Synthesis and Crystal Structure of a New Dinuclear Manganese(Ⅱ) Manganese(Ⅲ) Complex of a Macrocyclic Ligand

A mixed-valence dinuclear manganese complex, [MnⅡMnⅢL](ClO4)·1/2MeOH, where L is a macrocyclic ligand derived from the cyclocondensation of sodium 2,6-diformyl-4-methylphenolate with N,N-bis(2-aminoethyl)-2-hydroxybenzyl amine, was obtained and its structure was determined by X-ray diffraction. The orange crystal is a monoclinic system with space group P21/c and lattice parameters a=1.1617(4), b=1.4005(3), c=1.4641(3) nm, β=113.03(2)°, and Z=2. The crystal structure shows that each pendant-arm is bonded in a bidentate fashion to the adjacent metal atom and that both the arms are on the same side of the macrocycle. The two Mn atoms are bridged by two μ2-phenoxy oxygen atoms of the tetra-imine macrocycle, and each Mn atom, locating in a trigonal prismatic coordination environment(N3O3), is six-coordinated by the two imine nitrogen atoms, one tertiary nitrogen atom and a pendant phenol moiety apart from the two oxygen atoms.     

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.     

Crystal Structure of [Et_4N][Sm(S_2CNEt_2)_4]

The crystal structure of .[Et4N][Sm(S2CNEt2)4] was determined by X-ray diffraction technique. The crystal crystallizes in monoclinic system, space group P21/n with a= 1. 1695(3), b=2.0821(6), c=1.7420(7) nm, β=99. 79(3)°? Z=4, Dc= 1. 39 g/ cm3, μ(Mo/KTσ) = 18. 4 cm-1, F(000) = 1812. The structure was solved by Patterson and Fourier techniques and refined by least-squares method to a final conventional R of 0. 053 for 3116 (Ⅰ> 3σ- (Ⅰ)) reflections. Each asymmetric unit contains two ions [Sm (S2CNEt2)4]-1 and [Et4N] +1, having distance between central atoms N5 and Sm3+ to be 0. 6522 nm. The atom Sm is coordinated by eight sulphur atoms. The Sm-S distance lies in the range of 0. 285-0. 290 nm with an average of 0. 288 nm.     

Synthesis, Structure and Properties of (n-Bu_4N)_3[Mo_6O_18NNAr(NO_2)_2]

The title compound was synthesized and characterized by means of elemental analysis, IR, DTA-TG and UV. Its single crystal structure was solved by using direct methods. The compound crystallizes in the orthorhombic space group Pmc(?) with lattice parameters: a = 1. 7261(2), b=l. 7537(3), c=2. 4258(3) nm. V=7. 34220 nm3, F(000) = 3648, Z = 4. The structure was refined to conventional discrepancy factors of R=0. 060 for 3176 observed reflections [Ⅰ>3σ/(Ⅰ)]. The anion represents a modification of the well-known [Mo6O19]2- anion, in which a single terminal oxo group is replaced by a 2,4-dinitrophenyl hydrazine ligand while the structure integrity of the hexanuclear framework is maintained.     

三维超分子化合物[Ag4(L)4](PMBS)4·2H2O的合成、晶体结构和荧光性质

The title compound,[Ag4(L)4](PMBS)4·2H2O (1),where L=2,5-bis (4-pyridyl)-3,4-diaza-2A-hexadiene,PMBS =p-methylbenzenesulfonate was synthesized and its crystal structure was determined by X-ray diffraction structure analysis.The crystal is of triclinic,space group P1 with a=0.820 3(2) nm,b=1.3227(3) nm,c=2.0610(3) nm,α=76.155(2)°,β=78.651 (4)°,γ=89.993(3)°,V=2.126 2(8) nm3,Z=2,Dc= 1.644 g·cm-3,F(000)= 1068,R=0.052 4,wR=0.113 6.The Ag atoms are linear coordinated by two N atoms of two L ligands,while the p-methylben-zenesulfonate molecules are included in the lattice and connected to [Ag(L)]n by hydrogen bonding interactions to form a three-dimensional supramoleculur structure.CCDC:727587.     

