Syntheses and Structures of Two New Coordination Polymers:[Cu(C_(14)H_9O_4)(C_(14)H_(10)O_4)(C_(12)H_(12)N_2)_2] and [Ag(C_(14)H_9O_4)(C_(13)H_(14)N_2)]·0.5H_2O

1 INTRODUCTION Supramolecular approaches to self-assembly of infinite molecular solids with novel structural topo- logies attract considerable attention for their po- tential applications as functional materials and their fascinating architectures[1]. In…     

Ce(C_8H_8)_2和Ce(C_8H_8)_2~-的化学键性质

结合改进的重叠模型Xa-SW法和Ziegler过渡态法,通过将中心原子与配体的作用选成离子聚集、中心原子只有s和p轨道参与成键、中心原子只有d轨道参与成键、中心原子只有f轨道参与成键、中心原子的s、p、d和f轨道同时参与成键5种类型,从能量角度分析了Ce(C_8H_8)_2和Ce(C_8H_8)~-_2的化学键性质。     

ab initio calculation study on vibrational spectra of C_2B_(10)H_(12),NB_(11)H_(12) and C_2B_(10)H_(11)Cl

Geometrical optimization and theoretical calculation of the vibrational frequencies have been performed for C2B10H12, NB11H12 and C2B10Cl by using Gaussian 92 program at 6-31G basis set. The results obtained in this work are in agreement with experimental ones. The optimized geometry and vibrational spectra show that the icosahedral configuration remains unchanged upon converting from B12H122- to the title compounds. The vibrational spectrum of C2B10H11Cl features the absence of C-Cl stretching vibration. But the (C2B10H11)-Cl vibration mode in the low frequency region is as the case for two-atom molecules if the group (C2B10H11) is considered as a pseudoatom     

CRYSTAL STRUCTURE OF {Ni[(C_4H_9O)_2PS_2](C_(12)H_8N_2)_2} -[(C_4H_9O)_2PS_2]

<正> {Ni C(C4H9O)2PS2] (C12H8N2)2} [C(C4H9O)2PS2], Mr= 795. 60, Monocinic,P2,/n,a=16. 806(2), b=12. 720(2), c=21. 248(2) A. β=98. 454(7)°, V = 4493A3,Z=4,Dc= 1. 18g·cm-3,Mo Ka radiation,A=0. 71069A ,F(000) = 1664, R=0. 102 for 4154 reflections with I≥3σ(I).The crystal structure consists of complex cation {NiC(C4H9O)2PS2](C12H8N2)2}+ and complex anion C(C4H9O)2PS2]-. In the cation, nickel (Ⅱ) atom is coordinated by four nitrogen atoms and two sulfur atoms to form a distorted octahedron.     

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 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 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     

双核钴簇合物(C6H5C2R)Co2(CO)6的合成

羰基钴簇合物Co₂(CO)₈可用于有机合成的催化剂。但Co₂(CO)₈本身不稳定,易被氧化。因此,研究不向CO₂簇合物的稳定性及其催化性能具有一定的意义。     

CRYSTAL STRUCTURE OF [Ni((C)_6H_(11)O)_2PS_2)·(C_4H_9NH_2)_4]-(C_6H_(11)O)_2PS_2

<正> [Ni((C6H11O)2PS2)·(C4H9NH2)4](C6H11O)2PS2,Mr-=938. 05, triclinic,P1,a=13. 513(6),b=16. 040 (7), c= 12. 891(6) A , α= 95. 66 (4),β= 90. 23(4),γ= 75. 46(3)°,V = 2691 A3,Z=2,Dc= 1. 16 g·cm3.μ=6. 07cm-1,MoKa radiation, λ=0. 71069 A ,F(000) = 1020,R=0. 100 for 4595 reflections with I≥3σ(I). The title compound molecule consists of a complex cation [Ni((C6H11O)2PS2)(C4H9-NH2)4]+ and a complex anion (C6H11O)2PS2- . The Ni (Ⅱ) atom in the cation is octahedrally coordinated by four nitrogen atoms from four w-butylamine ligands and two sulfur atoms from one (C6H11O)2PS2 group.     

[Nd_2O(C_5H_5)_6](C_12H_9N_2)3Cl·mC_4H_8O的晶体结构

本文报告用单晶X-射线衍射法测定[Nd_2O(C-5H_5)_6](C_(12)H_9N_2)_3C1·mC_4H_5O的晶体结构。晶体属于单斜晶系,空间群为P2-1/c,晶胞参数为a=20.982(15),b=11.217(7),c=32.954(32),β=104.17(7)°;Z=4。Nd和C1原子坐标用直接法定出,其他原子坐标以差Fourier方法求得,经过最小二乘法修正,R因子为0.159。在分子中三个茂环皆通过η~5。键与Nd原子配位,两个Nd原子间存在桥氧原子,因而形成(Nd_2O(C_5H_5)_6)~(2-)阴离子,Nd-C键基本上属于离子键。三个邻菲罗啉基团通过氢键与C1原子连接形成大的阳离子[(C_(12)H_9N_2)3-C1]~(2+)。     

三元配合物Tm[(C_5H_8NS_2)_3(C_(12)H_8N_2)]的热化学性质研究

在无水乙醇中,用吡咯烷二硫代氨基甲酸铵(APDTC)和1,10-邻菲咯啉(o-phen·H2O)与TmCl3·3.65H2O作用,合成了未见文献报道的三元固态配合物,确定它的组成为Tm[(C5H8NS2)3(C12H8N2)]。用RD496-Ⅲ微量热计测定了298.15K下水合氯化铥及两个配体在无水乙醇中的溶解焓,两个配体醇溶液的混合焓及不同温度下标题化合物液相生成反应的焓变。在实验和计算基础上,得到了液相生成反应的热力学参数(活化焓、活化熵和活化自由能),速率常数和动力学参数(表现活化能、频率因子和反应级数)。通过合理的热化学循环,求得了298.15K时标题化合物的固相生成反应焓变;推导了用该热量计测定固态物质比热容的计算式,并测定了题目配合物298.15K的比热容。用RBC-Ⅱ精密转动弹热量计测定了题目配合物的恒容燃烧热,计算了它们的标准摩尔燃烧焓和标准摩尔生成焓。     

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.     

