STRUCTURE OF NOVEL DICOPPER(Ⅱ) COMPLEX Cu_2 (oxpn) (NCS)_2 (H_2O)(oxpn=N,N''''-bis(3-aminopropyl) oxamido)

<正> C10H10Cu2N6O4S2,Mr = 475. 41,monoclinic,space group P2/c,a = 8. 531 (2),b= 6. 870(1) ,c= 14. 463(2) A ,β=93. 84 (2), V= 845. 7 A3,Z=2,D = 1. 866 g·cm-3,μ=27. 799cm-1,F(000) = 484,R=0. 071. The molecules possesse basically a planar structure ,with the two aquamolecules displaced 2. 75 A to opposite sides of this plane and being at the apexpositions of the square pyramidal coordination of the two Cu atoms, respectively, the two carbonyls of the oxamide show the "trans-form".     

CRYSTAL AND MOLECULAR STRUCTURE OF AuCSC(NH_2)_2]_2CiO_4 CONTAINING TWO-COORDINATE COMPLEX CATION

<正> Au [SC(NH2)2]2C1O4, Mr,= 448. 66, orthorhombic, Pcca, α= 17. 873 (2),b = 8. 2933(7), c = 7. 196(2) A V=1066. 6A3,Z=4,DC = 2. 794g·cm-3,R= 0. 049,Rw=0. 068 for 807 observed reflections. The structure consists of complex cation Au[SC(NH2)2]2+ and perchlorate ion ClO4-. The gold atom( I ) in the cation has a slightly bent linear coordination geometry.     

STRUCTURE OF { CEu_2 (OOCCH_2NHCOCH_2NH_3)_4 (H_2O)_4]·(C1O_4)_6·4H_2O}_n

<正> {[Eu(OOCCH2NHCOCH2NH3)2(H2O)2]·(ClO4)3·2H2O}2,Mr = 1572,P21/n,a=12. 014(4),b=8. 910(5),c=22. 749(5)A ,β=91. 73(3)°,V = 2034 A3,Z=2,Dx=2. 15g·cm-3,λ(MoKa) = 0. 71073A,R=0. 060 for 3107 unique observed reflections (I≥3σ(I)). The complex cation is of one-dimensional chain structure in which the basic unit is a dinuclear complex and the gly-gly ligands are coordinated to metal atoms in two kinds of forms. The overall structure of the dinuclear unit is dioxo and dicarboxyl-bridged.     

Syntheses and Structures of Sil abridged Hafnocene Dichlorides

The present paper covers three silabridged hafnocene dichlorides(1, 2 and 3) prepared by sequential reactions of α, ω-dichloropermethyl polysilane with cyclopentadienyl sodium, n-butyl lithium and hafnium tetrachloride. Their structures were characterized by elemental analyses, UV, 1H(13C) NMR and MS. Furthermore the crystal and molecular structures of 1 and 2 were determined by X-ray diffraction method. The crystal of 1 is monoclinic, space group C2/c with a=1. 3401(4), b=0. 9977(3), c = 1. 0922(4) nm; β=94. 07(1)° V=3. 6342 nm3, Z = 2, Dc = 2.155 g·cm-3. The final deviation factor R = 0. 064. The crystal of 2 is monoclinic, space group P21/c with a=0.0847(1), b=1.5181(1), c=2.9824(2) nm; β= 94. 07(1)°? V=3.634 nm3; Dc= l. 805 g·cm-3. The final deviation factor R = 0. 033. The relationship between the silabridged structure and spectral properties is also discussed.     

