Syntheses, Crystal Structures and Magnetic Properties of a New Nitronyl Nitroxide Radical and Its Cu(Ⅱ) Complex

A new compound (NIT-mNO2 = 4,4,5,5-tetramethylimidazoline-2-yl-(2'-chlor-5'- nitrophenyl)-3-oxide-1-oxyl) 1 and its complex (Cu(NIT-mNO2)(hfac)2) 2 have been synthesized and structurally and magnetically characterized. Complex 1 crystallizes in monoclinic, space group P21/n with a = 10.6798(9), b = 11.2705(9), c = 12.9559(10) , β = 107.3770(10)o, V = 1488.3(2) 3, C13H15ClN3O4, Mr = 312.73, Z = 4, Dc = 1.396 g/cm3, μ(MoKa) = 0.276 mm-1, F(000) = 652, the final R = 0.0606 and wR = 0.1773 for 3405 independent reflections with Rint = 0.0203. The nitronyl nitroxide unit (imidazoline ring) is not coplanar with the phenyl ring with the dihedral angle between them of 55.75o. The compound results in a 1-D zig-zag chain structure by intermolecular H-bond interaction. Compound 2 crystallizes in triclinic, space group P1 with a = 10.3699(10), b = 10.6286(11), c = 15.1683(15), α = 77.5330(10), β = 773080(10), γ = 87.3420(10)o, V = 1592.5(3) 3, C23H17ClF12N3O8Cu, Mr = 790.39, Z = 2, Dc = 1.648 g/cm3, μ(MoKa) = 0.888 mm-1, F(000) = 788, the final R = 0.0793 and wR = 0.2153 for 5794 independent reflections with Rint = 0.0196. The Cu(II) ion is located at a center of symmetry, and each Cu(II) is surrounded by six oxygen atoms at the vertices of a distorted tetragonal octahedron. Four of the six oxygen atoms belong to two hfac ligands and occupy the equatorial coordination sites, while the other two of NIT-mNO2 act as μ-1,5 bridge between the Cu(II) ion, thus forming a 1-D chain structure. The magnetic susceptibility data indicate intermolecular antiferromagnetic interactions between compound 1 and intrachain ferromagnetic behaviors.     

Syntheses, Crystal Structures and Magnetic Properties of a New Nitronyl Nitroxide Radical and Its Cu（II） Complex

A new compound （NIT-mNO2 = 4,4,5,5-tetramethylimidazoline-2-yl-（2＇-chlor-5＇- nitrophenyl）-3-oxide-l-oxyl） 1 and its complex （Cu（NIT-mNO2）（hfac）2） 2 have been synthesized and structurally and magnetically characterized. Complex 1 crystallizes in monoclinic, space group P211n with a = 10.6798（9）, b = 11.2705（9）, c = 12.9559（10）A, β = 107.3770（10）°, V = 1488.3（2） A^3, C13H15ClN3O4, Mr = 312.73, Z = 4, Dc = 1.396 g/cm^3, g（MoKa） = 0.276 mm^-1, F（000） = 652, the final R = 0.0606 and wR = 0.1773 for 3405 independent reflections with Rint = 0.0203. The nitronyl nitroxide unit （imidazoline ring） is not coplanar with the phenyl ring with the dihedral angle between them of 55.75°. The compound results in a 1-D zig-zag chain structure by intermolecular H-bond interaction. Compound 2 crystallizes in triclinic, space group Pi with a = 10.3699（10）, b = 10.6286（11）, c = 15.1683（15）A, a = 77.5330（10）, ,β = 773080（10）, y = 87.3420（10）＊, V = 1592.5（3） A^3, C23HITCIFI2N3O8Cu, Mr = 790.39, Z = 2, Dc = 1.648 g/cm^3, μ（MoKa） = 0.888 mm^-1, F（000） = 788, the final R = 0.0793 and wR = 0.2153 for 5794 independent reflections with Rint = 0.0196. The Cu（Ⅱ） ion is located at a center of symmetry, and each Cu（Ⅱ） is surrounded by six oxygen atoms at the vertices of a distorted tetragonal octahedron. Four of the six oxygen atoms belong to two hfac ligands and occupy the equatorial coordination sites, while the other two of NIT-mNO2 act as μ-1,5 bridge between the Cu（Ⅱ） ion, thus forming a 1-D chain structure. The magnetic susceptibility data indicate intermolecular antiferromagnetic interactions between compound 1 and intrachain ferromagnetic behaviors.     

