STRUCTURE OF TARAXER-9,12,17-TRIENE-3β,23-DIOL,C_(29)H_(44)O_2

<正> The structure of the title compound, a pentacyclic triterpenoid isolated from Clinopodium Polycephalum (Vant.) C. Y. Wu et Hsuan, has been determined by X-ray crystallographic analysis. C29H44O2,Mr=424.67, monocli-nic, P21,a=10.753(2), b=7.705(2), c=15.336(2)A,β=101.47(1)°, V=1245.2(7) A3,Z=2, Dx=1.133gcm-3,μ(Mo-Kα)=0.64cm-1, F(000)=468, 294K. Ths structure was solved by direct methods and refined to R=0.050 for 2269 observed MoKd reflections.     

CRYSTAL AND MOLECULAR STRUCTURE OF BIS(L-VALINATO)COPPER(II) MONOHYDRATE Cu[(CH_3)_2CHCH(NH_2)COO]_2·H_2O

<正> Mr=313.8, monocllnic, C2, a=21.255(4), b=9.567(4), c=7.399(1)A, β=108.8(1)°, V=1423.8A3, Z=4, Dx=1.464 g.cm-3, MoKα , μ=15.496cm-1 , F(OOO) = 660, T=295K, final R=0.089 for 1644 observed reflections. Two amino acid ligands chelate to copper forming a planar-square configuration. An oxygen atom of water occupying the apical position makes the coordinating polyhedron of copper a square pyramid.     

CRYSTAL STRUCTURE OF 1-METHYL-6-(E-ETHOXYCAR-BONYLVINYL)-8-BENZOYL-2, 3-DIHYDRO-1H-IMIDAZO[1, 2-a] PYRIDIN-5-ONE

<正> The title compound C20H20N2O4(Mr=352.39)belongs to mono-clinic space group C2/c with a=9.208(4),b=11.714(3),c=32.336(8)A,β=100.83(2)°,V=7146.2(6)A3,Z=16,Dc=1.35 g/cm3,μ(Moka)=1.03 cm-1 and final R=0.06 for 1781 reflections with F≥2.5(F).There are two independent molecules in an asymmetric unit.Neither pyridinone nor phenyl ring is coplanar with the ketonic carbonyl group in the molecule.     

Crystal and Molecular Structure of 2-(2-Methoxycarboxyl) phenyloxy-5,7-dimethyl-1,2,4-triazolo[1,5-a]pyrimidine

The crystal structure of the title compound has been determined by single crystal X-ray diffraction analysis. C15H14N4O3, Mr=298.30, monoclinic, space group P21/n, a=9.483(9),b=11.078(9), c=13.700(9),β=100.19(7)°, V=1417(4)3, Z=4, Dx=1.399 g.cm-3, μ=0.0942 mm-1; F(000)=624, final R=0.074 and Rw=0.074 for 1502 observed reflections[I≥3σ(I)]. The results show that all ring atoms in the triazolopyrimidinyl moiety were coplanar with strong tensile force, which might be an important active site.     

Crystal and Molecular Structure of 2-(2, 6-Dinitro-4-Trifluoromethyl) phenylthio-5, 7-Dimethyl-1,2,4-Triazolo [1, 5-a] Pyrimidine

1INTRoDUCTIONItwasreportedthattheheterocycliccompoundscontainingl,2,4-triazolo[1,5-ajpyrimldinyldisplayedpotentialbioIogicalactivities['2i.Howeverltheherbicidalac-tivityofthethio-etherderivativesof1,2,4xtriazolo[1,5-ajpyrimidinewasrarelyre-ported"'.Inourpreviouspaper"',wedesignedandsynthesizedaseriesof2-arylthio-l,2,4-triazolo{l,5-ajpyrimidines,someofwhichdisplayedgoodherbicidalactivity.Inordertostudythestructure-activityrelationshipofthesecompounds,thestructureofthetitlecompound(1)wasan…     

Synthesis and Characterization of Tetrametal Cluster [Co2(CO)6][μ-HC2CH2OCH2C2H-μ][Co2(CO)6]

The treatment of dipropargyl ether HC2CH2OCH2C2H with Co2(CO)8 resulted in the formation of a novel cluster [Co2(CO)6][μ-HC2CH2OCH2C2H-μ][Co2(CO)6]. The cluster was characterized by C/H analyses, IR and 1H NMR spectroscopy and X-ray crystal structure determination. It belongs to monoclinic system, space group P21/c with the following crystallographic parameters: a=18.149(2), b=7.0111(7), c=20.897(2)(A), β=115.318(7)°, V=2403.7(5)(A)3, Z=4, Mr=665.97, Dc=1.840 g·cm-3, F(000)=1304.00, μ(Mo-Kα)=27.76 cm-1 and R=0.030 for 2372 observed reflections.     

