SYNTHESIS AND STRUCTURE DETERMINATION OF POLYMERIC CHAIN COMPLEX OF NEODYMIUM(Ⅲ) NITRATE WITH N,N'-BIS-SALICYLIDENE-ETHYLENEDIAMINE(H2salen) AND DMSO,[Nd(H_2salen)(DMSO)(NO_3)_3]n

<正> NdC18H22N5O12S, Mr = 676.68, monoclinic, space group P21/n, a = 16.342(3), b = 16.630(2), c= 9.677(2) A,β=102.88(1)°,V=2563.6A3,Z =4, Dc= 1.75gcm-3,R=0.056. A polymeric chain complex of Nd(Ⅲ) with N,N'-bissalicylidene-ethylenediamine(H2salen) is described. Each H2salen molecule links two Nd(Ⅲ) ions through oxygen atoms of OH groups, while nitrogen atoms of C=N groups do not take part in coordination.     

SYNTHESIS AND CRTYSTAL STRUCTURE OF LUTETIUM (Ⅲ) COMPLEX WITH 1,3,5-BENZENETRICARBOXYLIC ACID

<正> LuC9H3O6(H2O)5·4H2O, Mr = 528. 3, monoclinic, C2/c, a = 14. 673(3), b=16.930(4), c= 14. 383(4)(?) , β=118.77(2)°, Z = 8, 7 = 3132(1) (?)3, Dc = 2. 24g/cm3, μ(MoKα) = 67.0cm-1, F(000) = 2064, R = 0. 052 for 4080 observed reflections. The Lutetium ion is eight-coordinated by three oxygen atoms, one from a 1, 3, 5,-benzenetricarboxylate ligands, two from another one, and five aqua ligands,forming a polymeric zigzag chain along the [101] direction. The Lu -O distances fall in the range of 2. 229 -2. 404(?).     

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 AND CRYSTAL STRUCTURE OF MgCl_2(CH_3COOC_2H_5)_2

The crystal of the title compound was prepared and its structure determined by X-ray diffraction method.1672 independent reflections were collected. The crystal is orthogonal with space group P2_12_12, and a=7.353(3),b=25.111(10), c=8.631(2), Z=8. The structure was solved by using Patterson method and modified with LSM program.The final R= 0.0795. The structural features of the title compound are:Mg(Ⅱ) is octahedral and ethyl acetate is located on trans-position.Mg atoms are connected by double chloro-bridge and form polychains.     

SYNTHESIS AND CRYSTAL STRUCTURE OF THE MACROCYCLOOCTAONE, C_(28)H_(40)O_8

<正> INTRODUCTION. Macrocyclic compounds have attracked a lot of chemistsbecause of their diverse physical and chemical properties. There was anidealized method to synthesis macrocyclo polyketones compounds. Product(Ⅱ)was obtained by condensation reactions of furan with acetone followed byOxidative opening of furan rings in (Ⅰ) . The 2,2,7,7,12,12,17,17-octamethylcycloeicosan-1,3,6,8,11,13,16,18-octaone(Ⅲ) was obtained byhydrogenation of (Ⅱ) with 20% Pd carried on carbon.     

SYNTHESIS OF DIAMMINEPLATINUM(Ⅱ)ASCORBATE AND STRUCTURE COMPARISON WITH ITS DACH DERIVATIVES

An antitumour complex,cis-diammineplatinum(Ⅱ)ascorbate,has beensynthesized and its X-ray structure is given.Quantum chemistry calculationcompared with its diaminecyclohexane derivatives indicates that they havedifferent electron distribution.     

THE SYNTHESIS AND CRYSTAL STRUCTURE OF CIS-BIS(1,10-PHENANTHROLINE)GLYCINECOBALT(Ⅲ)

A new coordination compound of cis-bis(1,10-phenanthroline)glycinecobalt(Ⅲ)chloridate tetrahydrate,cis-[Co(phen)_2gly]Cl_2.4H_2O,has been prepared by glycinereacted with cis-[Co(phen)_2Cl_2]Cl,then isolated by SP-Sephadex C-25 H~+ form column.The crystal and molecular structure of the new compound has been determined by RIGAKUAFC5R four circle diffractometer,5032 independent reflections were collected ofwhich 3781 observable reflections were used for structure refinement.The crystal ismonoclinic,space group C2/c,with a=35.13(1),b=9.637(3),c=17.485(6),β=115.08(Z)~,V=5362(3),Z=8.The structure was refined by full matrix least-squaresprocedure to a final R=0.041 and R_=0.060.The molecular formula was CoC_(28)H_(28)N_5O_8Cl_2.with molecular weight M_r=636.38,D_c=1.58g/cm~3,μ=8.88cm~(-1)and F_((000))=2624.     