Isolation, Crystal Structure and Inhibitory Activity against Magnaporthe Grisea of （2R,3R）-3,5,7-trihydroxyflavanone 3-Acetate from Myoporum Bontioides A. Gray

The title compound, (2R,3R)-3,5,7-trihydroxyflavanone 3-acetate, is a flavanonol derivative which was first isolated from Myoporum bontioides A. Gray and characterized by MS, NMR and CD spectra. In addition, the structure was determined by X-ray single-crystal diffraction analysis. It crystallizes in the triclinic lattice, space group P21 with a = 10.686(3), b = 6.862(2), c = 11.267(3) , β = 107.46(1), V = 788.3(4) 3, Z = 2, C17H16O7, Mr = 332.30, Dc = 1.400 g/cm3, μ(MoKα) = 0.110 mm-1, F(000) = 348, the final R = 0.0283 and wR = 0.0826 for 3428 independent reflections (Rint = 0.017) and 1500 observed ones (I > 2σ(I)). The structure consists of one flavone and one water molecule. The flavone molecules form a 1D column by the p…π stacking interactions and C–H…O hydrogen bonds. The weak intermolecular/intermolecular O–H…O hydrogen bonds observed in the crystal give further rise to a complicated network structure. Primary bioassay showed that the title compound has high inhibitory activity against Magnaporthe grisea with the EC50 values of 199.41 μg/mL.     

A New Dinuclear Cu(Ⅱ) Complex of a Ligand with Benzimidazole Group─Synthesis and Crystal Structure

A new dinuclear copper complex, [Cu(C9H11N3)Cl2]2 (C18H22Cl4Cu2N6), has been synthe- sized and characterized by X-ray structure determination. It crystallizes in the triclinic P1 space group with a = 7.526(3), b = 9.473(4), c = 9.535(3) , α = 117.214(10), β = 108.251(9), γ = 91.560(6)o, V = 562.3(4) 3, Z = 1, Mr = 591.30, F(000) = 298, Dc = 1.746 g/cm3, μ(MoKα) = 2.385 mm-1, the final R = 0.0577 and wR = 0.1248 for 2188 unique reflections with 1629 observed ones (I > 2σ(I)). In the title complex, each copper(II) atom is located at the center of a distorted trigonal bipyramid of five coordination atoms (two nitrogen and three chlorine atoms). Two copper(II) atoms were bridged by two chlorine anions (Cl(2) and Cl(2a)) to form a Cu(II)-Cu(II) binuclear entity with the distance between two copper(II) atoms of 3.398 .     

Synthesis and Crystal Structure of 2-Hydroxybenzoic Acid [1-（3,5-Dibromo-2-hydroxyphenyl）methylidene]hydrazide Methanol

