Synthesis and Crystal Structure of Bis（barbiturato） triwater Complex of Copper（Ⅱ）

1 INTRODUCTION A variety of transition metal complexes with barbiturates have been prepared owing to their important roles in clinical detection and identi- fication of drug[1～5]. They have the general formula of M(Ⅱ)(barb)2L2, where M is a transition metal (Co, Cr, Zn, Cu etc), barb the anion of a substituted barbituratic acid and L an organic base, usually pyridine. In these complexes, the donor atom in the barbiturate anion is a deprotonated nitrogen atom and, the coordination …     

Preparation and Crystal Structure of Bis（2－thenoyltrifluoroacetone）Copper（Ⅱ）

ＰｒｅｐａｒａｔｉｏｎａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＢｉｓ（２－ｔｈｅｎｏｙｌｔｒｉｆｌｕｏｒｏａｃｅｔｏｎｅ）Ｃｏｐｐｅｒ（Ⅱ）ＷａｎｇＤｏｎｇ－Ｍｅｉ；ＹａｎｇＲｕｉ－Ｎａ；ＨｕＹｉ－Ｍｉｎ；ＪｉｎＤｏｕ－Ｍａｎ（ＨｅｎａｎＩｎｓｔｉ...     

Synthesis and Crystal Structure of aNovel Polymer Copper（ Ⅱ） Complex

1 INTRODUCTION One-dimensional coordination polymers of metal complexes have been extensively studied for many years owing to their unusual properties, and many efforts have been made to prepare these kinds of complexes. Study on these polymer complexes has an active field of coordination chemistry in recent years[1～5]. In this study we obtained a com- plex C14H9CuNO3CH3OH, of which the carboxy- late oxygen atom acts as the bridging ligands to coordinate to the second metal atom, fo…     

Synthesis and Crystal Structure of a New 2D O-bridged Copper(Ⅱ) Coordination Polymer Constructed from Sulfonate-derived Schiff Base

A new chain-like coordination polymer, namely, [CuL ]n(1, Na2 L = 2-[(2-hydroxybenzylidene)-amino]-benzenesulfonic acid sodium salt), has been synthesized and characterized by single-crystal X-ray diffraction, IR spectroscopy and elemental analysis. Complex 1 crystallizes in monoclinic system, space group P21/c with a = 9.2296(16), b = 10.4754(18), c = 12.200(2) A, β =102.392(2)°, V = 1152.0(3) A3, C13H9 CuN O4S, Mr = 338.83, Dc = 1.953 g/cm3, Z = 4, F(000) = 684,μ = 2.089 mm-1, the final R = 0.0376 and w R = 0.0956. X-ray diffraction analyses indicate that 1displays a square-pyramidal metal center with NO4 donor sets. The sulfonate-derived Schiff base serves as a common N,O,O′-tridentate and a unique O-bridged ligand connecting the metals.Dinuclear copper complexes serve as secondary building blocks(SBUs) to construct an unusual2 D coordination network. In the crystal, the components form a stable 3D supramolecular architecture by C–H···O interactions and π-stacking.     

Synthesis and Crystal Structure of Copper(Ⅱ) Compound with Didentate Schiff-base Ligand

1INTRODUCTIONTransitionmetalcomplexesofSchiff-baseligandswhichbindtwoormoremetalcentersincloseproximityareimportantaspotentialcatalysts[1]andasmodelsforanumberofmetalloproteins[2]duetotheopportunitytheyprovidefortheinvesti-gationofmagneticinteractions.The…     

Synthesis and Crystal Structure of a New Copper(II) Complex with 4-Cyanobenzoic Acid

1 INTRODUCTION Exploration on the syntheses and properties of car- boxylate complexes, especially aromatic carboxylate complexes, has always been a fascinating and chal- lenging research field for decades either in coor- dination chemistry or in functional materials[1, 2]. Cy- anobenzoic acid (Hcba) possessing two functional coordination groups should display structural diver- sities on the formation of complexes[3～15]. In particu- lar, the copper(II) carboxylate complexes bearing spe- …     

Synthesis and Crystal Structure of a New Mononuclear Copper(Ⅱ)Complex with 4,4',6,6'-Tetrabromo-2,2'-[ethylenedioxybis(nitrilomethylidyne)]diphenol