SYNTHESIS AND STRUCTURE OF DIAQUO-μ-TRIETHYLENETE-TRA AMINOHEX A ACETATODI ANTIMONY ( Ⅲ) , C(H_2O)Sb(ttha)Sb-(H_2O)]

<正> C_18H_28N_4O_14Sb_2, MT = 767. 94, monoclinic, space group P2_1/c, a = 13. 847(2),b=6.866(2),c=13. 846(2) A,β=116. 46(1)°,V=1180. 3A3,Z=2,Dc = 2. 161g/cm3, F(000) = 756,μ(MoKa) = 23. 83cm-1. R and Rw were 0.054 and 0. 060, respectively, for 1357 observed reflections at room temperature. Each binuclear complexes arranged so that the centre of the carbon-carbon bond in the ethylenediamine group lies on a crystallographic centre of inversion. The ethylenediamine group forms a bridge between the two halves of the title molecule. Each antimony atom is ψ-heptacoordi-nated by a lone electron pair,one O atom from a water molecucle,one O atom from an ac-etato group and two amino N atoms at the equatorial plane as well as two O atoms from the acetato groups at the axial positions forming a pentagonal bipyramid.     

SYNTHESIS AND TAUTOMERISM OF KETENE N,O-ACETALS WITH BENZOXAZOLINE RING

Benzoxazoline ring substituted ketene N,O-acetals 3 were synthesizedby the reaction of ketene S,S-acetals 2 with 2-aminophenol.Thetautomeric equilibrium of some 3 was also observed.     

SYNTHESIS AND CRYSTAL STRUCTURE OF S-BENZYL-N-(FERRO-CENYL) METHYLIDENEDITHIOCARBAZATE

<正> C_19H_18N_2S_2Fe, Mt = 394. 33, monoclinic, P2_1/c,a = 7. 726 ( 7) , b = 11. 098(1 ),c= 21. 300(6) A ,β=100. 40(7)°,V= 1796. 2 A3,Z = 4,DC = 1. 458g·cm-3;MoKa,(λ=0. 71073A),μ=10. 635cm-1,F(000) = 816,room temperature,final R=0. 098,Rw=0. 121 for 3250 unique reflections,2306 reflections with I>3σ(I). The title compound is a new Schiff base which is made by condensation of formoylferrocene, FC-CHO and S-benzyldithiocarbazate. The mean Fe-C distance is 2. 04 A. The mean C-C distances in the cyclopentadienyl rings with and without side chain are 1. 43 and 1. 38 A,respectively. Electron migration from cyclopentadienyl ring to side chain is evident. A substantial Kekule-type distortion of the phenyl ring on the side chain is indicated.     

SYNTHESIS,CRYSTAL STRUCTURE AND MAGNETISM OF THE COMPLEX:GdFe(CN)_64H_2O

ＳＹＮＴＨＥＳＩＳ，ＣＲＹＳＴＡＬ　ＳＴＲＵＣＴＵＲＥ　ＡＮＤ　ＭＡＧＮＥＴＩＳＭ　ＯＦ　ＴＨＥ　ＣＯＭＰＬＥＸ：ＧｄＦｅ（ＣＮ）_６４Ｈ_２ＯＳＹＮＴＨＥＳＩＳ，ＣＲＹＳＴＡＬＳＴＲＵＣＴＵＲＥＡＮＤＭＡＧＮＥＴＩＳＭＯＦＴＨＥＣＯＭＰＬＥＸ：ＧｄＦ...     

