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 …     

Synthesis, Spectroscopic Properties and Crystal Structures of Dibenzyltin（IV） Dithiobenzoate and Chlorodibenzyltin（IV） Thiobenzoate

Two dibenzyltin(IV) complexes with thiobenzoate ligand, (PhCH2)2Sn(SOCPh)2 (1) and (PhCH2)2Sn(C1)SOCPh (2), have been synthesized by the reaction of dibenzyltin(IV) dichloride with thiobenzoic acid in the presence of organic base Et3N and characterized by IR, ^1H NMR spectroscopy and elemental analysis. Their crystal structures were determined by X-ray single crystal diffraction analysis. In the crystals of 1, the tin atom is six-coordinated in a distorted octahedron configuration. In the crystals of 2, the molecular packing in unit cell reveals that the two adjacent molecules are symmetrically linked to each other to form a dimer with intermolecular Sn…C1 distances of 0.3591 (2) nm and the tin atom is five-coordinated in a distorted trigonal bipyramid configuration.     

Computational studies of σ-type weak interactions between NCO/NCS radicals and XY(X = H,Cl;Y = F,Cl,and Br)

The triatomic radicals NCO and NCS are of interest in atmospheric chemistry,and both the ends of these radicals can potentially serve as electron donors during the formation of σ-type hydrogen/halogen bonds with electron acceptors XY(X = H,Cl;Y = F,Cl,and Br).The geometries of the weakly bonded systems NCO/NCS···XY were determined at the MP2/aug-cc-pVDZ level of calculation.The results obtained indicate that the geometries in which the hydrogen/halogen atom is bonded at the N atom are more stable than those where it is bonded at the O/S atom,and that it is the molecular electrostatic potential(MEP)-not the electronegativity-that determines the stability of the hydrogen/halogen bond.For the same electron donor(N or O/S) in the triatomic radical and the same X atom in XY,the bond strength decreases in the order Y = F > Cl > Br.In the hydrogen/halogen bond formation process for all of the complexes studied in this work,transfer of spin electron density from the electron donor to the electron acceptor is negligible,but spin density rearranges within the triatomic radicals,being transferred to the terminal atom not interacting with XY.     

Preparation and Crystal Structure of Hetero—metal Clusters[η^5—C5H4C（O）CH2CH2C（O）OCH3]FeCoM（μ3—S）（CO）8（M=Mo or W）

1 INTRODUCTIONTransition metal clusters have been attracting intensive attention largely because they are suggested as active catalysts in a variety of homogeneous catalyzed reactions. However, no unequivocal proof exists that metal clusters themselves serve as the true catalysts among the catalytic process. In many cases it is known that fragments of the original clusters are the actual catalytic species. The unambiguous proof would be the use of a rigid chiral cluster to catalyze an asy…     

Synthesis and Crystal Structure of cis—[meso—1,3—Bis（propylsulfinyl）propane]dichloroplatinum（Ⅱ）

1 INTRODUCTION A number of Pt complexes with monosulfoxide have been isolated and characterized[1]. It was indicated that the sulfoxide group trends to coordinate to soft metals (Pt, Pd, etc.) by its sulfur atom[2]. Pt(Ⅱ) trends to bond to disulfoxides in cis-mode and such complexes have potential antitumor activity[2]. However, only few examples of such complexes have been structurally characterized[3]. We will report herein the crystal structure of a new Pt(Ⅱ) complex with a disulf…     

Synthesis and Crystal Structure of a New Chain Coordination Polymer [Cu（inio）2（H2O）]∞ （Inio = Isonicotinic Acid N-Oxide）

1 INTRODUCTION With deep studies on the complex biology system and syntheses of new functional complexes, people have paid more and more attention to the polynuclear complexes. In the construction of one to three dimensional frameworks, multi-dentate ligands are usually used to bridge the metal centers to form polymeric structures[1, 2]. The isonicotinic acid N-oxide can function as a good mono-dentate ligand[3～8] through one oxygen atom from the group of -NO or carboxyl, and the dep…     

Kinetics and Mechanism of Oxidation of Lactic Acid by Dihydroxyditelluratoargentate（Ⅲ）in Alkaline Medium

The kinetics of the oxidation of lactic acid(Lac) by dihydroxyditelluratoargentate(Ⅲ）[abbreviated as DDA of Ag(Ⅲ）]anions was studied in an aqueous alkaline medium by conventional spectrophotometry in a temperature range of 25-40℃.The order of the redox reaction of lactic acid and DDA was found to be first-order.The rates increased with the increase in [OH^-]and decreased with the increase in [tellurate].No free radical was detected.In the view of this the dihydroxymonotelluratoargentate(Ⅲ）species(DMA) is assumed to be the active species.A plausible mechanism involving a two-electron transfer is proposed,and the rate equation derived from the mechanism can be used to explain all the experimenttal results.The activation parameters(25℃）and the rate constants of the rate-determining step along with the preequilibrium constants at different temperatures were evaluated.     

