Molecular and Supramolecular Structures of a Nickel（Ⅱ） Complex with a Macrocyclic Ligand

1 INTRODUCTION The knowledge of all non-covalent interactions, such as strong and weak hydrogen bonds and p…p interactions, is important to the supramolecular chemistry, biochemistry, crystal engineering and material science[1～7]. Several mononuclear complexes of macrocyclic oxamido Schiff base ligands with phenyls have been used as 揷omplex ligands?to design polynuclear complexes[8～11]. Herein we report the molecular and crystal structures, CH贩稯 hy- drogen bonding and p…p stacki…     

Synthesis and Crystal Structure of Chloro(p-toluidine)[4-(p-tolyl)imino-2-pentanone-3-oximato]- palladium(Ⅱ), PdCl(p-CH_3C_6H_4NH_2)(p-CH_3C_6H_4-iai)

1 INTRODUCTION Transition metal complexes of N-R-isonitroso- b-ketoimine have received considerable interest, because the isonitroso (oximo) group can coordinate to metal atoms through its oxygen and/or nitrogen atoms to form several geometrical isomers[1～4]. Some palladium(Ⅱ) complexes with N-R-isonitro- soacetylacetoneimine (abbreviated to R-Hiai)[4] and N-R-isonitrosoethylacetoacetate (abbreviated to R- Hieai)[5] have been reported. Here we will report the structure of a palladi…     

Synthesis and Crystal Structure of a Dicopper(Ⅰ) Complex with Bis(diphenylphosphino)methane and Diethyldithiocarbamate

1 INTRODUCTION Dithiocarbamate derivatives and their metal complexes are extremely versatile compounds which have been used, for example, in the treatment of alcoholism, sarcoma cell and as possible pro- tection against the lethal effect of X-rays etc[1]. Owing to the striking structure features and diversified applications of the metal complexes with dithiocarbamate[2～6], it is of theoretical and practical significance to study the coordination chemistry much more adequately. The meta…     

Synthesis and Structure of a Novel Macrocyclic Complex [Cd2(phen)4(phth)2]·4H2O

A novel complex [Cd2(phen)4(phth)2]·4H2O has been synthesized by the reaction of H2phth(phthalic acid) and phen(1,10-phenanthroline) with Cd(Ⅱ) in ethanol-water solution. X-ray crystal structure analysis shows it crystallizes in triclinic, space group P1 with a = 10.619(3), b =12.560(4), c = 12.651(4) A, α = 98.775(5), β = 109.035(5), γ = 113.576(5)°, C32H24CdN4O6, Mr=672.95, V= 1381.7(7) A3, Rint = 0.0358, Z= 2, Dc= 1.618 g/cm3, μ = 0.845 mm-1, -6 ≤h≤13, -15≤k ≤13, -15≤l≤14, F(000) = 680, S = 1.038, R = 0.0480 and wR = 0.0849 for 3992 observed reflections (I ＞ 2σ(Ⅰ)). Phth bridges Cd(Ⅱ) to form a macrocyclic compound, and a 2D supramolecular motif is formed through hydrogen bonds and π-π interaction.     

Synthesis and Crystal Structure of （3R,4R）-5-（2,4-Dichlorobenzoyl）-4-（4-nitrophenyl）-6-（phenylamino）-3,4-dihydro-2H-thiopyran-3-carbonitrile

The title compound(C25H16Cl2N3O3S),as a thiopyran derivative,has been synthe-sized by the cyclization of an organic intermediate obtained from Baylis-Hillman adducts with a β-aroylthioamide using copper(I) salt as the catalyst.The crystal belongs to the monoclinic system,space group P21/c with a = 13.668(3),b = 8.4803(17) c = 21.999(4) ,β = 113.57(3)°,V = 2337.2(10) 3,Z = 4,Mr = 510.38,Dc = 1.451 g/cm3,μ = 0.401 mm-1,F(000) = 1048,the final R = 0.0487 and wR = 0.1079 for 3678 observed reflections with I > 2σ(I).     

