SYNTHESIS, CHARACTERIZATION AND STRUCTURE OF [Co(DBP)_2·3Py]_2·2CHCl_3

The mixed ligand complex of cobalt with dibutylphosphate (HDBP) and pyridine has been synthesized. Elemental analysis yields the result that the formula of this compound is Co(DBP)_2·3Py·CHCl_3 (Py=pyridine). The thermal analsyis, visible spectra and magnetic properties of it have been studied as well. Single crystal structural analysis shows that the crystal is triclinic with space group P and the unit cell parameters are as follows:a=14.490(10), α=90.37(4)°,b=15.721(7), β=96.04(5)°,c=20.109(12), γ=105.63(4)°.The final R factor is 0.0773. Two Co atoms are connected by two bridging DBP groups to form a dinuclear molecule [Co(DBP)_2·3Py]_2 which has a C_s, symmetry. Each cell contains two dinuclear molecules and four chloroform molecules. The cobalt is coordinated in an octahedral arrangement by three oxygen atoms and three nitrogen atoms, of which one oxygen atom comes from a monodentate DBP group, two oxygen atoms from two bridging DBP groups, and the three nitrogen atoms from the three pyridi     

CRYSTAL STRUCTURE OF A HETERONUCLEAR LANTHANIDE COMPLEX OF ERBIUM-YTTRIUM AND GLYCINE[ErY(GlY)_6(H_2O)_4](ClO_4)_65H_2O

The title complex [ErY(Gly)_6(H_2O)_4](ClO_4)_6 5H_2O has been synthesized.Its crystalstructure has been determined by X-ray diffraction method.The crystal is triclinic with space groupP1.The unit cell parameters are as follows:a=11.518(4),b=14.105(7),c=15.530(6) ,α=96.61(3),β=102.74(3),γ=105.70(3)°,V=2327.7(17) ~3,Z=2,Dc=2.091g/cm~3.The structure has been refinedto a final R of 0.0785.The crystal is an infinite chain complex,in which four carboxyl groups fromglycine molecules bridge the Er(Ⅲ)and Y(Ⅲ)ion,other two carboxyl groups bridge two adjacentEr(Ⅲ)or two Y(Ⅲ)ions.     

CRYSTAL STRUCTURE OF BIS-ETHYLENEDIAMINE TRITHIOCYANATE OF COPPER(Ⅱ) AND SILVER(Ⅰ) Cu(en)_2Ag(SCN)_3

Cu(en)_2Ag(SCN)_3 crystallizes in space group P2_12_12_1 with its cell parameters, a=7.126(2), b=12.587(5), c=17.585(5). There are four formula units per unit cell(ρ_obs.=1.90g/cm~3, ρ_(calc.=1.96g/cm~3). Diffraction data are collected on a CAD4 four-circle diffractometer using Mo-Ka radiation. The structure is determiued by heavy atom method, then refined by leastsquare method to a final R=0.036. It is shown that in the crystal the coordination of Cu atoms is square pyramidal with four N atoms of en groups in the square plane and oue Natom of thiocyanate group in the apical position. The Ag atom is coordinated tetrahedrally by four S atoms of thiocyanate groups, one of which links up two AgS_4 together, thus forming the infinite AgS_4 tetrahedron chains along a axis.     

STUDIES ON RARE EARTH COMPLEXES OF QUARTERNARY AMMONIUM SALT——SYNTHESIS AND CRYSTAL STRUCTURE OF TETRAKIS-(TRIMETHYL-HEXADECYL AMMONIUM)DECANITRATO DINEODYMATE,((CH_3)_3C_(16)H_(33)N)_4Nd_2(NO_3)_(10)

A series of binuclear eleven-coordinated rare earth complexes with long chain quarternary ammonium salt have been synthesized. The general formula of the complexes may be represented by((CH_3)_3 C_(16)H_(33)N)_4Ln_2(NO_3)_(10) where Ln is La, Ce, Pr, Nd, Sm, Eu, Ga, Ho, Er or Y. The TG curve, the magnetic moment and the dissociation degree of the Nd complexes in alcoholic solution have been determined.((CH_3)_3C_(16)H_(33)N)_4 Nd,_2NO_3)_(10) was chosen as a representative of the complexes for the crystal structure determination. The crystal is monoclinic with space group P. Each Nd atom is coordinated by four terminal nitrate groups bidentately, and two Nd atoms are connected through two O atoms of the nitrate groups forming binuclear complex. Therefore, each Nd atom is surrounded by eleven oxygen atoms. The average bond length of the eleven Nd-O bond is 2.57, while the Nd-O bond length on the oxygen-bridge is 2.62.     