STRUCTURE AND BONDING OF Sm_(0.27)Nb_(2.73)Se_4 BY SOLID STATE REACTION

<正> The title compound was prepared from the corresponding elements (Sm, Nb and Se) using transport reaction with iodine at a temperature gradient of 1100/1040℃. The crystal structure was established by the single crystal X-ray diffraction technique with the following crystal data: Sm0.27Nb2.73Se4, Mr = 609. 8, hexagonal, P63/m, a = 9.997(1), c=3.470(2) A , V = 300. 4(2)A3, Z = 2, Dc= 6. 75 g/cm3, F (000) = 529. 34,μ= 292. 6cm-1, R = 0. 018, Rw = 0. 019. The ternary compound was confirmed to be isostructural with the compound Nb3Se4, and was found to be a conductor.     

杂-双核配合物[CaCu(C3H2O4)2(H2O)4]n的合成、晶体结构及热稳定性

The title complex, [CaCu(C3H2O4)2(H2O)4]n, with a formula of C6H12CaCuO12 and Mr=379.78 has been sy-nthesized and characterized by single crystal X-ray diffraction structure analysis, elemental analysis, IR spectra and TG-DTG techniques. The results show that the crystal is Orthorhombic, space group Pbcn with a=0.669 21(5) nm, b=1.370 23(5) nm, c=1.322 39(10) nm, V=1.212 59(16) nm3, Dc=2.080 g·cm-3, μ=2.288 mm-1, F(000)=772 and Z=4. The final R=0.054 0 and wR=0.112 8 for 1 189 observed reflections with I>2σ(I). The structure of the title complex consists of CaO8 polyhedra and CuO6 elongated octahedra linked together by malonate ligands. The Ca(Ⅱ) cation, on a twofold axis, is coordinated by two water molecules and six malonate O atoms. The Cu(Ⅱ) cation, which lies in a centre of symmetry in an octahedral arrangement, is coordinated by four malonate O atoms and two water molecules. The structure comprises alternating layers along the [101] plane, with the shortest Cu…Cu distance of 0.762 46(6) nm. The whole 3D structure is maintained and stabilized by the presence of hydrogen bonds. Its thermo gravimetric analysis was determined by TG-DTG techniques. CCDC:663184.     

一维链状化合物[Ag(L)]·H2O的合成、晶体结构和荧光性质

The title compound,[Ag(L)]·H2O,1,where HL=4-(isonicotinamido)benzoic acid,was synthesized in methanol solution and its crystal structure was determined by X-ray diffraction analysis.The crystal is of monoclinic.space group P21/c with a=0.571 8(8)nm,b=1.357 2(18)nm,c=1.5580(2)nm,β=91.090(2)°,V=1.2090(3)nm3,Z=4,Dc=2.009 g·cm-3,F(000)=722,Rint=0.042 9,R=0.027 1,wR=0.055 6.In complex 1,the Ag atoms are linearly coordinated by one O atom and one N atom of two ligand molecules.Each I- ligand in turn uses its one carboxylate group and one pyridinyl groups to connect two metal centers,then the one-dimensional (1D) chains is formed.On the other hand,the 1D chains are further connected by O1W-H1WB…O2 hydrogen bonds and Ag-O weak interactions to give a two-dimensional (2D) layer,finally,the 2D net extents to three-dimensional (3D) supramolecular framework by O1W-H1WB…O1 as well as N2-H2…O2 interactions.CCDC:762259.     

双核Cd(Ⅱ)配合物[Cd2(C22H14N4)2Cl2(N3)2]2·H2O的合成与晶体结构

A dinuclear Cd(Ⅱ) complex [Cdz (N3)2LzCl2]2·H2O (1) [L=4'-(4-eyanophenyl)-2,2':6',2"-terpyridine]was synthesized by reaction of ligand L with CdCl2 and NaN3 using solvothermal method and its structure was determined by X-ray crystal structure analysis. The structure indicates that the complex crystallizes in monoclinic, space group C2/c with a=1.644 5(16) nm, b=1.441 9(12) nm, c=1.9181(18) nm,β=100.349(11)°. V=4474(7) nm3, Z=2, Dc=1.570Mg·m-3,μ=1.120 mm-l, F(000)=2 100, and final R1=0.039 3, wR2=0.0811. The result shows a Cd(Ⅱ) ion was sixcoordinated by a tridentate 4'-(4-cyanophenyl)-2,2' :6',2"-terpyridine ligand and one bridging nitrogen atom of the azide group in the basal position and an chloride atom and the other bridging nitrogen atom of the azide group in the axialone, to form a distorted octahedral-pyramidal geometry. CCDC: 673291.     

