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.     

STRUCTURAL CHEMISTRY STUDIES ON THE COMPLEXES OF INDIUM CHLORIDE AND BIDENTATE HETEROCYCLIC AMINE LIGANDS 1.COMPLEX OF INDIUM CHLORIDE WITH 1,10-PHENANTHROLINE AND DIMETHYL SULFOXIDE

<正> InC12H8N2(CH3)2SOCl3, Mr=477.5, Triclinic, P1, a=7.640(1), b=9.907(2), c=12.250(2)A,α=94.26(2),β=96.61(1),γ=105.19(2), V=883.6A3,Z=2, Dc=1.795g·cm-3.μ(MoKα)=18.9cm-1, 293K. The structure was solved by heavy-atom method and refined to R=0.028 for 3026 observed reflections with I>3α(I).     

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.     

THE CRYSTAL STRUCTURES OF ALKALOIDS FROM KOPSIA OFFICINALIS

<正> Kopsamine(I): Mr=456.50, orthorhombic, P212121, a=ll.245(3), b=12.547(2), c=15.043(3)A, Z=4, Dc=1.429g.cm-3, V=2122.5A3, final R=0.041 for 2008 observed reflections.N-carbomethoxy-11-methoxy-12-hydroxy-kopsinaline(Ⅱ): Mr=458.52, mono-clinic, P21,a=8.424(2), b=13.037(1), c=9.883(1)A,β=90.14(2)°, Z=2, Dc= 1.403g·cm-3, V=1085.4 A3, final R=0.039 for 1687 observed reflections.In the structures: The rings A,B and E(I) take envelop conformations. The ring C takes chair conformation and the ring D boat conformation. There are intramolecular hydrogen bonds 0(5)-HO(5)...0(1) both in molecule(I) and molecule(Ⅱ), which formed the distorted seven-membered ring with atoms C(22), N(1), C(2), and C(18).     

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.     

CRYSTAL STRUCTUER OF DEHYDRODICENTRINE

<正> C20H19O4N,Mr= 337. 38,monoclinic,P21/n,a= 16. 567(3),b= 6. 353 (13),c=15. 085(4)A,B=93. 74(2)0,V=1584. 1(7) A3,Z=4,Z)c= 1. 415g.cm-3,F (000) = 712, (MoKa) = 0. 71073A ,u=0. 92cm-1,R=0. 058(Ru= 0. 056) for 2643 observed reflections with I>3a(I). The molecular skeleton is a large conjugated plane.     

STRUCTURE OF CHLORO [2-2''''-PYRIDYL)-6-MSTHYLBEHZOTHIAZOLE] PYROCATECHOLATOANTIMONY(Ⅲ)

<正> C19H14N2O2ClSSb,Mr = 491.6, space group P1, a = 5.977(1), b= 8.708(1), c = 8.962(1) X, a=93.91(1),B= 103.25(1),r=94.80(1), V = 450.6 A3, Z = 1, Do = 1.79, DC = 1.812 g.cm-3,F(000) = 242,u(MoKa)= 18.1 cm-1,R=0.024 for 2903 reflections. The Sb atom is situated in a distorted square- pyramidal ( octahedral) environment, with Sb-Cl 2.546(2), Sb-0 2.004(2)/2.038(3), and Sb-N 2.442(3)/2.526(3)A.     

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 AND MOLECULAR STRUCTURE OF 2-PHBNYLQUINOXALINE

<正> C14H10N2,Mr =206.24, space group P21/n, a =5.861(3), b =10.230 (5), c =17.440(11) A,β=92.07(5)°,V= 1045(1) A3,Z=4, Dx=1.31 g.cm-3, MoKa radiation,u=0.73 cm-1,F(000)=432,R=0.063 for 1054 observed reflections. 2-Phenylquinoxaline molecule is approximately planar. The dihedral angle between the quinoxaline ring and the substituted phenyl ring is 7.0°. The C-C bond distance connecting these two rings is 1.495(4) A. The whole molecule is a conjugation system.     

