CRYSTAL STRUCTURES OF 1,2-BENZO[2.2]PARACYCLOPHANE AND 1,2-BENZO[2.2]PARACYCLOPHANE-1,7-DIENE

<正> C20H16 (1) Mr = 256.34 and C20H14 (2), Mr = 254.32 are isomorphous, orthorhombic, P212121, Z = 4. For (?), ?a= 7.116(1), b =7.874(2), c = 24.564(4) A, V = 1376.4(3) A3, Dx = 1.237 g cm-3, μ(Mo-K α) =0.65 cm-1 , final R = 0.047 for 1152 observed reflections; for 2, a=6.963(2), b = 7.985(4), c = 24.315(8) A, V = 1351.9(8) A3, Dx = 1.250 g cm-3,μ(Mo-Kα) = 0.66 cm-1 , final R = 0.076 for 886 observed data. Structuralfeatures are similar to those of the parent [2.2]paracyclophane and related derivatives.     

CRYSTAL AND MOLECULAR STRUCTURE OF STEMOTININE

<正> C18H25NO5, Mr = 335.40, tetragonal, P41212, a = 15.578(4), c =14.723(3) A, V =3573(2) A3, Z = 8, D = 1.247 g cm-3, MoKα,λ= 0.71069 A, μ = 0.;85 cm-1, T = 293K, final R .= 0.100 and RW (on F2) = 0.080 for 1095 observed data [|FO| > 2σ(|FO|)]. The structure confirms the spectrbscopic assignment of a pentacyclic skeleton containing two α-methyl-γ-lactone rings, one ether and one tertiary amine.     

CRYSTAL AND MOLECULAR STRUCTURE OF BIS(2-ME-THOXYETHYL-CYCLOPENTADIENYL) ERBIUM CHLORIDE

<正> Complex Cp'2 ErCl(Cp'=2-methoxyethylcyelopentadienyl)(I)has been synthesized by the reaction of Cp' Na and ErCl3 in THF It crystallizes in space group Pnma with a=12.269(0),b=11.742(6),c=11.197(2)A,V=1613.1A3,Dc=1.849 g/cm3,Z=4,A=0.71073 A,μ(MoKa)=54.38 cm-1,F(000)=876,R=0.043,Rw=0.046.The Er atom is formally nine-coordinated with a pseudo-trigonal bipyramidal geometry with the "equatorial" plane composed of the Er atom,the Cl atom and the centers(1)and(2)of the two Cp rings(Cp=cy-clopentadienyl).The molecule is located at the crystallographic mirror plane through the atom C(3),C(4),C(S),Er,O(1)and C(6).The atom Cl and the atoms of Cp'(2)(except C(16)and C(16'))are disordered with an occupancy of 0.5 each.     

STUDIES ON CHEMICAL CONSTITUENTS OF CHINESE MARINE FOLK REMEDIES-ISOLATION AND X-RAY STRUCTURAL CHARACTERIZATION OF CYCLO-L-PROLYL-GLYCYL FROM DIODON NOVEMACULATUS (BLEEKER)

<正> Cyclo-L-prolyl-glycyl was isolated from Diodon novemaculatus (Bleeker) and characterised by X-ray diffraction analysis. C7H10N2O2, MW 154.17, space group P212121, a = 5.869(1), b = 9.674(2), c = 13.076(3) A,V = 742.4(2) A3, Z = 4, D = 1.379 g cm-3, μ(MoKα) = 0.96 cm-1, final R =0.034 and Rg = 0.047 for 939 observed data. Intermolecular N-H...0hydrogen bonds link the molecules into infinite zigzag chains parallel tothe b axis.     

CRYSTAL AND MOLECULAR STRUCTURE OF N—ETHYLPHENOTHIAZINE RADICAL CATION HEXACHLOROANTIMONATE EPT^＋SbCl6^—

<正> C14H13Cl6NSSb, Mr =561.8, Monoclinic, C2/c1 8=15,32(1), b= 11.72(1), c= 11.10(1)A,β=99.31(3)°,V=1969(1)A3,Dc=1,902g.cm-3, Z=4,CuKα,λ=1.5418A,μ=200.95cm-1.Room temperature, final R=0.051 for 1197 unique reflections with I>, 3.0σ(I).Pronounced defornation of the Molecular structure has been observed when the neutral N-ethylphenothia-zine is transformed into its radical cation. The structural features of the radical cation are compared with those of N-methyl analogue.     

