STRUCTURE AND CATALYTIC PROPERTIES OF (ACETYLACETONATO-κ2O,O′)BIS(TRI(2-FURYL)PHOSPHINE) PALLADIUM(II) TETRAFLUOROBORATE

Journal of Structural Chemistry - Reaction of Pd(acac)2 with BF3·OEt2 in the presence of tri(2-furyl)phosphine in toluene yields complex [Pd(acac)(TFP)2]BF4 (I) (TFP is tri(2-furyl)phosphine)...     

PREPARATION, PROPERTIES, AND MOLECULAR STRUCTURE OF trans-DICYANO BIS[BIS(DIPHENYLPHOSPHINO) METHANE]PALLADIUM (Ⅱ)

<正> The crystal structure of the title compound has been determined. PdC52H44N2P4, Mr = 927. 2, monoclinic, space group P21 /n, a =12. 102(2), b = 9.997(2), c=20. 254(5)(?),β=93. 80(2)°, V = 2445. 0(?)3, Z = 2, R =0. 075 and Rw = 0. 095 for 3535 observed reflections (I>3σ(I)), The palladium atom is located on the symmetric center and adopts a square planar coordination surroundings with two biphosphine ligands and two cyanide groups. The molecular structure in crystals is different from that in solution in which the molecule is very fluxional, probably due to the rapid alteration in coordination sites between the coordinated and uncoordinated phosphorus atoms of the biphosphine ligands. Their properties are also reported.     

STUDIES ON THE REACTION OF d-ACETAMIDCCINNAMAMIDE WITH TRIS(DIETHYLAMINO)PHOSPHINE

d-Acetamidocinnamamide do not react with P(OMe)_3, with P(NEt_2)_3 they give rise to 2-methyl-4-hydroxy-5-d-[bis(diethylamino)phosphoryl] benzyl imidazole.The pathway is studied for the formation of Ⅰ. The two intermediates(Ⅱ) are isolated.The structures of Ⅰ and Ⅱ are confirmed by IR, ~1H NMR, ~(31)P NMR, Ms.     

CRYSTAL AND MOLECULAR STRUCTURE OF BIS(O,O'-DICYCLOHEXYLDITHIOPHOSPHATO)-NICKEL(Ⅱ)

<正> Ni[(C6H11O)2PS2]2, Mr=627.39, Monoclinic, P21/n, a=11.802(7), b= 9.336(2), c=14.177(5) A,B=96.72(4)°,V=1551.3A3, Z=2, Dc=1.343g·cm-3, MoKα radiation λ=0.71073A, F(000)=648e, R=0.068 for 2642 reflections. Ni(Ⅱ) atom is surrounded by four sulfur atoms, forming a square.     

SYNTHESIS,CRYSTAL STRUCTURE AND PROPERTIES OF TETRAETHYLAMMONIUM BIS[BIS(2-OXYPHENYL)DISULFIDE-O,O'''',S]MANGANESE

The synthesis,crystal structure and properties of the firstMn(III)-disulfide complex(Et_4N)[Mn(mp-mp)_2]were reported with the Mn(III)ion in a S_2O_4 octahedron distorted due to Jahn-Teller effect.Spectroscopicdata revealed its paramagnetic properties.     

CRYSTAL STRUCTURE OF ADDUCT OF BIS(O,O''''-DIBUTYLDITHIOPHOSPHATO)-NICKEL (II) WITH BIPYRIDYL

<正> Ni[(C8H9O)2PS2]2 bipy, Mr=697.57, triclinic, Ci-Pl, a=9.469(1)A, b=14.638(3)A, c=14.637(2)A, α=69.64(1)° , β=71.16(1)°, r=89.99(1)°, V= 1785.6A3, Z=2, Dc=1.297g.cm-3, Mo kα radiation, λ=0.71073A, F(000)=736e, R=0.081 for 4986 independent reflections. Ni(II) is coordinated by four sulfur atoms and two nitrogen atoms to form a distorted octahedron. The angles between each two among planes N2Ni, NiS(11)S(12) and NiS(21)S(22) are nearly 90°.     

