STRUCTURAL STUDIES OF trans-1,2 CYCLOHEXANEDIA-MINETETRAACETIC ACID HYDRATE]·C_(14)H_(22)N_2O_8·H_2O

<正> C14H22N2O8. H2O,Mr = 364. 4, monoclinic,P21/n,a =11.536(2),b= 10. 744(2),c=13. 271(3)A,B=99. 87(2) ,V=1620.5A3,Z=4,Do=1. 47,Dc= 1. 493gcm-3,F(000) = 776,u(MoKa) = 1. 17cm-1.The structure was solved by direct methods and refined to R=0. 059 for 2743 observed reflections with I>3 o(I).The molecule of trans-1,2-cyclohexanediaminetetraacetic acid exists in the crystal in a zwitte-rionic form -OOCCH2N+H(CH2COOH) C6H10N(CH2COOH)2. There is no intramolecular hydrogen bond,but intermolecular hydrogen bonds exist between water molecule and car-boxyl group as well as between the carboxyl groups.     

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.     

[Cu(TOL)_4]Cl_2·2C_2H_5OH·2H_2O的合成和晶体结构

三唑醇(Triadimenol,简写TOL)是一内吸性的广谱低毒杀菌剂,主要用于禾谷类作物,腥黑穗病、丝黑穗病、散黑穗病、白粉病、锈病等病害的防治犤1～3犦。其化学名称为1-(4-氯苯氧基)-3,3-二甲基-1-(1H-1,2,4三唑-1基)丁基-2-醇,结构式如下:以农药为配体的金属配合物近年来逐渐被人重视犤4,5犦,它不仅保持了某些金属离子的杀菌特性,扩大了杀菌谱,而且作为一种缓释技术,使农药具有提高持效、延长半衰期、降低对哺乳动物的毒性以及使农药从非内吸性转化为内吸性等优越性。铜化合物作为杀菌剂使用已有60多年的历史,至今仍无抗性,由于其广谱、低毒,…     

THEORETICAL STUDY ON THE CONFIGURATION OF [PdCl_2(C_2H_4OH)]-

The configuration of[PdCl_2(C_2H_4OH)]~- has been studied bypseudopotential ab initio method.A cis isomer was found to be the reactionintermediate in the Wacker process.     

利用氧化加成反应合成[Cu(C_6H_5COO)_2(C_5H_5N)_2(H_2O)]

室温下 ,金属铜粉和过氧化苯甲酰进行氧化加成反应合成了铜化合物 [Cu(C6H5COO) 2 (C5H5N) 2 (H2 O) ](1 )。通过元素分析、电导、红外光谱等方法对配合物进行了表征 ,并经X 射线单晶结构分析确定了配合物的结构 ,晶体属单斜晶系 ,空间群Cc ,a =0 .60 78(4) ,b =1 .5879(4) ,c =2 .30 91 (3)nm ,β =97.61 (2 )°,Z =4,V =2 .2 0 91nm3,R =0 .0 30 7,中心铜原子由单齿配位的苯甲酸根的氧原子和吡啶的氮原子及来自水分子的氧原子形成四方锥配位结构。     

THE CRYSTAL AND MOLECULAR STRUCTURE OP TRIS(u-SULFIDO)-(μ3-SULFIDO)-TETRAKIS (O,O-DIETHYLPHOSPHORODITHIOATO-S,S)-ETHANOL-TRI-MOLYBDENUM-ANTIMONOUSCHLORID ETHANOL SOLVATE {Mo_3(μ3-S)[(μ-S)_3·SbCl_3][S_2P(OEt)_2]_4·(C_2H_5OH)}·(C_2H_5OH)

<正> Mr = 1476.77, monpclinic. The apace group is P21/n with the unit cell parameters: a = 13.250(3), b=17.296(4), c=23.223(9) A; β=92.41(3)°; Z=4; Dc=1.844 g.cm-3. The final R factor is 0.078 for 2054 reflections with     

4[CuCl(C_5H_5N)_4]·[W_10O_(32)]·2(C_5H_5N)·3H_2O的合成及晶体结构

标题化合物是通过(NH_4)_2WS_4,CuCl_2·2H_2O在吡咤溶液中反应制得。晶体呈蓝色,属三斜晶系,空间群,晶胞参数为:a=13.555(7),b=13.666(5),c=17.860(13),a=69.08(4)°β=87.39(5)°,γ=70.72(4)。V=2907(3),Z=1,D_m=2.56g cm~(-3).结构由Patterson法和Fourier法测出。对5692个收集到的独立衍射数据进行计算,最后R= 0.046.结构测定表明,晶体由W_(10)O_(32)~(4-),[CuCl(C_5H_5N)_4]~+,C_5H_5N和H_2O所组成。W_(10)O_(32)~(4-)的结构见图1,W原子处在O原子的八面体配位中,彼此共边和共顶点相连。[CuCl(C_5H_5N)_4]~+的结构见图2,Cu原子由1个Cl和4个N原子配位,呈略有变形的四方锥形,这种离子是首次报导。C_5H_5N和H_2O填入正负离子堆积的空隙中。     