STUDIES ON THE MOLECULAR STRUCTURE OF WT-12 DERIVATIVE OF PYRAZOLO [3,4-d] - 1,3,2-DIAZAPHOSPHORIN-6-ONE

<正> The title compound was obtained by reaction of 1-phenyl-5-benzy-lamino-pyrazole-4-(N-methyl) carboxamide with p-fluorophenyl phosphorus dichloride and its molecular structure determined by X-ray diffraction method. The crystal is mono-clinic,space group P21/c,with a=11. 874(2),b= 12. 986(2),c=14. 587(2) A ,β= 106. 21(1)°,V=2159. 6A3,Mr = 430. 43(C24H20N4OFP),Z=4, Dx = 1. 324g/cm-3,μ(MoKa) = 1. 53cm-1 ,and F(000) = 896. The atoms in the pyrazolo[3,4-d] - 1,3,2-di-azaphosphorin-6-one are coplanar except the P atom.     

CRYSTAL AND MOLECULAR STRUCTURE OF HUMOSINE A

<正> The structure of humosine A, C20H19NO5, which represents a new kind of phthalide isoquinoline alkaloid,has been determined by X-ray diffraction analysis. The compound crystallized in the space group P212121 with a=7.654(2), b=12.926(2), c= 17.018(8) A, Z=4, V=1681.7A3, Dx=1.459g.cm-3, μ(Moke(?))=1.014 cm-1, F(000)=776. The structure was solved by direct methods, and refined by full-matrix least-squares with final R = 0.032 for 1517 observed reflections (I≥3σ).     

THE STRUCTURE OF YUEHCHUKENE: A NOVEL BIS-INDOLE ALKALOID FROM MURRAYA PANICULATA (L.) JACK

<正> The structure of yuehchukene, a new bis-indole alkaloid isolated from the root of Murraya paniculata (L.) Jack, has been determined by an X-ray crystallographic analysis of its mono-N-acetylated derivative. C28H28N2O,FW = 408.54, monoclinic, space group P21/n, a/3 = 8.032(2), b = 19.712(8), c =14.460(7) A, β = 101.22(2)°, U = 2245.7(9) A, Dm (flotation in KI/H2O) =1.20 g cm-3 , Z = 4, Dc = 1.208 g cm-3, F(OOO) = 871.86, μ(Mo-Ka) =0.68 cm-1 ,final R =0.079 and Rg = 0.084 for 1523 observed data.     

CRYSTAL AND MOLECULAR STRUCTURE OF NATURAL PRODUCT TOXOCAHOL

<正> Toxocarol C6H12O4 is a separated product from the plant of Toxocarpus (himalensis Falc. ex Hook. f.). It crystallizes in orthorhombic, the space group D2h-Pnca with a= 10.129(2), b= 11.297(3), c= 11.814(3)A, V=1351.9 A3, Z=8, Dc= 1.46 g.cm-3; m.p= 150.5°-151.5℃,μ(Mo)=1.3 cm-1. The result of structure analysis shows that the compound is a chair cyclohexan-tetrol .There is a complex net of hydrogen bonds in the crystal.     

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.     

含羧基的三核钨原子簇化合物的研究——Ⅰ.(Me_4N)[W_3(μ_3-O)(μ-Cl)_3(μ-HCOO)_3Cl_3]的合成和分子结构

用两种方法合成了标题化合物。晶体属正交晶系,空间群为Pnma,a=12.043(1),b=11.521(1),c=14.137(2)(?),V=1961.6(?)~3,Z=4,D_c=3.35g·cm~(-3),M=989.47,F(000)=1776,μ=194.06cm~(-1)。最终的R因子为0.064。簇阴离子的簇骼为W_3OCl_3,这是一个缺顶点的类立方烷构型。     

METAL COMPLEXES OF POLYCYCLIC TERTIARY AMINES. PART VI. PREPARATION AND CRYSTAL STRUCTURE OF HEXAMETHYLENETETRAMINE-SILVER(I) BROMIDE (1/4)

