STUDIES OF SYNTHESIS, STRUCTURE AND PROPERTIES OF CLUSTER COMPOUND [Fe_6S_9(SCH_2CH_2OH)Cl]~(4-)

By mixing appropriate quantity of FeCl_2, (NH_4)_2MoS_4 ano HSCH_2CH_2OH in MeOH--MeONa, the crystal [(C_2H_5)_4N]_4[Fe_6S_9(SCH_2CH_2OH)Cl] was obtained. The cluster compound crystallizes in triclinic, space gtoup, P1, and crystal cell constants:a = 12.818(4)A, b = 13.632(3)A, c = 18.328(7)A, α = 106.09(2)°, β = 100.75(2)°, γ = 102.69(2)°, Z = 2. On the basis of 7517 unique data (I>3σ(I)) the structure has been refined toR = 0.0818 by the block-diagonal least-squares. The result of structure analysis shows thatthe cluster compound [Fe_6S_9(SCH_2CH_2OH)CI]~(4-) includes doubly bridging μ_2-S, triply bridgingμ_3-S and quadruply bridging μ_4-S. The [Fe_6S_9]~(2-) core of [Fe_6S_9(SCH_2CH_2OH)CI]~(4-) consistsof eight nonplanar Fe_2S_3 rhombs that are fused edge-sharing to give four Fe(μ_2-S)(μ_3-S)Fe,two Fe(μ_2--S)(μ_4-S)Fe and two Fe(μ_3-S) (μ_4-S)Fe subunits. The quantum chemical calcu-lation of EHMO method was carried out for this cluster compound. The structure analysisgives a rule wit     

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 AND STRUCTURE OF THE FIRST TUNGSTEN-IRON-SULFUR CUBANE-LIKE CLUSTER [WFe_3S_4(S_2CNC_4H_8)s]·2DMF CONTAINING DITHIOCARBAMATO LIGANDS

<正> The title compound (Mr =1236.54) crystallizes in monoclinic space group C2/c with a =12.553(4),b=20.121(6),c=19.659(2)A,β=102.96(2)°,V=4839.1A3, Z = 4 and DC -1.697g/cm3. The structure was solved by direct methods.A full matrix least-squares refinement for 2197 reflections with I>3σ(I) gave final R and Rw of 0.064 and 0.076,respectively. The [WFe3S4] core of the cluster can be considered to be a [WFe3] tetrahedron capped by a sulfur atom on each face to fora a distorted cubane. The 57Fe Mossbauer spectrum indicates that there are two types of Fe atoms of ratio 2:1 in the cluster.     

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     

INVESTIGATIONS ON THE CRYSTAL STRUCTURE OF 2-(m-CYANOPHENYL)-5-CYANOBENZOTHIAZOLE AND CONFORMATIONS OF ITS ISOMERS

The crystal structure of 2-(m-cyanophenyl)-5-cyanobenzothiazole has been determined by X-ray single crystal diffraction method and its conformational analysis and its two isomers have been carried out by employing the PCILO method. The crystal of title compound belongs to the monoclinic system, space group P2_1/c, a=23.793(7), b=3.852(1), c=27.004(11), β=98.40°(3), Z=8, D_(calc). =1.42g/cm~3, F(000)=1072, the final β=0.048. The crystals of this molecule and its two isomers belong to a same space group, but the packing schemes of the molecules in the unit cell, the separations and the mutual orientation of-C≡N bonds are not same. From the detailed analysis and comparison of their packing schemes in crystal, it can be considered that they may be possible to polymerize to different extent in the solid state by appropriate energy stimulation.     

CRYSTAL STRUCTURE INVESTIGATION OF VANADYL COMPLEXES OF TRIDENTATE LIGAND (Ⅰ)——THE CRYSTAL STRUCTURES OF BIS[(1-(2,4-PENTANE- DIONATO(NITROBENZOYL) HYDRAZONE)-2- ETHOXY)OXOVANADIUM] AND BIS-[(1-(2, 4-PENTANEDIONATO-(3-NITROBENZOYL) HYDRAZONE)-2- METHO

The title complexes were obtained by the reactions of bis(2,4-pentanedionato)oxovanadium VO(Acac)_2 and m-nitrophenylhydrazide m-NO_2PhCONHNH_2 in the media EtOH and MeOH respectively. The compound (Ⅰ) crystallizes in the space group PT with unit cell dimensions a=8.123(2), b=10.409(5), c=10.822(4), α=65.78(3)°, β=85.50(3)°,γ=89.04(3)°. The compound (Ⅱ) crystallizes in the space group P2_1/a with unit cell dimensions a=7.745(2), b=19.164(5), c=10.787(4), β=107.87(2)°. The resuhs of structural analyses show that the two compounds have the same characteristics: the tridentate ligand formed by condensation occupies three of the four equatorial positions of vanadium and the rest equatorial position is occupied by alkoxy group RO~-. As RO~-group also bridges the sixth coordinated position of each vanadium atom, it brings about the formation of the new type binuclear complexes of vanadium.     

