STRUCTURE OF 1-CHLOROMETHYL-2,8,9-TRIOXA-5-AZA-3,4-BENZO-7,10- DIMETHYL-l-SILATRICYCLO-(3,3.3.O~(1,5))-UNDECANE

<正> Mr=299.8, triclinic, Pl, a=10.395(2), b=11.191(2), c=14.051(3)A, α=81.80(2), β=89.42(2), r=66.47(1)°, v=1481.4(5)A3, Z=4, μ(MoKα)=3.37 cm-1, F(000)=632, Dx=1.34 g/cm3, room temperature. The final R=0.058, with unit weights and s=1.33 for 2900 independent reflexions with |Fo| ≥2.5σ(|Fo|). There are two molecules in an asymmetric unit and the lengths of dative N→ Si bond for the two molecules are 2.185(4) and 2.177(4)A, respectively. The different conformations were observed due to the rotation of the chloro-methyl groups.     

2,8,9-三氧杂-5-氮杂-1-硼杂双环[3,3,3]十一碳烷的合成

本文报导了具有N→B配位键的2,8,9-三氧杂-5-氮杂-1-硼杂双环[3,3,3]十一碳烷的合成及性质。化合物(1)的制备已有报导,而化合物(2),(3)则为新的化合物。我们研究了它们的成环条件,制备的最佳条件及化学稳定性。     

CRYSTAL AND MOLECULAR STRUCTURE OF 1-PHENYLAMINOMETHYL-3,7,10-TRIMETHYL-2,8,9-TRIOXA-5-AZA-1-SILITRICYCLO(3,3,3,0~(1,5)) UNDECANE

<正> The transparent colourless crystal of the title compound crystallized in monoclinic system with space group P21/c and cell dimensions a=9.857(7), b=11.128(4), c=16.036(7) A, β=103.31(5)°, V=1711.7A3, Z=4, Dc= 1.25 g.cm-3, λ =-1.5418 A, μ= 13.067 cm-1. The structure was solved by direct methods and refined by full matrix least-squares, the final discrepancy factor R=0.061 and Rw=0.060. The skeleton of the molecule is composed of three five-membered rings with a common edge N(l)-Si(l), and the dihedral angles between each two of the three rings are 110.5°, 107.9° and 105.0° respectively. The N(l)-Si(l) coordination bond length is 2.143(3) A. In comparison with the structures of other related compounds, it was found the N-Si bond length varies with the electronegativities of the substitute groups R at Si atom.     

1-杂环芳酰氧基-2,8,9-三氧杂-5-氮杂-1-硅杂三环[3.3.3.0~(1,5)]十一碳烷的研究

本文合成了六个1-杂环芳酰氧基杂氮硅三环和三个1-杂环芳酰氧甲基杂氮硅三环,这些化合物均未见文献报道。通过1~H NMR、IR 和 X 射线衍射的方法,确证上述化台物为五配位结构,分子内的 N→Si 配键强度较大。这是一类低毒或中毒化合物。     

SYNTHESIS OF 1-(O,O-DIALKYLPHOSPHORYLAMIDO)PROPYL-5-AZA-2,8,9-TRIOXA-1 SILATRICYCLO-[3,3,3,01,5] UNDECANES

Ten 1-(O,O-dialkyl phosphorylamido)propyl-5-aza-2,8,9-trioxa-1-silatricyclo [3,3,3,0^1,5] undecanes were synthesized by the reaction of dialkoxy phosphoryl chlorides with aminopropyl silatrane and their structures were established by elemental analysis, IR, ¹HNMR, and MS measurement. The suitable reaction conditions are discussed based on the related reaction mechanism.     

THE ABSOLUTE CONFIGURATION OF S-(+)-1-p-CHLOROPHENYL-4-ETHYL-2,8,9-TRIOXA-5-AZA-1-SILATRANE(3.3.3.01.5) UNDBCANE

<正> The title compound crystallized in orthorhombic system with space group P212121 and cell dimensions a=9.805(2),b=11.381(4), c=13.865(4) A,V= 1547.0A3, Z=4,Dc=1.345 g.cm-3,λ=1.5418A,μ=13.067 cm-1.The structure was solved by direct methods and refined by block-diagonal least-squares method to the final discrepancy factors R=0.042 and Rw=0.042 for 1101 reflections with I>2.50σ(I). The absolute configuration was determined by utilizing the anomalous scattering of the Si and Cl atoms.It has the S configuration. The Si←N bond length is 2.146(5)A.     