Synthesis and Crystal Structure of [VO2（C17H11N3O2） ] [VO （C4H13N3）（C6H5N3O） ]（C2H5OH）

The reaction of VO（acac）2 with 2-hydroxyl-1-naphthaldehyde isonicotinyl hydrazone and amines （ethylenediamine or diethylenetriamine） in CH3OH yields crystals of novel vanadium compounds characterized by IR, NMR spectroscopic methods and X-ray single-crystal structure determination. Two different vanadium units exist in the crystal cell of [VO2（C17H11N3O2）][VO- （C4H13N3）（C6H5N3O）]（C2H5OH） which crystallizes in the triclinic system, space group P1 with a = 8.0104（17）, b = 13.898（3）, c = 14.955（3）A, α = 89.103（4）, β = 79.551（4）, γ = 78.352（4）°, V = 1603.3（6）A^3, Mr = 723.54, Dc = 1.499 g/cm^3, Z = 2, λ（MoKα） = 0.71073 ]A,μ= 0.644 mm^-1, F（000） = 748, the final R = 0.0547 and wR = 0.0997 for 8920 observed reflections with I 〉 2σ（I）. According to structure analysis, two different molecules are arranged in the lattice and the two vanadium atoms adopt octahedral and square pyramidal coordination geometries, respectively. The interactions between DNA and vanadium complexes have been investigated by UV-Vis absorption spectro- photometry.     

Synthesis and Crystal Structure of 3,3''-Bis(2-benzimidazolyl)-2,2''-dipyridine with Hydrated Zinc(Ⅱ) Perchlorate

The reaction of Zn(ClO4)2·6H2O with 3,3'-bis(2-benzimidazolyl)-2,2'-dipyridine (L) gave a mononuclear zinc(Ⅱ) complex: [ZnL2](ClO4)2·2DMF·4H2O, which was structurally characterized by EA, IR, UV, 1H NMR, fluorescence spectrum and single-crystal X-ray diffraction. The crystal (C54H54Cl2N14O14Zn, Mr=1259.38) belongs to the monoclinic system, space group C2/c with a=20.874(2), b=14.9953(16), c=20.462(3) (A), β=101.553(2)°, V=6274.8(13) (A)3, Z=4, Dc=1.333 g/cm3, F (000)=2608, μ(MoKα)=0.548 mm-1, R=0.0682 and Wr=0.1931 for 4984 observed reflections with Ⅰ ＞ 2σ(Ⅰ). The Zn(Ⅱ) is four-coordinated in a slightly distorted tetrahedral geometry through four N atoms from four benzimidazole units of two ligands. In the crystal lattice, the [ZnL2]2 cations are linked to each other by extensive intermolecular hydrogen bonds between nitrogen atoms of benzimidazole rings, water and DMF molecules.     

Synthesis and Crystal Structure of (E)-2-(1-(2-Hydroxy-4-methoxyphenyl)ethylideneamino)-3-(4-hydroxyphenyl)methyl Propionate

(E)-2-(1-(2-Hydroxy-4-methoxyphenyl)ethylideneamino)-3-(4-hydroxyphenyl)methyl propionate (C22H27O6N, Mr = 401.45) has been synthesized by a condensation reaction of paeonol with tyrosin methyl ester hydrochloride, and its structure was determined by IR, NMR, HR MS and X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P21/c, with a = 11.91291(15), b = 9.49947(12), c = 19.8727(3) , β = 106.1104(15)°, V = 2160.60(5)3, Z = 4, Dc = 1.234 g/cm3, μ = 0.739 mm-1, F(000) = 856, R = 0.0466 and wR = 0.1461 for 3859 observed reflections with (Ⅰ> 2σ(Ⅰ)). In the crystal structure, the title compound is constructed by a centrosymmetric dimmer unit composed of a pair of π-π stacking enantiomers, and such units are linked by intermolecular O(5)-H(5)…O(1) and intramolecular N(1)-H(1)…O(1) hydrogen bonds.     

