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 (μ-OXO)-BIS[BIS(DIETHYLDITHIOCARBAMATO)- OXO-MOLYBDENUM]

<正> INTRODUCTION. The reaction oF MoCl_3·3H_2O with dithiocarbamate in organic solvents is a interesting research area. Thus, several dinuclear and trinuclear molybdenum complexes have been synthesized The dinuclear oxo-dridged molybdenum compound was obtained by this reaction in acetonmethanol mixed solvent. The molecular configuration has been characterized     

CRYSTAL STRUCTURE OF BIS(μ-SULFIDO)-BIS[OXO-DIETHYL-DITHIOCARBAMATO-MOLYBDENUM(V)]

<正> INTRODUCTION. Reaction of MoCl_3·3H_2O with dithio-carbamate to synthesize dinuclear or trinuclear molybdenum complexes is an interesting topic. We have obtained sulfido-bridged molybdenum(V) complex Mo_2(μ-S)_2O_2(S_2CNEt_2)_2 by reacting MoCl_3·3H_2O with NadtcEt_2 in MeOH solvent. The molecular structure of the title compound was characterized by, X-ray structure determination. We report the result of the structure determination in this paper.     

DI-μ-CHLORO-BIS[l,2-BIS(DIPHENYLPHOSPHINO)-ETHANEPALLADIUM(II)]: SYNTHESIS AND CRYSTAL STRUCTURE

Abstract

On reacting 1,2-bis(diphenylphosphino)ethanedichloropalladium(II) with equimolar amount of silver perchlorate, a binuclear complex, di-μ-chloro-bis[1,2-bis(diphenylphosphino)ethane-palladium(II)] (1) is formed. The crystal structure of 1 has been solved. It crystallizes with two chloroform molecules. Chloro bridges are symmetrical and normal (Pd-Cl～2.414(3) Å). The immediate environment around palladium is slightly distorted square planar and the P-Pd-P angle is ～85°. IR bands at 290 and 270cm^?1 are observed for the chloro-bridged core of the complex.     

SYNTHESIS AND CRYSTAL STRUCTURE OF A ONE-DIMENSIONAL POLYMERIC CLUSTER[Mo(μ-S)_2Ag(μ-S)_2·α-MePyH]_n

Reaction of (NH_4)_2MoS_4 with AgI in α-MePy gives the title com-pound,an X-ray analysis of which shows that the molecule forms aone-dimensional polymeric chain with continuous metal-metal bonds.     

SYNTHESIS AND CRYSTAL STRUCTURE OF Mo_2OS(μ-S)_2[S_2CNC_4H_8]_2

Mo_2OS(μ-S)_2[S_2CNC_4H_8]_2, Mr=612.61, triclinic, PI, a=8.666(2)(?), b=17.366(6)(?), c=6.708(1)(?), α=98.29(2)°, β=97.27(2)°, γ=79.36(2)°, V=976.5(5)(?)~3, Z=2, Dc=2.03g/cm~3, MoKα(λ=0.71069(?)), μ=19.75cm~(-1), F(000)=588, Final R=0.064, Rw=0.073 for 1517 unique intensity data (I>3σ(I)). The binuclear unit of [Mo_2OS_3] has a new asymmetrically terminal coordinated configuration with Mo-Mo distance of 2.807(3)(?).     

THE CRYSTAL STRUCTURE OF BIS(TETRAETHYLAMMONIUM)(μ-OXO)BIS[TRIPHENYL-THIOLATO-IRON(Ⅲ)],(Et_4N)_2[Fe_2O(SPh)_6]

<正> Fe_2OSsN_2C_(52)H_(70),Mr=1043.23,monoclinic, P21/a, a=18.121(3), b=15.249(3), c=20.369(4)A,β=102.49(8)°,V=5495(1)A3, Z=4, Dc=1.261g.cm-3,MoKα(λ =0.710691), μ=17.816mm-1, F(000)=2208. R=0.073 for 4374 observed reflections with I≥3.0σ(I). The structure of the anion contains a linear Fe-O-Fe unit, with mean Fe-O distance of 1.766(2)A. The coordination geometry about each iron atom is close to tetrahedral with the angles O-Fe-S and S-Fe-S being 115.3° and 103.1°, respectively.     

CRYSTAL AND MOLECULAR STRUCTURE OF TETRACHLORO-BIS[BIS(2-ETHYLHEXYL)-SULFIDE]-PLATINUM(IV)

<正> C32H68Cl4S2Pt, Pt[(BEHS)2Cl4], Mr=853.9, space group P21/a, a =10.445(3), b=15.012(4), c = 13.506(5) A,β=101.43(3)°,V=2076(1) A3, Z=2, DC=1.37 g·cm-3, MoKa radiation, u= 39.3 cm-1, F(OOO) = 876 e, R = 0.053 for 1790 reflections. Pt(IV) is coordinated by four chloro atoms and two S atoms of BEHS, forming a somewhat distorted octahedron with Pt-S of 2.366 and Pt-Cl of 2.309A. The packing pattern of the long BEHS chain may allow the existence of conformational disorder.     