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.     

Synthesis and crystal structure of [V_2(μ-S_2)_2(S_2CNEt_2)_4]·2CH_3Cl

[V_2(μ-S_2)_2(S_2CNEt_2)_4].2CH_3Cl was synthesized by the reaction of NaS_2CNEt_2,Li_2S andVOCl_3 at room temperature.Crystal data:M=1061.3,space group Pbca,with the orthorhombicparameters:a=20.123(3),b=20.485(4),c=10.911(3),V=4497.7,Z=4,D_c=1.57g/cm~3,Mo Kσradiation(λ=0.71069()?),μ=13.2 cm~(-1),F(000)=2168.Final R=0.041 and R_w=0.047 for 2288 ob-served reflections with I>3σ(1).The coordination sphere of each V atom in title compound is a dis-torted tetragonal prism composed of two bidentate dithiocarbamate and two S_(2~((2-)) ligands.The V—Vdistance is 2.890 while the V—S distances fall in the range of 2.422—2.505.     

HETERONUCLEAR COMPLEX CONTAINING COPPER-LANTHANIDE ARRAYS: THE SYNTHESIS AND CRYSTAL STRUCTURE OF Ln_2Cu_4L_8 (HL)_4(OH)_2(CIO_4)_4(H_2O)_(10)·2CH_3COCH_3 (Ln = Tb (1), Y (2); HL = 2-Pyridone C_5H_5NO)

Reaction of 2-pyridone, copper acetate and terbium(or yttrium) perchlorate in acetone with the moleratio 6: 2: 1 results in the formation of heteronuclear complex Ln_2Cu_4L_8 (HL)_4 (OH)_2 (ClO_4)_4 (H_20)_(10)2CH_3COCH_3(Ln = Tb (1), Y (2)). By recrystallizing (1) in CHCl_3 single crystals were obtained and thestructure was determined by four-circle diffractometer. Data showed that the crystal is in space groupC2/m with a=27. 454(9)A, b=13, 608A, c=30. 556(11)A, β=99. 89(3)°, v=11245. 7(7. 5)A~3. Thestructure was solved by a combination of Patterson method and Fourier technique. The final R value is0. 103. In the structure, four copper and two terbium ions are bridged by 2-pyridone anions to form anessentially octahedral Cu_4Tb_2 core. The terbium atoms are each eight-coordinate and the copper atomsare five-coordinate.     

CRYSTAL STRUCTURE OF CK(C_(12)H_(24)O_6)]_2Pd(SCN)_4(H_2O)

<正> [K(C_12H_24O_6)]_2Pd(SCN)_4(H_2O),MT=963.59,monoclinic, P21/n,a= 11. 075(1),b= 12. 231(1),c= 15. 863(2) A ,β=93. 25(1)°,V=2145. 3A3,Z=2, Dc=1. 492gcm-3,λ(MoKa) = 0. 71073A μ=8. 64cm-1,F(000) = 996,final R=0. 045 for 1835 observable reflections. The Pd2+ ion coordinates with four S atoms from SCN- groups forming a regular square planar configuration. The K+ ion is surrounded by six ether oxygen atoms,one O atom from water molecule coordinated to two K+ions and one N atom from SCN- group to form a distorted hexagonal bipyramid. Two K atoms are linked with one Pd atom by two bridging SCN- groups forming a chain molecular array in the crystal.     

