Synthesis,Characterization, Oxygen Respiratory,Antibacterial Activity,and Photoluminescent Property Studies of One Novel Complex with Schiff-base Ligand

We have synthesized one novel Schiff-base ligand by modifying the aromatic aldehyde: H_2L~1(H_2L~1 = N,N?-bis(2-oxy-acetate-3-methoxyl)benzylpropylene-ethanediamine). [Co(Ⅱ)L~1]_2·2 EtOH(1) was prepared by the reaction between H_2L~1 and CoCl_2·6H_2O in the solvent of C_2H_5OH. The title compound was structurally characterized by elemental analysis, IR, H NMR and single-crystal X-ray diffraction. Complex 1 crystallizes in monoclinic, space group C2/c with a = 29.472(3), b = 13.4842(13), c = 15.1848(15) ?, β = 115.626(1)°, V = 5441.0(9) ?~3, C_(28)H_(22)CoN_2O_(8.50), Mr = 581.41, D_c = 1.420 g/cm~3, μ(Mo Kα) = 0.685 mm~(-1), F(000) = 2392, Z = 8, the final R = 0.0541 and wR = 0.1565(I 2s(I)). The Co(Ⅱ) atom is hexa-coordinated, furnishing a triangular prism geometry. It is interesting that the H-bond intersections formed a one-dimensional chain structure. In this paper, we research the synthesis, characterization, oxygen respiratory, antibacterial activity, and photoluminescent property of complex 1.     

4-((4-Chlorophenylsulfonamido)methyl)cyclohexanecarboxylic Acid: Synthesis,Crystal Structure and Biological Activities

In this study, a novel 4-((4-chlorophenylsulfonamido)methyl)cyclohexanecarboxylic acid(C_(14)H_(18)ClNO_4S) was synthesized by the reaction of tranexamic acid and 4-chlororbenzene sulfonyl chloride in basic medium at room temperature. The molecular structure was determined by FT-IR, NMR, elemental analysis and single-crystal X-ray analysis. The compound crystallizes in the monoclinic system, space group P21/c with a = 12.3120(11), b = 16.5987(19), c = 7.6873(7) ?, β = 90.495(6)o, Z = 4 and V = 1570.9(3) ?~3, crystal size(mm) = 0.38 × 0.16 × 0.14 and Rint = 0.045. In this compound, the carboxylic acid A(O(1)/C(1)/C(2)) and the sulfonyl B(O(3)/S(1)/O(4)) moieties are of course planar. The molecules are dimerized due to the O–H···O type of H-bonding with the R_2~2(8) ring motifs. The dimmers are interlinked through C–H···O and N–H···O types of H-bonding. The synthesized compound was screened against four bacterial and two fungal strains and inactive against all strains. Antioxidant activity was checked against DPPH. Enzyme inhibition activity was carried out using three different enzymes and the title compound was more potent α-chymotrypsin inhibitor.     

THE STUDY OF SPECTRA AND X-RAY CRYSTAL STRUCTURE OF A NOVEL BIONICS INSECTICIDE——(CH_3)_2NHCH(CH_2S_2O_3)_2Na·H_2O

IR and NMR spectra of novel bionics insecticide—C_5NS_4O_6H_(12)Na·H_2O have been studied. The molecular and crystal structures of the compound also have been determined. The compound crystallizes in the monoclinic space group C_(2h)~5, - P2_1/n with α= 8.0972. (9) , b =16.262(4), c = 10.370(3), β= 94.26(2)° and z = 4.The result shows that N atom in this compound captures a proton to form HN~ group, Na~ is in statistical disorder. Therefore, the structural formula of tho compound is (CH_3)_2HN~ —CH(CH_2S_2O_3~-)_2·1/2 (Na~ )_2·H_2O.     

