Synthesis and Crystal Structure of Bis(dicyanamide) (5,7,7,12,14,14-Hexamethyl-1,4,8,11-tetraazacyclotetradecane) Nickel(Ⅱ)

1 INTRODUCTION Crystal engineering is becoming an increase- ingly interest field by means of coordinated co- valent bonding or supramolecular contacts (such as hydrogen bonds, p-p interaction etc.)[1～7]. The ligand [N(CN)2]- is a remarkably versatile building block for constructing supramolecular architectures since it may act in uni-, biand tridentate manner. Additional ligands, such as coordinating amines (Lewis bases), in combination with dicyan- amide have been shown to produce n…     

Synthesis and Crystal Structure of Bis(dicyanamide)(5,7,7,12,14,14-Hexamethyl-1,4,8,11-tetraazacyclotetradecane) Nickel(Ⅱ)

The nickel ( Ⅱ ) complex [Ni(teta) { N(CN)2 } 2] (teta = 5,7,7,12, 1 4, 1 4-hexamehyl- 1,4,8,1 1-tetraazacyclotetradecane) was synthesized and its structure has been determined by singlecrystal X-ray diffraction. Crystal data: C20H36N10Ni, monoclinic, space group P21/c, a = 9.632(2), b = 11.833(2), c = 10.613(2) A, β= 93.46(3)°, V= 1207.4(4) A3, Mr = 475.30, Z= 2, Dc= 1.307 g/cm3,F(000) = 508,μ(MoKα) = 0.831 mm-1, R = 0.0446 and wR = 0.1274 for 2423 observed reflections with I ＞ 2σ(I). The center nickel ion is coordinated by six nitrogen atoms, four from the macrocyclic ligand teta and the other two from two dicyanamides. The dicyanamide is coordinated to the metal atoms as uni-dentate manner via nitrile nitrogen atom.     

铜锌异双核配合物[CuZn(fsan)(H_2O)]·H_2O的合成、晶体结构和电化学性质

合成了标题化合物[CuZn(fsan)(H2O)]H2O [H4(fsan)为N, N?- 二(3-羧基水杨醛叉)缩乙撑二胺],用单晶X-ray衍射法测定了它的晶体结构,该晶体属单斜晶系,空间群P21/n,a = 11.695(2), b = 14.646(3), c = 12.265(3) ? ?= 118.46(3)°, V = 1847.0(6) ?,C18H12CuN2O8Zn, Mr = 513.21, Z = 4, Dc = 1.846 g/cm3, (MoK? = 2.502mm-1,F(000) = 1028,R = 0.0478,wR = 0.0902 (I>2(I)), 2951个可观测衍射点。该分子结构为双核单元,铜原子位于“内部”由2个氮原子和2个酚氧原子构成的平面正方场中。“外部”锌原子与2个酚氧原子、2个端基羧氧原子及轴向水分子中的氧原子配位,锌原子处于变形四方锥几何构型之中。金属原子通过2个酚氧原子桥联在一起。结合晶体结构对配合物做了电化学研究。     

Synthesis and Crystal Structure of [Ni(C_5H_2N_2O_4)(2,2''''bipy)(H_2O)_2]·H_2O

1 INTRODUCTION Orotic acid (H3dtpc), an important pyrimidine derivative as the effective precursor in the biosynthesis of pyrimidine base of nucleic acids in living organisms, plays a unique role in bioinorganic and pharmaceutical. Aside from the biological interest, orotic acid is also interesting in coordination chemistry. Its ketonic and enolic tautomers along with asymmetric geometry make it to be a very good versatile polydentate ligand[1~5]. The incorporation of metals into supram…     

Crystal Structure Analysis of Tetras[L-tris(ethylenediamine) cobalt(Ⅲ)] tris[hexacyanoruthenate(Ⅱ)]