配合物[Tb(p-ClBA)_3(phen)]_2的结构和性能(英文)

Terbium p-chlorobenzoate complex with 1,10-phenanthroline, [Tb( p-ClBA)_3phen]_2 (1) has been obtained in the ethanol solution, where p-ClBA=p-chlorobenzoate and phen=1,10-phenanthroline. It crystallizes in the triclinic system, space group P1, a=1.008 1(2) nm, b=1.185 7(2) nm, c=1.431 1(3) nm, α=110.826(4)°, β=96.436(4)°, γ=101.737(4)°, Z=2. The two Tb(Ⅲ) ions are linked by four carboxylate groups through their bidentate bridging modes, forming a dimeric unit with crystallographic inversion center. Each terbium ion has an eight-coordinate geometry with four of the coordination sites occupied by four oxygen atoms from the four bridging carboxylates, respectively, two oxygen atoms from bidentate carboxylate, and the remaining positions occupied by two nitrogen atoms from a 1,10-phenanthroline molecule. The Tb(Ⅲ) ion adopt a distorted square antiprism coordination geometry. The excitation and luminescence data observed at room temperature show that the title complex emits very intensive green fluorescence under ultraviolet light. The result of thermal analysis indicates the complex [Tb(p-ClBA)_3phen]_2 is quite stable to heat. CCDC: 221921.     

CRYSTAL STRUCTURE OF ORGANOLANTHANIDE COMPLEX [Li~+(DME)_3]_2[(CpNd)_4(μ_2-CH_3)_2(μ_4-O)(μ_2-Cl)_6]~(2-)

<正> The crystal and molecular structure of [Li+(DME)3]2[(CpNd)4 (μ2-CH3)2(μ4-O) (μ2-Cl)6]2~was determined from single crystal X-ray diffraction. The complex crystallizes in the monoclinic space group P21/n with lattice parameters a= 14. 614(5), b= 18. 683 (5),c= 24. 595 (6) A, β = ,91-85(2)°, V = 6712(3) A3,2 = 4,DC = 1. 63g/cm3,F(000) = 3256,Mr=1650. 85. The structure was solved by direct methods and Fourier techniques and refined by least-squares to a final R=0. 047,RW = 0. 049 for 3761 with I>3σ(I). The result revealed that the anion [(CpNd)4(μ4-O) (μ2-Cl)6(μ2-CH3)2]2- is composed of four neodymium (Ⅲ) atoms bridged by six Cl atoms, two methyl groups and one oxygen atom, and every Nd is bonded to a cyclopentadienyl group. The four Nd atoms form a distorted tetrahedron. The cations are composed of two Li+(DME)3 with average Li-O distance of 2. 120(40) A.     

SYNTHESIS AND STRUCTURE OF A NEW TYPE OF COORDINA-TION COMPOUND OF Gd(Ⅲ) WITH H_2 CCH_2CH_2C(~+NH_2)C-HCOO-

<正> The crystal structure of gadolinium L-proline (Pro) complex [Gd2-(C5H9NO2)6 (H2O)6] (ClO4)6 has been determined. The complex crystallizes in the triclinic space group PI with following crystal data: a = 9. 906(3), b=13. 052(5), c = 13.703(5) A. α=109. 63(3), β=110.31(2), γ=100. 73(3)°, V=1470.3(9) A3.Mr=1710. 1, F(000) = 854,μ=26. 30 cm-1, Dc = 1. 931 g/cm3, Z=1.The structure was refined to the final R of 0. 048 for 3804 reflections. The structure is of one-dimensional chain, in which each gadolinium ion lies at the center of a distorted square antiprism of the eight oxygen atoms provided by four bridging carboxylate groups from four Pro ligands, a terminal carboxylate group from one terminal Pro ligand and three water molecules and the two neighbouring gadolinium ions are linked to each other through the two bridging carboxylate groups from the two Pro ligands. The prolines exist in the form of H2 CCH2CH2(+NH2)CHCOO-, and the complexions in the crystal are linked together by the net of hydrogen bo     

Synthesis, Crystal Structure and Photoluminescent Properties of a New Dinuclear Copper(I) Complex [Cu_2(μ_2-dppm)_2(MeCN)_2(μ_2-MeCN)](ClO_4)_2·MeCN

