Synthesis and Crystal Structure of a New Lanthanum（Ⅲ） 4-Cyanobenzoate Complex

A new dinuclear La（Ⅲ） complex [La2（4-cba）4[H（4-cba）2]2（phen）2（H2O）4] （4-Hcba = 4-cyanobenzoic acid and phen = 1,10-phenanthroline） 1 has been synthesized by solvothermal reaction in an ethanol/water mixed solution at 100 ℃ and structurally characterized by singlecrystal X-ray diffraction. Crystallographic data： C88H58La2N12O20, Mr = 1881.28, triclinic P1, a = 7.518（3）, b = 17.033（6）, c = 17.551（6）A, α = 115.333（4）, β = 92.9910（10）, γ = 99.366（5）°, V = 1985.3（12）A^3, Z = 1, Dc = 1.574 g/cm^3, F（000） = 944 μ = 1.145 mm^–1, the final R = 0.0281 and wR = 0.0686 for 6708 reflections with Ⅰ 〉 2σ（I）. In 1, two nine-coordinated La（Ⅲ） ions are connected by two 4-cba ligands in a syn-syn bidentate coordination mode, and the other six 4-cba ligands terminate the La（Ⅲ） ions, resulting in an isolated dinuclear structure. Two different types of intramolecular hydrogen bonds, asymmetrical O-H…O and symmetrical O…H…O, exist in the crystal. The title complex molecules are connected through hydrogen bonds and weak π-π stacking interactions to generate a 2-D layered network. The thermogravimetric analysis of 1 has also been discussed.     

Synthesis,Crystal Structure and Optical Properties of a Cerium（IV） Complex with Chelidamic Acid

A new cerium complex, （C7H8）[Ce（C7H3NO5）2（H2O）3]·2H2O or （C7Hs）[Ce（HChel）2· （H2O）3]·2H2O （1, H3Chel = 4-hydroxypyridine-2,6-dicarboxylic （chelidamic） acid）, has been prepared by the hydrothermal reaction, and its crystal structure was determined based on single-crystal diffraction data. Compound I crystallizes in monoclinic, space group P21/c with a = 12.4267（9）, b = 10.8195（7）, c = 19.5650（13）A, β = 92.898（3）°, V = 2627.2（3） A^3, Dc = 1.733 g/cm^3, Z = 4, Mr = 685.55, μ = 1.809 mm^-1, λ（MoKa） = 0.71073A and F（000） = 1372. The final R = 0.0455 and wR = 0.1984 for 5983 observed reflections with I 〉 2σ（I）, and R = 0.0490 and wR = 0.2053 for all data. Complex 1 contains one cerium ion, two chelidamic acid ligands, three coordinated water molecules, one discrete toluene molecule, and two discrete water molecules. The Ce（IV） ion is nine-coordinate with the coordination polyhedron made up of four oxygen atoms and two nitrogen atoms from two tridentate chelating chelidamic acid ligands, and three coordinated water molecules. A three-dimensional network is formed by the H-bonds. Moreover, optical properties are investigated and the results show that this complex has sharp optical absorption at 221,396 and 571 nm but no marked fluorescent emission.     

Synthesis and Crystal Structure of a New Oxovanadium（V） Multicomponent Complex with Acylhydrazone and Benzoylhydrazine

A new oxovanadium（V） complex with the mixed ligand of 2-oxopropionic acid benzoylhydrazone （C10H10N2O3） and benzoylhydrazine （C7H8N2O）, VO（C7H7N2O）（C10H9N2O3）, has been synthesized. Its structure was determined by single crystal X-ray diffraction analysis. The crystal belongs to monoclinic system with space group P21/n and cell parameters： a=1.1136（4） nm, b=0.6217（2） nm, c=2.6038（9） nm, β=97.182（6）°, V= 1.7887（11） nm^3, Z=4, F（000）=836, Mr=407.28, Dc= 1.512 g/cm^3,μ （Mo Kα） =0.592 mm^-1, R1 =0.0445, wR2= 0.1203. Vanadium atom is 6-coordinated by carboxyl and carbonyl O atoms and N atom of one tridentate C10H10N2O3 to form two stable five-membered rings with the same edge, and the other coordinated atoms of N and O come from one bidentate benzoylhydrazine C7H8N2O. The title complex has a six-coordinated V center [VO（N2O3）] with a distorted octahedral arrangement. In the crystal lattice, there are hydrogen bonding interactions between two molecules.     