1 INTRODUCTION The tris(ethylenediamine) cobalt (Ⅲ) complex in which there are L and D configurations is one of the very interest cations due to the chirality among research complexes and the characterization of reaction on the ion-pair charge-transfer transitions. It has been mentioned in a lot of examples on the chirality and the structure, such as [L-Co(en)3]- [?Co(edta)]2Cl?0H2O[1], [(+)DCo(en)3]Cl3稨2O[2], [(+)-Co(en)3?-)-Cr(en)3]Cl?.1H2O[3], [()-Co(en)3] (SCN)3[4], [(+)D…     

Structural Evidence of Anion's Effect on the Ion Packing of [Ni2(teta)3]4+ in the View of H-bonding Interaction

Two dinuclear nickel(II) complexes [Ni2(teta)3]Cl4·2H2O 1 and [Ni2(teta)3](NO3)4 2 (teta = triethylenetetramine) were synthesized by a solvothermal method and structurally characterized. Complex 1: orthorhombic, Pbca, a = 13.791(3), b = 13.078(3), c = 18.323(4) , V = 3304.8(12) 3, Z = 4, Mr = 733.98, Dc = 1.475 g/cm3, μ = 1.500 mm-1, F(000) = 1560, R = 0.0585 (I > 2σ(I)) and wR = 0.1243. Complex 2: orthorhombic, P212121, a = 7.8279(14), b = 14.209(3), c = 31.163(6) , V = 3466.2(11) 3, Z = 4, Mr = 804.19, Dc = 1.541 g/cm3, μ = 1.164 mm-1, F(000) = 1704, R = 0.0401 and wR = 0.0840 for 5950 observed reflections (I > 2σ(I)). Two Ni2+ ions are connected by one linear bridging teta ligand, forming a dinuclear [Ni2(teta)3]4+ cation. Each Ni2+ ion in 1 and 2 takes a distorted octahedral geometry with six coordinated N atoms from two teta ligands. The effect of different anions on the arrangement of [Ni2(teta)3]4+ cations has been discussed in view of H-bonding interactions. Thermal stability of 1 and 2 was also investigated.     

Synthesis and Structure of [Cu（OH）2（H2O）2（4—C5H4N—COOH）2]

1 INTRODUCTION Supramolecular chemistry and crystal engineering of coordination compounds have attracted considerable interests nowadays owing to the fascinating structural diversity and potential applications as functional materials[1,2]. Generally, architectures of supramolecules are formed through hydrogen bonds, ?- ?stacking interaction or other weak interactions between the molecules. Recently, many supramolecular compounds containing silver(I) and copper(II) species have been re-…     

Synthesis and Crystal Structure of Tri(4-(3-hydroxy2-ethyl-4-pyridinone-1-yl)-aniline Condensation Salicylaldehydato) Monohydratotricopper(II)Dimethylformamide Monohydrate Solvate

1 INTRODUCTION Synthesis of transition-metal complexes with Schiff-base has been a subject of considerable im- portance[1, 2]. These complexes are not only good coordination agents for Schiff-base, but also good bactericide and antitumour agent[3, 4]. A number of hydroxypyridinones are nontoxic compounds that have been applied in bioinorganic chemistry over many years[5], and their iron(III) complexes have been assessed for the amelioration of anaemia[6]. They have also been examined …     

Crystal Structure Analysis of Tetras[(-tris(ethylenediamine) cobalt(Ⅲ)] tris[hexacyanoruthenate(Ⅱ)]

The crystal of the title compound, [Co(en)3]4[Ru(CN)6]3(10H2O (en = ethylenediamine, C2H8N2), is formed from the octahedral cations of Co(en)33+ and anions of Ru(CN)64-. The Co atom is coordinated to six nitrogen atoms of ethylenediamines in a ( configuration and the Ru atom is also coordinated to six carbon atoms of cyanides. There is no bridging-cyanide between the metal ions in the structure. The crystal is of monoclinic, space group P21/c with a = 17.686(4), b = 14.496(4), c = 18.019(7) (A。）, β = 116.07(2), V = 4150(2) (A。）3, Z = 2, Mr = 1908.60, C42H116N42O10Co4Ru3, ((MoK() = 1.391 mm-1, Dc = 1.527 g/cm3, F(000) = 2084, R = 0.0520 and wR = 0.1070 for 5443 observed reflections (I > 2((I)).     