A new mononuclear Cu(Ⅱ)complex,[Cu(L)](H2L=4,4',6,6'tetrabromo-2,2'-[ethylenedioxybis(nitrilomethylidyne)]diphenol),has been synthesized and structurally characteri-zed.X-ray crystal stucture of the complex reveals that the Cu(Ⅱ)ion is four-coordinated by two oxygen atoms and two nitrogen atoms from L2-unit.Crystallographic data:monoclinic,space group P21/n with a=14.076(2),b=6.9801(14),c=19.858(2)(A),β=107.613(2)°,C16H10Br4CuN2O4,Mr =677.44,V=1859.6(5)(A)3,Dc=2.420 g/cm3,μ=9.796 mm-1,F(000)=1284,Z=4,the final R=0.0516 and wR=0.0938 for 1879 observed reflections with I＞20(I).The dihedral angel between the two coordination planes of Cu(1)-N(2)-O(4)and Cu(1)-N(1)-O(3))is 30.08(6)°.     

Hydrothermal Synthesis,Crystal Structure and Magnetic Behavior of a Novel 3D Supramolecular Complex [Cu（HDPPZC）（SO4）（H2 O）]2

In the title coordination compound,[Cu(HDPPZC)(SO4)(H2O)]2 (1,HDPPZC=dipyrido[3,2-a:2,3-c]-phenazine-2-carboxylic acid),has been hydrothermally synthesized and characterized by single-crystal X-ray diffraction,elemental analysis and magnetic susceptibility measurement.It crystallizes in triclinic,space group P1 with a=0.69485(6),b=0.76878(4),c=1.76638(13)nm,α=99.437(6),β=94.690(6),γ=95.735(6)o,V=0.92151(12) nm 3,Z=1,Cu2C38 H24 N 8S2O14,Mr=1007.85,Dc= 1.816 g·cm-3,F(000)=510,GOOF=0.988,the final R=0.0580 and wR=0.0689.The structural analyses reveal that complex 1 shows discrete dinuclear clusters,which are further linked by hydrogen bonding and π·π stacking interactions to form a three-dimensional supramolecular compound.Magnetic measurement shows ferromagnetic and antiferromagnetic exchange interactions in the sample.     

Synthesis and Crystal Structure of a New Three-dimensional Supramolecule of Copper（Ⅱ） Schiff Base Complex

A new three-dimensional supramolecule composed of copper-Schiff base complex, [Cu（naphdien）]Cl·H2O, where naphdien is Schiff base of 2-hydroxy-1-naphthaldehyde and diethylenetriamine, has been synthesized and determined by single-crystal X-ray diffraction. It belongs to the monoclinic system, space group P21/c, with a = 7.3490（15）, b = 7.0847（16）, c = 30.845（3）A, β= 95.33（3）°, V = 1599.0（5）A3, Z = 4, C15 H20ClCuN3O2, Mr = 373.33, De = 1.551 g/cm3, μ = 1.543 mm^-1, F（000） = 772, R = 0.0536 and wR = 0.0927 for 2788 unique reflections with 1659 observed ones （I 〉2σ（I））. In the crystal structure, mononuclear units [Cu（naphdien）]Cl·H2O are linked into a two-dimensional framework via strong hydrogen bonds, and extended into a three-dimensional supramolecular structure through π-π stacking interactions.     

Synthesis and Crystal Structure of a Novel Fe(Ⅲ) Schiff Base Complex

A novel Fe(Ⅲ) Schiff base complex,FeⅢ(HL) {H4L = 1,1,1,1-tetrakis[(salicylaldimino)methyl]methane},has been prepared and characterized by elemental analyses,IR spectrum,and single-crystal X-ray diffraction analysis.The crystal belongs to the monoclinic system,space group P21/n with a = 12.569(3),b = 12.955(3),c = 17.647(4) ,β = 91.896(9)°,V = 2871.9(1) 3,Z = 4,Dc = 1.391 g/cm3,F(000) = 1252.0,Mr = 601.45,R = 0.0383 and wR = 0.1025.The structural analysis reveals that the Fe(Ⅲ) ions are six-coordinated by imine nitrogen atoms and phenolic oxygen atoms form three pendant arms of Schiff base ligands,and one of the salicylaldimine chelating units remains uncoordinated.Discrete complex molecules were further assembled into 1D supramolecular aggregations by C-H…O hydrogen bonding and C-H…π interactions.     