RESEARCH ON CRYSTAL STRUCTURE AND OPTICAL PROPERTIES OF TRIHYDROXYL METHYL-AMINOMETHANE(TAM),H_2NC(CH_2OH)_3

<正> H2NC(CH2OH)3,Mr=121.14, orthorhombic, space group P21cn a= 7.786(2), b=8.785(1), c=8.835(1)A,V=604.4(3)A3, Do=1.326g.cm-3, Z=4. Dc= 1.331g.cm-3, F(000)=264e,λ(MoKα)=0.71073A, graphite monochromator, R= 0.049, Rw=0.057 for 651 observed reflections.     

SYNTHESIS AND STRUCTURE OF PERCHLORATOBIS-(2,2''''-BIPYRIDYL) COPPER (Ⅱ) PERCHLORATE

<正> C20H16Cl2CuN4O8,JMr = 574. 82,triclinic,space group PI,a =7. 397 (1),b=11. 172(3),c=15. 185(5)A,α=66. 28(2),β=76. 91(1),γ= 80. 74(2)°,V = 1115. 6A3,Z = 2,D=1. 71g·cm-3,μ=12. 76cm-1,F(000) = 582,R=0. 045,Rw = 0. 048. The Cu atom is coordinated by four N atoms from the two 2,2'-bipyridyls and two O atoms from two ClO4- groups,forming a distorted octahedron. A chain structure is developed through the coordinated ClO4-.     

CRYSTAL AND MOLECULAR STRUCTURE OF N-CYANOMETHYL PH-THALIMIDE AND N-CYANOMETHYL SUCCIMIDE

<正> Diethylaminoacetonitrile (1) reacts with phthalimide (2) or succirnide (3) to produce N-cyanomethyl phthalimide (4) C10H6O2N2 (Mr = 186. 168) or N-cyanomethyl succirnide (5) C6H6O2N2(Mr= 138. 128),respectively. Their molecular and crystal structures were determined by IR, 1H NMR, MS and X-ray diffraction analysis, compound (4) crystallizes in monoclinic space group P21/a(P21/c) ,with cell dimensions 0=8. 225(4) ,6= 10. 956(4),c= 10. 041(5) A .β=102. 43(4)°,V=883. 1A3, μ= 0. 90cm-1, F (000) = 384, Z = 4; compound (5) crystallizes in monoclinic space group P1,with a=8. 404(2),b = 9. 710(2),c= 10. 093(2) A ,α= 104. 73(2)°,β = 108. 55(2)°, γ= 112. 03(2)°,V= 655. 2 A3,μ= 1.0cm-1 ,F(000) = 288,Z= 4. The average inner angles of the five-membered ring of (4) and (5) are about 108°. The imide and the carbon atom of the methylene radical of N-cyanomethyl and phenyl ring are all in one plane . so the bonds are delocalized and the α-hydrogen atoms of N-cyanomethyl are activated. The syntheses and crysta     

CRYSTAL AND MOLECULAR STRUCTURE OF (CYANOETHYLOXY-FERROCENYL)-p-FLUOROPHENYL METHANE

<正> The crystal structure of (Cyanoethyloxy-ferrocenyl)-p-fluoro-phenyl methane (Fc-C(H)OCH2CH2CN, Mr=363.23) belongs to the monoclinic spacegroup P21/c with unit cell parameters: a =9.751(3), b =18.448(4), c =9.891(4)A,β= 105.71(3)°,V= 1712.7A3,Z=4,Dc=1.409g/cm3,μ=8.930cm-1,λ=0.71073A (MoKα),R=0.05. The structure and reactivities of the title compound are compared with those of its isomer.     