Synthesis and Crystal Structure of Complex {[Cu(N-men)_2(cda)_2]·[Cu(N-men)_2]·(ClO_4)_2}(N-men=N-Methylethylenediamine,cda=Carbamyldicyanomethanide Anion)

<正>Mononuclear complex {[Cu(N-men)2(cda)2]·[Cu(N-men)2]-(ClO4)2} was synthesized by sodium carbamyldicyanomethanide Na(cda), N-methylethylenediamine and hydrate copper perchlorate. The crystal belongs to the triclinic system, space group P 1 with a = 7.229(2), b = 8.114(2), c = 15.936(4) A, α = 80.511(4), β = 78.993(4), r= 72.118(4)°, V = 867.6(3) A3, Z = 1, C20H44Cl2Cu2N14O10, Mr = 838.68, Dc = 1.605 g/cm3, F(000) = 434 and μ = 1.449 mm-1. The structure was refined to R = 0.0480 and wR = 0.1289 for 2503 observed reflections (I > 2σ(I)). In the complex there exist two kinds of coordination models for Cu (II) ions. One is that the Cu (II) ion is coordinated by four nitrogen atoms which are from two N-men molecules, and a slightly distorted square planar coordinate environment is formed around the Cu (II) ion; the other is that the Cu (II) ion is coordinated by six nitrogen atoms, of which four are from two N-men molecules and the left from nitrile groups, resulting in a distorted octahedron around the     

Synthesis and Crystal Structure of[Ni(C5H2N2O4)(2, 2'-bipy)(H2O)2]·2H2O

The crystal structure of [Ni(C5H2N2O4)(2, 2?-bipy)(H2O)2]·2H2O 1 has been determined by X-ray diffraction. Crystal data: triclinic system, space group P ī with a = 7.9424(3), b = 9.9417(3), c = 12.1867(3) (A。）, α = 84.771(1), β = 77.375(2), γ = 68.993(2)°, C15H18N4O8Ni, Mr = 440.7, V = 876.16(5) (A。）3, Z = 2, Dc = 1.672 g/cm3, F(000) = 456, ((MoK() = 1.162 mm-1, the final R = 0.0464 and wR = 0.1055 for 3026 observed reflections with I > 2((I). In the title compound, the nickel ion is coordinated by a nitrogen atom and an oxygen atom from the orotate ligand, two nitrogen atoms from 2, 2'-bipy and two oxygen atoms from the coordinated water molecules in a distorted octahedral geometry. The presence of intermolecular hydrogen bonding and (-( stacking interaction of aromatic rings from 2, 2'-bipy results in a 3D structure.     

Hydrothermal Synthesis and Structure Characterization of Compound Zn（Hpydc）2（H2O）（pydc=pyridine—2,5—dicarboxylate）

1 INTRODUCTION The researches in zinc complexes have been rapidly expanding because of their fascinating structural diversity and potential applications as functional materials and bioloenzymes[1~5]. A lot of compounds of different structural types containing zinc metal have been synthesized and reported[6~9]. In these complexes, the multifunction ligand, such as polyamine, polyacid, and so on, were often elected. In order to obtain more compounds having novel structures, recently, we ch…     

Synthesis and Crystal Structure of a Dinuclear Cu(Ⅱ) Complex [Cu(C_(13)H_9N_2O)Cl]_2·(CH_3CN)_2 with Ligand 2-Benzimidazol

A new dinuclear copper complex, [Cu(C13H9N2O)Cl]2·(CH3CN)2 (C30H24Cl2Cu2N6O2), has been synthesized and characterized by X-ray structure determination. It crystallizes in the tricli- nic system, space group P1, with a = 7.6677(14), b = 9.2375(17), c = 11.227(2) , α = 81.338(3), β = 88.173(4), γ = 66.199(3)o, V = 718.9(2) 3, Z = 1, Mr = 698.53, F(000) = 354, Dc = 1.613 g/cm3, μ(MoKα) = 1.705 mm-1, the final R = 0.0645 and wR = 0.1364 for 2474 unique reflections with 1809 observed ones (I > 2σ(I)). In the title complex, each copper(II) atom is located at the center of a distorted tetrahedron consisting of four coordinate atoms (one nitrogen atom, two oxygen anions, and one chlorine atom). Two copper(II) atoms are bridged by two oxygen anions (O(1) and O(1a)) of two phenolates to form a Cu(II)–Cu(II) binuclear entity, and the distance between two copper(II) atoms is 3.0144(15) .     

