II) with calix[4]arene-tetraphosphineoxide

Monomeric and polymeric 1:2 complexes of a novel calix[4]arene-tetraphosphineoxide with Co(II) or Ni(II) nitrates were synthesized and analyzed by the X-ray method. In the monomeric complexes each metal cation is coordinated by two bidentate NO₃-ligands as well as by two proximal P=O groups at the calixarene skeleton. In the nickel metallopolymer one sort of the cations is bound by the two proximal P=O-groups but other cations link neighboring calixarene molecules through Р=О···Ni···O=P chains. The complexes possess molecular cavities or channels filled by solvent molecules. Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Heterovalent trinuclear Co(III)-Co(II)-Co(III) complexes with N-(2-Carboxyethyl)salicylaldimines

The heterovalent trinuclear cobalt complexes [Co₂^IIIL₄ ⁱ · Co^II(H₂O)₄] · nXmY (L ⁱ are deprotonated Schiff bases derived from substituted salicylaldehydes and β-alanine; i = 1–3) were obtained and characterized. An X-ray diffraction study of the trinuclear cobalt complex with N-(2-carboxyethyl)salicylaldimine showed that the central Co(II) ion and the terminal Co(III) ions are linked by bridging carboxylate groups. Either terminal Co(III) atom is coordinated to two ligand molecules. They form an octahedral environment consisting of two azomethine N atoms, two phenolate O atoms, and two O atoms of two carboxylate groups. The central Co(II) atom is coordinated to four water molecules and to two O atoms of two bridging carboxylate ligands involved in the coordination sphere of the terminal Co(III) atoms.     

Syntheses and Crystal Structures of Two Cyano-bridged Bimetallic Complexes [Ce(DMSO)_4(H_2O)_3Fe(CN)_6]·H_2O and [La(DMSO)_4(H_2O)_3Co(CN)_6]·H_2O(DMSO = Dimethylsulfoxide)

1INTRODUCTION Recently,cyano-bridged lanthanide-transition me-tal complexes have been extensively investigateddue to their potential applications as precursors in the preparation of rare earth orthoferrites,fluores-cent and magnetic materials[1].Various complexes of this system have been obtained in order to ex-plore the relations between structures and pro-perties by using different ligands,such as DMF,4,4?-bipy,and so on,to fill the coordination sites of lanthanide ions[2～9].But up to…     

Synthesis, Crystal Structure and Luminescence Property of [Co(hmz)_2(H_2O)_4]·2H_2O

A new mononuclear Co(II) complex, [Co(hmz)2(H2O)4]·2H2O, has been synthesized by the reaction of Co(CH3COO)2·4H2O with 1-(4-hydroxyphenyl)-5-mercaptotetrazole (Hhmz). It crystallizes in the monoclinic system, space group P21/n with a = 13.502(5), b = 6.718(3), c = 13.972(6) , β = 117.532(4)o, V = 1123.9(8) 3, Z = 2, M r = 553.45, F(000) = 570, Dc = 1.635 g/cm3, μ = 1.008 mm–1, the final R = 0.0272 and wR = 0.0684 for 2194 observed reflections (I > 2σ(I)). The Co(II) is six-coordinated by two nitrogen atoms from two hmz–1 ligands and four water molecules, forming an octahedral geometry. The intermolecular hydrogen bonding and offset-panel π-π stacking interactions between the adjacent molecules extend the compound into a three- dimensional supramolecular framework. The title compound emits strong blue fluorescent light (λem(max) = 427 nm) at room temperature and is red-shifted compared with free ligand Hhmz (λem(max) = 342 nm).     

Synthesis and Crystal Structure of Tetraaquacopper(II) Bis(5-fluorouracil-1-acetate) Tetrahydrate

1 INTRODUCTION 5-Fluorouracil (5-FU) is an antimetabolite with good antimicrobial and antitumor activities but has toxic side effects[1~4]. In order to improve the topical delivery of 5-FU and reduce the side effects, many derivatives of 5-FU have been synthesized, some of which are of improved activity. 5-Fluorou- racil-1-acetic acid is a member of the family[5~8], which belongs to the pyrimidine base and is a cyto-toxic analogue of the natural base thymine, and has proven useful in th…     

Synthesis and Crystal Structure of a Co(II) Complex with Schiff Base and Imidazole Ligand

1 INTRODUCTION The chemical behavior of metal complexes with Schiff base ligand has attracted much attention be- cause of their catalytic activity in some industrial[1, 2] and biochemical processes[3~5]. As some metal com- plexes have shown the catalytic activity in some polymerization reactions[2, 6], we are recently inte- rested in polymerizartion of organo-silicon com- pounds catalyzed by Schiff base complexes of tran- sition metals. A series of Schiff base complexes have been prepare…     

咪唑桥Cu(Ⅱ)-Co(Ⅱ)异双核配合物晶体结构与电子结构研究

本文报导了咪唑桥异双核配合物[(Ida)CuImCo(NH_3)_5](ClO_)4)_2·4H_2O(Ida为亚氨基二乙酸,Im=咪唑)的晶体结构。晶体属单斜晶系,空间群为P2_1/c,M_r=676.5,Z=4,D_c=1.911g/cm~3,晶胞参数为a=13.024(2),b=15.400(2),c=13.198(4)A,β=111.28(2)°。结构用直接法解出,经全矩阵最小二乘法修正,最后R因子为0.062。在分子中Cu(Ⅱ)处于Ida的两个0和一个N,咪唑的一个N及稍远处一个H_2O的O组成的变形四方锥配位环境中;Co(Ⅱ)则与5个NH_3及咪唑的另一个N配位,形成略有变形的八面体构型。对配位阳离子的CNDO/2计算表明,该配合物具有一定的催化O_(2-)歧化活性。     