THE CRYSTAL STRUCTURE OF BIS(N-METHYLIMIDAZOL)- PALLADIUM OXALATE MONOHYDRATE

<正> INTRODUCTION. In recent years, Zhang Liangfu et al. were successful in using complexes composed of chelate ligand of diphosphine, dinitrogen and transition metal elements of lower valence multi-electrons to activate C-H bond. Recently, we synthesized complexes of bis(N-methylimidazol) ligand with palladium(Ⅱ) or platinum(Ⅱ) oxalate. These compounds activate also     

CHARACTERIZATION AND CATALYTIC BEHAVIOR OF WATER-SOLUBLE PHOSPHINE RHODIUM (I) COMPLEX

IntroductionInhomogcncouscatal}-sis*arccurrentproblcmisthcseparationofthcorganicproductsfromtheactivecatal}'stThcapplicationoft`atersolubletransitionmctalcomplcxcsf0rcataI}ticrcactionshasrcccntl}'attractcdconsidcrablcattcntio.lI~3l.Thcx"atcr-solubleligandsarcslightl}'solublcinorganicmcdia-allot"ingthccatal}'sistobccarricdoutinat\"o-phascs}'stcm.Catal\'strccovcry'isthuscasil}'achievcdb}'dccantationandseparationofthctx"ophascs.Thctris(sodiumm-sulfophcn}-l)-phosphinc,P(m-C6fuS03Na)3(abbr.asTP…     

CATALYTIC PROPERTIES AND SURFACE STRUCTURE OF MgO PREPARED FROM VARIOUS PRECURSORS

ＣＡＴＡＬＹＴＩＣＰＲＯＰＥＲＴＩＥＳＡＮＤＳＵＲＦＡＣＥＳＴＲＵＣＴＵＲＥＯＦＭｇＯＰＲＥＰＡＲＥＤＦＲＯＭＶＡＲＩＯＵＳＰＲＥＣＵＲＳＯＲＳ￥ＪｉａｎＷｅｎＤＡａｎｄＳｈｉＫｏｎｇＳＨＥＮ（ＳｔａｔｅＫｅｙＬａｂｏｒａｔｏｒｙｏｆＯｘｏＳｙｎｔｈ...     

THE STRUCTURE OF TETRABUTYLAMMONIUM BIS(1,3-DITHIO-2-THION-CYCLOPENTENE-4, 5-DITHIOLATE)PALLADIUM(Ⅱ)

<正> Mr=984.05 monoclinic P21/c a=8.474(1),b=14.768(3), c=19.494(3) A,6=96.42(1)0, V=2424.5(7)A3, Z=2, (Mokα)=8.Hem-1, F(000)=1039.91, room temperature. The final R=0.0357 for 2696 independant reflections. The Pd(C3S5)22-ion is nearly planar and the Palladium(Ⅱ)-sulfur coordination polyhedron is square planar with Pd-S distances of 2.315A and 2.311A.     

SYNTHESIS AND PROPERTIES OF POLYMERIC BIS (ETHYLENEDITHIO)-TETRATHIAFULVALENES

A polymer containing bis(ethylenedithio)-tetrathiafulvalene moiety wassynthesized and its electrochemical properties were studied by cyclic voltammetry. Thecharge transfer complexes of the polymer with TCNQ and I_2 were obtained by chemicaloxidation in dichlorobenzene. All of them are semi-conductors. A film of the polymer wasobtained by casting. Its conductivity, after oxidation with iodine, is 2.24×10~(-6)S·cm~(-1)and its conducting state is stable in air.     