Synthesis and crystal structure of ethyl benzimidazole-2-yl phosphonate

When N-cyanoimido-( O,O-diethyl)phosphonyl/S-methyl thiocarbonate (1) was treated with o-phenylenediamine in the presence of Et3N in ethanol,diethyl benzimidazole-2-yl phos-phonate (2) was obtained and hydrolyzed during the recrys-tallization in MeOH/H2O,generating ethyl benzimidazole-2-yl phosphonate (3).Hie crystal structure of compound 3 was determined by X-ray diffraction method.The crystals belong to monoclinic,space group C2/c,a = 1.78408(18) ,6 = 0.83725(9),c= 1.67401(18) nm,β= 118.997(2),V = 2.1870(4) nm3,Z = 8,Dc=1.374 g/cm3,F(000)=944.The final R and wR are 0.0499 and 0.1436,respectively.The mechanism of the above reaction is also discussed.     

离子对化合物[(IBz)_2Im](TCNQ)的合成与结构表征(英文)

A novel compound [(IBz)2Im](TCNQ) [(IBz)2Im=1,3-bis(4-iodobenzyl) imidazole cation, TCNQ-=7,7,8,8-tetracyanoquinodimethanide anion] was synthesized by the reaction of [(IBz)2Im]Br and LiTCNQ in CH3OH and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c with a=1.147 35(18) nm, b=2.028 1(3) nm, c=1.264 1(2) nm, β=104.73(0)°, V=2.666(65) nm3, Z=4, C29H19I2N6, Mr= 705.30, Dc=1.757 g·cm-3, R1=0.053 2 and wR2=0.111 2. The structure analysis shows that the anions are stacked into column with isolated π-dimers, and there is one type of TCNQ entries (TCNQ-), in agreement with the IR spectra analysis of the compound. The most prominent structural features are the completely segregated stacking columns of the TCNQ-anions and [(IBz)2Im]+ cations. CCDC: 759523.     

Synthesis,Crystal Structure and Electrochemical Property of a Dinuclear Manganese（Ⅱ） Complex [Mn_2（C_（12）H_8N_2）_4（C_8H_5O_4）_2]（C_8H_4O_4）·H_2O

One dinuclear manganese(II)complex [Mn2(C12H8N2)4(C8H5O4)2](C8H4O4)·H2O has been synthesized with o-phthalic acid and 1,10-phenanthroline.The crystal structure was determined by X-ray diffraction.The crystal belongs to the triclinic system,space group P1 with a = 1.17767(3),b = 1.22292(2),c = 1.35860(3)nm,α = 110.5300(10),β = 97.6140(10),γ = 93.7300(10)o,V = 1.80307(7)nm3,Dc = 1.404 g/cm3,Z = 2,F(000)= 784,the final GOOF = 1.047,R = 0.0398 and wR = 0.1038.The crystal structure of the title complex consists of one [Mn2(C12H8N2)4(C8H5O4)2]2+ cation,one uncoordinate o-phthalate anion(C8H4O4)2-and one uncoordinate water molecule.In [Mn2(C12H8N2)4(C8H5O4)2]2+,the central Mn(II)ion is coordinated by four nitrogen atoms and two oxygen atoms to give a distorted octahedral coordination geometry.The electrochemical property of the title complex was also studied.     