Mixed-solvothermal Synthesis,Crystal Structure and Luminescence of a New Dinuclear Yttrium(Ⅲ) Coordination Polymer with 1-D Wave-like Infinite Chains

A new dinuclear Y~(3+) coordination polymer{[Y_2(H_2O)_2(C_(14)H_8O_4)_3(C_(12)H_8N_2)_2]·3 H_2O}_n (1, C_(14)H_8 O_4 = 2,2?-biphenyldicarboxylate, phen = 1,10-phenanthroline), has been obtained by means of a mixed-solvothermal method using ethylene glycol and water as solvent. The compound was characterized by elemental analysis, energy-dispersive X-ray spectroscopy(EDS), IR spectrum and single-crystal X-ray diffraction. The results reveal that 1 belongs to monoclinic system, space group C2/c with a = 24.249(3), b = 12.069(48), c = 22.7304(08) ?, β = 113.480(7)°, Z = 4, V = 6102(2) ?~3, Dc = 1.462 g·cm~(-3), F(000) = 2728, μ = 1.968 mm~(-1), the final R = 0.0673, w R = 0.1508 and S = 1.085. Its structure can be regarded as a 1-D coordination polymer constructed by Y~(3+) cations, 2,2?-biphenyldicarboxylate, 1,10-phenanthroline and water molecules. The compound not only contains two kinds of organic ligands, but also exhibits interesting wave-like infinite chains and 18-MR windows with the diameter of 4.070(7)? × 5.326(9)?. The structure is further stabilized by means of O–H···O hydrogen bonds and π-π stacking interactions. Furthermore, the luminescent properties(including emission spectrum, CIE chromaticity coordinate and decay curve) of 1 were also investigated in the solid-state at room temperature.     

苯四甲酸桥连的镍配合物[Ni(btec)(H2O)4][Ni(imi)2(H2O)4]·2H2O的合成及结构

At room temperature, a coordination polymer [Ni(btec)(H2O)4][Ni(imi)2(H2O)4]·2H2O was synthesized by reaction of NiCl2·6H2O, 1,2,4,5-benzenetetracarboxylic dianhydridc and imidazole in a water/THF solution. The structure was determined by X-ray diffraction crystal structure analysis. It crystallizes in triclinic P1 space group with the crystal cell parameters of a=0.67542 (2) nm, b=1.000 14 (1) nm, c=1.09088 (3) nm, α=74.140(2)°, β= 74.388(1)°, y=73.239(2)°, and V=0.664 09(3) nm3, Z=1. The crystal structure shows that Ni1 atom is coordinated by four water and two imidazole molecules, while Ni2 is coordinated by four water molecules and two carboxyl oxygen atoms. The 1,2,4,5-benzenetetracarboxylate ions bridge Ni2 coordination centers to form one-dimensional chain structure. Moreover, the chains are further linked together by hydrogen bonds to form a two-dimensional network. CCDC: 295873.     

A 3D Nickel(Ⅱ) Complex Constructed by Bis(2-dimethylaminoethyl) Ether: Solvothermal Synthesis,Crystal Structure and Catalytic Properties

Treatment of bis(2-dimethylaminoethyl) ether(BDMAE) with nickel acetate afforded a novel 3D nickel(Ⅱ) complex [Ni(BDMAE)(H_2O)_3·(CH_3COO)_2·(H_2O)_2] under solvothermal conditions. Its crystal structure was characterized by elemental analysis, IR spectrum, PXRD and single-crystal X-ray diffraction analysis. The complex belongs to the orthorhombic system, space group C2221 with a=8.823(2), b=13.932(3), c=17.563(4) ?, V=2158.9(8) ?~3, Z=4, C_(12)H_(36)N_2NiO_(10), Mr=427.14, Dc=1.314 g/cm~3, F(000)=920 and μ=0.944 mm~(-1). Single-crystal X-ray diffraction reveals that the mononuclear nickel(Ⅱ) ion is six-coordinated to one oxygen, two nitrogen atoms of the BDMAE ligand and three oxygen atoms of coordinated water molecules. The complex exhibits a 3D supramolecular structure through a variety of intermolecular and intramolecular hydrogen bonding interactions. In addition, the complex has been investigated for catalytic properties towards the Henry reaction of nitromethane with p-nitrobenzaldehyde, and the results indicated that the 1-p-nitrophenyl-2-nitroethanol product was obtained in excellent yield under optimum conditions with the complex as the catalyst.     