STRUCTURAL STUDIES OF THE METAL HYDRIDE Ti_2Cu_(0.8)Ni_(0.2)H_(0.65)

<正> The metal hydride Ti2Cu0.8Ni0.2H0.65, studied by X-ray diffraction and EXAFS speetroscopy, was found to have the same phase as Ti2Cu,both belonging to the tetragonal system and the I 4/mmm space group. The nearest-neighbour distance of Cu-Ti was found to be considerably shorter than, while the those of Cu-Cu and Cu-Ni almost equal to,the corresponding values in unhydrided alloy Ti2Cu0.8Ni0.2.These results suggest that the hydrogen atom occupies the tetrahedral interstitial site defined by four Ti atoms in a unit cell of Ti2Cu0.8Ni0.2H0.65.The H-Ti nearest-neighbour distance of 1. 86A is much shorter than the sum of the atomic radii of H and Ti, indicating a strong H-Ti bond . This may be an important reason for the high thermal stability of the title hydride.     

[C_5H_5Fe(CO)_2]LnCl_2·nTHF和[C_5H_5Fe(CO)_2][C_5H_4(SiMe_3)]LnCl·nTHF双核配合物的合成

合成了稀土铁双核配合物:〔C_5H_5Fe(CO)_2〕LnCl_2·nTHF(Ln=Nd,Sm,Gd;n=1,2)和〔C_5H_5Fe(CO)_2〕〔C_5H_4(SiMe_3)〕·LnCl·nTHF(Ln=Nd,Sm,Gd;n=0,1,2)。元素分析,热分析,红外光谱和质谱分析确认了这两种配合物。红外光谱数据表明铁与稀土原子是以羰基桥连接。晶体结构分析表明〔(C_5H_5Fe(CO)_2〕Na·4THF是〔C_5H_5Fe(CO)_2〕LnCl_2·nTHF合成的中间体。     

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.     

Cr(CNR)_3Cl_3和Cr(CNR)_3Cl_2B(C_8H_5)_4·H_2O(R=CH_2C_8H_5)的合成和性质研究

长期以来人们对羰基配合物进行了较为充分的研究,但忽略了与之对应的异腈配合物领域。本文在四氢呋喃溶剂中制得两个过渡金属异腈配合物,初步研究了它们的性质,并讨论了它们的红外光谱和热重分析。 1 实验部分 1。1 试剂和仪器 CrCl_3(thf)_3按文献合成。CNCH_2C_6H_5和NaB(C_6H_5)_4购自Aldrich试剂     

ELECTRONIC STRUCTURE OF(C_5H_5)_aCe(OCMe_a)

The electronic structure of(C_σH_σ)_σCe(OCMe_a)have beenstudied by INDO method.Some interesting results hays been obtained.     

INDO STUDIES ON THE ELECTRONIC STRUCTURE OF[Ln(CCl_3COO)_3·phen·C_2H_5OH]_2(Ln=Pr,Sm)

The electronic structure and chemical bonding of the title comp-lexes have been studied by an unrestricted INDO program made applicable forthe lanthanoid compounds.The results indicated:(1)In coordinated bonds O-Lnand N-Ln,5d orbitals of Ln have large contribution in all valence orbitalsof Ln and 4f orbitals have very small contribution.(2)The covalent chara-cter and ionic character are almost equal in the chemical bond which iscomparatively weak between phen,C_2H_5OH and Ln are mainly ionic with somecovalent character.     