The title compound [Cu_2(μ_2-dppm)_2(MeCN)_2(μ_2-MeCN)](ClO_4)_2·MeCN (dppm = bis(diphenylphosphino)methane) has been prepared and characterized. It crystallizes in the monoclinic system, space group P2_1/n, with a = 11.904(6), b = 20.755(11), c = 24.744(13) (A),β = 98.226(12)°, C_(58)H_(56)Cl_2Cu_2N_4O_8P_4,M_r= 1258.93, V=6051(5) (A)~3, Z = 4,D_c= 1.382 g/cm~3,μ = 9.52 mm~(-1), F(000) = 2592, R = 0.0533 and wR = 0.1295 for 6175 observed reflections with I > 2σ(I). Each Cu(I) center is tetrahedrally coordinated by two phosphine atoms from two bridging dppm ligands, one nitrogen atom from a terminally coordinated acetonitrile molecule, and another nitrogen atom from a μ_2-acetonitrile molecule. The two Cu(I) centers are bridged by two dppm ligands as well as a unique acetonitrile molecule. The full molecule exhibits a 'chair-like' configuration. This dinuclear complex exhibits intense or middle photoluminescence at room temperature in the solid state or actonitrile solution at 486 nm.     

MOLYBDENUM-IRON MIXED METAL CLUSTERS (Ⅰ)——THE SYNTHESIS AND STRUCTURAL CHARACTERIZATION OF (η~5-C_5H_5)_2Mo_2Fe_2(μ_4-Te)(μ_3-Te)_2(CO)_6

The reaction of Fe_2(μ_3-Te)_2(CO)_9 with Mo_2(CO)_6(η~5-C_5H_5) affords the title compound. Its X-ray analysis shows a butterfly structure for the Mo_2Fe_2 core; the two molybdenum atoms occupy the hinge with a Mo—Mo bond distance of 2.819 and the two iron atoms are on the tops of the wings with an average Mo—Fe bond distance of 2.932(2). Each molybdenum is bonded to a Cp ring, and three CO ligands are terminally bonded to each iron atom. One tellurium atom quadruply bridges Mo_Fe_2 with Mo—Te(μ_4)=2.625(2). and Fe—Te(μ_4)=2.713(2). Two tellurium atoms triply bridge the two triangular Mo_2Fe faces with Mo—Te(μ_3)=2.678(1) and Fe—Te(μ_3)=2.513(3). The molecule has C_(2v) symmetry and a bicapped triangle bipyramidal skeleton. Crystallographic parameters are as follows: space groupImm2(orthorhombic), a=14.562(3), b=10.391(1), c=7.139(4), V=1080.2(i)~3, Z=2, ρ(cald)=1.819g·cm~(-3). The final R factor was 2.2％ for 620 independent reflections(I>2σ(I)).     

MOLECULAR AND CRYSTAL STRUCTURE OF (μ-HOCH_2 CH_2 S)_2 Fe_2 (CO)_4(PPh_3)_2

<正> The molecular and crystal structure of the complex (μ-HOCH2CH2-S)2 Fe2(CO)4(PPh3)2 synthesized by reaction of ethylene epoxide with (μ-Lis)2Fe2(CO)6, followed by EtOH alcoholysis and PPh3 substitution,was determined by X-ray diffraction technique. The crystals are triclinic,space group P 1,with a= 10. 902(2),b=12. 106 (2),c=16. 123(4) A ,V= 2079. 36A3,α=78. 13(1),β=89. 37(2),γ=87. 93(1)°, Z = 2,Dx=1. 44 g/cm3.μ(MoKa) = 9. 149cm-1, F(000) = 940. The final R and Rw equal to 0. 055 and 0. 068,respectively,for 3598 observed independent reflections. In this molecule two PPh3 ligands are trans to the Fe - Fe bond and axially coordinated to two iron atoms. In addition,two hydroxylethyl groups are attached to bridging sulfur atoms by e-type of bond and thus this molecule is an ee conformer.     