A new Schiff base compound, 2-hydroxybenzoic acid [1-(3,5-dibromo-2-hydroxy- phenyl) methylidene]hydrazide methanol (C14H10Br2N2O3·CH3OH), has been synthesized by the condensation of equimolar 3,5-dibromosalicylaldehyde and 2-hydroxybenzoic acid hydrazide in a methanol solution. The compound was characterized by elemental analysis, IR spectra, and single- crystal X-ray diffraction. The compound consists of a Schiff base moiety 2-hydroxybenzoic acid [1-(3,5-dibromo-2-hydroxyphenyl)methylidene]hydrazide and a lattice methanol molecule. The crystal belongs to the monoclinic system, space group P21/n with a = 7.183(1), b = 15.673(2), c = 15.001(2) , β = 98.345(2)o, Z = 4, V = 1670.9(4) 3, Dc = 1.773 g/cm3, Mr = 446.10, λ(MoKα) = 0.71073 , μ = 4.872 mm-1, F(000) = 880, R = 0.0458 and wR = 0.0963. A total of 3445 unique reflections were collected, of which 2236 with I > 2σ(I) were observed. As expected, the molecule adopts a trans configuration about the C=N double bond. The two benzene rings are nearly coplanar (mean deviation from the combined plane is 0.061(4) ), with the dihedral angle of 7.9(3)o. The preliminary biological tests show that the compound has moderate antibacterial activities.     

Synthesis and Crystal Structure of a 1-D Chain Zinc（Ⅱ） Coordinated Polymer with N-p-Tolysulfonyl-glutamine

A novel coordination polymer {[Zn(ts-gln)(bipy)]3H2O}n (ts-glnH2=N-p-toly-sulfonyl-glutamine,bipy=2,2-bipyridine) has been prepared and structurally characterized by X-ray diffraction method. It crystallizes in orthorhombic,space group P212121 with a=8.2622(5),b=16.6244(10),c=18.2807(10) ,V=2510.9(3) 3,C22H28N4O8SZn,Mr=573.91,Z=4,Dc= 1.518 g/cm3,μ(MoKa)=1.115 mm-1,F(000)=1192,the final R=0.0262 and wR=0.0662 for 5691 independent reflections with Rint=0.0240. The zinc(Ⅱ) atom is coordinated by N(3) and N(4) atoms of a bipy molecule,two carboxylate O(1) and O(2A) and amino N(1) atoms of ts-gln ligands,resulting in a square-pyramidal geometry. The title complex consists of an infinite zigzag chain of zinc(Ⅱ) ions linked by the carboxylate of N-p-tolysulfonyl-glutamine.     

Synthesis and Crystal Structure of 2,5-Di- （pyridin-3-yl）-1,3,4-oxadiazolendium Nitrate

In order to continue our studies on the synthesis, properties and coordination of s-tetrazine, 3,6-di-(pyridin-3-yl)-s-tetrazine (II, 3-dptz) was synthesized and characterized by 1H- NMR, MS and IR spectra. And the coordination reaction of 3-dptz with nitrate of Cu(II) was studied. 3-dptz reacting with CuII salt [Cu(NO3)2·2H2O] generates a new salt, nitrate of 2,5-di-(pyridin-3- yl)-1,3,4-oxadiazolene (III). III was determined by IR spectra and single-crystal X-ray diffraction to give the following crystal data: space group P21/c, a = 4.9112(1), b = 8.4101(3), c = 29.499(1) , β = 93.266(2)o, V = 1216.44(7) nm3, Mr = 287.24, Z = 4, Dc = 1.568 g/cm3,μ= 0.122 mm-1, F(000) = 592, R = 0.0430 and wR = 0.1240. The results show that III is composed of one cation and one nitrate anion. The cation consists of one H+ and one 2,5-di-(pyridin-3-yl)-1,3,4-oxadiazol molecule, with the former being attached to the latter via electrovalent bond with N3 atom. And the O(42) atom in the nitrate anion is disordered. Intra- and intermolecular H-bonds are observed in the crystal of the title compound. The mechanism of metal-assisted decomposition was also discussed briefly.     

