CRYSTAL STRUCTURE OF BIS(η~5-CYCLOPENTADIENYL-η~6-ISOPROPYLBENZENE-IRON(II)) DODECAHYDRO-DODECABORATE(C_(14)H_(17)Fe~+)_2·B_(12)H_(12)~(2-)

<正> Introduction. It is well known that both cyclopentadienyl-aromatic sandwich complexes of metal and boronhydrides have special and interesting Structures. Recently we have studied the structures of some of the compounds which simultaneously contain the two Structural units, i. e. sandwich and borane polyhedron (Chen and Pan, 1983, Fu and Pan, 1982, Zhang et al., 1982). The present work is a continuation of our previous studies.     

CRYSTAL STRUCTURE OF BIS (η~5-CYCLOPENTADIENYL)(1,3-PROPANEDIYL-BIS(DIPHENYL-PHOSPHINE)-P,P')NICKEL(II) DODECAHYDEO-DODECABORATE (C_5H_5Ni(C_6H_5)_2PC_3H_6P-(C_6H_5)_2)_2~ ·B_(12)H_(12)~(2-)

<正> Introduction. Tertiary diphosphine-cyclopentadienyl-nickel(Ⅱ) complexes were first synthesized by Sato (Sato, et al., 1971), and their boronhydrides were prepared by Zhang (Zhang, et al., 1983). Here we report the crystal structure of the title compound in Order to correlate the reactivity of this type of compounds with their structures and bondings.     

CRYSTAL STRUCTURE OF AgSCN·C_5H_5N

<正> INTRODUCTION. The structure of the title compound has been determined as a part of our systematic studies on the structural chemistry of silver. CRYSTAL DATA. The compound AgSCN'C_5H_5N crystallized from a pyridine     

FORMATION AND X-RAY CRYSTAL STRUCTURE OF MONOMERIC(η~5-C_5H_5)_2 LuCl·OC_4 H_8

The di(η~5-cyclopentadienyl)lutetium chloride was first prepared by Dubeck et al.in 1963.However,to our knowledge no report on its structrual information has beengiven up to date.The crystal structure of its four analogies which exist as chlorine-bri-     

CRYSTAL AND MOLECULAR STRUCTURE OF IPOHARDINE PICRATE, C_(15)H_(16)NO·C_6H_2N_3O_7

<正> INTRODUCTION. Ipomoea Hardwickii Hemsl (Ⅰ) belongs to Convolvulaceae, and its seed may be used as an anodyne. Ipoharine and Ipohardine were obtained by Reinickate method from the aqueous solution of Ⅰ. The structure of the title compound has been determined by X-ray crystal structure analysis. The structure of the cation (C_(15)H_(16)NO)~+ is reported here for the first time.     

CRYSTAL STRUCTURE OF FeaTe_2(CO)_6(NO)(η_5-C_5H_5)

<正> The title compound belongs to triclinic system, space group PI, with dimensions: a = 9.237(1), b = 9.589(1), c = 10.424(1) A ; <*= 72.09(2)?ft- 88.79(2)? 3r=80.28(l)? Z = 2, V = 865.5 A3, Dx = 2.626 gcnr3. Final R = 0.026 and Rw = 0.036 for 2531 reflections.     

SYNTHESIS of(η~5-C_9H_7)Ln(η~8-C_8H_8)·2THF AND CRYSTAL STRUCTURE OF(η~5-C_9H_7)Pr(η~8-C_8H_8)·2THF

The reaction of LnCl_3 with K _9H_7(C_9H_7=indenyl)andK_2C_8H_8(C_8H_8=cyclooctatetraene)in tetrahydrofuran(THF)give thecorresponding complexes(η~5-C_9H_7)Ln(η~8-C_8H_8)·2THF.The synthesis of(η~5-C_9H_7)Ln(η~8-C_8H_8)·2THF(Ln=Pr,Nd)and crystal structure of(η~5-C_9H_7)Pr(η~8-C_8H_8)·2THF are described.     