Synthesis and Crystal Structure of a Rubidium Lanthanum Borate Rb3La3（BO3）4

The title compound was obtained by the flux method and its structure was determined. It crystallizes in monoclinic, space group P2/c with a = 11.0024（17）, b = 9.2979（14）, c = 14.500（2） A, β = 110.879（2）°, V = 1385.9（4） A^3, Z = 4, Mr= 908.38, F（000） = 1592, p = 19.601 mm^-1, Dc = 4.353 g/cm^3, the final R = 0.0481 and wR = 0.1257 for 2532 observed reflections with I 〉 2σ（I）, The Rb3La3（BO3）4 structure can be viewed as a 3-dimensional scaffold-like framework constructed by La-O polyhedra and BO3 groups. Two Rb＋ ions locate in a channel along the a direction and the rest one in a cavity.     

Synthesis and Crystal Structure of a Copper（Ⅱ） Complex with Benzilic Acid and 1,10-Phenanthroline

A new complex [Cu（phen）3][（C6H4）2C（OH）COO]2·6H2O was prepared by selfassembly of benzilic acid, 1,10-phenanthroline （phen）, and copper perchlorate. It crystallizes in triclinic, space group P1-, with a = 1.14661（17）, b = 1.6455（2）, c = 1.6457（2） nm, α= 74.779（2）, β = 74.904（3）, γ = 84.424（3）°, V = 2.8914（7） nm^3, Dc = 1.340 g/cm^3, Z = 2, F（000） = 1218, GOOF = 1.018, the final R = 0.0643 and wR= 0.1633. The crystal structure shows that the copper ion is coordinated with six nitrogen atoms from six 1,10-phenanthroline molecules, forming a distorted octahedral coordination geometry.     

Hydrothermal Synthesis, Crystal Structure and Electrochemical Properties of Complex Cu（α-Furacrylic acid）2（phen）

The title complex (C26H18CuN2O6,Mr=517.96) has been synthesized by the reac-tion of α-furanacrylic acid with 1,10-phenanthroline (phen) in the solvent mixture of water and methanol. Crystal data: monoclinic,space group C2/c with a =2.2927(4),b=1.01248(18),c=1.05061(18) nm,β=111.188(3)o,V=2.274(7) nm3,Dc=1.513 g/cm3,Z=4,F(000)=1060,μ= 1.007mm?1,R=0.0320 and wR=0.0781. The crystal structural analysis shows that the copper atom is coordinated with four oxygen atoms from two α-furacrylic acids and two nitrogen atoms from 1,10-phenanthroline,giving a distorted octahedral coordination geometry. The result of electroche-mical analysis shows that the electron transfer in the electrode reaction is quasi-reversible.     

Synthesis and Crystal Structure of Di-n-butyltin（Ⅳ） Complex with 2-Oxo-propionic Acid （4-Pyridinecarbonyl） Hydrazone

The novel complex di‐n‐butyltin(IV) 2‐oxo‐propionic acid (4‐pyridinecarbonyl) hydrazone, (n‐C₄H₉)₂Sn‐[O₂CC(CH₃)=N‐N=C(‐O)C₅N‐4] (H₂O) has been synthesized and its structure has been determined by X‐ray diffraction analysis. The complex crystallizes in orthorhombic system with space group Pca2₁. Crystal data: a=2.7540(9) nm, b=0.9676(3) nm, c= 1.5750(5) nm, V=4.197(2) nm³, D_c= 1.444 g/cm³, Z=8. μ= 1.241 mm^?1. F(000)= 1856, R₁=0.0462 and wR₂=0.1001. In the crystals of the title complex, the tin atom is in six‐coordination with a distorted octahedral geometry, three oxygen atoms [O(1), O(3) and O(4)] and one nitrogen atom N(1) forming the equatorial plane and C(10)‐Sn(1)‐C(14) being the axis. Two molecules form a dimer with weak interactions of Sn‐O bonding and hydrogen bonds.     