Synthesis and Crystal Structure of a 1-D Chain Zinc(Ⅱ) Coordinated Polymer with N-p-Tolysulfonyl-glutamine

A novel coordination polymer {[Zn(ts-gln)(bipy)]3H2O}n (ts-glnH2=N-p-toly-sulfonyl-glutamine,bipy=2,2-bipyridine) has been prepared and structurally characterized by X-ray diffraction method. It crystallizes in orthorhombic,space group P212121 with a=8.2622(5),b=16.6244(10),c=18.2807(10) ,V=2510.9(3) 3,C22H28N4O8SZn,Mr=573.91,Z=4,Dc= 1.518 g/cm3,μ(MoKa)=1.115 mm-1,F(000)=1192,the final R=0.0262 and wR=0.0662 for 5691 independent reflections with Rint=0.0240. The zinc(Ⅱ) atom is coordinated by N(3) and N(4) atoms of a bipy molecule,two carboxylate O(1) and O(2A) and amino N(1) atoms of ts-gln ligands,resulting in a square-pyramidal geometry. The title complex consists of an infinite zigzag chain of zinc(Ⅱ) ions linked by the carboxylate of N-p-tolysulfonyl-glutamine.     

Co-crystallization of Resorcin[4]arene Tetracarboxylic Acid with Triethylamine: Synthesis and Crystal Structure

Treatment of resorcin[4]arene tetracarboxylic acid 1 with triethylamine in the presence of Co(CH3COO)2·4H2O and 4,4'-bipyridine gave a co-crystallization 14-·4Et3NH+(C32H20O164-·4Et3NH+,Mr=1069.27) from ethanol and water.The compound was structurally determined by single-crystal X-ray diffraction.The crystal belongs to monoclinic,space group P21/n,with a=8.1763(18),b=12.913(3),c=28.724(7) ,β=97.574(4)o,V=3006.3(12) 3,Z=2,Dc=1.181 g/cm3,F(000)=1152,Rint=0.0275,T=293(2) K,μ=0.086 mm-1,the final R=0.0634 and wR=0.1752 for 5082 observed reflections with Ⅰ 2σ(Ⅰ).The co-crystallization is very stable at room temperature.Possibly,a network of N-H···O(=C) plays an important role in the structure.Meanwhile,the compound emits a weak cyan luminescence with peak maximum band at 458 nm.     

Synthesis,Crystal Structure and DNA Binding Studies of α,α'-Bis(3,5-bismethyl-1-pyrozolyl)-carbene-acetyl-isopropenyl Hydrazine

The title compound α,α'-bis(3,5-bismethyl-pyrozole-N-yl)-carbene-acetyl-isopro- penyl hydrazine (C16H22N6O, Mr = 314.40) has been prepared. It was characterized by elemental analysis as well as IR, MS, 1H-NMR and 13C-NMR spectra. Its crystal structure was determined by single-crystal X-ray diffraction, getting the following data: triclinic, space group P1 with a = 6.9734(16), b = 10.773(3), c = 12.001(3) , α = 75.311(4), β = 82.695(4), γ = 77.143(4)o, Z = 2, V = 847.9(3) 3, Dc = 1.231 g/cm3, F(000) = 336 and μ(MoKα) = 0.082 mm-1 (λ = 0.71073 ). The results of crystal structure determination show that there exist intermolecular and intramolecular hydrogen bonds, resulting in a two-dimensional supramolecular framework of the title compound. The binding of the title compound to DNA was investigated by absorption, emission, and viscosity measurements. The title compound shows absorption hyperchromicity accompanied by a blue shift at about 254 nm. The binding constant Kb for the title compound has been determined to be 1.89 × 104 M-1 from absorption measurements. The addition of the title compound to DNA pretreated with EB causes appreciable reduction in the emission intensity, indicating that the DNA-bound EB fluorophore is partially replaced by the title compound. The value of K is 3.093 × 104 M-1. The relative viscosity of DNA decreased with the addition of the title compound. Results suggest that the title compound binds to DNA with a non-classical intercalative or groove interaction mode. The observed efficient nuclease activity of the title compound is interesting and may have further influences on the chemistry of DNA minor groove binders. Keywords: α,α'-bis(3,5-bismethyl-pyrozole-N-yl)-carbene-acetyl-isopropenyl, preparation, crystal structure, DNA binding     