MOLECULAR RECOGNITION OF AN ORGANIC MOLECULE BY BIS(TETRAFLUOROBORATE)ZINC(II). SYNTHESIS AND CRYSTAL STRUCTURE OF {[Zn(phen)3](BF4)2}2·MNA·(H2O)1.5

Abstract

The 2:1 adduct {[Zn(phen)₃](BF₄)₂}₂·MNA·(H₂O)_1.5 (1) (where phen = 1,10-phenanthroline and MNA = 2-methyl-4-nitrobenzenamine) was prepared by self-assembly and characterized by X-ray crystallography. The central zinc atom in two non-equivalent [Zn(phen)₃]²⁺ cations exhibits distorted octahedral geometry with Zn-N bond distances of 2.151(6)-2.194(6) Å and 2.136(6)-2.210(6) Å, respectively. The 2-methyl-4-nitrobenzenamine molecule is connected with bis(tetrafluoroborate)tris(1,10-phenanthroline)zinc(II) through a hydrogen bond (N13-H13a…F23? 3.044 Å, ?1 - x, 1 - y, - z). High shape specificity was observed in the recognition process.     

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

<正> Preliminary information. The vanadyl complexes are found to be increasingly used in the areas of catalysis, new materials research as well as in bio chemistry. Therefore, more attentions have been paid to such compounds. The title complex K_2[VO(C_2H_3O-3)_2(C_2H_2O_3)] H_2O has been prepared by reaction of VOSO_4 with hydroxyacetic acid in aqueous solution, with KOH added to a suitable PH value.     

STRUCTURE AND THERMAL MECHANICAL PROPERTIES OF ORIENTED POLYIMIDE (PEI-E)

The strain induced crystallization behaviour in polyimide from 1,4-bis (3', 4'- dicarboxyphenoxy)benzene and 4,4'-oxydianiline (PEI-E)has been investigated by WAXD, DSC and FTIR. The results obtained show that crystallization in PEI-E did take place just after tensile yielding. Meanwhile, the effect of strain induced crystallization on the thermomechanical properties was studied by DMA and TMA, the results of which indicate that the crystallization and hot stretching have a certain influence on the dynamic mechanical properties, such as weakening the βrelaxation and decreasing the glass transition temperature. The TMA results confirm the shifting of glass transition temperature to lower temperature region after hot stretching. This phenomenon could be well explained by the effect of residual stress according to Eyring's theory.     

CRYSTAL AND MOLECULAR STRUCTURE OF TRIS (HYDROX-YMETHYL) AMINOM ETHANE ARSENATE (THAMAS)

<正> (CH2OH)3CNH3H2AsO4, M, = 263. 08, monoclinic, space group P21, with a = 8. 232(2), b = 6. 180(2), c=9. 856(3)(?) , β=104. 77(2)°, Z = 2, V = 484. 81(?)3, Dc= 1. 80 g/cm3, MoKα radiation, μ = 35. 02cm-1, F(000) = 268. The final R and Rw are 0. 040 and 0. 037, respectively. The molecule of THAMAS is composed of TAMH+ and H2AsO4- which are held together by a hydrogen bond. Adjacent molecules in THAMAS crystals are connected by intermolecular hydrogen bonds.     

CRYSTAL STRUCTURE OF TRIS(DIBENZYI SULPHOXIDE)-METHANOL-TRINITRATOLANTHANUM

<正> INTRODUCTION. The complexes of rare-earth metal with sulphoxides are a class of compounds that possess properties of extraction, catalysis and luminescence. It would be condutive to understanding the relationship between structure an4 property to clarify the influenece of lanthanide contraction and sulphoxide ligands with differe(?) substitution groups upon coordination geometry and neighbouring environment of rare-earth ion. We are carrying out systematic investigations of lanthanide complexes with dibenzyl sulphoxide(DBSO). The structure of La(NO_3)_3·(DBSO)3·CH_3OH reported herein is a part of our studies.     