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 AND CRYSTAL STRUCTURE OF La（NO3）3（16—C—5）

<正> The title complex LaC11H22O14N3 (Mr = 559. 27) crystallizes in the monoclinic space group P21/c with a=14. 452(7) ,b=8. 260(2),c= 16. 641(8) A ,β= 90. 85(4)°, Z = 4, V=1986. 2(1) A3,Dc=1. 87g·cm-3, F(000) = 1112,μ(MoKa) = 22. 7cm-1. The final refinement converged with R=0. 036 and Rw = 0. 038 for 2996 observed independent reflectios. The average La-O(crown) bond length of 2. 683 A (2. 660-2. 701A)is shorter than that in La(NO3)3(15-C-5)(2. 694A).The distances between opposite O atoms (3. 47~4. 68A) indicate that the cavity of 16-C-5 in the complex is elliptic.     

SYNTHESIS AND CRYSTAL STRUCTURE OF SODIUM ETHYLENEDIAME-TETRAACETATOVANADYL(IV) TETRAHYDRATE Na[VO(C_(10)H_(13)N_2O_8)]·4H_2O

<正> Mr=451,orthorhombic,P212121, a=6.524(2), b=13.910(2),c= 19.694(5)A,V=1787.4A3,Z=4,Dx=1.670 g·cm-3,MoKd,λ=0.71073A,μ=6.270 cm-1,F(000)=928, room temperature, final R=0.052 for 1643 unique reflections.The VO2+ ion is coordinated by three O and two N atoms of one ethylenediaminetetraacetate (EDTA) ligand, which acts in quinquedentate chelate fasion. The coordination geometry of V atom is roughly octahedral.     

CRYSTAL STRUCTURES OF Ln(o-HOC_6H_4CO_2)_3 (H_2O)_2·2H_2O [Ln =Tb,Ho]

<正> Ln(o-HOC6H4CO2)3(H2O)2·2H2O [Ln = Tb, Ho], Mr = 642. 32 (648. 33 )**,monoclinic, space group Cc,a=16. 280(4)(16. 217 (2)) ,b= 14. 889(3) (14. 877(2)),c = 9.867(1)(9. 835(2)) A,β=101.49(1)(101. 46(1))°,Z= 4,V= 2343. 8(7)(2325. 3(6)) A3,Dc=1. 8(1. 85)g·cm-3,μ=31. 6(36. 1)cm-1(MoKa), F(000) = 1272(1280).The final R=0. 031(0. 031),Rw = 0. 029(0. 031). There is no discrete molecules of the compounds in the crystal structures. The compounds are in linear polymeric arrangements, each metal ion is bridged to the next by two bridging carboxyl groups from salicylato ions.     

CRYSTAL AND MOLECULAR STRUCTURE OF (μ-PhS) (μ-σ,π-CH_3CH = CH)Fe_2(CO)_6

<正> The crystal and molecular structure of (μ-PhS) (μ-σ, n-CH3CH = CH)-Fe2(CO)6 has been determined by X - ray diffraction technique. The complex has chemical formula of C15H10O6SFe2 and Mr=129. 99. The crystals are monoclinic,space group P21/c,with α=11. 789(2),b= 7. 159(1),c = 20. 890(4) A ;β = 100. 89(2);V = 1731. 32 A3;Z=4,Dc=1. 65g·cm-3;F(000) = 863. 86. The final R and Rw equal 0. 0315 and 0. 0405 respectively for 2527 observed unique reflections.     

SYNTHESIS AND STRUCTURE OF (Et_4N)_2[Ni_2(OSC_5H_4)_2(μ-SC_6H_4OH)_2]

<正> The synthesis and structure of cluster compound(Et4N)2[Ni2-(OSC6H4)2(u-SC6H4OH)2] are reported. Mr = 876.54,space group P21/n, a = 9.179(4), b = 17.487(6), c = 12.840(4) A;B=92.87(3)°;V=2058.6(2)A3; Z = 2; DC = 1.182g·cm-3.     