Synthesis and Structure of a NovelTetranuclear Erbium( Ⅲ) Complex with α-Alanine [Er4(Hala)6·(μ3-OH)4(H2O)8](ClO4)8·3H2O

The title complex was synthesized in an aqueous solution and its crystal structure was determined by X-ray diffraction. The crystal crystallizes in a triclinic system, space group P1 with a=1.306 3(2) nm, b=1.319 4(4) nm, c=1.950 2(4) nm, α=90.597(14)°, β=93.998(11)°, γ=94.093(13)°, V=3.344 1(12) nm3, Z=2, the final R indices are R1=0.065 4, wR2=0.126 2 respectively. The complex contains a novel tetranuclear cluster cation with four Er3+ ions connected by four μ3-OH ions and six bridging carboxyl groups. Each erbium ion is coordinated by three μ3-OH, three carboxylic oxygen atoms from three α-alanine and two oxygen atoms from water molecules, forming a square-antiprismatic coordination polyhedron.     

THE SYNTHESIS AND CRYSTAL STRUCTURE OF A NOVEL MOLYBDENUM-COPPER-SULFUR CLUSTER COMPOUND [(CH_3CH_2 )_4N]_2 [(μs-S)CusS_6(S_2)_6Mo_6O_6].DMF

The synthesis and crystal structure of a novel molybdenum-copper cluster compound with [(μs-S)Cus] core is reported. It was prepared from Cu2Br2 upon reaction with molybdenum sulfur compound [CH3CH2)4N]2[Mo2O2S2-(S2)(S4)]. The title compound crystallizes in the monoclinic system space group Cc with cell dimensions: a=21.320(5), b=21.869(3), c=13.029(5)A,β=118.28(1)°,Z=4, V=5349A3 and Dc=2.48 g.m-3. The structure has been determined by Patterson and Fourier methods and then refined by the least squares method to a final R of 0.053. There are some distortions from octahedron in configuration of the [(μs-S)Cu6]6 core with three weak Cu-Cu bonds.     

Synthesis and Crystal Structure of a Novel Compound of （C2N2H8O2） H6V10O28

A novel vanadate decamer, involving all vanadium atoms present in +5 oxidation and one formhydroxamic acid dimer cation readical, has been synthesized. The single-crystal X-ray diffraction shows that the orange crystal is formed in the triclinic system, space group Pi, a = 8. 4960 (17), b = 10.447 (2), c = 11.299 (2) A, α= 68. 82 (3)°,β= 87.35 (3)°, γ = 66.97(3)°. V = 855. 3(3) A3, Z = 8, R1 = 0. 0857, wR2=0. 2551. X-ray crystallographic and packing in superlattice studies showed that the crystal structure was constructed by electrostatic attraction of O-H…O hydrogen bonds between formhydroxamic acid dimer cation and decavanadate polyanion. Formhydroxamic acid dimer is got through controlling the condition of the reaction using formhydroxamic acid.     

THE CRYSTAL STRUCTURE OF A NOVEL TETRANUCLEAR SILVER CLUSTER COMPLEX Ag_4(α-C_(10)H_7CS_2)_4(Py)_4·2Py

The title compound has been synthesized by the reaction of α-dithionaphthoic acidwith AgNO_3 in an organic solvent. The single crystals were obtained by recrystallizingfrom pyridine. We obtained two kinds of crystal with different colours (A and B), usingdifferent ratios of silver nitrate and α-dithionaphthoic acid (1:2,1:4) in the reactions. The structures of the two kinds of crystal were determined by a single-crystal X-raydiffraction analysis. The crystal (A) belongs to monoclinic space group C_(2h)~5-P2_1/a withunit cell parameters: a = 22.822(4) A, b = 12.803 (4) A, c = 24.444 (7) A, β = 103.90 (2)°V = 6933.14 A~3, Z = 4. The crystal (B) belongs to monoclinic space group C_(2h)~6-C2/c witha = 29.150 (2) A, b = 12.799 (3) A, c = 24.413 (2) A, β = 130.56 (4)°, V = 6914.38 A~3,Z = 4. Both crystals (A) and (B) have the same molecular configuration, but they havedifferent symmetry. In crystal (B), the molecule possesses a C_2 symmetry. This paperreports the structure determination and parameters o     