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     

MOLECULAR AND CRYSTAL STRUCTURE OF (η~6-BENZOPHENONE)TRICARBONYLCHROMIUM(0)

<正> The crystal of (η6-C6H5C(O)C6H5)Cr(CO)3 belongs to monoclinic system with space group P21/n. The cell parameters are: a=ll.068(2), b= 7.501(2), c=17.174(2) A, β=91.22(2)0, V=1425.4(8) A3, Z=4. The structure was solved by the analysis of 1745 observed reflections recorded on CAD-4 diffractometer. The final R=0.053.     

CRYSTAL AND MOLECULAR STRUCTURE OF ο-(2-CYANOETHYL)-BENZOYL FERROCENE OXIME, C_5H_5FeC_5H_4C(C_6H_5)NOC_2H_4CN

<正> INTRODUCTION. The derivatives of ferrocene are found to be increasingly used in the area of the catalysis of combustion reactions of high energy fuels and new material research. Therefore, more attention has been paid to these compounds. This work is a part of our systematic investigation on a     

THE FORMATION AND CRYSTAL STRUCTURE OF (η~5-C_5H_5)_3Nd·OC_4H_8 AND (η~5-C_5H_5)_3Pr·OC_4H_8

Under suitable reactant ratios without sublimation or reerystallization, single crystals of(η~5-C_5,H_5)_3 Ln-OC_4H_8(In = La, Pr, Nd) could be prepared by the reaction of cyclopentadienylsodium with respective lanthanide trichlorides in THF. Using low temperature technique wehave collected the X-ray data of single crystals of the title compounds at -60℃ under N_2and determined crystal structures. (η~5-C_5H_5)_3 Pr·OC_4H_8, [(η_5-C_5H_5)_3 Nd·OC_4H_8] recrystallizesin the monoclinic space group P2_1/n[P2_1/n] with unit cell parameters a = 8.406(3) [8.364(3)],b = 24. 510(9) [24.467(9)], c = 8. 284(3) [8.254(3)] A, β= 101.60(3) [101.42 (3)], D_c = 1. 62 [1.65]gem~(-3) for z = 4 [4]. Least-square refinement has led to a final R value of 0.056 [0.063],R_W = 0.049 [0.062]. The THF molecule is coordinated to the Pr [Nd] atom at a Pr-O [Nd-O]bond length of 2.16(1) [2.54(1)], A. The Pr-C (Cp) [Nd-C(Cp)] bond distances average 2.80(2) [2.78(2)] A. The title compounds are isostructaral with (η~5-C_5H_5)_3     

SYNTHESIS AND CRYSTAL STRUCTURE OF COMPLEX [Cu_2(CH_3COO)_4(C_8H_(11)NO)_2] · (C_6H_(11)NO)_2 · (C_8H_(12))

<正> SYNTHESIS AND CRYSTAL STRUCTURE OF COMPLEX [Cu_2(CH_3COO)_4(C_8H_(11)NO)_2] · (C_6H_(11)NO)_2 · (C_8H_(12)), where C6H11 = caprolactam, Mr = 900. 07, triclinic,space group P1, a = 11. 103(4), b= 11. 865(6), c=9. 912(3)(?), α=94. 85(4), β=115.20(2), γ=103. 25(4)°, V = 1125(2)(?)3, Z = l, Dx = 1. 33g. cm-3, λ(MoKa) = 0. 71069(?), T = 295K , μ = 10. 45cm-1, F(000) = 478, final R=0. 063 for 2098 observed reflections with I>3σ (I). The two Cu atoms in the molecule are held together by four carboxylate groups. Each Cu atom is bound in a square-pyramidal configuration to four carboxyl oxygen atoms and to the O atom of a caprolactam molecule.     

CRYSTAL STRUCTURE OF [PdCl_2 (DMAF)_2]·C_7H_8

<正> C33H42 Fe2PdCl2N2 (dichloro-bis (dimethylaminomethylferrocene) pal-ladium(Ⅰ) toluene solvate) ,Mr = 755. 72,monoclinic,P21/c,a=7. 521(1),b= 11. 128 (2),c=19. 260(7) A ,β=91. 77(2)°,V=1611. 1A3,Z=2,Dc = 1. 56g·cm-3,D0 = 1. 58g·cm-3,μ=76. 3cm-1, The least-squares refinement gave a final R value of 0. 062 for 2192 observed reflections. The Pd atom is of squareplanar coordination. The ferrocene ligand of in DMAF has an approximately eclipsed conformation.     