七配位K[InⅢ(Hdtpa)]·3.5H2O配合物的合成及结构测定

In this paper, the title complex K[InⅢ (Hdtpa)] · 3.5H2O(dtpa=diethylenetriaminepentaacetic acid) was synthesized and its crystal structure was determined by single-crystal X-ray structure analysis.The crystal belongs to monoclinic system, P21/c(No. 14) space group with a= 0. 978 1 (2) nm,b=0. 733 8(1) nm, c＝2. 962 9(6) nm, β=91.81(3)°, V=0. 212 6(1) nm3, Z=4, M=606.31, Dx=1.895 g · cm-3, μ=1. 382 1 mm-1, F(000)=1 228, R=0. 035 and Rw=0. 041 for 2 802 unique reflections. The complex anion [InⅢ (Hdtpa)]- has a pseudo-monocapped trigonal prismatic sevencoordination structure in which the seven coordinate atoms, three N and four O atoms, are all from a ligand dtpa. In addition, it can be seen that the complex anion [InⅢ (Hdtpa)]－ can furnish a free carboxyl group(-CH2COOH) being used for molecular embellishment to form the target diagnosis- and treat-drug of anticancer.     

Hydrothermal Synthesis and Crystal Structure of Binuclear Copper(Ⅱ) Complex Bridged by 1,2,4,5-Benzenetetracarboxylato Trivalent Anion

The title complex [(phen)2Cu(Htcb)Cu(phen)2]H3tcb(tcb=1,2,4,5-benzenetetracarboxylato tetravalent anion; phen=1,10-phenanthroline) was synthesized by the hydrothermal synthesis method. The crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in the triclinic system with space group P1, a=1.04174(8) nm, b=1.07119(8) nm, c=1.26360(10) nm, α=98.169(2)°, β=99.679(10)°, γ=93.658(10)°, V=1.37031(18) nm3, Z=1. The two copper(Ⅱ) cations are bridged by Htcb in the monodentate fashion, and have the same five-coordinated environment completed by the four N atoms from the two phen molecules and one O atom from the carboxylic group of Htcb respectively, which can be best described as distorted trigonal-bipyramid geometry. Moreover, the three dimensional network is formed by H-bonding interactions [O…O distance from 0.2506(10) nm to 0.3176(11) nm] and π-π stacking interactions between the phen rings of adjacent binuclear entities with a face-to-face separation of ca. 0.354 nm.     

Synthesis and Crystal Structure of Compound [ZnS6 (C12H8N2)]

The title compound ZnS6(C12H8N2) was obtained by reaction of zinic powder with sulfur and 1,10-phenathtroline in DMF solvent, and its structure has been determined by single crystal X-ray diffraction analysis. The crystal data for the compound: triclinic, P-1, Z = 2, a = 8. 159(2), b = 9. 485(2), c = 11. 997(2)A , α =110. 00(3)°,β = 99.22(3)°, γ = 100.57(3)°, V = 832A3, Dc =1. 748g/cm3, μ(MoKa)=0. 2219 cm-1, F(000)=440. The structure was refined to R = 0. 0723 and Rw = 0. 0865 for 1427 independent observed reflections. The tilte crystal consists of a discrete molecules, in which the core of ZnS2N2 shows a distorted tetrahedral geometry.     

SYNTHESIS AND CRYSTAL STRUCTURE OF [(η~5-C_5H_5)_2NdCl·OC_4H_8]_2

All attempts to prepare light lanthanide dicyclopeutadienyt chloride failed,due to the disproportionation reaction. The crystal complex of [(η~5-C_5H_5)_2NdCl.OC_4H_8]_2 was successfully prepared by the reaction of NdCl_3·2C_4H_8O with cyclopentadienyl sodium (molar ratio 1:1.8)in tetrahydrofuran at room temperatureThe composition of the title compound was determined by the methods of elemental analysis, infrared spectroscopy and photoelectron spectroscopy. The crystal structure of [(η~5-C_5H_5)_2NdCl·OC_4H_8]_2 was determined from single crystal X-ray diffraction. Data were collected at-60℃ under dry nitrogen atmosphere.The complex crystallizes in the monoclinic space group P2_1/c,with Z=2. Lattice parameters are: a=8.201(3), b=21.589(6),c=8.596(3),β=109.10(3)°.The structure was solved by Patterson and Fourier techniques and refined by least-squares to a final conventional R=0.0636 for 1680 reflections. There are two Nd atoms in the dimeric unit which are bridged asymmetrically by the two chlori     

Synthesis,Crystal Structure and Bioactivity of N-（phenethylcarbamothioyl）cyclopent-1-enecarboxamide