Thermal decomposition of Pr[(C_5H_8NS_2)_3(C_(12)H_8N_2)]

The thermal behavior of the complex Pr[(C5H8NS2)3(C12H8N2)] in a dry nitrogen flow was examined by TG-DTG analysis. The TG-DTG investigations indicated that Pr[(C5H8NS2)3-(C12H8N2)] was decomposed into Pr2S3 and deposited carbon in one step where Pr2S3 predominated in the final products. The results of non-isothermal kinetic calculations showed that the decomposition stage was the random nucleation and subsequent growth mechanism (n = 2/3), the corresponding apparent activation energy ?was 115.89 kJ·mol-1 and the pre-expo-nential constant ln[A/s] was 7.8697. The empirical kinetics model equation was proposed as/(α) =3/2(1-α)[-ln(1-α)]1/3.The X-ray powder diffraction patterns of the thermal decomposition products at 800℃under N2 atmosphere show that the product can be indexed to the cubic Pr2S3 phase. The transmission electron microscopy (TEM) of the final product reveals the particle appearance of a diameter within 40 nm. The experimental results show that the praseodymium sulfide nanocrystal can be prepared from thermal decomposition of Pr[(C5H8NS2)3(C12H8N2)].     

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     

STRUCTURE OF DIAQUA(DEMETHYLCANTHARATE)ZINC(II) Zn(C_8H_8O_5)·2H_20

<正> Mr=258.57, Monoclinic, P21/a, a=10.907(5), b=8.502(3) ,c=11.083(4) A, β=107.15(3)°, V=982.09A3, Z=4, Dx=1.729 Mgm-3, λ(MoKα)=0.71069A, μ=26.74 cm-1, F(000)=583.90, T=293K. The final R=0.0406 for 1587 unique observed reflections. The demethylcantharate ion acts as a tridentate ligand towards Zn(II) and a monodentate ligand towards another. The oxygen atoms in one carboxylate group bind with two different Zn(II) to form a chain-structure. There are four different types of oxygen coordinating with Zn(II).     

CRYSTAL STRUCTURE OF [Ce~(Ⅲ)Cl_2(THF)_5][Ce~ⅣC15(THF)]

<正> INTRODUCTION. The attempt to prepare C_9H_7CeCl_2. nTHF(C_9H_7=indenyl) by the reaction of CeCl_4 3THF with C_9H_7Na in THF(tetrahydrofuran) has failed, but an unexpected orange crystal was obtained and determined by single cryntal X-ray diffraction to be a new complex [Ce~ⅢCl_2 (THF)_5]~+[Ce~ⅣCl_5 THF]~-. The valence state of the cerium atom in the cation is different from that in the anion, the former being trivalent while the latter quadrivalent. In this paper the crystal structure of the new complex is reported.     

CRYSTAL AND MOLECULAR STRUCTURE OF DICHLOROBIS-(PYRIDINIOPROPIONATO)ZINC(Ⅱ) ,Zn(C_5H_5NCH_2CH_2CO_2)_2Cl_2

<正> A 1:2 adduct of ZnCl2 with pyridiniopropionate (C5H5N + CH2CH2CO2-,ppBET ) has been prepared and characterized by single-crystal X-ray analysis. The complex crystallizes in the monoclinic space group P21/c(No. 14) with a = 13. 524(2), 6 = 9.322(3), 15. 474(2) A, β=106. 34(2)°, V = 1871. 9(5) A3, Z = 4, Dm = 1. 554gcm-3, Dc=1. 557gcm-3, and μ = 16. 5cm-1. The crystal structure comprises discrete [Zn(ppBET)2Cl2] molecules in which the Zn atom is tetrahe-drally coordinated by two unidentate;carboxylato groups [Zn - O = 1. 965(4) , 1. 969 (4)A] and two chloro ligands [Zn-Cl=2. 269(2),2. 266(1)A].     

Synthesis and Structure Characterization of [HgCl(η~5-C_5H_3C(CH_3)=N-3- C_5H_4N)Fe(η~5-C_5H_5)]·(1/2)CH_2Cl_2

1INTRODUCTIONThechemistryofcyclomercuratedferrocenyl-imineshasbeenofgeneralinterestfordecades,owingtotheirvariousapplicationsinorganicsynthesis,materialscience,catalysisandphoto-chemistry[1].Wehavealsostudiedalotofthesekindsofcompounds[2].Moreover,itisrep…     

Synthesis and Crystal Structure of Ni_3(admt)_6(NCS)_6·C_2H_5OH·2H_2O

1　INTRODUCTIONCoordination compounds with 1 ,2 ,4 triazole as a ligand have interesting fea tures,notonly because ofthe very interesting magnetic propertiesofthese complex es,but also because ofrich modes ofcoordination〔1〕.Particularly,the coordinationbehavioroftriazoletowardsa numberoftransition metalthiocyanatesshowsremark abledifferences〔2 - 6〕.On unsubstitution at N4 ,thetriazole ring hasmonodentate,1 ,2 and 2 ,4 bridging forms.These three modes were all observed in the Ni( II)…