Crystal Structure and Magnetic Property of Heteronuclear Copper—Lanthanum Carboxylate Complex

ＥｘｐｅｒｉｍｅｎｔａｌＳｙｎｔｈｅｓｉｓａｎｄｅｌｅｍｅｎｔａｌａｎａｌｙｓｉｓＬａＬ3·2Ｈ2 Ｏ (86 0ｍｇ ,2 0ｍｍｏｌ ;ＨＬ =ＣＨ2 Ｃ(ＣＨ3) ＣＯＯＨ)ａｎｄＣｕ(ＮＯ3) 2 ·3Ｈ2 Ｏ (2 4 2ｍｇ ,1 0ｍｍｏｌ)ｗｅｒｅｄｉｓｓｏｌｖｅｄｉｎｔｏ 2 0ｍＬｏｆＨ2 ＯａｎｄａｄｊｕｓｔｅｄｔｏｐＨ 4 1ｗｉｔｈＨＬ (0 1ｍｍｏｌ/ｃｍ3) .Ａｎｅｔｈａｎｏｌｓｏｌｕｔｉｏｎｏｆ 1,10 ｐｈｅｎａｎｔｈｒｏｌｉｎｅ (2 0 0ｍｇ ,1 0ｍｍｏｌ)ｗａｓａｄｄｅｄｉｎｔｏｔｈｅｍｉｘｅｄｓｏｌｕｔｉｏｎｗｉｔｈｓｔｉ…     

Synthesis and Crystal Structure of a Mixed （Phthalocyaninato）（porphyrinato） Yttrium Double-decker Complex

The title compound,a mixed(phthalocyaninato)(porphyrinato) yttrium double-decker complex 1,has been synthesized and structurally characterized by X-ray single-crystal diffraction method.Crystal data:monoclinic,space group C2/c,Z = 8,C79H52Cl10N12O4Y,Mr = 1676.74,a = 38.217(3),b = 18.9867(13),c = 26.200(3) ,β = 128.0190(10)°,V = 14977(2) 3,Dc = 1.487 g/cm3,μ(MoKα) = 1.196 mm-1,F(000) = 6808,R = 0.0745 and wR = 0.2208 for observed reflections with I > 2σ(I).X-ray analysis reveals that the coordination polyhedron adopts a slightly distorted square-antiprismatic structure around the metal center.Both phthalocyanine and porphyrin ligands are saucer-shaped,with the skew angle of the two ligand planes approximately 45°.     

Synthesis,Characterization and Crystal Structure Determination of a Thiocyanato Bridged One-dimensional Polymeric Complex of Cadmium（Ⅱ）

A new one-dimensional polymeric complex [Cd（SCN）2（H2O）]L （L = N,N′-bis（furan- 2-ylmethylene）hydrazine） has been synthesized and characterized by IR, UV spectra, TG-DTA technique and single-crystal X-ray diffraction analysis. It crystallizes in triclinic, pace group P1^- with a = 5.9268（8）, b = 10.8678（15）, c = 13.3671（19） A, α = 109.295（2）, β = 95.092（2）, γ = 97.8580（10）°, V = 796.70（19）A^3, Z = 2, C12H10CdN4O3S2, Mr = 434.76, μ = 1.648 mm^-1, Dc = 1.812 g/cm^3, F（000） = 428, R = 0.0308 and wR = 0.0769. The crystal structure reveals that the structure of [Cd（SCN）2（H2O）]n features di-μ-1,3-thiocyante bridges and 1D chains. The octahedrally coordinated Cd atom is surrounded by one oxygen atom from water molecule, three S atoms and two N atoms from five di-μ-1,3 thiocyanato bridges. The Cd atoms are connected by two di-μ-1,3 thiocyanato bridges with the Cd（1）…Cd（1A） separation of 4.239（1） A and Cd（1）...Cd（1B） of 5.852（1）/~. In addition, the one-dimensional straight chain structure is further connected by multiform intermolecular N-H…O hydrogen bonds and π-π interactions to form a three-dimensional supramolecular structure.     