Synthesis and Crystal Structure of Complex {[Cu(N-men)_2(cda)_2]·[Cu(N-men)_2]·(ClO_4)_2}(N-men=N-Methylethylenediamine,cda=Carbamyldicyanomethanide Anion)

<正>Mononuclear complex {[Cu(N-men)2(cda)2]·[Cu(N-men)2]-(ClO4)2} was synthesized by sodium carbamyldicyanomethanide Na(cda), N-methylethylenediamine and hydrate copper perchlorate. The crystal belongs to the triclinic system, space group P 1 with a = 7.229(2), b = 8.114(2), c = 15.936(4) A, α = 80.511(4), β = 78.993(4), r= 72.118(4)°, V = 867.6(3) A3, Z = 1, C20H44Cl2Cu2N14O10, Mr = 838.68, Dc = 1.605 g/cm3, F(000) = 434 and μ = 1.449 mm-1. The structure was refined to R = 0.0480 and wR = 0.1289 for 2503 observed reflections (I > 2σ(I)). In the complex there exist two kinds of coordination models for Cu (II) ions. One is that the Cu (II) ion is coordinated by four nitrogen atoms which are from two N-men molecules, and a slightly distorted square planar coordinate environment is formed around the Cu (II) ion; the other is that the Cu (II) ion is coordinated by six nitrogen atoms, of which four are from two N-men molecules and the left from nitrile groups, resulting in a distorted octahedron around the     

Density Functional Theory Investigation on the Reaction Mechanisms of Ti(~3F) with CH_2Cl_2 and CHCl_3 to CH_2=TiCl_2 and HC÷TiCl_3

The reaction mechanisms of Ti(~3F) + CH_2C1_2→CH_2=TiCl_2 and Ti(~3F) + CHC1_3→HC÷TiCl_3 were investigated with Gaussian 03 program package at the B3PW91/6-311++G(d,p)level.The computational results revealed that:1) Both reaction systems are initiated by Ti(~3F) atom attacking the C atom of CH_2C1_2 and CHCl_3 to activate a C-Cl bond;2) Both reaction systems were carried out via triplet reaction channels;3) CH_2=TiCl_2 has singlet and triplet isomers,and the singlet one is more stable;4) The HOMO of CH_2=TiCl_2(S) illustrates a π-bonding interaction between C and Ti;5) Only singlet HC÷TiCl_3 was located,and the Mulliken atomic spin densities show that the two single electrons are mostly on the C atom.     

STUDY ON TRINUCLEAR MOLYBDENUM CLUSTER COMPOUNDS——THE CRYSTAL AND MOLECULAR STRUCTURE OF THE TWO TRINUCLEAR MOLYBDENUM CLUSTERS(C_5H_7S_2)[Mo_3(μ_3-O )(μ-X)_3(μ-OAc)_3Cl_3](X=Cl,Br)

The crystal structure of two isomorphic cluster compounds with formula (C_5H_7S_2)-[Mo_3(μ_3-O)(μ-X)_3(μ-OAc)_3Cl_3] (X=Cl for compound (Ⅰ) and compound (Ⅱ)) has been investigated by X-ray diffraction method. The parameters of two crystals are: a=10.423(1),b=17.095(4), c=14.062(7), β=97.54(4)(°); Dc=2.20gcm~(-3), D_o=2.17g cm~(-3) for compound (Ⅰ). and a=10.511(3), b=11.213(2), c=14.053(3), β=96.12(2)(°); D_c=2.52g cm~(-3), D_o=2.53gcm~(-3) for compound (Ⅱ). The space groups are P2_1/C. Z=4. The 2621 and 2548 independent reflections with I>3σ(I) were collected on a CAD-4 four-circle diffractometer by means of MoKα radiation. The crystal structures were solved by heavy atom method and refined by full-matrix least-squares technique to a final discrepancy factors of R=0.061 and 0.051 respectively. The results of investigation show that the molecule consists of the cation (C_5H_7S_2)+ and the trinuclear Mo cluster anion, the configuration of which is similar to that of (Et_4N)_2[Mo_3(μ_3-O)(μ     