STRUCTURE OF 1-PHENYL-3,4-BENZO-7,10-DIMETHYL-2,8,9-TRIOXA-5-A2A- SILATRICYCLO(3.3.3.0~(1,5))UNDECANE

<正> Mr=327.49, monoclinic,C2/c,a=17.211(11), b=12.300(7),c=17.079(10)A,β=99.41(5)°,V=3567(4)A3,Z=8,μ(MoKα)=1.5cm-1,F(000)=1392,Dx=1.22g/cm3, room temperature.The final R=0.085,Rw=0.077 and s=1.27 for 1471 independent reflections with |Fo|>2.5σ(|Fo|).The length of the dative bond N→Si is 2.193(5)A.The structure Is disordered at C(7),C(13),C(10), C(12)positions.     

STRUCTURE OF ALKALOID WILFORGINE, C_(41)H_(47)NO_(19) 2C_2H_5OH

<正> INTRODUCTION. Tripterygium hypoglaucum(Levl)Hutch growing in Hunan,Guangxi,Yunan and Guizhou provinces of China is a plant used as a medicinetreating rheumarthritis. All alkaloids contained within this plant arecharacterzed by antiinflammatory and analgetic. Using column partitionchromatography of silica gel, we have separated out the wilforine and wilforgine from root of this plant.     

STRUCTURE OF（C6H5COCHCOC6H5）SmI2（THF）3

<正> (C6H5COCHCOC6H5)SmI2(THF)3,Mr= 843. 75,triclinic space group P1,a=13. 274(3),b=9. 886(3),c= 12. 526(4)A,a= 110. 89(3),B=93. 98(2),y=85. 16(2) ,V=1528. 9(8)A3,Z=2,Dc=1. 83g/cm3, (MoKa) = 0. 71069A,u= 40. 3cm-1,F(000) - 810. The structure was solved by Patterson and Fourier techniques and refined by least-squares method to a final conventional R value of 0.082(Rw= 0. 083). The central Sm(III) ion is coordinated by two iodine ions, two oxygen atoms from C6H5COCHCOC6H5 and three oxygen atoms from three THF molecules to form a distorted pentagonal bipyramid. The Sm-I distances are 3. 103 and 3. 092 A ,The Sm-O (O atom from C6H5COCHCOC6H5) distances are 2. 273 and 2. 307 A and the average Sm -O(THF) distance is 2. 500A.     

THE CRYSTAL STRUCTURE OP 1-p-CRESOXYSILATRANE, C_(13)H_(19)NO_4Si

<正> INTRODUCTION. The five-coordinated silicon atoms in the 1-aryloxy derivatives of the silatrane series are surrounded by four oxygen atoms (three in equatorial- and one in apical position). The only known crystal structure of the 1-aryloxy silatrane derivatives is that of 1-m-chlorophenoxysilatrane and we performed the structure determination of the title compound to throw light upon the effect of the phenyl ring substituent on the Si←N dative bond.     

STRUCTURE OF 3-(N-METHYL- β-NAPHTHYLAMINO)-ACROLEIN,C_(14)H_(13)NO

<正> M=211.28, monoclinic, P21/c, a=10.268(2), b=11.581(2), c=9.605(2)A, β=100.40(2)°, V=1123.5(4)A3, 2=4, Dx=1.25 g/cm3, λ=0.71069A, u=0.73 cm-1, F(000)=448, room temperature, R=0.041. The planes of the formylvinyl groupand the naphthyl ring are tilted with respect to the plane of nitrogen frameN by 8.6 and 33.6 , respectively. The O atom and the methyl group are in Z position.     

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     

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.     

STRUCTURE OF MACROSPEGATRINE, [C_(40)H_(46)N_4O_3]Cl_2·3(H_2O)

<正> Mr=322.9, orthorhombic, P212121,a=19.867(4), b=15.793(3),c= 12.997(2)A, Z=4, Dc=1.23gcm-3,λ(CuKα)=1.5418A,μ=17.06cm-1, F(000)=1552. Final R=0.096 for 2764 unique diffractions with I≥3σ(I). Macrospegatrine obtained from the root of raurolfia Verticillata(Lour) Baill.f.rubrocarpa H. T.Chang.mss is a complex which involves double skeletons. It is a new alkaloid.     