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. ,     

SYNTHESES AND CRYSTAL STRUCTURES, REACTION OF α -THIOPI-COLIN-o-TOLUIDIDE AND ITS ORGANOTIN COMPLEX

<正> α-thiopicolin-o-toluidide and its organotin complex have been synthesized, and both crystal structures have been determined by X-ray analysis. The ligand:C13 H12N2S,Mr = 228. 3,monoclinic,P21/n,a=16. 387(1),b = 7. 752(2),c=18. 334(1) A ,β=95. 52(1),V = 2324. 8A3,Z = 8,DC=1. 305g·cm-3,F(000) = 960e. The final R= 0. 053 for 3291 observed unique reflections. There are two molecules in the asymmetric unit,which are confirmed to exist as the keto,cis-N configuration in the solid state. The complex:C17H21N2SClSn,Mr = 439. 6,orthorhombic,P212121,a = 8. 801(3),b = 9. 188 (2),c=24. 087(6) A,V=1947. 9A3,Z = 4,DC=1. 499g·cm-3,F(000) = 880e. The final R = 0. 041 for 1694 observed unique reflections. The tin atom is surrounded by an irregular (5 + 1) coordination geometry with five normal bonds and one weak bond [Sn....C1]. The molecules join each other through the weak bonds to form infinite polymeric chains parallel to the a axis. In addition, the possible reaction mechanism in coordination is discussed.     

CRYSTAL AND MOLECULAR STRUCTURE OF N-CYANOMETHYI,BENZOIC SULFIMIDE

<正> C9HsN2O3S, Mr=222.218,monoclinic space group P21/n,B=12,584 (4).b =10.788(3), c= 15.124(4)A,β=106.83(2)°,V=1965.3A3,Dc= 0,75 g/cm3,Z=8,μ(MoKα)=1.5cm-1, F(OOO)=456(e),λ=0.7107A,R=0.067, Rw=0.059. Two Bolecules are in an asymmetric unit in the crystal. Structural analysis showed that all atoms of the two rings of benzoic sulfinide are in the sane plane which is normal to plane S(1)O(1)O(2). The C=N group is above the plane of the two rings.     

SYNTHESIS AND CRYSTAL STRUCTURE OF BaGa_4

<正> BaGa4,tetragonal space group I4/mmm with lattice parameters a=b=4.5650(8), c=10.786(2)A, V=224.77(7)A3,Dc=6.15 gcm-3,and Z=2,λ(MoKα)=0.71069A,μ=335.93cm-1,F(OOO) =360. The final R = 0.045, Rw=0.069.The distribution of valence electrons in crystal Ba6a4 is described and a suggestion that two different types of gallium atoms form covalent bonds by utilizing sp3 and dsp3 hybrid orbitals respectively is proposed.     

ISOLATION AND X-RAY STRUCTURE CHARACTERIZATION OF (+)-ONONITOL FROM CHINESE CAESALPINIA CRISTAL

<正> The compound (+)-Ononitol was isolated from Chinese Caesalpinia Cristal and identified by X-ray structure analysis to be 4-0-methyl-myo-inositol-hydrate. C7H1406·H2O,Mr=212.2, triclinic, space group Pl,a=5.074 (1), b = 6.599(1), c = 7.750(1)A,α=106.02(1),β=93.47(1),γ= 109.09(2)°,V = 232.5 A3,Z=1, Dc=1.516 gcm-3, u(MoKa)=1.28 cm-1, R=0.034 for 1431 observed reflections. There is no intramolecular hydrogen bond in (+)-Ononitol, but intermolecular hydrogen bonds exist between water molecule and hydroxy group as well as between hydroxy groups.     

METAL COMPLEXES OF POLYCYCLIC TERTIARY. AMINES. PART VIII. SYNTHESIS AND CRYSTAL STRUCTURE OF 1,4-DIAZABICYCLO[2.2.2]OCTANEPENTACARBONYLMOLYBDENUM(0), (CH_2)_6N_2·Mo(CO)_5

<正> C11H12N2MoO5, Mr = 348.17, orthorhombic, space group p212121,a= 7.048(1), b = 11.060(4), c = 18.039(7) A, V = 1406.2(8) A3, Z = 4, D x=1.645, Dm = 1.61 (flotation in aqueous KI) g cm-3 , graphite-monochromatizedMo-Kα,λ = 0.71069 A, μ = 9.25 cm-1, F(OOO) = 695.73, T = 295°K, final RF =0.035 and RwF2 = 0.051 for 1335 observed reflections with |F0| > 3σ(|F0|). The measured molecular dimensions.reflect the trans influence and steric bulk of the organic cage ligand.     