Syntheses of (C_5H_9C_5H_4)_2LnCl(THF)_n (Ln=Nd, Sm, Er, Yb) and crystal structure of [(C_5H_9C_5H_4)_2-LnCl(THF)_n]_2(Ln=Sm, n=1; Ln=Er, n=0)

Reactions of lanthanoid trichlorides with sodium cyclopentylcyclopentadienyl in THFafford bis(cyclopentylcyclopentadienyl) lanthanoid chloride complexes (C_5H_9C_5H_4)_2LnCl(THF)_n (Ln=Nd, Sm, n=1; Ln= Er, Yb, n= 0). The compound [CP'_2SmCl(THF)]_2 (2) (Cp' =cyclopentylcy-clopentadienyl) crystallizes from mixed solvent of hexane and THF in monoclinic space group P_2_1/cwith a = 11.583 (3), b = 23.019(6), c = 8.227 (2), β= 90.26 (2)°, V= 2194 (1)~3, D_c= 1.59 g/cm~3.μ= 28.6 cm~(-1), F(000) = 1060, Z= 2 (dimers). Its crystal molecule is a dimer with a crystallographicsymmetry center. The central metal atom Sm is coordinated to two Cp' rings, two bridging chlorineatoms and one THF forming a distorted trigonal bipyramid. The crystal of [Cp'_2ErCl]_2 (3) belongs tothe triclinic space group P with a = 11.264 (2), b= 13.296(5), c = 14.296(6), a = 96.99 (3), β=112.47(2), γ= 102.78(2)°, V= 1865(1)~3, D_c= 1.67 g /cm~3, μ= 48.0 cm~(-1), F(000) = 924, Z = 2 (dimers).The molecule is a dimer consisting of two Cp'_2 ErCl species bridged by two Cl atoms. The centralmetal atom Er is coordinated to two Cp' rings and two bridging chlorine atoms forming a pseudo-tetrahedron. All these complexes are soluble in THF, DME, Et_2O, toluene and hexane.     

CRYSTAL STRUCTURE OF [Sm(CCl_3COO)_3(H_2O)_2]·2H_2O

<正> Biaqua-trichloroacetate-samarium dihydrate, [Sm(CCl3COO)3(H2O)2]-2H2O, Mr=707.54, orthorhombic, space group Pnne, with a = 19.158(5), b = 22.176(4), c= 9.798(4)A, Z= 8, V= 4162.7A3.F{000)= 2696,λ(MoKα)=0.71069A, Dx = 2.258 g/cm3, final R=0.061. The title compound has non-molecular structural character, and its structural units Sm(μ-CCl3COO)s/2-(H2O>2 constitute 2-dinensional infinite chains of Sm(μ-CCl3COO)4Sm(μ-CCl3-COO)2Sm.The Sa(Ⅲ) atom in each unit is bound to two O atoms from aqua-molecules and six 0 atoms from six bridging CCl3COO groups (four of which are shared with the SB atom of another unit, two shared with the Sm atom of a third unit) forming a square antiprism.     

SYNTHESIS AND CRYSTAL STRUCTURE OF COMPLEX [Cu_2(CH_3COO)_4(C_8H_(11)NO)_2] · (C_6H_(11)NO)_2 · (C_8H_(12))

<正> SYNTHESIS AND CRYSTAL STRUCTURE OF COMPLEX [Cu_2(CH_3COO)_4(C_8H_(11)NO)_2] · (C_6H_(11)NO)_2 · (C_8H_(12)), where C6H11 = caprolactam, Mr = 900. 07, triclinic,space group P1, a = 11. 103(4), b= 11. 865(6), c=9. 912(3)(?), α=94. 85(4), β=115.20(2), γ=103. 25(4)°, V = 1125(2)(?)3, Z = l, Dx = 1. 33g. cm-3, λ(MoKa) = 0. 71069(?), T = 295K , μ = 10. 45cm-1, F(000) = 478, final R=0. 063 for 2098 observed reflections with I>3σ (I). The two Cu atoms in the molecule are held together by four carboxylate groups. Each Cu atom is bound in a square-pyramidal configuration to four carboxyl oxygen atoms and to the O atom of a caprolactam molecule.