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     

CRYSTAL STRUCTURE OF CHUANLIANSU C_(30)H_(38)O_(11)·3H_20

<正> Introduction. Chuanliansu(1), C_(30)H_(38)O_(11)·3H_2O, isolated from the bark of Melia toosendan S. et Z., is an active anthelimintic against ascaris (Chung, 1975; Shu, 1980). In the course-of our systematic investigation on the relationship between the structure and biological activity of its analogues (Ochi, 1976; Arnoux, 1980), we have undertaken an X-ray structural, determination of the title compound. The'molecule belongs to the triterpene group with a furan ring and a hemiacetai bridge between C(19) and C(28). Its colorless crystals have been obtained by slow evaporation of an alcohol-water solution.     

CRYSTAL STRUCTURE OF ERBIUM (HI) COMPLEX WITH 5-SUL-FOSALICYLIC ACID[Er (SO_3C_8H_3(OH)CO_2) (H_2O)_7] [Er (SO_3C_6H_3-(OH)CO_2)_2(H_2O)_6]·8H_2O

<正> [Er(SSA)(H2O)7][Er(SSA)2(H2O)6]·8H2O (H2SSA = 5-sul-fosalicylic acid), Mr=1361.3, monoclinic,P21/c, a = 21.459(7), b = 10.125(2), c = 22. 033(5)(?), β=109. 07(2)°, V = 4524(2)(?)3, Z = 4, D,= 1. 998g/cm3, μ (MoKa) = 40. 6cm-1, F(000)=2704, R = 0. 038 for 5805 observed reflections. The Er(Ⅲ) ions in-both complex cation and anion are coordinated by unidentate SSA ligand(s) and water molecules in a trigondodecahedral geometry. The coordination polyhedra are connected with each other by hydrogen bonds involving the uncoordinated carboxylato oxygen atoms and the coordinated water molecules. Stacking interactions between the phenyl rings further stabilize the structure.     

Crystal Structure of 3－hydroxyl－1，5－diazacycloheptane Dihydrobromide C_5H_（12）N_2O·2HBr

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆ３－ｈｙｄｒｏｘｙｌ－１，５－ｄｉａｚａｃｙｃｌｏｈｅｐｔａｎｅＤｉｈｙｄｒｏｂｒｏｍｉｄｅＣ_５Ｈ_（１２）Ｎ_２Ｏ·２ＨＢｒＬＩＵＹｏｎｇ；ＸＵＥＧｕｏ－Ｐｉｎｇ；ＷＵＣｈｅｎｇ－Ｔａｉ（Ｄｅｐａｒｔｍｅｎｔｏｆ?..     

[Zn(C_6H_(14)N_5O)Cl_3]的合成、表征和晶体结构的测定

本文合成了吗啉双胍合锌配合物。经分析鉴定,锌离子、吗啉双胍、氯离子组成比为1:1:3,分子式确定为[Zn(C_6H_(14)N_5O)Cl_3]。对该配合物的红外光谱、核磁共振氢谱、~(13)C、~(15)N谱进行了研究。获得了该配合物的单晶体,结构研究表明,该晶体属于三斜晶系,空间群为P1,晶胞参数:a=7.696(3)、b=7.773(2)、c=12。074(5)A;α=74.95(3),β=81.29(3),γ=66.89(3)度。晶胞中含有二个[Zn(C_6H_(14)N_5O)Cl_3]分子,锌与吗啉双胍呈单齿配位,每个锌离子除与吗啉双胍中N(3)原子配位外,还有三个氯离子参与配位成四面体构型.     

三苯基氧化膦与氯金酸配合物的热分解反应动力学

本文报道了三苯基氧化膦与氯金酸形成的配合物 HAu Cl4.H2 O.4(C6H5) 3 PO的非等温热分解动力学 ,采用微分与积分相结合的方法 ,推断出了它的热分解反应机理 ,其热分解动力学方程为 :dα/dt=AΦe-E/ RT(32 ) (1 α) ( 2 / 3 ) [(1 α) ( 1 / 3 ) - 1 ] -1