Synthesis and Crystal Structure of 4-Oxo-1,2,4-triazino[4,5-a]benzimidazole

The title compound 4-oxo-1,2,4-triazino[4,5-a]benzimidazole(C9H6N4O,Mr = 186.18) has been synthesized and structurally characterized by IR,NMR and single-crystal X-ray diffraction. The crystal belongs to monoclinic,space group P21/c,with a = 9.1530(18) ,b = 7.2260(14),c = 12.604(3) ,β = 106.92(3) ,V = 797.5(3) 3,Z = 4,Dc = 1.551 g/cm3,λ(MoKa) = 0.71073,F(000) = 384,μ(MoKa) = 0.109 mm-1,the final R = 0.0632 and wR = 0.1095. A total of 1444 unique reflections were collected,of which 767 with I > 2σ(I) were observed. The structure of the title compound is planar. In packing,the molecules are intersected to each other to form chains along three dimensions,together by intermolecular N-H…O and C-H…N hydrogen bonds. The whole structure is further stabilized by π…π interaction between two adjacent tricyclic ring systems,with the centroid-to-centroid distance of 3.369(4) .     

Synthesis and Crystal Structure of Isonicotinic Acid [1-（3,5-Dibromo-2- hydroxyphenyl）methylidene]hydrazide Methanol

A new Schiff base compound, C13H9Br2N3O2·CH3OH, isonicotinic acid [1-(3,5- dibromo-2-hydroxyphenyl)methylidene]hydrazide methanol, has been synthesized and characterized by elemental analysis, IR spectra, and single-crystal X-ray diffraction. The compound comprises a Schiff base moiety isonicotinic acid [1-(3,5-dibromo-2-hydroxyphenyl) methylidene]hydrazide and a methanol molecule. The crystal belongs to the triclinic system, space group P1 with a = 8.464(1), b = 9.511(2), c = 10.901(2) , α = 92.940(2), β = 110.456(2), γ = 96.040(2)o, Z = 2, V = 814.0(2) 3, Dc = 1.759 g/cm3, Mr = 431.09, λ(MoKα) = 0.71073 , μ = 4.994 mm-1, F(000) = 424, R = 0.0440 and wR = 0.1061. A total of 3284 unique reflections were collected, of which 2197 with I > 2σ(I) were observed. The molecule adopts a trans configuration about the C=N double bond. The dihedral angle between the benzene and pyridine rings is 22.0(4)o. The crystal structure is stabilized by intermolecular O-H···N and C-H···O hydrogen bonds, forming layers parallel to the ac plane. The preliminary biological tests show that the compound has potential antibacterial activities.     

Synthesis and Crystal Structure of 2-[（2-Chloropyridin-4-yl）oxy]-3,3-diphenyl-3-methoxypropionic Acid

The title compound was synthesized and its crystal structure was determined by single-crystal X-ray diffraction.The crystal is of orthorhombic system(C21H18ClNO4,Mr = 383.81),space group Pca21 with a = 13.913(3),b = 10.273(2),c = 26.488(5),V = 3786.1(13) 3,Z = 8,Dc = 1.347 g/cm3,F(000) = 1600,μ = 0.228 mm-1,the final R = 0.0550 and wR = 0.1278 for 5065 observed reflections(I > 2σ(I)).The title compound in a racemic form was found to exist as a mixture of two enantiomers in an equal ratio in the unit cell.The intermolecular hydrogen bonds link the molecules in a head-to-end manner to generate an infinite chain.     

Syntheses and Crystal Structures of Two Copper(Ⅱ) Coordination Polymers Derived from Aromatic Carboxylic Acids and Bis(imidazoles) Ligands

