Synthesis and Crystal Structure of a Mn(II) Complex with Thiosemicarbazone Derivative of Pyridine-3-carbaldehyde Showing Unusual Coordination Mode of Tridentate Thiosemicarbazone

1 INTRODUCTION Heterocyclic thiosemicarbazones as well as their metal complexes have been attracting considerable interest due to their biological activities, such as antiviral, antibacterial, antimalarial, antifungal, and antitumoral activities[1～5]. This prompted us to carry out structural studies of these complexes to provide a basis for understanding their behaviors in living systems. Although quite a number of investigations on the 2-heterocyclic thiosemicarbazones have ap- peared[6…     

Synthesis and Crystal Structure of Copper(Ⅱ)Complex with N-Acetoxyl-picolinamide

Using Cu(Ⅱ) as the template, a complex {[Cu2L2(H2O)2] 4H2O}n (L = N-acetoxyl- picolinamide) has been successfully synthesized and characterized by single-crystal X-ray diffrac tion. The crystal is of monoclinic, space group C2/c, with a = 24.144(5), b = 7.1622(14), c = 17.283(4) (A), C16H24Cu2N4O12, Mr = 591.47, β = 131.73(3)°, V = 2230.3(8) (A)3, Z = 4, Dc= 1.761 g/cm3, F(000) = 1208,μ = 1.978 mm-1, R = 0.0400 and wR = 0.1099. The copper (Ⅱ) ion is five coordinated with a distorted square pyramidal geometry. The complex can be viewed as a one dimensional chain structure by carboxylic bridges among copper atoms. In the complex there exist hydrogen bonding interactions to stabilize the structure.     

Synthesis and Crystal Structure of a Dinuclear Cu(II) Complex with Tridentate Schiff Base and Azido Bridge

1 INTRODUCTION The azido ligand is an efficient superexchange path-way for propagating magnetic interaction between theparamagnetic centers, such as copper(II), giving di-nuclear, tetranuclear, 1D, 2D and 3D complexes[1～4].The versatility of this ligand due to its diverse bin-ding modes leads to the variation in magnetic pro-perties that depend on its orientation with respect tothe magnetic centers. In general, the bridging modesobserved for the azido group are endtoend and en-don. In…     

Synthesis and Crystal Structure of Ni(Ⅱ) Complex with N-Salicylaldehyde-N''''-phenoxyacetylhydrazine Ligand

1INTRODUCTIONHydrazoneshavebeenattractingmuchatten-tionfromchemistsinrecentyearsbecauseoftheirbiologicalactivities,chemicalandindustrialversa-tility,andstrongtendencytochelatetotransitionmetals[1,2],lanthanidemetals[3]andmaingroupmetals[4,5].Inthehydrazonecomplexes,thehydra-zoneligandcanactasaneutralormononegativebidentateligand,orevenasadianionictridentateliganddependingonthedonoratomsoftheligandsandthereactionconditions.Ontheotherhand,variouscompoundsderivedfromphenoxyaceticacidareveryus…     

Synthesis and Crystal Structure of a Novel Terpyridine-based Cd(Ⅱ) Complex

A novel terpyridine-based complex CdL'S2 (L'= oxide of L; L = 10-hexyl-3-(2,6-di(pyridine-2-yl)pyridine-4-yl)-10H-phenothiazine) has been solvothermally synthesized and characterized by FT-IR spectroscopy, elemental analysis, 1 H NMR and X-ray crystallography. The sulfur of phenothiazine moiety was oxidized when the crystal is formed. The complex C36H37CdN5O2S3 crystallizes in triclinic, space group P1 with a = 9.4452(9), b = 13.0181(14), c = 14.6721(18), α = 73.872(1), β = 81.531(1), γ = 87.547(2)°, V = 1714.2(3)3 , Mr = 780.29, Dc = 1.512 g·cm-3 , μ = 0.861 mm-1 , F(000) = 800, Z = 2, the final R = 0.0456 and wR = 0.1059 for Ⅰ > 2σ(Ⅰ). The Cd(Ⅱ) is coordinated by two terminal sulfur ions and three pyridyl nitrogen atoms in a distorted trigonal bipyramidal geometry. Universal hydrogen bonds between the neighboring molecules have generated a supramolecular arrangement which contributes to the stability of the title complex. Fluorescence property and thermogravimetry of the complex have also been investigated and discussed.     

Synthesis and Crystal Structure of a Novd Nickel (Ⅱ) Coordination Polymer with Chiral Schiff-base

以手性对称的Shiff碱为配体,合成了手性镍配合物[Ni2(salen)2(1)],其结构经X-单晶射线衍射和元素分析表征.1属单斜晶系,C2空间群,晶胞参数a ＝25.060(5)(A),b=13.508(3)(A),c＝ 11.938(2)(A),α=90(3)°,β=104.82(3)°,γ=90(3)°,V=3906.7(14)(A)3,Z=4,Mr=828.24,Dc=1.429 g·cm-3,F(000)=1808,μ=1.027mm-1,GOF=1.068,R1=0.051 0,wR2=0.1289.在1的分子结构中,环己胺和苯环之间通过分子间CH…π作用形成二维结构.     