Synthesis and Crystal Structure of a New Mononuclear Cobalt（Ⅲ） Complex with 2,2＇-Dipyridylamine and Glycine as Ligands

A new mononuclear cobalt(Ⅲ) complex [Co(dpa)2(Gly)](ClO4)2·4H2O was synthesized by the reaction of Co2 , glycine (gly) and 2,2'-dipyridylamine (dpa) in a methanol-water solution, and its structure was characterized by IR, EA, ES-MS and X-ray structure analysis. The compound crystallizes in the monoclinic system, space group P21/n with a = 12.8795(2), b =13.2904(2), c = 19.1104(2) (A),β= 109.378(1)°, V= 3085.89(8) (A)3, Z = 4, Mr = 746.36, Dc = 1.606g/cm3,μ= 0.808 mm-1, F(000) = 1536, the final R = 0.0543 and wR = 0.1306 for 5393 independent reflections. The magnetic measurement of the compound at room temperature shows that it is diamagnetic and the cobalt ion is in low spin 3 oxidation state. ES-MS experiments show that the [Co(dpa)2(Gly)]2 cation is very stable in the methanol solution.     

Synthesis and Crystal Structure of a Hexameric Organooxotin Cluster from Benzilic Acid

1 INTRODUCTION There is great interest in the study of organotin carboxylic ester compounds due to their consider- able biological activities and structural diversities[1~3]. Since Holmes, R. R.[4] first reported the hexameric drum organotin compound, many organotin carboxy- lic ester compounds with drum-shape have been syn- thesized in recent years[5, 6]. It has been revealed that organotin compounds containing carboxylate ligands with additional donor atoms that are available for coord…     

Synthesis and Crystal Structure of a Zinc（Ⅱ）Complex with 2,2＇-Diphenic Acid and Benzimidazole Ligands

A new complex [Zn1.5(dpa)1.5(bim)]2n(dpa = 2,2-diphenic acid,bim = benzimida-zole)1 has been hydrothermally synthesized and structurally characterized by elemental analysis,IR,fluorescence spectrum and single-crystal X-ray diffraction.The complex crystallizes in monoclinic,space group C2/c with a = 18.773(8),b = 16.560(7),c = 16.417(9),β = 94.737(9)o,V = 5086(4)3,C56H36N4O12Zn3,Mr = 1153.00,Dc = 1.506 g/cm3,μ(MoKα)= 1.472 mm1,F(000)= 2344,Z = 4,the final R = 0.0573 and wR = 0.1164 for 2968 observed reflections(I > 2σ(I)).It exhibits a one-dimensional chain-like structure and shows luminescent property in the blue region.     

Hydrothermal Synthesis,Crystal Structure and Properties of a Lanthanum（III） Complex Based on a N,O-Donor Ligand①

A novel metal-organic complex [La（o-NCP）3]n （o-HNCP = 2-（2-carboxyphen- yl）imidazo（4,5- f）（1,10）-phenanthroline） has been hydrothermally synthesized and characterized by elemental analysis, infrared analysis and X-ray single-crystal diffraction. The complex crystallizes in triclinic, space group P1 with a = 9.898（2）, b = 16.193（3）, c = 16.909（3） A, a = 67.68（3）, β = 80.85（3）, y = 78.78（3）°, V= 2448.2（8） A3, Z = 2, Mr = 1156.9, Dc = 1.569 g/cm3,μ = 0.71073 A, F（000） = 1164, GOOF = 1.065, the final R = 0.051 and wR = 0.123 for 8539 observed reflections with I 〉 2o（I）. The complex exhibits a one-dimensional double chain structure. The adjacent chains are further connected by N-H...N hydrogen bonds which help to form a two-dimensional suprarnolecular architecture. Furthermore, the complex exhibits excellent thermal stability and luminescent property.