Two compounds have been obtained by the reaction of metal(Cu(II)), 4,4?-bis(imidazol-l-yl)diphenyl thioether(BIDPT) with two carboxylic acids, 4,4?-oxydibenzoic acid(H_2oba) and phthalic acid(H_2pht). The crystal structures of the resulting compounds, namely {[Cu(BIDPT)(oba)]·H2O}n(1) and {Cu(BIDPT)(pht)}n(2), have been determined by single-crystal X-ray diffraction analysis. Compound 1 is of orthorhombic system, space group Pbcn with a = 27.8310(3), b = 10.7791(1), c = 19.3913(2) ?, V = 5817.0(3) ?3 and Mr = 656.15. Compound 2 belongs to the monoclinic system, space group C2/c with a = 18.2678(2), b = 11.0259(1), c = 22.906(2) ?, β = 97.727(2)o, V = 4571.8(8) ?3 and Mr = 545.04. Structural analyses reveal that compounds 1 and 2 respectively exhibit two-dimensional(2D) wavy and corrugated layer structures. Through intermolecular hydrogen bonding, compound 1 is assembled into a 3D supramolecular structure. The thermal stability and ultraviolet spectroscopy properties of the two compounds are also investigated.     

Synthesis and Crystal Structure of N-(Biphenyl-2-thiocarbamoyl)-4-(1,3-dichlorophenyl) Carboxamide

The synthesis of the title molecule was achieved by the reaction of 2,4-dichlorobenzoyl chloride with potassium thiocyanate in 1:1 molar ratio in dry acetonitrile to afford the corresponding isothiocyante in situ followed by the treatment with 2-aminobiphenyl. The structure of the target compound was established by elemental analysis, FTIR, 1H, 13 C NMR and mass spectroscopy and unequivocally confirmed by the crystallographic data. The title compound crystallizes in the monoclinic space group P21/n with a = 13.356(2), b = 7.0761(11), c = 20.539(3) , β = 105.723(4)°, V = 1868.5(5) 3 and Z = 4.     

Synthesis and Crystal Structure of [Cu_2(DMF)(H_2O)(C_7H_4NO_4)_2(C_7H_3NO_4)]_2·3.5DMF

A new copper(II) complex [Cu2(DMF)(H2O)(C7H4NO4)2(C7H3NO4)]2·3.5DMF has been synthesized and its structure was determined by single-crystal X-ray diffraction.The crystal is of triclinic,space group P1 with a = 10.722(3),b = 18.170(4),c = 20.923(7),α = 105.297(9),β = 101.701(10),γ = 105.74(1)°,V = 3615(1) 3,Z = 2,C58.50H64.50Cu4N11.50O31.50,Mr = 1686.90,Dc = 1.550 g/cm3,μ = 1.255 mm-1,F(000) = 1728.00,T = 150(2) K,the final R = 0.0640 and wR = 0.173 for 11310 observed reflections with I > 2σ(I).In the crystal,each formular unit consists of two dinuclear copper(II) compounds,between which the O-H···O hydrogen bonds exist.Each CuII cation is six-coordinated in an octahedral geometry.The intermolecular hydrogen-bonding interaction leads to a 3-D framework of the title compound.     

Synthesis and Crystal Structure of Ethyl 1-（2-bromoethyl）-3-（4-meth-oxyphenyl）-1H-pyrazole-5-carboxylate

The title compound ethyl 1-(2-bromoethyl)-3-(4-methoxyphenyl)-1H-pyrazole-5-carboxylate 1 has been synthesized and structurally characterized by single-crystal X-ray diffraction.The crystal is of monoclinic(C15H17BrN2O3,Mr = 353.22),space group C21 with a = 24.691(7),b = 6.7678(17),c = 17.884(5) ,β = 97.184(5)o,V = 2965.1(13) 3,Z = 8,Dc = 1.583 g.cm-3,F(000) = 1440,μ = 2.784 mm-1,the final R = 0.0260 and wR = 0.0596 for 2684 observed reflections with I > 2σ(I).All the carbon atoms in the molecule are nearly coplanar except C(15),with a large conjugated system among the carbonyl group,pyrazole ring and the benzene ring.Three non-classical intermolecular hydrogen bonds help to stabilize the crystal lattice.The regioselectivity was rationalized based on the coordination of potassium ion with the N-anion and the carbonyl oxygen atom.     