Synthesis,Crystal Structure and Luminescence Study of a New Two-dimensional Mn(Ⅱ) Coordination Polymer

The coordination polymer [Mn_2(cipt)_2(aic)_2]_n(cipt = 2-(3-chlorophenyl)-1Himidazo[4,5-f][1,10]phenanthroline, aic = 5-amino-isophthalic acid) has been obtained from hydrothermal reaction and characterized by elemental analysis, IR, TG and single-crystal X-ray diffraction. The title compound crystallizes in the triclinic system, space group P1, with a = 11.523(3), b = 12.162(3), c = 18.706(5) ?, β = 81.789(5)o, V = 2455.2(1) ?3, C_(54)H_(32)Cl_2Mn_2N_(10)O_8, Mr = 1129.68, Z = 2, Dc = 1.528 g/cm3, μ = 0.692 mm-1, F(000) = 1148, R = 0.064 and wR = 0.145 for 9571 observed reflections(I 2σ(I)). In this polymer, the Mn(Ⅱ) atoms adopt different coordination modes. The Mn(1) atom is five-coordinated, forming a distorted tetragonal pyramidal geometry. Mn(2) atom is six-coordinated to get a distorted octahedral geometry, which is different from the Mn(1) atom. Each Mn(Ⅱ) atom is linked by aic ligands with neighboring Mn(Ⅱ) atoms, forming an infinite one-dimensional(1D) double-chain structure. The existence of N–H···O hydrogen bonding interactions leads the 1D chains to generate a 2D structure. Luminescent properties for the ligand cipt and compound 1 have also been discussed in detail.     

Synthesis and Crystal Structure of Zn(Ⅱ) Complex with Tridentate Ligand N-(2-Hydroxy-1-naphthylidene)-L-serine

A new Zn(Ⅱ) complex, [Zn(L)2(H2O)2], where H2L = N-(2-hydroxy-l-naphthylidene)-L-serine, has been synthesized and characterized by single-crystal X-ray diffraction. The crystal belongs to monoclinic system, space group C2/c with a = 13.669(2), b = 6.4657(9), c =31.463(5) (A), β = 98.010(2)°, V = 2753.6(7) (A)3, Z = 8, Mr = 358.64, Dc = 1.730 g/cm3, F(000) =1472,μ(MoKa) = 1.814 mm-1, the final R = 0.0355 and wR = 0.0706. The Zn(Ⅱ) atom adopts a square-pyramidal geometry coordinated by the tridentate ligand and two water molecules.Intermolecular hydrogen bonds link the complex molecules into a two-dimensional layer.     

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

A new Cu(Ⅱ) complex [Cu(4-cba)(l,10-phen)(H2O)2](NO3) (4-Hcba = 4-cyanobenzoic acid) has been synthesized by solvothermal reaction in an ethanol/water mixed solution at 100℃ and structurally characterized by single-crystal X-ray diffraction. Crystallographic data: C20H16CuN4O7, Mr= 487.91, triclinic, space group P1, a = 7.8420(2), b = 9.1070(2), c = 15.1140(6) A,α=76.889(9), β = 81.332( 11 ), γ = 74.844(11 )°, V = 1009.89(5) A3, Z = 2, Dc = 1.605 g/cm3, F(000)=498,μ=1.134 mm-1,the final R = 0.0379 and wR = 0.0865 for 2977 observed reflections with I ＞ 2σ(Ⅰ).The Cu(Ⅱ) atom is coordinated by two terminal water molecules, one chelating 1,10-phen molecule and one monodentate 4-cba ligand to form a slightly distorted square pyramid. The title complex molecules are connected through hydrogen bonds and π-π stacking interactions to generate a 2D layered network. The thermogravimetric analysis of the title complex has also been discussed.     

Synthesis, Crystal Structure, and Spectral Properties of a Novel Co(Ⅱ) Complex Containing Imidazole Derivative

A novel imidazole derivative with functional group and π-conjugated system, 1- [trans-4-(4-diethylaminostyryl)phenyl]imidazole (abbreviated as L), and its CoII complex (CoCl2L4)2 (Co2C168H184N24Cl4, Mr = 2799.05 ) have been synthesized and the crystal structure of the latter was determined by X-ray diffraction. The crystal is of triclinic, space group P with a = 8.823(3), b = 18.799(7), c = 23.065(9) (A), α = 77.349(6), β = 83.128(7), γ = 80.942(3)°,V = 3671.5(12)(A)3, Z = 1, Dc = 1.266 g/cm3, μ = 0.361 mm-1, F(000) = 1482, the final R = 0.0587 and Wr = 0.1284 for 6562 observed reflections with Ⅰ ＞ 2б(Ⅰ). In the molecular structure of (CoCl2L4)2, there are two crystallographically unique units. The CoII atoms are six-coordinated by four N atoms from four imidazole ligands (L) and two Cl atoms to form a distorted octahedral geometry. The optical properties of complex (CoCl2L4)2 have been experimentally studied.     