Synthesis and Crystal Structure of a Novel Binuclear Cu（ Ⅱ ） Complex with Tetradentate Schiff-base Ligand

1 INTRODUCTION Many metalloenzymes containing in their active sites two copper ions that operate cooperatively occur in plants and animals. They are utilized for dioxygen transport or activation, electron transfer, reduction of nitrogen oxides, and hydrolytic che- mistry[1]. Consequently binuclear copper complexes with two ions in close proximity have received a great deal of attention[2～4]. These complexes are particularly of interest in the field of biomimetic chemistry to provide impr…     

A New Dinuclear Cu(Ⅱ) Complex of a Ligand with Benzimidazole Group─Synthesis and Crystal Structure

A new dinuclear copper complex, [Cu(C9H11N3)Cl2]2 (C18H22Cl4Cu2N6), has been synthe- sized and characterized by X-ray structure determination. It crystallizes in the triclinic P1 space group with a = 7.526(3), b = 9.473(4), c = 9.535(3) , α = 117.214(10), β = 108.251(9), γ = 91.560(6)o, V = 562.3(4) 3, Z = 1, Mr = 591.30, F(000) = 298, Dc = 1.746 g/cm3, μ(MoKα) = 2.385 mm-1, the final R = 0.0577 and wR = 0.1248 for 2188 unique reflections with 1629 observed ones (I > 2σ(I)). In the title complex, each copper(II) atom is located at the center of a distorted trigonal bipyramid of five coordination atoms (two nitrogen and three chlorine atoms). Two copper(II) atoms were bridged by two chlorine anions (Cl(2) and Cl(2a)) to form a Cu(II)-Cu(II) binuclear entity with the distance between two copper(II) atoms of 3.398 .     

Synthesis and Crystal Structure of a New Cadmium（Ⅱ） Coordination Polymer with Ethylenediaminetetraacetic Acid

A new cadmium(Ⅱ) coordination polymer,namely,[KCd2(edta)I]n(1,H4edta = ethylenediaminetetraacetic acid),has been prepared and structurally characterized by single-crystal X-ray diffraction.Crystallographic data for 1:C10H12Cd2IKN2O8,Mr = 679.02,monoclinic,space group P21/n,a = 9.870(5),b = 8.989(4),c = 19.082(10) ,β = 104.581(10)o,V = 1638.5(13) 3,Z = 4,Dc = 2.753 g/cm3,μ = 4.776 mm-1,F(000) = 1272,the final R = 0.0473 and wR = 0.1311 for 2846 observed reflections with I > 2σ(I).Polymer 1 features a 2-D layered structure,in which each edta4-ligand chelates/bridges five adjacent six-/seven-coordinated Cd(Ⅱ) centers with all ten donors(eight oxygen and two nitrogen) involved with coordination.Additional iodide I-ions as counterions are bound to the Cd(Ⅱ) centers in a terminal mode and the potassium K+ ions are located in the layers and surrounded by O and I atoms from neighboring environment.The thermal stability of 1 has been 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.     

Synthesis and Crystal Structure of a Novel Binuclear Cu(Ⅱ) Complex with Tetradentate Schiff-base Ligand

A novel binuclear complex ([Cu2(μ2-shed)(hshed)]·(ClO4)·H2O, h2shed = N-salicylidene-N′-(2-hydroxyethyl)ethylenediamine) has been synthesized and structurally characterized by X-ray diffraction analysis. It crystallizes in monoclinic, space group P21/c with a = 12.511(10), b =15.750(12), c = 14.281(12) (A), β = 100.564(14)°, C22H31ClN4O9Cu2, Mr = 658.04, V= 2766(4) (A)3, Z =4, Dc = 1.580 g/cm3, μ(MoKα) = 1.689 mm-1, F(000) = 1352, the final R = 0.0528 and wR = 0.1433 for 4880 independent reflections with Rint = 0.0577. The complex is a binuclear copper compound,and two Cu(Ⅱ ) ions in the binuclear cation are in different coordination environments. The Cu(1) ion adopts a distorted square pyramidal geometry (τ = 0.22) with four donor atoms (N2O2) of the ligand in the basal plane, and one hydroxyl oxygen atom with protonated form occupying the apical position.The Cu(2) ion assumes the geometry of a distorted square plane with four donor atoms (N2O2) of the ligand. The Cu…Cu separation is 3.103 (A). In addition, N-H…O and C-H…O intermolecular hydrogen bonding interactions link these binuclear cations into a quasi one-dimensional chain along the a axis.     