A Cu(II) Complex with IM-MeImz-κ~2 N,O Mode in [Cu(IM-MeImz)_2]·(SCN)_2: Synthesis, Crystal Structure and Magnetic Properties

A new copper(II) compound with imino nitroxide radicals [Cu(IM-MeImz)2]?(SCN)2 (IM-meImz =2-(5-methylimidazol-4-yl)-4,4,5,5-tetramethyl-2-imidazoline-1-oxyl) has been synthesized and characterized structurally and magnetically. It crystallizes in monoclinic, space group P21/c with a = 9.3604(7), b = 10.3012(7), c = 16.6684(12) , β = 105.0290(10)o, V = 1552.25(19) 3, C24H34CuN10O2S2, Mr = 622.27, Z = 2, Dc = 1.331 g/cm3, μ(MoKα) = 0.876 mm-1, F(000) = 650, the final R = 0.0374 and wR = 0.1079. X-ray analysis demonstrates that the IM-MeImz ligand is coordinated to the copper(II) ion as an unusual didentate chelate with a κ2 N(MeImz),O(IM) mode in the complex. The square-planar coordination sites at Cu(II) are occupied by two O and two N atoms from the imino nitroxide radicals. The complex molecules are connected as a onedimensional polymer structure by intermolecular interactions. Magnetic measurements show that there are intramolecular antiferromagnetic interactions between the Cu(II) ion and radicals.     

Microwave-assisted Synthesis and Crystal Structure of 3-Acetamido-1-phenyl-4-（2,6-dichloro）benzylidene-5-pyrazolone

The title compound,3-acetamido-1-phenyl-4-(2,6-dichloro)benzylidene-5-pyrazolone(C18H13Cl2N3O2,Mr = 374.21),has been synthesized by one-step condensation of 2,6-dichloroben-zaldehyde with acetic anhydride and 3-amino-1-phenyl-5-pyrazolone under microwave irradiation.The compound was characterized by means of IR and 1H NMR.Its crystal and molecular structure were determined by X-ray diffractometry.It belongs to the orthorhombic system,space group Pbca,with a = 12.5312(13),b = 8.5495(9),c = 31.110(3) ,V = 3332.9(6) 3,Z = 8,Dc = 1.492 g/cm3,λ = 0.71073 ,μ(MoKα) = 0.407 mm-1,F(000) = 1536,the final R = 0.0394 and wR = 0.0984.A total of 15894 reflections were collected,of which 3630 were independent(Rint = 0.0362).There exist three planes in the molecular structure.X-ray analysis reveals that the dihedral angles between planes 1 and 2,1 and 3 and 3 and 2 are 80.89,74.29 and 20.57°,respectively.     

Synthesis,Structure and Spectral Properties of a Novel Triaryl Substituted Triazole and Its Co(Ⅱ) Complex

The new compound 3-(2-pyridyl)-4-(p-methoxyphenyl)-5-(2-thienyl)-1,2,4-triazole L was synthesized and characterized by elemental analysis,IR,1H NMR,13C NMR,MS,UV and photoluminescent spectra.The complex CoL2(NCS)2 was prepared by the reaction of ligand L with Co(SCN)2,and its structure was characterized by single-crystal X-ray diffraction,IR,UV,elemental analysis and MS.The complex crystallizes in monoclinic,space group P21/n with a=13.7639(19),b=7.6641(11),c=18.409(3),β=101.549(3)o,V = 1902.6(5) 3,Z=2,C38H28CoN10O2S4,Mr=843.87,Dc=1.473 g/cm3,μ=0.720 mm-1,S=1.075,F(000)=866.0,the final R=0.0825 and wR=0.2149 for 2566 observed reflections(I2σ(I)).In the crystal structure,the cobalt atom adopts a distorted octahedral environment with two NCS-ions in the axial positions and two bidentate chelating L ligands in the equatorial plane.The extended 2D network of the complex is formed by intermolecular C-H…N hydrogen bonds together with π-π stacking interactions.