CRYSTAL AND MOLECULAR STRUCTURE OF 1，2，3，4—TETRAKIS（6‘,7’—DIMETHYL）BENZOXAZOLYL CYCLOBUTANE

<正> 1,2,3,4-Tetrakis(6',7'--dimethyl)benzoxazolyl cyclobutane was obtained by irradiation of E-l,2-bis(6',7'-dimethyl-1',3'-benzoxazolyly-2')-ethene in ethanol with a 450-watt high pressure mercury lamp. Its crystal and molecular structure has been determined by X-ray diffraction method. The crystal is triclinic, space group A with a = 7.008(2), b=9.586(1), c = 13.174(2)A,α= 104.08(1),β= 98.56(2),γ=99.97(2)°,V= 828.4A3, Mr= 636.76, (C40H36N4O4), Z =1, Dx =1.28g/cm3,μ= 0.78 cm-1 and F(OOO)=336.     

CRYSTAL AND MOLECULAR STRUCTURE OF cis-ISOMER OF 1-N-PROPYL-3-iso-PHOPYL-2-PHENYL-4-ETHOXY-4,5-DIOXO-2-THIO-1,3,2,4-DIAZADIPHOSPHOLANE

<正> PhP(S)N(C3H5-i)-PO(OEt)CON(C3H5) Mr=358.34, monoclinic, space group P21/c, a=8.654(3), b=15.390(2), c=15.235(3)A,β=101.48(2)°;Z=4, Dx=1.20g/cm3, λ(No Kα)=0.71069A,μ=3.24cm-1. The final refinement converged with R=0.047 and Rw=0.051 for 1326 observed independent reflections.     

SYNTHESIS AND MOLECULAR STRUCTURE OF METHYL 1—BENZYL—6—PHENYLPIPERIDIN—2—ONE—5—CARBOXYLATE

<正> C20H21NO3,Mr=323.39,monoclinic, space group P21, a= 7. 338(2), b=15. 419(3),c=7. 515(1)A,β=95.98(1)°,V= 845. 7(2)A3,Dm(flotation in aq. KL)=1.267,Dx(Z=2)=1.270gcm-3,λ(MoKα)=0.71069A,μ=0.08cm-1,F(000)=344,T=295°K,final RF=0. 042 for 1651 observed reflections. The title compound was synthesized and established as the trans isomer, with the phenyl and carbomethoxy substituents occupying pseudo-axial and axial positions, respectively, of the piperidin-2-one ring in a half-chair conformation.     

CRYSTAL STRUCTURE OF COMPLEX OF p-METHOXY-ARYLDIAZONIUM SALT WITH DTBENZO-24-CROWN-8

<正> Mr=448.5, monoclinic P21/c, a=8.531(3), B=12.076(4), C=33.309(13) A, β=95.41(1)°, V=3416.2(2) A3, Z=4, μ(MoKα)= 1.2 cm-1, F(000)=1408, room temperature, R=0.086, Rw=0.084 (W=1/(σ2(F) + 0.0001 x F2)) for 1759 independent reflections with I > 3σ(I).     

CRYSTAL AND MOLECULAR STRUCTURE OF(μ-PhCH_2S)(μ-CH_3C(0)CH_2S)Fe_2(CO)_6

<正> The crystal and molecular structures of (μ-PhCH2S)(μ-CH3C(O)CH2S)-Fe2(CO)6 have been determined by X-ray diffraction technique. The complex has chemical formula of C16H12O7S2Fe2 and Mr=492.08. The crystals are tri-clinic, space group P1,with a=8.461(5), b=10.937(5), c=ll.419(4)A,α=81.61 (3), β=78.21(4),γ=71.04(4)°,V=974.5A3, Dc=1.68 gcm-3,μ(MoKα)=17.3cm-1, Z=2,F(000)=495.93. The final R was 0.038 for 2874 independent reflections.