Synthesis,Crystal Structure and Antitumor Activity of a Novel Zn(Ⅱ) Complex with 2-(Nicotinoyloxy)acetic Acid Ligand

A novel Zn(Ⅱ) complex, [ZnL_2(H_2O)_4]·H_2O(1, HL = 2-(nicotinoyloxy)acetic acid), was synthesized using Zn(OAc)_2·2H_2O and 2-(nicotinoyloxy)acetic acid as raw materials. Its structure has been elucidated by elemental analysis, IR and single-crystal X-ray diffraction. The structural analysis revealed that complex 1 crystallizes in triclinic, space group P1 and the Zn(Ⅱ) atom is six-coordinated with two N atoms from two different 2-(nicotinoyloxy)acetate anion ligands and four O atoms from coordinated water molecules. Complex 1 forms a 3D network structure by O–H···O hydrogen bonds. The antitumor activities of 2-(nicotinoyloxy)acetic acid ligand and its Zn(Ⅱ) complex were evaluated against human lung adenocarcinoma A549 cells, human hepatoma SMMC-7721 cells and human colon carcinoma Wi Dr cells.     

A Novel Hydrogen-bonded Three-dimensional Network Complex Containing Nickel

A novel complex, (H3O)2[Ni(2,6-pydc)2] · 2H2O was synthesized in an aqueous solution and characterized by means of single-crystal X-ray diffraction, elemental analyses and IR spectra. The X-ray structural analysis revealed that the novel compound forms three-dimensional(3D) networks by both π-π stacking and hydrogen-bonding interactions. The crystal data for the complex are a = 13. 853 (3) nm, b= 9. 6892 (19) nm,c=13.732(3) nm, α=90. 00°, β=115.52(3)°, γ=90.00°, Z=3, R1=0. 0786, wR2=0.1522.     

Synthesis, Crystal Structure and Pyrolysis of a Heterobimetallic Peroxo-titanium（IV） Nitrilotriacetate Complex

A new heterobimetallic nitrilotriacetatoperoxotitanate complex with the formula of [Mn(H2O)5]2[Ti(O2)2O(nta)2]·7H2O (1, C6H6O6N = H3nta) has been isolated in pure crystals. It was characterized by elemental analyses, IR, thermal analysis (TGA) and single-crystal X-ray diffraction. Complex 1 crystallizes in monoclinic, space group C2/c with a = 15.088(3), b = 13.311(3), c = 17.741(4) , β = 100.92(3)°, Z = 4, V = 3498.6(12) 3, Mr = 968.19, Dc = 1.838 g/cm3, μ = 1.266 mm-1, F(000) = 1992, R = 0.0337 and wR = 0.0819. Single-crystal X-ray analysis reveals that the titanium atom is N,O,O',O'-chelated by the nitrilotriacetate and O,O'-chelated by the peroxo group, and is coordinated to the bridging O atom in an overall pentagonal-bipyramidal geometry. The manganese ions in the compound are both 6-coordinated by five water molecules and one bridged carboxylato oxygen atom. A decameric water cluster consisting of a cyclic water hexamer in a boat fashion is also found in complex 1. The TGA and XRD results prove that 1 undergoes facile thermal decomposition to form the mixture of Mn2O3 and TiO2 at 600～800 ℃, and pure MnTiO3 at 900 ℃.     

Synthesis, Crystal Structure and Thermal Stability of Homopolytungstate Supporting Nickel(Ⅱ) Coordination Fragments

The organo-inorganic hybrid compound [ Ni(phen)3 ] [ ( H2W12O40 ) { Ni(phen)2H2O } { Ni(trien) } ]·2H2O was synthesized from Na2WO4·2H2O, NiSO4·6H2O, CH3COOK,triethylenetetramine and 1,10-phenanthroline in water by the hydrothernal reaction, and characterized by IR, X-ray single crystal diffraction, and TG-DTA analysis.This compound crystallized in the monoclinic system, space group P2 ( 1 )/n, with lattice constants: a = 1. 80998 (6) nm, b =2.36504(8) nm, c=2.29199(7) nm, β=110.2220(10)°, V=9.2065(5) nm, Z=4. Final R indices R1 =0.0532, wR2 =0.1295. The compound is decomposed at 593 ℃.     