CRYSTAL STRUCTURE OF μ-[meso-1, 2-BIS(PHENYLSULFINYL)-ETHANE]-(O,O'''')-BIS[DIPHENYLTIN(Ⅳ) DICHLORIDE]

<正> The title complex is of triclinic system space group P1 with its cell parameters: a = 9. 386(1), b = 9. 412(2), c=11. 549(2)(?), α=97. 91(2), β = 81.70(1), γ= 102. 63(1)°, V= 979.2(?)3, Z = l, Mr = 966. 01, Dx =1. 638 gcm-3, μ(MoKα) = 16. 896cm-1, F (000) = 478, final R = 0. 033 and Rw = 0. 046 for 3424 reflections with I≥3σ(I). The two O atoms of the ligand are bonded to two Sn atoms to form a bridged binuclear species which lies on the crystallographic centre of symmetry situated at the centre of the ethylene C -C bond. The unique Sn atom exhibits a trigonalbipyramidal geometry.     

THE STRUCTURE OF BIS (TETRAETHYLAMMONIUM)(DICHLORODITHIOFERRATO- S,S')-DIOXOMOLYBDATE, (Et_4N)_2[Cl_2FeS_2MoO_2]

<正> (Et4N)2[Cl2FeS2MoO2], Mr = 579.3, monoclinic, P21, a = 13.531(2) b = 8.912(2), c = 11.095(2)A, β= 95.39(4)°, V r 1331.9(8)A3, Z = 2, DC =1.444 gcm-3, MoK , radiation, λ= 0.71069A, R = 0.065 for 1725 observed reflections. The complex anion (OaMoSzFeCl2)2- contains a cluster core (MoS2Fe) with the Mo-Fe distance of 2.859A.     

SYNTHESIS AND CRYSTAL STRUCTURE OF 3-(METHYLMER-CAPTO)PHENANTHRO[9,10-e] 1,2,4-TRIAZINE

<正> The title compound was synthesized by a new method and its crystal structure was determined by X-ray diffraction analysis. C16H11N3S, Mr = 277. 34, triclinic system, space group P1, cell parameters: a = 10. 410(4), b = 17. 953(5), c = 7. 468(3)(?), α=101. 47(3)°,β=110. 85(3)°, γ = 81. 53(3)°, V = 1273.8(8) (?)3, Z = 4 and Dc=1. 45gcm-3. Refinements of full-matrix least-squares converged at R = 0. 053 and Kw = 0.065 for 2794 observed reflections. There are two independent molecules in an asymmetric unit. All non-hydrogen atoms of phenanthro[9,10-e]-1,2,4-triazine make up a 18 18 large conjugated plane.     

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.     

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.     

STRUCTURE OF BIS(TETRAETHYLAMMONIUM)BIS[BIS(PHENYLTHIOLATO) (μ-SULFIDO)-IRON(Ⅲ)],(Et4N)2[Fe2S2(SC6H5)4]

<正> Mr= 873.02, orthorhombic P21212, a= 16.153(3), b= 15.718(2), c= 8.847(3) A, V= 2246.2(14)A3, Z=2, Dx? 1.291gcm-3, MoK(?), radiation, λ= 0.71069A, μ= 9.417mm-1, F(000)= 924, R(Rw)= 0.073(0.069) for 1936 observed reflections. The structure of the anion contains a FesSz core, in which each iron atom is coordinated by two μ2-S atoms and two thiolate sulfur atoms to form a distorted tetrahedron.     

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.     

CRYSTAL STRUCTURE OF BIS(TETRAETHYLAMMONIUM) BIS-[BIS(p-CHLOROPHEN- THIOLATO)(μ-SULFIDO) IRON(Ⅲ)], (Et4N)_2[Fe_2S_2(SC_6H_4Cl-p)_4]

<正> (Et_4N)_2[Fe_2S_2(SC_6H_4Cl-p)_4], Mr=939.89, F(000)=492, triclinic, P1,a=9.358(4), b=10.535(3), c=14.537(2)A,α=64.96(2),β=70.29(2),γ= 68.22(2)°, V=1177.8(13)A3, Z=1,Dc=1.325 gcm-3, MoKα ,λ=0.71069A. Final R= 0.061,Rw=0.076, for 1794 independent observed reflections. The anion contains a planar Fe2S2 core. Each iron atom is coordinated by two μ2-S atoms and two thiolate sulfur atoms to form the tetrahedral geometry. The structure of the cation has its positional disorder.     

CRYSTAL STRUCTURE OF [Et_4N]_2[Mo_2O_2(μ-S)_2(S_2)_2]

<正> [(C2H5)4N]2[Mo2o2S2(S2)2], Mr = 676. 74, monoclinic, P21/c, a = 13.510(2), b = 14.373(2), c=14. 777(3)(?), β = 97.53(2)°, V = 2844.7(9) (?)3, Z = 4, Dc= 1. 58g/cm3, μ(MoKα) = 13.0cm-1, F(000) = 1384, R =0. 033 for 1803 observed reflections. The structure contains discrete [Mo2O2S2(S2)2]2- anions and Et4N+ cations. The two oxygen atoms bonded to the Mo atoms are in cis-form with respect to the Mo2S2 bridging unit, with an average Mo- O distance of 1. 678 (?), The Mo…Mo distance is 2. 832(1)(?).     

CRYSTAL STRUCTURE OF (μ-PYRAZINE)-BIS[DIAQUA(IMINODIACETATO) COPPBR(Ⅱ)] DIHYDRATE

<正> PRELIMINARY INFORMATION. Recently multinuclear complexes with bridging ligand have been found possibly to possess special catalytical and special electric properties. Therefore more attention has been paid to such complexes. This study is a part of systimatic investigations on structures and properties of the kind of complexes, which have been carred out previously.