Coordination polymer incorporating cobalt(II) and glycine acid: structure and magnetism

We report the structure and magnetism of a cobalt(II) compound with glycine acid, Co(C₂H₄NO₂)₂ · H₂O (1). It crystallizes in the orthorhombic system, space group P2(1)2(1)2(1) with a = 5.2301(10) Å, b = 10.837(2) Å, c = 13.542(3) Å, R ₁ = 0.0448, wR ₂ = 0.1151. In 1, Co(II) has a slightly distorted square-pyramidal geometry defined by two O atoms and two N atoms from two glycine ligands, and by one O atom from an aqua ligand in the apical position. The molecules form a three-dimensional supramolecular network through O–H ··· O and N–H ··· O hydrogen bonds. Magnetic characterization shows 1 exhibits a negative Curie–Weiss constant and dominant spin-orbit coupling for Co(II).     

Synthesis and Extended 3D Hydrogen-bonded Structure of Complex Tris(violurato-N,O) Cobalt(III) Hexahydrate

1 INTRODUCTION The study of cobalt complexes plays an important role in pharmacology, coordination chemistry and bio- inorganic chemistry. The recent work on organoco- baloximes shows that it has outgrown its initial rele- vance of Vitamin B12 model and acquired an indepen- dent research field because of its rich chemistry[1~4]. At the same time, research on the complexes with oxime ligands has considerable interest owning to their special catalytic, electric, magnetic properties and bio…     

Synthesis and crystal structure of aquachlorobis(1,10-phenanthroline)manganese(II) nitrobenzoate trihydrate

The title compound has been prepared and its crystal structure determined by X-ray diffraction methods. The complex salt consists of Mn(II) complex cations, benzoate anions and lattice water molecules. Mn(II) assumes a distorted octahedral geometry defined by two 1,10-phenanthroline (phen) ligands, a Cl^? ion and a water molecule. A comparison of bond distances and bond angles suggests electrostatic interaction between Mn(II) and coordinated N atoms. The nitrobenzoate anion does not coordinate to the Mn atom but links with the complex cation via O?H···O hydrogen bonds. Aromatic stacking occurs between phen rings and between phen and benzoate.     

CRYSTAL STRUCTURES OF COPPER (Ⅱ) AND COBALT (Ⅲ) COM- PLEXES OF o-HYDROXYBENZYLGLYCINATE (HBG)

<正> The structures of two complexes C(CuOC6H4CH2NHCH2COO)2 (H2 O)]·H2P(1) and [Co(NH3)6[Co(OC6H4CH2NHCH2COO)2]2[C1]·10H2O (2) were determined by X-ray analyses. Compound (1) crystallizes in the orthorhombic space group P212121 with a=11. 357(1),b= 24. 304(2),c=7.317(4) A,Z= 4;While compound (2) in the monoclinic space group A2/a(C2/c) with a=23. 486(9) ,b=26. 605(6) ,c= 10. 542(1) A,γ= 128. 42(4)°,Z= 4. In compound (1),two Cu(Ⅱ) ions are bonded together by the phenolic oxygen atoms of two tridentate chelating ligands and each of them is separately coordinated by the carboxyl oxygen,amino nitrogen of each chelate ligand and by the fifth oxygen atom as well (from aqua or the carbonyl group in adjacent molecule). Thus the coordination of each Cu(Ⅱ) is a square pyramid with distances of 1. 93- 1. 97A to the four corner atoms and 2. 30 and 2. 32 A to the apex atoms. The whole molecule has an approximately planar configuratioir with the two pyramid apexes pointing towards one side. Compound (2) consists of     

THE SYNTHESIS AND STRUCTURE OF THE IMIDAZOLATE-BRIDGED HETEROTRINUCLEAR COMPLEX (en)_2Ni[(Im)Co-(NH_3)_5]_2(CIO_4)_6·5H_2O

<正> (H2NC2H4NH2)2Ni [(C3H3N2) Co (NH3)5]2 (CIO4)6 · 5H2O,NiCo2Cl6O29N18C10H62, Mr = 1288. 00, monoclinic, C2/c, a = 31. 832(4), b = 9. 691 (1), c=15. 425(4)(?),β=90. 71(2)°, Z = 4, V = 4758. 0(?)3, Dc=1. 798g/cm3, μ (MoKa) = 15. 22cm-1, F(000)=2656. The three metal nuclei, one Ni( Ⅱ ) and two Co( Ⅲ ), bridged by two imidazolyl anions (Im = C3H3N2), form an isosceles triangle. The Ni( Ⅱ ) atom is situated on the two-fold axis and coordinated by six nitrogen atoms to form a distorted octahedron with two nitrogen atoms from two Im in cis-positions. The two Co( Ⅲ ) atoms are related by C2 symmetry and each Co( Ⅲ ) is coordinated by six nitrogen atoms to form an octahedral configuration.