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.     

Hydrothermal Synthesis, Crystal Structure and Electrochemical Properties of the Complex Cu(o-Methylbenzoic acid)2(2,2''-bipy)·(H2O)

The title complex (C26H24CuN2O5, Mr = 508.01) has been synthesized by o-methylbenzoic acid, 2,2'-bipyridine (bipy) and copper perchlorate in the mixed solvent of water and methanol. It crystallizes in orthorhombic, space group P212121 with a = 0.70814(10), b = 1.6953(3),c = 1.9539(3) nm, V= 2.3457(6) nm3, Dc= 1.439 g/cm3, Z= 4,μ = 0.971 mm-1, F(000) = 1052, R= 0.0432 and wR = 0.0860. The structural determination shows that the copper atom is coordinated by three oxygen atoms from two o-methylbenzoic acids and one water molecule together with two nitrogen atoms from 2,2'-bipyridine, giving a distorted square-pyramidal coordination geometry.The cyclic voltammetric behavior of the complex is also discussed.     

Synthesis and Crystal Structure of [Cu（bbtz）（HCOO）2（H2O）2]n

1 INTRODUCTION Crystal engineering principles have been employ- yed in recent years to produce a variety of coordi- nation networks[1], which are of great current interest not only for their potential properties as functional solid materials[2] in host-guest chemistry, ion ex- change and catalysis, but also for their often com- plicated intriguing architectures and topologies. Ra- tional control the construction of polymeric net- works remains a great challenge in crystal engineer- ing. Mu…     

Hydrothermal Synthesis, Crystal Structure and Electrochemical Properties of the Complex Cu(o-Methylbenzoic acid)_2(2,2′-bipy)·(H_2O)

The title complex (C26H24CuN2O5, Mr = 508.01) has been synthesized by o-me- thylbenzoic acid, 2,2′-bipyridine (bipy) and copper perchlorate in the mixed solvent of water and methanol. It crystallizes in orthorhombic, space group P212121 with a = 0.70814(10), b = 1.6953(3), c = 1.9539(3) nm, V = 2.3457(6) nm3, Dc = 1.439 g/cm3, Z = 4, μ = 0.971 mm-1, F(000) = 1052, R = 0.0432 and wR = 0.0860. The structural determination shows that the copper atom is coordinated by three oxygen atoms from two o-methylbenzoic acids and one water molecule together with two nitrogen atoms from 2,2′-bipyridine, giving a distorted square-pyramidal coordination geometry. The cyclic voltammetric behavior of the complex is also discussed.     

乙二胺双缩3-醛基水杨酸Schiff碱铜镍异双核配合物的晶体结构

合成了乙二胺双缩3-醛基水杨酸Sch iff碱铜镍异双核配合物CuN i(ES)(H2O)2.H2O[H4ES为N,N′-二(3-醛基水杨酸)缩乙撑二胺],用单晶X-ray衍射法测定了晶体结构,该晶体属六方晶系,空间群P322I,晶胞参数a=1.283 90(18)nm,b=1.283 90(18)nm,c=0.995 7(2)nm,α=90°,β=90°,γ=120°,V=1.421 4(4)nm3,C18H18CuN iN2O9,Mr=528.59,Z=3,ρ=1.853 g/cm3.在配合物中,Cu处于由两个氮原子和两个酚氧原子所形成的平面四方场中,N i处于由两个酚氧原子、两个羧基氧原子和两个轴向水分子氧所形成的六配位变形八面体场中,且内部铜原子和外部镍原子通过两个酚氧原子桥联起来.     