Synthesis, Crystal Structure and Thermal Stability of Homopolytungstate Supporting Nickel（Ⅱ） Coordination Fragments

The organo-inorganic hybrid compound [Ni(phen)3] [(H2W12O40){Ni(phen)2H2O} {Ni(trien)}]·2H2O was synthesized from Na2WO4·2H2O,NiSO4·6H2O,CH3COOK,triethylenetetramine and 1,10-phenanthroline in water by the hydrothermal reaction,and characterized by IR,X-ray single crystal diffraction,and TG-DTA analysis.This compound crystallized in the monoclinic system,space group P2(1)/n,with lattice constants:a=1.80998(6)nm,b=2.36504(8)nm,c=2.29199(7)nm,β=110.2220(10)°,V=9.2065(5)nm,Z=4.Final R indices R1=0.0532,wR2=0.1295.The compound is decomposed at 593 ℃.     

一种新型含三苯胺的喹啉衍生物及其金属配合物的合成与表征

A new 8-hydroxyquinoline derivative(5)was synthesized and characterized by ESI-MS,~1H NMR spectroscopy,elemental analysis and IR spectroscopy.The photophysical properties of compounds 5,6 and 7 were also deteminedby UV-vis and FL spectroscopy.The vibrational frequency of ligand 5 predicted by using B3LYP method is in goodagreement with experimentally determined values.The compositions of the corresponding copper(Ⅱ)and zinc(Ⅱ)complexes were confirmed to be Cu(C_(29)H_(21)N_2O)_2·H_2O(6)and Zn(C_(29)H_(21)N_2O)_2·H_2O(7)by elementary analysis,thermogravimetry analysis and IR spectroscopy.     

Crystal Structure and Theoretical Studies of Tetrahytrate(1-H-1,2,4-triazole-3,5-dicarboxylicacid)nickel

A new compound, [Ni(Hdctrz)(H_2O)_4](1, H_3dctrz = 1-H-1,2,4-triazole-3,5-dicarboxylic acid), has been successfully synthesized via slow evaporation. The structure of 1 was characterized by FT-IR, elemental analysis and single-crystal X-ray diffraction. Compound 1 crystallizes in monoclinic, space group P21/c with a = 6.871(1), b = 11.468(1), c = 12.178(1) ?, b = 101.291(1)o, V = 941.01(16) ?~3, Z = 4, C_4H_9N_3O_8Ni, M_r = 285.85, D_c = 2.018 g·cm~(–3), m = 2.10 mm~(–1), F(000) = 584, GOOF = 1.025, the final R = 0.0515 and wR = 0.2125 for 1404 observed reflections(I 2s(I)). The crystal structure is assembled by a slightly distorted {NiNO_5} octahedral geometry and hydrogen bonds viz. N–H···O, O–H···O, C–O···π and π···π weak interactions. A rare π···π interaction from triazolate and carboxylate is affirmed through the molecular orbitals(MO) of three adjacent Ni CN molecules. The 3D Hirshfeld surface analysis was employed to gain additional insight into the interactions responsible for the packing of compound 1. Quantitative examination of 2D fingerprint plots revealed, amongst others, the dominating participation of O···H, N···H and π···π interactions in the molecular packing.     

Synthesis,Crystal Structure and Flame Retardance of 2-(3-Silatranylpropylamino)-4-phenyl-5,5-dimethyl-1,3,2-dioxaphosphorinane-2-oxide

The title compound, 2-(3-silatranylpropylamino)-4-dichlorophenyl-5,5-dimethyl-1,3,2-dioxaphosphorinane-2-oxide(2(C_(20)H_(33)N_2O_6Psi)·C_2H_6O·CH_4O, Mr = 991.20), has been synthesized by the nucleophilic substitution reaction of 2-chloro-4-phenyl-5,5-dimethyl-1,3,2-dioxaphosphorinane-2-oxide with γ-aminopropylsilatrane, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1 with a = 10.3783(15), b = 11.2402(17), c = 12.1675(18) ?, a = 70.653(4), b = 82.908(4), g = 85.690(4)°, V = 1328.1(3) ?3, Z = 1, Dc = 1.239 g/cm~3, μ = 0.19 mm~(-1), F(000) = 532, the final R = 0.0640 and wR = 0.2090 for 3615 observed reflections with I 2s(I). The cyclic dioxaphosphorinane ring in the molecule adopts a thermodynamically stable cis conformation, while the silatrane fragment forms a cage-like structure in which there exists an intramolecular Si?N donor-acceptor bond. In the crystal structure, centrosymmetrically related molecules are linked by pairs of N–H···O hydrogen bonds into dimers, generating rings with graph-set motif R22(8). Furthermore, a couple of O(7)–H(10)···O(3) hydrogen bonds were formed by O atom of P=O and H atom from hydroxyl in the solvent ethanol. Thermal property of the compound was also studied by means of thermogravimetry(TGA). The thermal analysis and preliminary fireproofing test show that the title compound has good flame retardance.     