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.     

CRYSTAL STRUCTURE OF TETRAMETHLAMMONIUM BIS(TETRATHIOCYANATOVANADYL) MONOHYDRATE

<正> Preliminary informatiom. The title compound [(CH_3)_4N]_4[VO(NCS)_4VO(NCS)_4.H_2O] is a member of a series of vanadyl complexes, currently being investigated. It was prepared by the reaction of VOSO_4 with NH_4SCN in aqueous solution. Crystal data. (from single, crystal diffractometry, MoKα, λ=0.71073) M=945.16, orthogonal, a=23.252(6), b=13.015(2), c=30.621(6), space group Pcab, Z=8, D_m=1.32, D_c=1.34 g.cm~-3     

CRYSTAL STRUCTURE OF RhCl(dppm)_2·H_2O

<正> C50H46OP4ClRh, RhCl(dppm)2 · H2O, Mr = 922. 2, monoclinic, P21/2, a=10. 532(3), b=22.574(8), c=18. 641(8) A, β=93. 41(3)°, V = 4424 (3) A3, Z = 4, Dc=1. 386 g. cm-3, λ(MoKα) = 0. 71073A , F(000) = 1904. The structure was determined by direct methods and difference Fourier syntheses and refined by full-matrix least-squares to final R = 0. 037 and Rw = 0. 036 for 3432 (F> 6. 0σ(F) ) observed reflections. The structure of the title compound contains RhCl-(dppm)2 and non-coordinated H2O molecules. The rhodium atom is coordinated by one chlorine atom and four phosphorus atoms of two DPPM ligands forming a tetragonal pyramidal configuration.     

CRYSTAL STRUCTURE OF MOLYBDENUM-CARBENE COMPLEX (CO)_5Mo=C(OC_2H_5)C_6H_4-p-CH_3

<正> INTRODUCTION. Recently, researches on carbene metal complexes are very active, as they are of great importance in both theoretical study and catalytic activity. In a systematic research, the crystal structure of the title complex was analyzed and reported here to the advantage of understanding the catalytic action and searching for new and better carbene catalysts of novel kinds.     

THE CRYSTAL STRUCTURE AND SECOND-HARMONIC EFFECT OF COMPOUND C_9H_9N_3O_6· C_5H_5N

<正> The title compound (PAP) with excellent nonlinear optical prpper-ties has been synthesized. CHCHSCOO , monoclinic with space group P21, a = 4. 521(1), b = 9.601(6), c=17. 892(2)(?) , β=96. 12(1)°, V =772.8(?)3, Z = 2, Dc=1.44g · cm-3, F(000)-348, μ= 1.24cm-1. The second-harmonic intensities of PAP, MAP and NaAP HAP were measured,with the values which are 100, 50, 5. 0 times as large as that of KDP, respectively, Indicating that PAP is a new NLO crystal.     

STRUCTURE OF DIAQUA(DEMETHYLCANTHARATE)ZINC(II) Zn(C_8H_8O_5)·2H_20

<正> Mr=258.57, Monoclinic, P21/a, a=10.907(5), b=8.502(3) ,c=11.083(4) A, β=107.15(3)°, V=982.09A3, Z=4, Dx=1.729 Mgm-3, λ(MoKα)=0.71069A, μ=26.74 cm-1, F(000)=583.90, T=293K. The final R=0.0406 for 1587 unique observed reflections. The demethylcantharate ion acts as a tridentate ligand towards Zn(II) and a monodentate ligand towards another. The oxygen atoms in one carboxylate group bind with two different Zn(II) to form a chain-structure. There are four different types of oxygen coordinating with Zn(II).     

CRYSTAL AND MOLECULAR STRUCTURE OF IPOHARDINE CHLORIDE, C_(15)H_(16)NOCl

<正> INTRODUCTION. Ipohardine is an alkaloid which can be dissolved in water. It was obtained by Reineckate method from the aqueous solution of Ipomoea Hardwickii Hemsl. In the previous paper we have reported the crystal and molecular structure of Ipohardine Picrate. The structure determination of the title compound is described here. The structure analysis shows that the structure of the title compound is slightly different from the former.