CRYSTAL AND MOLECULAR STRUCTURE OF MOLYBDENUM COM-PLEX MoO_2Cl_2(C_4H_3OCOOH)_2

<正> The crystal and molecular structure of the title compound was determined by single crystal X-ray diffraction method. The complex crystallizes in the mono-clinic space group P21/n with a = 10. 306 ( 3) , b = 10. 161 (2), c = 14. 798 ( 4) A . β= 108. 52(2)°, V= 1469. 4(6)A3,Z= 4. The structure was solved by direct methods. Least-squares refinement converged to a final value of R = 0. 043 and Rw= 0. 040 for 1237 reflections. The molybdenum (Ⅵ) ion is bonded to two chlorine atoms, two oxo atoms and two oxygen atoms from two monodentately and weakly coordinated carboxyl groups of molecules C4H3OCOOH, forming a octahedron. The Mo-O distances are in the range 1. 66 - 2. 39A ,the Mo-Cl distances fall in the range 2. 33-2. 34A.     

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 A MOLYBDENUM-COPPER-SULFUR CLUSTER COMPLEX WITH DITHIOBENZOATE LIGAND [Bu_4N]_2[MoCu_2S_4(C_6H_5CS_2)_2]

<正> The title compound has been synthesized by the reaction of (Bu4N)2MoS4, CuCl and (C6H5CS2)(Bu4N) in DMF and recrystallized from DMF/ Et2O. The red black crystal belongs to the triclinic space group P1 with a = 12. 021 (6), b = 17.045(8), c=17. 136(7)(?) , α=110.05(3), β=108.64(4), γ=103.87 (4)°, V = 2873(3)(?)3, Dc=1. 321gcm-3, Z = 2. The structure was refined to R = 0. 065 for .4783 reflections. The anion of the title compound can be described as a MoS42- tetrahedron coordinated by two [Cu(C6H5CS2)] units with the three metal atoms lying on a line. The coordination number of each Cu atom is three.     

THE CRYSTAL AND MOLECULAR STRUCTURE OF CHLORO(BIS-2,2''''-DIPYRIDYL) COPPER7,7'''',8,8''''-TETRACYANOQUINODIMETHANE [Cu(bipy)_2Cl]·TCNQ_2

The crystals of title compound are prepared by the electrochemical method and its structure has been determined by X-ray diffractions method. The crystals are triclinic with space group P(?). a=7.920, b=13.140, c=19.126; a=100.77°, β=94.45° and γ=101.08° ; Z=2, Calculating of electronic structure of TCNQ and its packing mode are discussed.     

SYNTHESIS AND STRUCTURE OF TETRANUCLEAR MOLYBDENUM CLUSTER COMPOUND[Mo_4S_4(μ-O_2CC_6H_5)_2(dtp)_4]

The cluster compound[Mo_4S_4(μ-O_2CC_5H_5)_2(dtp)_4](dtp=S_2P(OEt)_2)wasobtained by the ligand substitution reaction of tetranuclear molybdenum cluster[Mo_4S_4(μ-dtp)_2(dtp)_4]in the mixed solvent of acetone,ethanol and water in thepresence of C_6H_5CO_2Na.It is monoclinic and crystallizes in space group C2/c,Mr=1495.09,a=12.175(5),b=22.01(1),c=20.875(9),β=99.04(4)°;V=5575(5);Z=4;Dc=1.78g/cm~3.Final R factor is 0.066.The result reveals that the[Mo_4S_4]clustercore and t-(dtp)~(-1)ligands are retained and only μ-bridged(dtp)~(-1)ligands aresubstituted by(C_6H_5CO_2)~(-1)in the substitution reaction,thus producing the newtitle cluster compound,the structure of which contains two species of bidentateligand.     

The synthesis and crystal structure of heteronuclear complex of lanthanide with sulfo-salicylic acid [Na3YLa2(C7H3SO6)4.26H2O]n

The titled complex has been synthesized by the reaction of sodium sulfo-salicylate with lanthanum and yttrium perchlorate. The crystal structure has been determined by single crystal X-ray diffractometry. The crystal is monoclinic with space group C2/c. The unit cell parameters are as follows: a=16.289(8), b=18.323(8), c=22.044(8) A, β=106.34(2)°, V=6314(6) A3, Z=4 and Dc=1.764 g/cm3. The structure was solved by direct method. The least-square refinement based on 3776 observed reflections [F > 6σ(F)] converged to a final R=8.6% and F(000) is 3548. Yttrium ion with eight-coordinate is located in central of the molecule, the two lanthanum ions with ten-coordinate are located at the two sides of yttrium ion. There are two positions for Na in the molecule, one is in the C2 axis with six coordinate, the other one is in a general position with five-coordinate.     