THE SYNTHESIS AND X-RAY CRYSTAL STRUCTURE STUDIES OF (DI-3-INDOL YL )M ETH YLFERROCENE

<正> A novel anhydrous zinc chloride catalyzed condensation reaction of ferrocenealdehyde with indole in solid state gave the title compound (Di-3-indolyl) methylferrocene ((C8H6N)2CHC5H4FeC5H5) selectively, and its crystal structure has been determined by X-ray diffraction analysis. The crystal belongs to triclinic system, space group P1, with cell parameters a = 9. 624(2), b = 9. 957(2), c=11. 295 (4)A,α=92. 17(2), β=92. 23(2), γ=111. 30(1)°, V=985. 4A3, Mr = 430. 33, Z = 2, Dx = 1. 44g/cm3,μ= 7. 8cm-1, F(000) = 444. The final R = 0. 056 for 3027 observed reflections.     

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).     

Synthesis and Crystal Structure of (E)-[1-Ferrocenyl-2-(4-Chlorophenyl) ethylene]

1INTRoDUCTIoNCurrently,thereisaconsiderableinterestintheinvestigationoforganicandorganometallicmaterialsshowinglargenonlinearopticalresponse.Theirpotentialusehasbeenresearchedindeviceapplicationswhicharerelatedtothetelecommuni-cations,opticalcomputingandopticalinformationprocessing"2i.Onamicroscopiclevel,oneofthemajorphysicalparameterstodecidethenonlinearopticalpropertiesofmaterialsisthemolecularhyperpolarizability,avaluedeterminedbyelectronicandgeometricstructureofmolecule.Thetitlecompoun…     

双环[2.2.2]辛-7-烯-2，3，5，6-四羧酸铜配合物的合成和晶体结构研究

以双环[2.2.2]辛-7-烯-2,3,5,6-四羧酸(H4L)为配体,采用水热法合成了个铜配合物[Cu2L2(H2O)2](2),并得到单晶,同时在水热条件下得到了化合物H4L.2H2O(1)的晶体。分别对化合物1和2进行了元素分析、红外光谱等分析,并用X-射线单晶衍射测定了化合物的单晶结构。化合物1属于三斜晶系,P1空间群,化合物1的晶体学数据为:a=0.88554(15)nm,b=0.95566(16)nm,c=1.043 88(17)nm,α=110.863(3)°,β=91.127(3)°,γ=91.429(3)°,V=0.824 9(2)nm3,Z=2,Mr=366.32,Dc=1.475 g.cm-3,F(000)=388,μ=0.129,R1=0.067 0,wR2=0.189 3;配合物2属于正交晶系,Pnnm空间群,配合物2的晶体学数据为:a=2.766 8(6)nm,b=0.638 75(14)nm,c=0.737 32(16)nm,V=1.303 1(5)nm3,Z=4,Mr=442.31,Dc=2.254 g.cm-3,F(000)=884,μ=3.324,R1=0.059 4和wR2=0.191 7。化合物1通过氢键形成三维网状结构,配合物2中的中心离子有3种配位方式,通过不同的配位方式也形成三维结构。     

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.     

Synthesis and Crystal Structure of H2Mo8O26[(n-Bu)4N]2[(CH3)2COHCH2COCH3]2

The title compound 4-methyl-4-hydroxy-2-pentone is obtained by the condensed reaction of acetone, and co-crystallized with octamolybdate anion and tetrabutyl-ammonium cation. The crystal structure belongs to triclinic system, space group P1, Mo8C44H98O30N2 Mr= 1902.77, a=11. 512(6), b=12. 790(3), c=13. 395(4)A, α=65. 22(2), β=78. 26(4), γ=71. 12(3), V=1689(1) A3, Z=1, Dx=1. 869g/cm3, F(000)=950, μ=14.79 cm-1, final R=0. 053 and Rw=0. 067. Theorbital hybridization of C (53) and C (55) are sp3 and sp2 separately in (CH3)2COHCH2COCH3 and the catalysis of β-octamolybdate anion might be present for the condensed reaction of acetone.     

CRYSTAL STRUCTURE OF VANADIUM（V） COMPLEX OF SCHIFF BASE

<正> The complex C23H29N2O6V crystallizes as a dark red crystal in monoclinic space group P21/a, with a = 10. 233(2), b = 24.805(8), c= 10. 423(2) (?). β=117. 93(2)°, V =2337.1 (?)3. Mr = 480.43, Z = 4, Dx =1. 368g/cm3, μ = 4. 463cm-1,. F(000) = 1061. The final R is 0. 054 for 1778 observed reflections. X-ray crystallography demonstrates that the ligand in the complex is a condensation pro-suet from l:l 4-tert-butyl-6-formyl salicylaldehyde to benzoyl hydrazine. The compound has a five-coordinated square pyramidal VO3+ gump.     