CRYSTAL STRUCTURE OF A LINEAR TETRANUCLEAR Mo-Fe-S CLUSTER, (Et_4N)_4C(MoS_4)_2Fe_2S_2D·(CH_3OH)_2

<正> C_34H_88O_2N_4Mo_2Fe_2S_10, Mt= 1209. 25,monoclinic, P2_1/a,a= 17. 722 (7) ,b= 11. 857(5),c= 13. 743(5) A .β= 112. 29 (3)°, V= 2672. 0A3,Z = 2,Dc = 1. 503 g·cm-33,μ(Moka) = 14. 0 cm-1,T=193 K. Final R=0. 045 for 1943 observed reflections (I≥3σ(I)). In the anion [(MoS4)_2Fe2S2]4- ,the two Fe atoms, each attached with a chelating MoS42- unit, are bridged by two sulfur atoms. The metal atoms are arranged in a linear fashion with Mo-Fe-Fe angle of 179. 1(1)°, and Fe-Fe and Fe-Mo distances of 2. 746(2) and 2. 801(2) A, respectively. The long Fe-S distances (average 2. 246A) in Fe2S2 ring could be a result of the hydrogen-bonding interaction between the sulfur atom and the methanolic hydrogen atom.     

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 [Tm_4(p-NO_2C_6H_4CO_2)_(12)(H_2O)_(10)·2H_2O

<正> [Tm4 (p-NO2C6H4CO2)12 (H2O)10]·2H2O, Mr = 2885. 28, triclinic, space group P1 with a=14. 109(4) ,b= 14. 594(3) ,c= 13. 638(3) A ,α= 107. 04 (2), β=103. 36(2),γ= 93. 93(2)°, Z=1,V = 2584(1) A3.F(000) = l416,μ = 36. 4cm-1(Moka) ,Dc=1. 85g·cm3. The final R factor is 0. 034. The crystal structure is composed of tetrameric units in which four metal ions are bridged by carboxyl groups in chain form.     

BINUCLBAB COPPER(Ⅱ) COMPLEXES OF SOME PLANT GROWTH-STIMULATING SUBSTANCES.Ⅰ.SYNTHESIS AND STRUCTURE OF BIS(N,N-DIMETHYLFORMAMIDE)-TETHAKIS(μ-INDOLYL-3-ACETOXY) DICOPPER(Ⅱ)

<正> The structure of the title compound (Mr = 969.99) has been determined by X-ray analysis. The crystals are monoclinic, space group P21/n with a =14.746(2),b= 10.782(7), c = 15.531(3) A,β=113.74(2)°,Z=2,and DC=1.425g·cm-3. The final refinement converged with R = 0.067 and Hw=0.080 for 4491 observed reflections with I>3σ(I).     

CRYSTAL AND MOLECULAR STRUCTURE OF [K(C_(14)H_(20)O_5)_2]_2[Co(NCS)_4]

<正> The title complex (Mr= 1442.6) crystallizes in the monoclinic, space group PC, with a =14.515(7),b =15.773(5), c =16.287(11)51,β=95.13(5)°,Z=2,V=3713.8A3,Dc=1.29 g·cm-3. The structure was solved by Patterson method and the final R=0.068. The potassium atom in the cation lies between the two planes of the oxygen atoms from two benzo-15-crown-5 molecules.     

CRYSTAL STRUCTURE OF Fe4S4[SC（CH3）3]4[（C4H9）4N]2

<正> Fe_4S_4[SC(CH_3)_3]_4[(C1H_9)_2,Mr=1193. 23,tetragonal,142d,a = 23. 272(2), c= 13. 080(5) A ,V=7084(3) A3,Z=4,DC=1. 12g·cm-3,UUUU(MoKa) = 10. 8cm-1,F(000) = 2568,R=0. 058 for 1005 observed reflections. The cluster anion contains a cubane-type Fe4S4 core compressed along the 4 axis which is crystallographically imposed. Compared to other salts with different cations ,the core is subject to slight structural distortions in different crystalline environments and crystallographic symmetry of the anion is related to that of the cation.     