Non-Isothermal Decomposion Kinetics of Supermolecule Compound [Eu(C_(10)H_9N_2O_4)(C_(10)H_8N_2O_4)(H_2O)_3]_2·phen·4H_2O

Europium(Ⅲ) compound with 2-oxopropionic acid salicyloyl hydrazone (C_(10)H_(10)N_2O_4,H_3L) and 1,10-phenan-throline (C_(12)H_8N_2,phen) has been prepared.A yellow prismatic crystal of the compound was obtained,and themolecule crystallized in the triclinic space group P-1.There are two 9-coordinated complex molecules in everystructure unit,where every Eu atom is coordinated by three water molecules and two tridentate C_(10)H_(10)N_2O_4 ligands,forming two stable pentacycles.The coordination polyhedron around Eu~(3+) was described as a single cap squareantiprism.In the crystal cell,there are one free 1,10-phenanthroline and four water molecules.The thermaldecomposition of the compound and its kinetics were studied by non-isothermal thermogravimetry.The Kissinger'smethod and Ozawa's method were used to calculate the activation energy value of the first-step decomposition.Thestages of the decompositions were identified by TG-DTG-DSC curve.The non-isothermal kinetic data were ana-lyzed by means of integral and differential methods.The possible reaction mechanism and the kinetic equationswere investigated by comparing the kinetic parameters.     

THE CRYSTAL AND MOLECULAR STRUCTURE OF DIPOTASSIUM TRIS(HYDROXYACETATO) VANADYL(ⅠⅩ) MONOHYDRATE

The title compound has been prepared by reaction of VOSO_4 with hydroxyacetic acid in aqueous solution, adding KOH to a suitable pH value. The crystals are monoclinic, space group P2_1/b with cell parameters: α=10.075(2), b=9.857(3), c=14.314(3), γ=115.29(2)°, Z=4. Intensities of 1714 independent reflexions having I≥3σ(I) were collected on a CAD4 diffractometer with MoKα radiation. The structure was solved by Patterson and direct methods and refined by full matrix least-squares method to R=0.060. In the complex the ratio of centric V atom to hydroxyacetate ligands is M:L=1:3, two hydroxyacetate ligands are chelated to V atom in a cis arrangement, the other is monodentate ligand with a carboxyl O atom to grasp the cation VO~(2+).     

Anti-tumor Metastasis and Crystal Structure of N1（1,3,4-Thiadiazole-2-yl）-N3-m-chlorobenzoyl-urea

The title compound N 1-(1,3,4-thiadiazole-2-yl)-N 3-m-chlorobenzoyl-urea (C 9 H 7 N 4 OSCl,M r=254.70) was prepared by the reaction of m-chlorophenyl isocyanate with 2-amino-1,3,4-thiadiazole in dry acetonitrile.The effect of the title compound on tumor metastasis was analyzed by Lewis-lung-carcinoma model.The bioassay showed that the title compound significantly reduced the number of lung metastasis.The crystal structure has been determined by X-ray diffraction.The crystal belongs to the monoclinic system,space group P2 1 /c with a=11.565(2),b=9.5616(19),c=10.221(2),β=111.75(3)°,Z=4,V=1049.8(4)3,D c=1.612 Mg/m 3,F(000)=520,μ(MoKa)=0.544 mm-1,R=0.0468 and wR=0.0922 for 1236 observed reflections (I > 2σ(I)).     

THE SYNTHESIS AND CRYSTAL STRUCTURE OF A NOVEL TETRANUCLEAR COPPER (Ⅰ) CLUSTER COMPLEX, Cu_4(α-C_(10)H_7CSS_2)_4·1/2CS_2

The title compound has been synthesized by the reaction of sodium α-dithionaphthoatewith CuCl_2 in an alkaline aqueous solution or by the reaction of α-dithionaphthoic acid withCuCl_2 in an organic solvent, The crude product was recrystallized in a mixture of CS_2 andC_2H_5OH. The crystals obtained are red and stable in air. The structure of the title compound is determined by a single-crystal X-ray diffractionanalysis. The crystal belongs to monoclinic space group C_(2h)~5- P(2_1/a) with unit cell parameters:a= 16.453(3)A, b=12.651(4)A, c=23.182(7)A, β=100.5(2)°, V=4744.6A~3,Z=4. Thestructure was refined to R=0.06 for 4707 reflections. In the molecule, Cu_4 cluster has a distorted tetrahedral configuration. Surrounding thistetrahydron are four α-perthionaphthoate ligands, coordinated to copper through the sulfuratoms. One of the sulfur atoms in each ligand forms sulfur bridge with copper atoms,while the other is coordinated to only one copper. The three Cu--S bonds formed by thethree sulfur atoms with a given copper atom are approximately coplanar. Each group--C--S_2 with Cu atom on a vertex of the tetetrahedron forms a five-member ring. Thesefive-member rings are also approximately cooplanar. The molecule possesses an approachingS_4 point symmetry. The mechanism for the formation of the title compound involves a redox reaction.which is discussed in this paper.