Structure of Palladium( Ⅱ ) Complex with 2-Hydroxy-propane 1, 3-diamine-N,N,N'''' N'''',-tetraacetic Acid

The reaction of PdCl2 in water with 2-hydroxypropane-1, 3-diaminetetraacetic acid (HPDTA) gave the complex Pd (C11H16N2O9)·1. 5H2O, which was characterized by elemental analysis, IR, NMR and single-crystal X-ray diffraction. The spectroscopic and X-ray diffraction data show that Pd ( Ⅱ ) is coordinated by two nitrogen atoms and two car-boxylic oxygen atoms. The complex crystallizes in monoclinic space group Pc with a = 1. 1240(2), b=1. 1183(2), c=1. 2597(3) nm, β=96. 33(2)°V=1. 5737(6) nm3, Z = 4, R= 0.038. The structure contains two crystallographically independent molecules which have slightly different orientations and are connected by hydrogen bonds.     

Synthesis,Crystal Structure and Antimicrobial Activity of Ethyl 2-（1-cyclohexyl-4-phenyl-1H-1,2,3-triazol-5-yl）-2-oxoacetate

A novel 1,4,5-trisubstituted 1,2,3-triazole(C18H21N3O3) was synthesized by a one-pot three component reaction of 1-azidocyclohexane, 1-copper(I) phenylethyne and ethoxalyl chloride at room temperature. The molecular structure was determined by single-crystal X-ray analysis. The compound crystallizes in the monoclinic system, space group P21/n with a = 12.8167(9), b = 8.0966(6), c = 16.7079(9) , β = 98.716(2)o, Z = 4 and V = 1713.8(2). In the crystal, the molecules are related by inversion and paired into dimers via C–H···O and C–O···C interactions involving(oxo) acetate groups. Furthermore, X-ray analysis results are compared with the optimized structure computed by using B3 LYP method with 6-311 G basis set. The calculated results showed that optimized geometry can well reproduce the crystal structure parameters. The bioassay results indicate that the compound has good antibacterial and antifungal activities.     

Hydrothermal Synthesis,Crystal Structure and Thermal Stability of a Novel Water Cluster [Mn(phen)_2·H_2O·Cl]·p-FBA·3H_2O

A novel water cluster [Mn(phen)2·H2O·Cl]·p-FBA·3H2O (p-FBA = p-fluorobenzoic acid and phen = 1,10-phenanthroline) was synthesized by the hydrothermal reaction of MnCl2 with p-FBA and phen at 150 ℃ and characterized by elemental analysis,IR spectra and TG. Its crystal structure was determined by X-ray single-crystal diffraction study. The crystal belongs to the triclinic system,space group P1,with a = 10.5768(1),b = 11.5960(1),c = 12.9916(2) ,α = 101.816(2),β = 95.397(2),γ = 103.052(2)o,V = 1502.8(3) 3,Z = 2,Dc = 1.463 g/cm3,R = 0.0399 and wR = 0.0997. The crystal structure shows that the manganese(Ⅱ ) ion is six-coordinated by four nitrogen atoms,one chloride ion and one oxygen atom forming a distorted octahedral coordination geometry. The structure includes three acyclically connected water molecules and one coordinated water molecule thus forming a (H2O)4 water cluster. This water pattern forms a cross-linked discrete ring. The steady (H2O)4 is further extended into a cage-like structure by the hydrogen-bonding interaction formed by dissociative aqua molecule and Cl-ligand. The dimer structure is further extended into a one-dimensional (1D) structure through C-H···O interaction. π···π Stacking interaction among adjacent phen aromatic rings further stabilizes the crystal structure.     