Structures of 1-（3,4-Dihydroxyphenyl）-2-（3,4-dimethoxyphenyl） ethanone and Its Hydrate Complex

The title compounds, C16H16O5 (I) and C16H16O5·H2O (II), were structurally characterized by single-crystal X-ray diffraction. Compound I crystallizes in monoclinic space group P21/c with a = 10.5574(10), b = 8.3576(9), c = 16.5528(16) , β = 91.762(3)°, Z = 4, R = 0.0524 and wR = 0.1084. The molecules are jointed into a chain by intermolecular O-H···O and C-H···O hydrogen bonds, which form layers parallel to (001). The chains run along the [110] and [110] directions alternatively layer by layer, and are assembled into a network by intermolecular O-H···O (carboxyl) hydrogen bonds. On the other hand, the hydrate complex (II) crystallizes in the triclinic space group P1 with a = 5.1451(2), b = 10.4583(4), c = 14.8267(5) , α = 70.900(2), β = 82.478(2), γ = 81.359(2)°, Z = 2, R = 0.0393 and wR = 0.0983. The molecules are linked into infinite two-dimensional ribbons by O-H···O (carbonyl) and solvent-bridged O-H···O hydrogen bonds.     

Synthesis and Structural Characterization of Co( Ⅱ ) Coordination Polymer [Co(μ-phth)(imi)2]n

A new cobalt( Ⅱ ) complex [Co(μ-phth)(imi)2]n (phth = o-phthalato, imi = imidazole)has been synthesized by the reaction of CoCl2 with disodium o-phthalate and imidazole. The crystal structure of the compound has been determined by single-crystal X-ray diffraction. The crystal is of monoclinic system, space group Pn with a = 8.405(1), b = 9.995(1), c = 9.996(2) (A),β= 104.479(2),V= 813.0(2) (A)3, Dc= 1.467 g/cm3, C14H12N4O4Co, Mr= 359.21, F(000) = 366,μ = 1.079 mm-1, Z = 2, R = 0.0483 and wR = 0.1209 for 1583 observed reflections (Ⅰ＞ 2σ(Ⅰ)). In the title complex, the Co(Ⅱ) ions are bridged by o-phthalate ligands in a bidentate mode, producing a zigzag infinite chain structure. Each four-coordinated cobalt( Ⅱ ) center was coordinated by two oxygen atoms and two nitrogen atoms to give a distorted tetrahedral geometry. The chains are linked by hydrogen bonds between oxygen atoms belonging to carboxylate groups and hydrogen atoms of imidazole molecules, forming an unusual two-dimensional coordination polymer.     

Synthesis and Structural Characterization of a Copper Complex with Furaldehyde Salicylylhydrazone

The copper complex Cu（C12H9N2O3）2 has been synthesized by the reaction of furaldehyde salicylylhydrazone （Hfs） and copper acetylacetonate and characterized by X-ray crystal diffraction and spectroscopic studies. The crystal crystallizes in space group P211n with a = 5.9765（3）, b = 15.7196（9）, c = 12.0514（6）A,β= 101.618（3）^o, V = 1109.0（1）A^3, C24H18CuN4O6, Mr = 521.96, Z = 2, Dc = 1.563 g/cm^3, μ = 1.035 mm^-1, F（000） = 534, R = 0.0373 and wR = 0.1058 for 2283 observed reflections （I 〉 2σ（I））. The copper atom has a square-planar CuN2O2 coordination and should be in an octahedral coordination if considering Cu-O （phenol） with distances of 2.796（2）A as weak bonds. The neighboring copper complex molecules are linked together by these weak Cu-O （phenol） bonds, resulting in an extended 1D chain. The title compound exhibits paramagnetic property and fluorescence behavior at room temperature supported by the EPR and fluorescence spectra.     

Synthesis and properties of one-dimensional Ni(Ⅱ) and Ni(Ⅱ)Cu(Ⅱ) complexes linked by hydrogen bond

Four dithiooxalato (Dto) bridged one-dimensional Ni(ll) and Ni(ll)Cu(ll) complexes (Me6[14]dieneN4)Ni2(Dto)2) (1), (Me6[14]dieneN4)CuNi(Dto)2 (2), (Me6[14]aneN4)Ni2(Dto)2 (3), and (Me6[14]aneN4)CuNi(Dto)2(4), were synthesized. These complexes have been characterized by elemental analysis, IR, UV and ESR spectra. The crystal structure of complex 3 was determined. It crystallizes in the monoclinic system, space group C2/c with a = 2.2425(4) nm, b = 1.0088(2) nm, c=1.4665(3) nm, β= 125.32(3)° ;Z=4; R = 0.076, Rw = 0.079. In the complex, Ni(1) coordinates four sulphur atoms of two Dto ligands in plane square environment. Ni(2) lies in the center of mac-rocyclic ligand. For Dto ligand, two sulphur atoms coordinate Ni(1), and O(1) coordinates Ni(2) and forms weak coordination bond. O(2) is linked to N(2) of macrocyclic ligand through hydrogen bond.     