Synthesis and Crystal Structure of 2,5—Bis（morpholino）—3,4—bis（p—chlorophenyl）thiophene

1 INTRODUCTION -Thiocarbonylthioformamide synthesized in 1980[1, 2] is a class of stable and almost unexplored compounds[3]. We have reported the reaction of - thiocarbonylthioformamides in our previous paper[4]. Here, we will report a novel synthesis of 2 by the reaction of 1 and trimethyl phosphite in refluxing xylene. In order to determine the structure of 2, X- ray crystallographic study was carried out. 2 EXPERIMENTAL 2. 1 Preparation of the title compound Trimethyl phosph…     

Synthesis and Structure of [Cu2（μ—NO2）（aepy）4]（ClO4）3 （aepy=2—（2—Aminoethyl）pyridine）

1 INTRODUCTION There has been great and considerable interest in the study of copper nitrite complexes because they are relevant to the study of copper-containing enzymes involved in the denitrification process[1]; in particular, copper-nitrite complexes are potentially relevant to the nitrite reductases[2] (the enzyme from Achromobacter Cycloclastes) which convert NO2－ to NO and/or N2O. Many attempts have been made to synthesize a variety of copper-nitrite complexes, in which the n…     

Syntheses of Two Chiral Clusters [η5—C5H4C（NR）CH3]—RuNiM（CO）5（μ3—S）（R=NH—C6H3—2,4—（NO2）2,M=Mo,3;M=W,4）and the Single—crystal Structure of Cluster 3

1 INTRODUCTION The synthesis of chiral clusters containing four different atoms at the vertexes of the tetrahedron has been extensively studied because the chiral cluster can induce an asymmetric catalysis potentially[1]. Until now, many tetrahedron-type chiral clusters have been reported, but only a few of the reactions about the organic group in these clusters were investi- gated[2～4]. In this paper, we described the syntheses of clusters 3 and 4, and the structure of the former. 2 …     

One and Two-dimensional Structures of a New Oxamido Copper(II) Complex with Phthalato Bridged

1 INTRODUCTION Coordination polymers are a family of materials composed of 1D chains, 2D sheets, and 3D networks of metal-organic building blocks connected via co- valent and hydrogen bonds. Recently, they have re- ceived increasing attention for their fascinating struc- tures and topological features[1～4]. The complex as ligands approach is one of the best strategies to de- sign and synthesize polynuclear species, and a good example of ‘complex ligand’ is represented by mono- nuclear…     

Hydrothermal Synthesis and Structure of a Mixed-valence Polyoxotungstate Decorated by Copper(I) Coordination Group, [Cu(en)_2H_2O]_2[{Cu(en)_2}HPW_(12)O_(40)]·2H_2O

1 INTRODUCTION Polyoxometalates (POMs) are early transition metal oxygen clusters and have aroused much inte- rest because of their discrete structures of definite sizes, shapes[1] and potential applications in cata- lysis, medicine, materials science, g…     

Hydrothermal Synthesis and Structure of a Mixed-valence Polyoxotungstate Decorated by Copper(I) Coordination Group, [Cu(en)2H2O]2[{Cu(en)2}HPW12O40]·2H2O

A complex [Cu(en)2H2O]2[{Cu(en)2}HPW12O40]·2H2O (C12H57Cu3N12O44PW12, Mr = 3501.49) has been synthesized under hydrothermal conditions and its crystal structure was determined by X-ray diffraction.It crystallizes in the orthorhombic system, space group Pbca with a = 21.680(4), b = 20.680(4), c = 26.120(5) (A), V = 11711(4) (A)3, Dc = 3.972 g/cm3, Z = 8, μ(MoKa) = 24.661 mm-1, F(000) = 12440, the final R = 0.0527 and wR = 0.1416 for 11527 observed reflec- tions with I > 2σ(I).The crystal structure is composed of [{Cu(en)2}HPW12O40]2- anions, discrete [Cu(en)2H2O]+ complex cations and crystal water molecules, which are held together into a three- dimensional network through hydrogen-bonding interactions.The anionic [{Cu(en)2}HPW12O40]2- is formed by the mixed valance {HPWVI11WVO40}3- Keggin unit covalently linked by a {Cu(en)2}+ group.     