A Unique Heteronuclear Metal Organic Framework Based on Amino-acid and N-donor Ancillary Ligand: Synthesis,Structure and Characterization

A novel heteronuclear metal organic framework(MOF) incorporating both transition and alkali metal ions, namely, {(Ni_2K_2L_2·bipy]×6 H_2O]×2 H_2O}n(1, L = N-phosphonomethyl amino diacetic acid, bipy = 4,4?-dipyridine) has been obtained. Its structure was established by single-crystal X-ray diffraction analysis and further characterized by elemental analysis and IR spectroscopy. The complex crystallizes in orthorhombic system, space group Pccn with a = 14.650(11), b = 36.56(3), c = 7.112(5) ? and V = 3809.3(8) ?~3. In this framework, bipy connects adjacent Ni–K heteronuclear coordination units into 1 D railway type chains, which are further propagated into 2 D deck-like array bearing large tunnels through the carboxylic oxygen from N-phosphonomethyl amino diacetic acid. The molar electrical conductivity of heteronuclear complex increases gradually with increasing the temperature. Complex 1 also exhibits strong photoluminescent emission in the visible region.     

Synthesis, Crystal Structure and Electrochemistry Properties of a (N,N'-Ethylene-bis(salicylaldiminato)) Nickel(Ⅱ) Complex, [Ni2(salen)2]·NCS-NH4

A new Ni(Ⅱ) complex [Ni2(salen)2]·(NCS)·NH4 (salen = N,N'-bis(salicylidenea-mino)ethanato) has been prepared and structurally characterized by elemental analysis, IR spectra and single crystal X-ray diffraction. It crystallizes in the orthorhombic system, space group Pbca with a = 16.8725(13), b = 19.0046(15), c = 20.0583(16) (A), Z = 8, V = 6431.8(9) (A)3, C33H32N6Ni2O4S1, Mr= 726.13, Dc = 1.500 g/cm3, F(000) = 3008, μ = 1.284 mm-1, the final R = 0.0394 and wR = 0.0767 for 4449 observed reflections with Ⅰ＞2σ(Ⅰ). The complex involves a N,N'-ethylene-bis(salicylaldiminato) Schiff base, an isothiocyanato anion and an ammonium cation. The nickle(Ⅱ) ion adopts a distorted square coordination geometry with N2O2 set of Schiff base ligand. The complexes are linked into a dimmer via intermolecular hydrogen bonds and the [Ni(salen)] moieties are connected together to form a 2-D layer structure by intermolecular N-H…O hydrogen bonds and π-π stacking. Cyclic-voltammetry method was used to characterize electrochemically the complex.     

Mn(Ⅱ) Based Coordination Polymer Involving 1,2,4,5-Benzenetetraboxylic Acid and 4,4-Bis(imidazol-1-ylmethyl)biphenyl: Synthetic,Structure and Magnetic Property

A novel Mn(Ⅱ)coordination polymer(CP),[Mn(BBA)_(0.5)(BIYB)]_n(1),was gained by the 1,2,4,5-benzenetetracarboxylic acid(H_4BBA),4,4-bis(imidazol-1-ylmethyl)biphenyl(BIYB),and Mn(CH_3COO)_2·4H_2O under hydrothermal reaction.CP 1 was characterized and structurally determined by elemental analyses,PXRD,IR spectra,thermal behaviors,and X-ray single-crystal diffraction.The framework structure of 1 shows a novel(2,5,6)-connected 3Dnetwork with a Schlafli symbol of(4~3.6~6.8)~2(4~6.6~9)(6)~2.It crystallizes in triclinic system,space group ■,with a=7.5898(5),b=9.8201(6),c=14.1307(9)?,α=97.5850(10),β=99.6810(10),γ=111.6580(10)o,V=943.01(10)?~3,Z=2,C_(23)H_(15)MnN _4O_4,M_r=466.33,D_c=1.462 g/cm~3,F(000)=476,S=1.082,R=0.0361 and wR=0.1008.The magnetic property of CP 1 was investigated.The weak antiferromagnetic interactions are observed between the Mn(Ⅱ)ions.