CRYSTALLOGRAPHIC STRUCTURE AND MAGNETIC PROPERTIES OF R_(2)Fe_(17)N_(2.4)

By a proper thermal treatment, the nitrogen atoms can enter the R2Fe17 structure. The crystallographic and intrinsic magnetic properties as well as their relationship have been studied by magnetic measurements, X-ray and neutron diffraction techniques. The neutron data indicate that the nitrogen atoms occupy the interstitial sites in the Th2Zn17-type rhom-bohedral structure. The inserting nitrogen atoms are found to dilate the cell volume, increase the Curie temperature and enhance the saturation moment by raising the difference in the electron number between the spin-up and spin-down 3d subbands of the Fe atoms. Furthermore, the nitrogen atoms have an important effect on the magnetocrystallic anisotropy, which results in an easy axis with Sm2Fe17N2.4. All these make Sm2Fe17N2.4 favorable for permanent magnet applications.     

CRYSTAL STRUCTURE AND NLO PROPERTIES OF 4,4'''' -DIAMIN-ODIPHENYLSULFONE (DAPS)

<正> 4, 4'-Diaminodiphenylsulfone (DAPS) (NH2C6H4)2SO2, Mr= 248. 3, orthorhombic, space group P212121, a = 8. 057(2), b = 25. 554(6), c = 5. 759(2)(?), V = 1185. 7(6)(?)3, Z = 4, Dc=1. 39g/cm, λ(MoKa) = 0. 71069(?) , μ= 2. 51cm-1, F (000) = 520, T = 296K, R = 0. 044 for 1022 observed reflections (I >3σ(I)). In the crystal there is one intermolecular hydrogen bond O(2)a…H(10)b- N(1)b between molecule (a) and (b), with Oa…Nbdistance of 2. 86(?) and Oa…Hb- N(1)b angle of 161. 7°, which is formed between the - NH2 group of molecule (b) and the atom. O(2) of the molecule (a). A large dihefral angle (78. 31°) exists between the two phenyl planes. Its SHG efficiency of crystalline powders is about 2. 5×KDP and the cut-off wavelength is 335nm in 0. 1mM ethanol solution.     

CRYSTAL AND MOLECULAR STRUCTURE OF THE ADDUCT OF BIS (1,1,1 TRIFLUORO 3-2-2'''' THENOYLACETONATO) COPPER (II) WITH PYRIDINE

<正> Mr=666.12, triclinic, Pl, a=8.868(1), b=9.719(2), c=10.861(1) A,α=58.23(1)°, β =64.06(1)° r =71.63(1)°; V =711.2 A3; 2=1, Dc=1.555 g.cm-3,for 3724 reflections with I≥ 3σ(I). In the title compound, the copper atomhas a distorted octahedral coordination with four Cu-O long bonds and twoCu-N short bonds. ,     

STUDIES ON ORGANOMETALLIC COMPOUNDS OF TITANIUM,ZIRCONIUM AND HAFNIUM——THE SYNTHESES AND PROPERTIES OF BIS (CYCLOPENTADIENYL) AND BIS (METHYLCYCLOPENTADIENYL) DI(ARYL)-METAL DERIVATIVES

Aryllithium reacts with Cp_2MCl_2 and Cp'_2 MCl_2 (C_p=η~5-C_5H_5, C_P′=η~5-CH_3C_5H_4:M=Ti, Zr, Hf) respectively to prepare a series of new bis (cyclopentadienyl), bis (methy-lcyclopentadienyl) diaryl derivatives of titanium, zirconium and hafnium. The hydrolysicreaction of these organometallic compounds are studied, the derivatives of zirconium andhafnium can be easily hydrolyzed with the exception of that of titanium. They react withhydrogen chloride, acetyl chloride, bromine and haloacids to form the respective bis(cyclo-pentadionyl) dihalides of these metals. The NMR and IR spectra were discussed in regardto the structure of (η~5--CH_3C_5H_4)_2 MAr_2 and (η~5--CH_3C_5H_4)_2 MX_2.