Synthesis and Crystal Structure of Cluster [C6H4-1,2-(CO2CH2C2H-μ)2][Co2(CO)6]2

The reaction of dipropargyl phthalate C6H4-1,2-(CO2CH2C2H-μ)2 1 with octacarbonyldicobalt 2 resulted in the formation of red complex [C6H4-1,2-(CO2CH2C2H-μ)2][Co2(CO)6]2 3, in which each Co2(CO)6 group coordinates to one of the two C≡C bonds of 1. Molecular structure of complex 3 was determined by single crystal X-ray analyses. The crystal belongs to the monoclinic system, space group P21/a with the following crystallographic parameters: a=8.521(2), b=29.143(6), c=12.918(7)(A), β= 100.12(3)°, V=3158(2)(A)3, Z=4, Mr=814.09, Dc=1.712 g.cm-3, F(000)=1608, μ(Mo-Kα)=21.37 cm-1 and final R=0.044 for 3151 observations.     

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.     

CRYSTAL AND MOLECULAR STRUCTURE OF 1- ETHOXYCAR-BONYLMETHYL-2-(α-PHENYl-β-NITRO) PROPYL-3-n-PROPYL-2, 4-DIOXO-1,3,2-BENZODI ZAPHOSPHORIN

<正> C23H28N3O6P,Mr, = 473. 47,orthorhombic,space group Pbca, α=10. 412 (1),b=18. 498(6), c=24. 860(4) A,V= 4787. 9 A3,Z = 8 , Dx= 1. 315g/cm3, λ(Mo Kα) = 0. 71073A ,μ=1. 51cm-1,F(000) = 2000. The final refinement converged with R=0. 074 and Rw=0. 090. Stable conformations of the title compound are discussed.     

STRUCTURE OF MOLECULAR COMPOUND CRYSTAL A_2B(A =1, 6, 7, 8,-TETRA-PHENYL (3, 4-BENZO)BICYCLO[4, 2, 0]OCTA-7-ENE, B=CIS, CIS-1,2,3,4,-TETRAPHENYLBUTADIENE)

<正> C100H78, (A: C36H28, B: C28H22) Mr = 1279. 74, monoclinic, P21/a, a=17. 282(3), b=10. 669(4), c= 19, 927(3) A , β =102. 99(1)°,V = 3580. 1(2) A3, Z=2, μ(MoKα) = 0. 623cm-1, F(000) = 1356, Dc=1. 187g/cm3, room temperature. The final R=0. 084, Rw = 0. 086 for 1255 independent observed reflections (I≥3σ(I)). Owing to the existence of 1,6,7, 8-Tetraphenyl (3,4-benzo)-bicyclo[4, 2, 0]octa-7-ene(A) , cis, cts-1, 2, 3, 4-Tetraphenylbutadiene (B) in A2B can take the different conformation from the one in the pure B crystal. The reason of the formation of this molecular compound crystal is put forward.     

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 AND MOLECULAR STRUCTURE OF O,O-DI-ISO-PROPYL-α-(1, 3, 4, 6-TETRA-O-ACETYL-2-DEOXY-β-D-GLU- COPYRANOSYL ) AMINO-α-p-METHYLPHENYLMETHYLPHOS-PHONATE

<正> The crystal C28H42O12NP is the monoclinic space group P21, with a = 10. 158(1), b=9. 069(1), c=18. 147(3) A , β=90. 72(1)% V=1671. 6 A3, Mr=615. 61, Z=2, Dx=1.23 g/cm3, μ=2.16 cm-1, F(000) = 660. The final R = 0. 071 and Rw = 0. 073 for 1860 observed reflections [I≥3σ(I)]. The results of structure analysis indicate that the configuration of the chiral carbon atom C(41) formed in the reaction is R *.     

多齿配体2,5-二羟基-1,4-苯醌缩氨基脲 (C_6H_4O_3NNHCONH_2.CHON(CH3_)_2)的合成及晶体结构

报道了含1个溶剂DMF的多齿配体2,5-二羟基-1,4-苯醌缩氨基脲的合成和晶体结构。该化合物(C10N4O5H14)属正交晶系,其空间群为P212121 a=13.221(6),b=17.709(5),c=5.347(4)?, V=1252.0(1)3,Z=4,F(000)=568, Dx=1.434g/cm3,Mr=270.25, m (MoKα)= 1.16 cm-1, 结构由直接法解出,全矩阵最小二乘法修正,最终的偏离因子R=0.0319,wR=0.0748。结构测定表明溶剂DMF分子和2,5-二羟基-1,4苯醌缩氨基脲间形成很强的氢键,后者可看作是两条共轭链的偶合物。