Synthesis and Crystal Structure of a Mononuclear Zn(II) Complex with Tridentate Schiff Base,Zn(C_(12)H_(18)N_2O)(NCS)_2

1 INTRODUCTION In recent years there has been considerable and increasing interest in the synthesis of transition metal complexes with multidentate Schiff base ligands[1~4] because such ligands can accommodate one, two or more metal centers and may synthesize homo and/or heteronuclear metal complexes with interesting ste- reochemistry[5, 6]. In addition, these metal complexes can be used for biological modeling applications, catalysis, design of molecular ferromagnet and mate- rials chemis…     

Ligand effects on the structures and magnetic properties of tricyanomethanide-containing copper(II) complexes

The preparation, crystal structure and magnetic properties of four heteroleptic copper(II) complexes with the tricyanomethanide (tcm(-)) and the heterocyclic nitrogen donors 3,6-bis(2-pyridyl)pyridazine (dppn), 2,5-bis(2-pyridyl)pyrazine (2,5-dpp), 2,3-bis(2-pyridyl)pyrazine (2,3-dpp) and 2,3-bis(2-pyridyl)quinoxaline (2,3-dpq) are reported, {[Cu(2)(dppn)(OH)(tcm)(2)] x tcm}(n) (1), {[Cu(2,5-dpp)(tcm)] x tcm}(n) (2), {[Cu(2)(2,3-dpp)(2)(tcm)(3)(H(2)O)(0.5)] x tcm x 0.5H(2)O}(n) (3) and [Cu(2,3-dpq)(tcm)(2)](n) (4). 1 has a ladder-like structure with single mu-1,5-tcm ligands forming the sides and a bis-bidentate dppn and a single mu-hydroxo providing the rung. Each copper atom in 1 exhibits a distorted square pyramidal CuN(4)O surrounding: the basal plane is built by the hydroxo-oxygen, a nitrile-nitrogen atom from a tcm group and one pyrazine and a pyridyl nitrogen atoms from the dppn whereas the apical position is filled by a nitrile-nitrogen atom from a symmetry-related tcm ligand. The structures of 2-4 consists of zig-zag (2 and 3)/linear (4) chains of copper(II) ions which are bridged by either bis-bidentate 2,5-dpp (2) and 2,3-dpp (3) molecules or single mu-1,5-tcm (4) groups. The copper atoms in 2 and 4 are five coordinated with distorted trigonal bipyramidal (2) and square pyramidal (4) CuN(5) surroundings. The axial positions in 2 are occupied by two pyridyl-nitrogen atoms from two 2,5-dpp ligands whereas the trigonal plane is built by a nitrile-nitrogen from a terminally bound tcm group and two pyrazine nitrogen atoms from two 2,5-dpp molecules. The basal plane in 4 is defined by a pyridyl and a pyrazine nitrogen atoms from the bidentate 2,3-dpq ligand and two nitrile nitrogen atoms from two tcm groups (one terminal and the other bridging) whereas the apical position is filled by a nitrile nitrogen from another tcm ligand. The crystallographically independent copper atoms in 3 [Cu(1) and Cu(2)] exhibit elongated octahedral geometries being defined by four nitrogen atoms from two 2,3-dpp groups [Cu(1) and Cu(2)] either two terminally bound tcm ligands [Cu(1)] or a water molecule and a monodentate tcm ligand [Cu(2)] in cis positions. Magnetic susceptibility measurements for 1-4 in the temperature range 1.9-295 K reveal the occurrence of strong [J ca.-1000 cm(-1) (1); H = -JS(A) x S(B)] and weak [J = -0.13 (2), -0.67 (3) and -0.18 cm(-1) (4); H = -J Sigma(I)S(i) x S(i+1)] antiferromagnetic interactions in agreement with the different nature of the exchange pathways involved, diazine and single mu-hydroxo (1) and the extended 2,5-dpp (2), 2,3-dpp (3) and single mu-1,5-tcm (4) bridges with copper-copper separations of 3.363(8) (1), 7.111(1) (2), 6.823(1) and 7.056(1) (3) and 7.446(1) A (4).