Synthesis, Crystal Structure and Luminescent Properties of [Zn（bipy）_2（H_2O）_4]·L·3H_2O

A novel coordination complex [Zn(bipy)2(H2O)4]·L·3H2O (1, bipy = 4,4'-bipyridine, LHNa = aniline-2,5-disulfonic acid monosodium salt) has been synthesized from LHNa by using hydrothermal method and structurally characterized. The result indicates that complex 1 belongs to the monoclinic system, space group P21/c with a = 20.392(3), b = 7.4052(12), c = 23.843(3) , β = 116.253(10)°, V = 3.2291(8) 3, Z = 4, Dc = 1.553 g·cm-3, μ = 0.962 mm-1, F(000) = 1568, and the final R = 0.0497 and wR = 0.1290. The complex 1 has a 0-D discrete structure, and generates an infinite 3-D network with the aid of O–H…O hydrogen bonds and π-π interactions.     

SYNTHESIS AND STRUCTURE OF CU8S[S2P（OC2H5）2]6

<正> Cu8C24H60O12P6S13,Mt= 1651. 73,trigonal,R3,a=b = c= 12. 667(4) A,α= β=γ=111. 42(1)°.V=1441(2)A3,Z=1,Dc=1. 903g·cm-3,λ(MoKa) = 0. 71073 A ,μ(MoKa) = 35. 671cm-1, F ( 000 ) = 830, 293K. Final R = 0. 066,Rw= 0. 077 for 850 unique intensity data (I≥3σ(I)). Each unit cell of the crystal comprises of a neutral molecule of formula Cu8S(dtp)6[dtp=S2P(OEt)2],wherein the eight copper atoms are arranged at the corners of regular cube,with each dtp ligand μ4-bridged to each face of the cube and a μ8-S in the center bonded to all the eight copper atoms. Each copper atom is coordinated by four sulfur atoms in a tetrahedral configuration. The bond lengths of Cu-(μ8-S) are in the range of 2. 627(2)-2. 543(2) A ,those of Cu-S(dtp)in the range of 2. 251-2. 280A.The adjacent Cu-Cu bond lengths (2. 950(5)-3. 070(2) A) show a weak interaction between the copper atoms     

CRYSTAL STRUCTURE OF A TRINUCLEAR COBALT COMPLEX Co_3(bdt)_3(PBu_3~n)_3 · ~2CH_2C1 (bdt = S_2C_6H_4~2- ) WITH MIXED o-BEN-ZENEDITHIOLATE AND TRIBUTYLPHOSPHINE LIGANDS

<正> Co3(S2C6H4)3{P(C4H9)3}3 ·2CH2Cl2, Mr = 1373. 45, mono-clinic, space group P21/c, a = 16. 110(5), b=36.313(10), c=13. 502(5) A , β= 105. 69(4)% V=7604. 4 A3, Z = 4, Dc = 1. 20 g. cm-3, μ=10. 03 cm-1, and F (000) = 2990. R(Rw) is 0. 086(0. 091) for 4559 observed unique reflections. The three cobalt atoms in the complex form an isosceles triangle with an average Co -Co bond distance of 2. 504(5) A. The average values of Co - S and Co - P bond distances are 2. 271(7) A , and 2. 198(8) A , respectively.     

STUDIES ON THE CRYSTAL STRUCTURE OF THIS(HYDROXYMETHYL)METHYLAMMONIUM SALT Ⅰ.THE CRYSTAL STRUCTURE OF THIS(HYDROXYMETHYL)METHYLAMMONIUM DIHYDROGEN PHOSPHATE(HOH2C)3CNH3H2PO4

<正> The crystal structure of tris(hydroxymethyl)methylammonium di-hydrogen phosphate(TAMP) has been determined by X-ray structural analysis.Mr = 219.13, nonoclinic, space group P21, a=8.179(l), b=6.170(2), c=9.576(5)A,β=106.32(3)°,DC= 1.57g·cm-3, Do = 1.56 g·cm3, Z = 2, MoKα radiation,λ=0.71073A, F(000)=232e,R=0.033,Rw=0.050 for 1102 reflections (I)3σ(I)).