Crystal Structure of 3-(4-nitro-) phenylsulfonyloxyisothiazole NO_2C_6H_4SO_3C_3H_2NS

1INTRoDUCTIONFollowingpublicationofthefirstsynthesisofamononuclearisothiazoleinl956(li,thisringsystemhasattractedconsiderableinterest.Especially,thistenden-....1cyisincreasingsincealotOfreportsaboutexcellentbiologicalactivitiesofcompoundscontainingisothiazolemoietyemergerecently"~".Theincreasingunderstandingofthefundamentalchemistryoftheisothiazolesystemhasenabledchemiststoincorpo-ratetheringintoawidevarietyofcompoundswithpotentialbiologicalactivity.Inanattempttolookforbiologicallyactivec…     

C_2H_3Cl分子团簇内部离子-分子反应产生C_4H_5Cl~ 的研究

用同步辐射对（C2H3Cl）分子团簇进行了光电离研究，发现该团簇内部发生了离子－分子化学反应，生成了十分稳定的反应产物C4H5Cl＋，不再是varderWaals弱键络合物．本文对反应机理进行了初步探讨     

[(C_5H_4CH_3)_2HoN_4CPh]_2·[(C_5H_4CH_3)(C_5H_5)HoN_4CPh]_2的合成和晶体结构

（C5H4CH3）3Ho和（C5H4CH3）2Ho（C5H5）与5-苯基四唑（HN4CPh）在THF中反应，得到复合产物[（C5H4CH3）2HoN4CPh]2·[（C5H4CH3）（C5H5）HoN4CPh]2，该晶体属三斜晶系，P1空间群，晶胞参数为a=9．386（3），b=13．071（3），c=16.571（2）A，a=86．90（1），β=74．61（2），γ=77.30（2）°，V=1912．2（8）A3，Z=1，Dc=1.602g／cm3，Mr=922．61，μ=41．92cm－1，F（000）=896，最终偏离因子R=0．041，Rw=0．056．晶体数据显示，在同一个晶胞里有两个组成不同的分子，每一个分子都是具有对称中心的四唑基桥二聚体结构，其桥环单元-HoN3HoN3-是平面型的。每个钬原子分别被两个茂基和3个四唑基氮原子配位，形成1个边桥变形四面体构型。     

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 [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.     

HRh[(C_6H_5)_2PCH_2CH_2P(C_6H_5)_2]_2的晶体和分子结构

HRh[(C_6H_5)_2PCH_2CH_2P(C_6H_5)_2]_2(分子量900.8)晶体属单斜晶系,空间群P21/n,晶胞参数a=21.319(2),b=20.844(2),c=10.130(3),β=91.255(2)°,V=4500.4,Z=4,D_c=1.15g·cm~(-3),F(000)=1864,μ(CuKα)=44.97cm~(-1)。共收集独立衍射点数7636个,其I>3σ(1)的衍射点数6810个。最终的R=0.045,R_w=0.050(W=1/σ~2(F)+(F)+g|F|~2)。其分子结构呈畸变的三角双锥构型。     

［Cu_2（C_6H_5COO）_4（C_3H_4N_2S）_2］的合成、晶体结

在２－氨基噻唑存在下，利用铜粉和过氧化苯甲酰的氧比加成反应，在丙酮中合成了双核铜（Ⅱ）配合物［Ｃｕ_２（Ｃ_６Ｈ_５ＣＯＯ）_４（Ｃ_３Ｈ_４Ｎ_２Ｓ）２］．晶体属单斜晶系，Ｐ２１／ｎ空间群，晶胞参数：ａ＝１．０６８５（１）ｎｍ，ｂ＝１．９０２８（６）ｎｍ，ｃ＝１．７０４６（９）ｎｍ；α＝γ＝９０°，β＝９６．４９（３）°，Ｖ＝３．４４３（４）ｎｍ~３，Ｚ＝４．Ｆ（０００）＝８２４，Ｄｃ＝１．５５５８ｇ／ｃｍ~３，μ＝１４．０７８ｃｍ~（－１），最终偏离因子Ｒ＝０．０４８２１，Ｒｗ＝０．０５３１４．通过元素分析、ＩＲ、ＴＧ、Ｘ射线粉末衍射表征了配合物的结构．     

SYNTHESIS AND CRYSTAL STRUCTURE OF （C5H5）2Ti（o—NHPhC6H4CO2）2

<正> Cp2Ti(o-NHPhC6H4CO2)2, Mr = 602. 54, space group C2/c, a = 33. 77(2), b = 12. 611(6), c=14. 486(9) A ,β=103. 28(4)°,V = 6004(5) (?)3,Z = 8, Dc= 1. 33gcm-1, MoKa(λ=0. 71069(?)) radiation, μ = 3. 21cm-1, F(000) = 2512e, R = 0. 066, Rw= 0. 085 for 2511 radiations. The Ti atom in the molecule is coordinated by two C5H5 groups and two monodentate carboxyl ligands in a distorted tetrahedral geometry with the bonds in the range of Ti-C = 2. 334 - 2. 41(?) ; Ti-O = 1. 914(5) and 1. 919(5)(?);and the bond angles O-Ti-O = 91. 7(2)°; (cent-C5H5)-Ti-(cent-C5H5) = 135. 9(6)°.