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.     

Synthesis and Structure of L-Aspartato-nickel(II) Complex with Benzimidazole

1INTRODUCTIONThereisgreatinterestinthecoordinationabili-tyofaminoacidtometalionsandhydrogenbondinginvolvedintheaminoacid[1].Asabinaryaminoacid,theasparticacidisespeciallyimportantfromeitherbiologicalorsimplecoordinativepointofview.Somereportsshowedthechan…     

One and Two-dimensional Structures of a New Oxamido Copper(Ⅱ) Complex with Phthalato Bridged

A new o-phthalato-bridged oxamide copper(Ⅱ) complex 1, {[Cu2(oxap)](pht)4H2O}n (oxap = N, N'-bis(2-aminopropyl)oxamide, pht = phthalate dianion), has been prepared and structurally characterized. It crystallizes in monoclinic, space group C2/c with a = 23.424(4), b = 7.9696(14), c = 15.727(3) (A), β = 129.617(2)°, C16H28Cu2N4O10, Mr = 563.50, V = 2261.6(7) (A)3, Z = 4, Dc = 1.655 g/cm3,μ(MoKα) = 1.939 mm 1, F(000) = 1160, the final R = 0.0393 and wR = 0.0928 for 1707 observed reflections with I ＞ 2σ(Ⅰ). Single-crystal X-ray analysis reveals that 1 displays a one-dimensional zigzag chain structure, in which each Cu(oxap) moiety adopting trans-conformation is connected by μ1,6-phthalate anion bridges, and these zigzag chains are further linked by anotherμ1,6-phthalate anion bridge to form a 2D sheet structure. The polar guest water molecules reside in the inter- and intrasheets to stabilize the whole crystal structure.     

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

1INTRODUCTION There has been considerable interest in the designand synthesis of transition metal complexes withcarboxylate ligands in coordination chemistry due tothe fact that this type of complexes has potentialapplications in molecule-based magnets,catalysis,supramolecular chemistry and biological systems[1～3].As an important flexibility dicarboxylate ligand,malonate dianion may act as momodentate,chelatedbidentate and tridentate bridging ligands to formvarious1D,2D and3D structures[…     

Hydrothermal Synthesis and Crystal Structure of a Square Grid Coordination Copper(II) Polymer from 1,4-Bis(imidazole-1-ylmethyl)benzene

1INTRODUCTION The employment of transition metal ions and ap-propriate bridging ligands has become a dominant theme in the construction of some interesting ar-rays[1,2],especially for the large square grid net-works.Recently,considerable research effort has been focused on the studies of polymeric frame-works with the ligands based on imidazole.These polymers are of great interest not only due to their intriguing topologies but also the potential applications in ion exchange,magnetic and e…     

Hydrothermal Synthesis, Crystal Structure and Magnetic Property of a Novel Pentanuclear Copper(II) Complex:[Cu_5(SIP)_2(HSIP)_2(H_2O)_(18)](H_2O)_5

The pentanuclear complex, Cu5(SIP)2(HSIP)2(H2O)18(H2O)5(H3SIP = 5-sulfoi-sophthalic acid), has been synthesized by the hydrothermal reaction of CuCl2 with NaH2SIP at 160 ℃, and characterized by single-crystal X-ray diffraction and IR spectrum.The crystal of the complex crystallizes in a triclinic system, space group P1-, with a = 7.0018(5), b = 11.9725(8), c = 19.0424(13) , α = 78.8540(10), β = 85.1710(10), γ = 83.6080(10)o, V = 1553.24(19) 3, Z = 1, C32H60O51S4Cu5, Mr = 1706.74, Dc = 1.825 g/cm3, μ = 1.937 mm-1, F(000) = 869, the final R = 0.0709 and wR = 0.1503 for 4235 observed reflections with I > 2σ(I).The five Cu2+ ions are connected by two symmetry-related tridentate SIP3-ligands and charge-balanced by two monodentate HSIP2-ligands, giving a discrete pentanuclear structure.The pentanuclear copper molecules are linked by hydrogen bonds to form a three-dimensional supramolecular structure.The temperature-dependent magnetic susceptibility data revealed weak ferromagnetic magnetic interactions between the Cu2+ ions.