The compound N-(phenethylcarbamothioyl)cyclopent-1-enecarboxamide was synthesized by the reaction of cyclopent-1-enecarbonyl isothiocyanate with phenethylamine in acetone, and its structure was characterized by IR, 1H NMR and X-ray crystal structure determination. The crystal of the title compound belongs to triclinic, space group P1 with a = 6.9500(7), b = 9.4618(9), c = 11.3256(11), α = 71.522(9), β = 81.830(8), γ = 89.237(8)o, Z = 2, V = 698.80(12)3, Dc = 1.304 g/cm3, μ = 0.225 mm-1, F(000) = 292, R = 0.0413 and wR = 0.1073 for 1996 observed reflections with I 2σ(I). Intramolecular N(2)–H(2)···O(1) interactions as well as intermolecular N(2)–H(2)···O(1), N(1)–H(1)···S(1) and C(12)–H(12)···S(1) hydrogen bonds help to stabilize the crystal structure. X-ray diffraction analysis reveals that the structure of the new compound exhibits a one-dimensional infinite chain-like structure. The cytotoxicity of the compound was investigated by MTT assay. The results show that the compound is toxic to A549 tumor cell.     

Crystal structure and thermal decomposition mechanism of the supramolecular complex of barium chloride with inositol

The single crystal of [Ba(H2O)2(C6H12O6)2Cl2] was obtained based on the phase equilibrium results. Its structure was determined by X-ray crystallographic analysis. The crystals are monoclinic and in space group C2/c with a=1.901 7(2) nm, b = 0.682 13(8) nm, c = 0.162 60(2) nm,β=96.593(2)°and V= 2.095 3(4) nm3, Z= 4, DC=1.917 g·cm-3. In its solid state, this supramolecular complex is a three-dimensional network with double layers connected by hydrogen bondings. The molecule structure of [Ba(H2O)2(C6H12O6)2Cl2] has a central barium ion that is coordinated to two water molecules, two chlorides, and four hydroxyls from the two inosi-tols. Losing the coordinating water is controlled by random nucleation and growth mechanism (n = 2/3) and 3-dimensional diffusion mechanism (n=2).     

CRYSTAL STRUCTURE OF CYCLOOCTADIENYL POTASSIUM TE- TRAHYDROFURANATE ,C_8H_(11)K(OC_4H_8)_2

<正> The title compound, cyclooctadienyl potassium tetrahydrofuranate was prepared by the reaction of cycloocta-1,5-diene with metallic potassium in tetrahydrof u-ran(THF) in the presence of triethylamine. Its crystal structure was determined by a low temperature X-ray diffraction analysis method. The crystal is monoclinic with space group Pc,a=6. 192(3),b=9. 444(8),c=14. 543(1) A ,β=94. 92(5)°,V = 847. 24 A3,Z = 2,DC= 1. 14 g/cm3 and μ(MoKa) = 5. 58cm-1. The structure was solved by heavy-atom methods and refined by least-squares to a final R value of 0. 049. The potassium cations, each with two complex THF molecules attached,are linked by bridging cyclooctadienyl an-ions,while the anions are connected to the bridging cations to form a puckered chain.     

Synthesis and Crystal Structure of N-[(3aR,4R,4aR,5aS,6S,6aS)-1,3-Dioxooctahydro-4,6-ethenocyclopropa[f]isoindol-2(1H)yl]-4-(trifiuoromethyl)phenylmethanimine Monohydrate

The crystal structure of the title compound (C19H17F3N2O4,Mr=394.35) was determined by single-crystal X-ray diffraction.The crystal belongs to monoclinic,space group C2/c with a=28.383(6),b=10.355(2),c=12.799(3)(A),β=111.74(3)°,V=3493.8(12)(A)3,Z=8,De=1.499 g/cm3,λ(MoKα)=0.71073,F(000)=1632,μ= 0.127 mm-1,R=0.0412 and wR=0.1019.In the title compound,there exist three intennolecular hydrogen interactions (O(4)...O(1),O(4)...O(3) and O(4)...N(1)) between water.The neighboring molecules are linked to each other generating a two-dimensional network structure via the three intermolecular hydrogen bonds and π-π interactions shaped by phen-phen with centroid distance of 4.049 (A).