Synthesisand Crystal Structure of a Cu（II） Complex with Reduced Schiff-base N-（2-Hydroxybenzyl）-D,L-alanine and 4,4＇-Bipyridine

A new complex [Cu2(sala)2(H2O)2(4,4'-bipy)]·H2O (sala = N-(2-hydroxybenzyl)- D,L-alaninate, 4,4'-bipy = 4,4'-bipyridine) has been synthesized and characterized by elemental analysis, IR spectroscopy, thermogravimetric analysis and single-crystal X-ray diffraction. The complex crystallizes in monoclinic system, space group C2/c with a = 42.44(3), b = 10.416(8), c = 15.487(13), β = 97.455(14)o, C30H36Cu2N4O9, Mr = 723.71, V = 6789(9)3, Dc = 1.416 g/cm3, Z = 8, F(000) = 2992, μ(MoKα) = 1.308 mm-1, R = 0.0493 and wR = 0.1004 for 4878 observed reflections (I > 2σ(I)). Structural analysis shows that each copper(II) atom displays a distorted square-based pyramidal coordination geometry with two oxygen atoms and one nitrogen atom from one N-(2-hydroxybenzyl)-D,L-alaninate, one nitrogen atom from 4,4'-bipyridine ligand and one water molecule. 4,4'-Bipyridine ligand bridges two Cu(II) ions to form a dinuclear compound. The molecular structure is extended into a one-dimensional wavy chain through hydrogen bonds. These 1D chains are further expanded into 2D networks through hydrogen bonds.     

Synthesis,Crystal Structure and Properties of a Nanotubular Metal-organic Framework（MOFs） Based on Cu（Ⅱ） Oxide Chains and Benzenedicarboxylates

A new cooper benzenedicarboxylate metal-organic coordination polymer,[Cu(μH2O)(BDC)]n·nDMF(1,H2BDC = 1,4-benzenedicarboxylate acid,DMF = N,N'-dimethylfor-mamide),has been successfully synthesized under hydrothermal conditions and characterized by IR spectroscopy,elemental analysis,thermogravimetric analysis and single-crystal X-ray diffraction.This complex crystallizes in triclinic,space group P1 with a = 6.605,b = 10.44780(10),c = 11.0881(6) ,α = 62.064(11),β = 73.410(15),γ = 78.404(16)°,C11H13CuNO6,Mr = 318.76,V = 645.79(8) 3,Z = 2,Dc = 1.639 g/cm3,F(000) = 326,μ = 1.712 mm-1,the final R = 0.0362 and wR = 0.1330 for 2055 observed reflections with I > 2σ(I).The title compound contains infinite inorganic chains constructed by Cu oxygen octahedra by sharing corners and edges.Each chain is connected by BDC linkers to four other chains to form a three-dimensional framework with irregular rhombic channels where the DMF molecules are encapsulated.     

Synthesis and Crystal Structure of Dinuclear Copper(Ⅱ)Complex Cu_2(μ-PhCOO)_4(amet)_2·2CH_3COCH_3

1INTRODUCT1ONFormode1ingcompoundsofcertaincopper-containingenzymes,theinvestigationofdinuclearcoppercomplexeshasattractedtheattentionofinorganicandbiologicchemistst1i.Actingasoxygentransportproteinsforinvertebrates,oxyhemocyanin(oxyHc)hasadinuclearcoppersitewithaCu-Cuseparationofca.3.6A[2'3i(Fig.1).In1984,Karlinetal-[4ireportedthesynthesisofadinuclearcopper(I)com-plexwithabidentateligand.Thecomplexreactswithdioxygenquasireversibly,whichproducesaperoxodinuclearcopper(I)complex(Nallo=8O3…     

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.     

Synthesis, Crystal Structure and Properties of a Novel Vanadium（Ⅴ） Oxoperoxo Complex Incorporating a Tridentate Hydrazone Ligand

A novel vanadium(V) oxoperoxo complex [VOO2(APTCH)(CH3OH)] (HAPTCH = 2-acetylpyridine thiophene-2-carboxylic hydrazone) has been synthesized and characterized by IR, TGA and X-ray single-crystal structure determination. The complex crystallizes in the monoclinic system, space group P21/c with a = 11.232(2), b = 10.762(2), c = 112.613(3), β = 99.44(3)°, V = 1504.1(5)3, Dc = 1.657 g·cm-3, Z = 4, F(000) = 768, μ = 0.827 mm-1, the final R = 0.0392 and wR = 0.1073 for 2266 observed reflections with I > 2σ(I). Single-crystal X-ray diffraction studies reveal that the vanadium(V) is coordinated by a tridentate ligand, methanol molecule and peroxo group to form a pentagonal-bipyramidal geometry. The crystal structure is stabilized by intermolecular hydrogen bonds of O-H···N and C-H···O.