<正> C6H12N4Br4Ag4,Mr = 891.31, orthorhombic, Pnma, a = 8.778(2),b = 9.80.5(2), c = 16.906(3) A, V = 1455.1(4) A3, Z = 4, Dx = 4.069, Dm (displacement of H2O) = 4.03 g cm-3 , A(Mo-Ka) = 161.3 cm-1 , F(OOO) = 1615.77,T = 295°, final R = 0.052 arid Rw = 0.062 for 1472 observed reflections.All four lone pairs of each (CH2)6N4 molecule serve as ligand sites in a polymeric framework comprising octahedral AgBr5N, tetrahedral AgBr3N, and tetragonal pyramidal AgBr4N coordination polyhedra. The Ag-N and Ag-Br bond lengths lie in the ranges 2.366(12)-2.454(12) and 2.640(2)-3.178(2) A, respectively.     

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-.     

STRUCTURAL STUDIES OF DICHLORO-(4,7-DIPHENYLPHENANTHBOLINE)DIBUTYLTIN(Ⅳ) ETHANOL SOLVATE,[SnBu_2Cl_2(DPphen)]·C_2H_5OH

<正> C34H40N2OCl2Sn,Mr=682.3, triclinic, P1, a = 10.082(1),b= 10.932(1), c=15.666(2) A,α= 79.85(1),β=84.19(1),γ=84.92(1)°;V =1686.5 A3,Z = 2,Dc = 1.344 g.cm-3,μ(MoKα) = 9.5 cm-1, T=294(1)K. The coordination of tin is essentially octahedral, with the nitrogen atoms from bidentate ligand DPphen and cis-chlorine atoms lying in the equatorial plane and the two carbon atoms from trans-butyl groups in the axial positions. The average Sn-N distance of 2.39A happens to be in the shortest limit for this kind of complexes exhibiting antitumor activity.     

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. ,     

Structure and properties of dinuclear manganese(III) complexes with pentaanionic pentadentate ligands including alkoxo, amido, and phenoxo donors

Doubly bridged mu-alkoxo-mu-X (X = pyrazolato or acetato) dinuclear MnIII complexes of 2-hydroxy-N-{2-hydroxy-3-[(2-hydroxybenzoyl)amino]propyl}benzamide) (H5L1) and 2-hydroxy-N-{2-hydroxy-4-[(2-hydroxybenzoyl)amino]butyl}benzamide (H5L2), [Mn2(L)(pz)(MeOH)4].xMeOH (1, L = L1, x = 0.5; 2, L = L2, x = 0; Hpz = pyrazole) and [Mn2(L1)(OAc)(MeOH)4] (3), have been prepared, and their structure and magnetic properties have been studied. The X-ray diffraction analysis of 1 (C24.5H34Mn2N4O9.5, triclinic, P, a = 12.2050(7) A, b = 12.7360(8) A, c = 19.2780(10) A, alpha = 99.735(5) degrees , beta = 96.003(4) degrees , gamma = 101.221(5) degrees , V = 2867.6(3) A3, Z = 4), 2 (C25H34Mn2N4O9, triclinic, P, a = 9.4560(5) A, b = 11.0112(5) A, c = 13.8831(6) A, alpha = 90.821(4) degrees , beta = 92.597(4) degrees , gamma = 93.403(4) degrees , V = 1441.29(12) A3, Z = 2), and 3 (C23H32Mn2N2O11, triclinic, P, a = 10.511(5) A, b = 11.713(5) A, c = 13.135(5) A, alpha = 64.401(5) degrees , beta = 74.000(5) degrees , gamma = 66.774(5) degrees , V = 1329.3(10) A3, Z = 2) revealed that all complexes consist of dinuclear units which are further extended into 1D (1 and 3) and 2D (2) supramolecular networks via hydrogen-bonding interactions. Magnetic susceptibility data evidence antiferromagnetic interactions for all three complexes: J = -3.6 cm-1, D approximately 0 cm-1, g = 1.93 (1); J = -2.7 cm-1, D = 0.8 cm-1, g = 1.93 (2); J = -4.9 cm-1, D = 3.8 cm-1, g = 1.95 (3).