Synthesis and Crystal Structure of Zn(Ⅱ) Complex with 2-Aminopyridine and Acetylacetone

A mixed complex [Zn(C5H6N2)(HL)2] (C5H6N2 = 2-aminopyridine, H2L = acetyl- acetone) has been synthesized and characterized by IR, elemental analysis and X-ray single-crystal diffraction analysis. The crystal belongs to monoclinic, space group P21/c with a = 7.4490(15), b = 8.2650(17), c = 27.615(6)(A),β = 101.69(3)°, V = 1664.9(6)(A)3, Z = 4, Mr = 357.70, Dc = 1.427 g/cm3, F(000) = 744, μ = 1.493 mm-1, R = 0.0309 and wR = 0.0771. The Zn(II) is coordinated by one nitrogen atom from 2-aminopyridine and four oxygen atoms from two acetylacetone anions to furnish a distorted square pyramid geometry. The complex forms a three-dimensional network through intermolecular hydrogen bonds.     

Synthesis and Crystal Structure of a 3-Arylamino-3-Deoxy Sugar Derivative

1INTRODUCTION Amino sugars in which a hydroxyl group of a mo-nosaccharide is replaced by an amino group play a wide variety of important biological roles[1]and have broad applications in chemical,biochemical,medi-cinal,and pharmaceutical fields[2,3].Amino sugars are chiral synthon of azasugar and polyose,many of which are found to be potential chemotherapeutic agents for the treatment of diseases,such as diabetes and cancer,inflammation and viral infections,inclu-ding HIV[4].Particularly…     

Synthesis and Crystal Structure of Binuclear Complex of Copper(Ⅱ)Chloroacetate with Acetamine

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Urothermal Synthesis and Crystal Structure of a Zn（Ⅱ） Coordination Polymer with a 3-D Supramolecular Structure

A new metal-organic coordination polymer [Zn(hfipbb)(e-urea)]n(1,H2hfipbb = 4,4'-(hexafluoroisopropylidene)bis(benzoic acid),e-urea = ethylene urea) has been urothermally synthesized and characterized by elemental analysis and single-crystal X-ray diffraction.The title complex crystallizes in monoclinic,space group P21/c with a = 13.302(4),b = 10.981(3),c = 13.804(4) ,β = 93.587(5)°,V = 2012.3(10) 3,C20H14N2O5F6Zn,Mr = 541.72,Z = 4,Dc = 0.447 g/cm3, = 0.328 mm-1,F(000) = 272,R = 0.0340 and wR = 0.1107 for 4528 observed reflections(I >2σ(I)).In the structure of compound 1,two Zn(Ⅱ) ions are bridged by two carboxylate groups from two hfipbb ligands to form a dinuclear unit,and each dinuclear Zn(Ⅱ) unit is linked with its two adjacent dinuclear units through four hfipbb ligands into an infinite one-dimensional double-chain.The interesting structural feature of compound 1 is that the one-D double-chains are self-interconnected into a three-D supramolecular structure through hydrogen bonds between the coordinated e-urea molecules and carboxylate oxygen atoms(N1 and O2,N2 and O4).     

Antitumor Metallothiosemicarbazonate:Synthesis,Crystal Structure,Spectra and Antitumor Studies of Co(Ⅲ) Complex with Thiosemicarbazone Derivative of 2-Benzoylpyridine

The title complex Co(L)2Cl·4H2O I has been achieved via self-assembly by incorporating cobalt into 2-benzoylpyridine thiosemicarbazonate ligand, and characterized by elemental analysis, infrared spectra, mass spectra and single-crystal X-ray diffraction study. The crystal crystallizes in monoclinic, space group P21/n, with a=10.227(3), b=17.363(4), c=17.459(4), β=100.408(4)o, V=3049.2(13)3, Z=4, Mr=677.08, Dc=1.475 g/cm3, μ(MoKα)=0.834 mm-1, F(000)=1400, the final R=0.0747 and wR=0.0896 for 1663 observed reflections with I > 2σ(I). The complex contains one six-coordinated cobalt ion connected by two thiosemicarbazone ligands which act as a tridentate ligand to coordinate with the center metal atoms via two pyridyl nitrogen atoms, two imine nitrogen atoms and two sulfur atoms giving rise to a mononuclear structure. Hydrogen bonds existing in the complex link the different com-ponents to stabilize the crystal structure. The antitumor activity of the title complex was tested against A549 lung cancer cell line. Complex I exhibits antitumor activity.     

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.     

Synthesis and Crystal Structure of Copper(II) Complex with N-Acetoxyl-picolinamide

1 INTRODUCTION The picoloylhydrazide compounds are close to thebiologic environment and can react with microele-ments in organism so as to have antitubercular andantineoplastic activities. However, owing to the exis-tence of amino group, this kind of compounds aretoxic to some extent[1]. In order to decrease theirtoxicity, hydrazone or hydrazide compounds synthe-sized by the condensation reaction of amino and car-bonyl groups have been well studied in recentyears[1～7]. Herein we report t…