Synthesis and Crystal Structure of a Mixed－Valence Trinuclear Manganese Complex：Mn_3O（O_2CPh）_6（Py）_3

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆａＭｉｘｅｄ－ＶａｌｅｎｃｅＴｒｉｎｕｃｌｅａｒＭａｎｇａｎｅｓｅＣｏｍｐｌｅｘ：Ｍｎ_３Ｏ（Ｏ_２ＣＰｈ）_６（Ｐｙ）_３ＸｕＨａｏ；ＬｉＪｉｎ－Ｙｕ；ＬｉｕＱｉ；ＸｕＺｈｅｎｇ；ＹｏｕＸｉａ...     

Synthesis and Crystal Structure of the Novel Chiral o—Hydroxyphenyloxazoline Metal Complexes

1 INTRODUCTION Optically active oxazolines have been extensi- vely used as valuable chiral ligands for transition metals in asymmetric catalysis[1]. The design and syntheses of new chiral oxazoline ligands have inspired many scientists to work with great efforts during the recent years. Our interest has been focus- ed on the studies of enantioselective transition- metal catalysis of heterocyclic ligands. In the pre- sent work, we choose o-hydroxyphenyloxazoline ligand for it has a rigi…     

Synthesis and Crystal Structure of 1＇-Methyl-4＇-（4-chlorophenyl）-1H-indole-3-spiro-2＇-pyrrolidine-3＇-spiro-4＂-（2＂-phenyloxazole）-2,5＂（3H,4＂H）-dione

The title compound （C26H20ClN3O3） has been synthesized by 1,3-dipolar cycloaddition reaction from isatin, sarcosine and （Z）-4-（4-chlorobenzylidene）-2-phenyloxazol-5（4H）-one through a one-pot procedure, and its structure was confirmed by IR, IH NMR, elemental analysis and single-crystal X-ray diffraction analysis. The crystal belongs to the triclinic system, space group PI, with a = 9.3903（19）, b = 11.398（2）, c = 12.603（3） A, α = 83.495（3）, β = 68.988（3）, γ = 67.178（3）^o, V= 1160.1（4）A^3 Z = 2, Mr= 457.90, Dc= 1.311 g/cm^3, p = 0.198 mm ^-1, F（000） = 476, the final R = 0.0489 and wR = 0.1144 for 3109 observed reflections with I 〉 2σ（I）.     

Synthesis and Crystal Structure of Diaquabis{2,4-dibromo-6-[(2-ethylaminoethylimino)methyl]-phenolato}nickel(Ⅱ) Dinitrate Diacetonitrile

The title mononuclear Schiff base nickel(Ⅱ) complex [Ni(C11H14Br2N2O)2(H2O)2]· 2NO3·2C2H3N was prepared and characterized by elemental analysis,IR spectrum,and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system,space group P21/n with a=15.534(2),b=7.647(1),c=16.435(2),β=103.252(2)o,V=1900.3(4)3,Z=2,Dc=1.750 g/cm3,Mr=1000.99,λ(MoKα)=0.71073,μ=4.776 mm-1,F(000)=996,the final R=0.0368 and wR=0.0724. A total of 3988 unique reflections were collected,of which 2764 with I > 2σ(I) were observed. The complex consists of a mononuclear [Ni(C11H14Br2N2O)2(H2O)2]2+ cation,two nitrate anions and two acetonitrile molecules. The Ni atom,lying on the inversion centre,is six-coordinated by two Schiff bases and two water molecules to assume an octahedral coordination geometry. The molecules in the crystal are linked through intermolecular hydrogen bonds of N–H…O,N–H…Br,O–H…O,O–H…N and C–H…O to form layers.     