SYNTHESIS, STRUCTURE AND ELECTRICAL PROPERTIES OF POLY(PHENYLENE VINYLENE) FILM DOPED WITH FERRIC CHLORIDE

Poly(phenylene vinylene) (PPV) film was synthesized via a soluble precursor poly-mer. Strong fluorescence at 500-600nm was observed in both precursor and PPV film.Room-temperature conductivity of PPV film doped with FeCl_3 depends on the eliminationtemperature, the concentration of FeCl_3 and doping time. The maximum conductivity ofdoped PPV at room-temperature can reach about 40 S·cm~(-1). The temperature depen-dence of conductivity was controlled by 1D-VRH (1 Dimension Variable Range Hopping)model with T_0 value of 3.9×10~3 K. Non-Ohmic conductivity resulting from Schottky effectwas observed and the value of converted voltage from Ohmic region into non-Ohmic regionat the current-voltage characteristic was found to be dependent upon the work function ofelectrodes.     

SYNTHESIS, STRUCTURE AND PROPERTIES OF INTERPENETRATING SULFONIC ACID RESINS WITH HIGH CAPACITY

Two series of interpenetrating sulfonic acid resins (ISAR), 10×n and n×10, were prepared by means of the wet method, and the physicochemical, thermodynamic and kinetic properties of the ISAR were measured. The results show: 10×n resins exhibit better properties than n×10 ones, mainly in higher apparent degree of crosslinking and larger conformational entropy effect, among which, 10×1 resin exhibits the best thermodynamic and kinetic properties. In the DTA graphs of n×10 resins, there are two T_g and two T_(ox), but in those of 10×n, only one T_g and one T_(ox). This result well supports the conclusion that 10×n resins have much better interpenetrating structural aspects.     

SYNTHESIS AND CRYSTAL STRUCTURE OF (β-PHENYL) CAR-BOXYLETHYLTRICHLOROGERMANIUM

<正> The crystal and molecular structure of the title compound was determined by single crystal X-ray diffraction. The complex crystallizes in the triclinic space group P1,a=8. 450(4),b=11. 730(3),c=14. 718(6)A ,α=104. 50(3),β=103. 71 (4),γ=69. 20(3)°,Z=4,V=1302. 4(9) A3,Dc,= 1.67g/cm3, λ(MoKa) = 0. 71069 A ,μ=30. 7/cm,F(000) = 646,Mr = 327. 6,final R=0. 037 for 2198 reflections with I<3σ(I). There are two molecules of different conformation in an asymmetric unit. Atom Ge is coordinated by three chlorine atoms and one carbon atom to form an irregular tetrahedron.     

THE SYNTHESIS AND CRYSTAL STRUCTURE OF B-(32) MODEL COMPOUND: 1-C_4H_9Co(salen)(Py)

The title complex i-C_4H_9Co(salen)(Py) (Py=pyridine. salen=dianion of disalicylideneethylenediamine) has been first synthesized. Its crystal structure has been determined by X-ray diffraction method. The crystsis are monoclinic with space group P2_1/ C. The unit cell parametes are presented. The structure has been refined to a final R of 0.038.     

SYNTHESIS OF N,N''''-DISUBSTITUTED MONOTHIOXAMIDE AND STUDY OF THEIR REACTIONS WITH DIAMINES

In this paper, six N,N'-disubstituted aonothioxamides were synthesized and the reactions between these monothioxamines and diamines (1,2-diamino ethane and 1,3-diamino propane) were studied. Some new compounds were synthesized by using these reactions.     

SYNTHESIS AND STRUCTURE OF A NEW TYPE OF COORDINATION COMPOUND OF Tb（Ⅲ）WITH BENZOIC ACID

<正> The synthesis and crystal structure of a novel rare earth coordination compound are reported. [TbL3(HL)H2O]2 (HL=henzoic acid) Mr=1324. 81, triclinic, space group P1, a=9. 148(1), b=11. 4 60(2), c=13. 506(2) A ;a=112. 76(1), B=91.83(1),y=91. 99(1) ;Z=1 ;V=1303. 3(4)A3;Dc=1.69g.cm-3;F(000)= 656;u=28. 4cm-1(MoKa). The final R is 0. 024. Each rare-earth ion in the title complex is nine-coordinated by seven oxygen atoms from five benzoate groups, one benzoic acid, and one aqua molecule, forming a distorted monocapped square antiprism.