混合三烃基锡有机酸酯化合物构效关系 （Ⅰ）二环己基－甲基－2，4－二溴－β－甲基苯氧乙酸锡酯 及二环己基－甲基－2－甲氧基－4－丙烯基苯氧乙酸锡酯的晶体结构和分子结构

报道２，４－Ｂｒ２Ｃ６Ｈ３ＯＣＨ（ＣＮ３）ＣＯ２Ｓｎ（Ｃ６Ｈ１１）２ＣＵ３（１）和２－ＯＣＨ３－４－ＣＨ３ＣＨ＝ＣＨＣ６Ｈ３ＯＣＨ２ＣＯ２Ｓｎ（Ｃ６Ｈ１１）２ＣＨ３（Ｈ２Ｏ）（Ⅱ）的晶体结构和分子结构。（Ⅰ）单斜晶系，空间群Ｐ２１／ｃ，ａ＝１３．０６７（３），ｂ＝１０．５９４（３），ｃ＝１８．１５７（４），β＝１０６．９９（２）°，Ｚ＝４，Ｄｃ＝１．６７２ｇ／ｃｍ３，Ｖ＝２４０３．７３，μ＝４３．７３１ｃｍ－１，Ｍｒ＝６２２．９９，Ｆ（０００）＝１２３２；（Ⅱ）单斜晶系，空间群Ｐ２１／ｎ，ａ＝１０．４０９（１），ｂ＝　１２．５７０（２），ｃ＝２０．６６４（２），β＝８３．５１（１）°，Ｚ＝４，Ｄｃ＝１．２８１ｇ／ｃｍ３，Ｖ＝２６８６．４Ａ３，μ＝９．７６１ｃｍ－１，Ｍｒ＝５３９．２８，Ｆ（０００）＝１１２０．最后的偏离因子，化合物（Ⅰ）Ｒ＝０．０４６，Ｒω＝０．０４６；化合物（Ⅱ）Ｒ＝０．０４９，Ｒω＝０．０４７。晶体结构解析表明，化合物（Ⅰ）和（Ⅱ）中的锡均被配体的３个碳和２个氧原子配位，配位原子呈畸变三角双锥构型；化合物中的环己基均为椅式构象；化合物（Ⅱ）中，配位水分子和另一分子的羰基氧与芳环上的甲基氧?     

Synthesis and Structure of (Oxydiacetato)-nickel(II) Complex with Diaminobithiazole

1 INTRODUCTION The transition metal complexes with 2,2-diamino-4,4-bi-1,3-thiazole (DABT) and their derivatives are excellent soft mag- netic materials[1]. Structural investigation of these complexes is helpful to under- standing the relationship betwee…     

Synthesis, Structure and Spectral Characterization of a Discrete Binuclear Copper (II) Complex

1　ＩＮＴＲＯＤＵＣＴＩＯＮＲｅｃｅｎｔｌｙ,ｂｒｉｄｇｅｄｂｉｎｕｃｌｅａｒｃｏｍｐｌｅｘｅｓｏｆｆｉｒｓｔｒｏｗｔｒａｎｓｉｔｉｏｎｍｅｔａｌｓｈａｖｅｒｅｃｅｉｖｅｄｍｕｃｈａｔｔｅｎｔｉｏｎｏｎａｃｃｏｕｎｔｏｆｔｈｅｉｒｂｉｏｌｏｇｉｃａｌｒｅｌｅｖａｎｃｅａｎｄｃｏｎｄｅｎｓｅｄｐｈａｓｅｍａｇｎｅｔｉｃｐｒｏｐｅｒｔｉｅｓ[1,2].Ｉｎｔｈｅｓｅｒｅｓｅａｒｃｈｅｓ,ｍａｎｙｂｒｉｄｇｅｄｌｉｇａｎｄｓｗｈｉｃｈｐｌａｙｉｍｐｏｒｔａｎｔｒｏｌｅｓｈａｖｅｂｅｅｎｕｓｅｄａｓｕｓｅｆｕｌ…     

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…