软X-射线分光晶体马来酸氢十八酯的晶体结构

测定了标题化合物C_(22)H_(40)O_4的晶体结构，属空间群Pī，a=0.6833(2)，b=3.1662(5)，c=0.5392(1) nm，α＝90.63(2)．β=102.61(2)，γ＝89.03(2)°，Z=2偏离因子R=0.0465，晶体中分子通过氢键形成二聚体，二聚体在晶体中排列成层，进而这些层堆垛成晶体结构，层内二聚体之间相互作用比层之间的相互作用强．分子中的十八烷基的碳原子基本共面．其碳链呈锯齿状伸展，初步解释了晶体生长过程中的一些现象．     

双(甲基环戊二烯基)二(2,6—二氯苯氧基)锆的晶体和分子结构

标题化合物的晶体是单斜晶系,所属的空间群为P2_1/c,晶胞参数为:a=17.050,b=8.603,c=16.332,β=101.05°,Z=4。在PW1100四圆衍射仪上用CuKα射线在3°≤θ≤68°范围内收录了4266个独立的衍射数据,其中3802个衍射数据大于3σ(Ⅰ)。结构用重原子法和Fottrier合成法解出,经全矩阵和块对角矩阵最小二乘法修正,最后的偏离因子R=0.068。结构测定表明,分子内具有非结晶学二次旋转轴对称性,锆原子周围的二(甲基环戊二烯基)和二氧原子构戍一个畸变的四面体配位。     

[C_5H_7S_2]_2[(SbCl_3)_2S]的晶体结构

[C_5H_7S_2]_2[(SbC1_3)_2S]的晶体结构采用x射线衍射法测定。晶体属于卑斜晶系,空间群C2/c,a=14.531(2),b=11.265(2),c=15.364(3),B=112.72(1)°,Z=4。在CAD-4四圆衍射仪上收集数据,用重原子法解出结构并经全矩阵最小二乘法修正。R=0.067。研究表明,该离子晶体中,[C_5H_7S_2]~+的C、S骨架具有平面构型,而[(SbCl_3)_2S]~(2-)的构型是:Sb原子周围形成缺位的准三角双锥构型,两个Sb准三角双锥通过共用S桥形成二聚体,∠Sb-S-Sb=98°,整个阴离子具有C_2对称性。     

二氯二L-天门冬氨酸二乙酯合铂的晶体结构及分子结构

本文报道二氯二L-天门冬氨酸二乙酯合铂的晶体结构及分子结构。使用美国Syntex R3四圆衍射仪收集到3978个独立的三维强度数据.晶体属单斜品系,空间群为P21,晶胞参数a=8.074(1)A,b=11.309(4)A,c=27.793(9)A,β=106.84°(2),z=4,分子式为Pt(C8H15O4N)2Cl2.用Patterson法解出结构,用块矩阵最小二乘程序修正,最后的R值为0.039结构分析结果表明,Pt(Ⅱ)原子取dsp2杂化轨道正方形配位,二个Cl及L-天门冬氨酸乙二酯分别处于对位位置.N原子采取sp3杂化四面体构型以孤对电子与Pt(Ⅱ)成配键.由于络合物分子内氢键及堆积上的原因使络合物中的L-天门冬氨酸的构型比L型及DL型天门冬氨酸有较大的扭曲.     

六氯三(烯丙基硫脲)一水合二钨(Ⅲ)的晶体与分子结构

六氯三(烯丙基硫脉)一水合二钨(III)晶体属单斜晶系,空间群为P2_1;晶胞参数:a=8.496(1)A,b=18.760(2)A,c=8.591(1)A,β=91.36(1)°;Z=2;D_C=2.297g·cm~3。在CAD-4四圆衍射仪上录得独立衍射3069个。晶体结构用重原子法和差值Fourier法解出,经全矩阵最小二乘方修正,R=0.038。研究结果表明,这是由三个烯丙基硫脲的硫原子桥联的双核钨原子簇化合物,W—W间距2.443(1)A,显示出较强的金属—金属相互作用。     

新型氧桥和多硫基杂桥联的双核钼硫亚硝基化合物〔(CH_3)_4N〕_2K〔Mo_2OS_2(NO)_2(S_2)_2S_5)·H_2O的合成和晶体结构

本文报导[(CH_3)_4N]_2K[Mo_2OS_2(NO)_2(S_2)S_5]·H_2O的合成和晶体结构。该化合物晶体属于单斜晶系,所属的空间群为P2_1/c。晶胞参数为:a=13.320(2),b=17.377(2),c=13.269(3),β=107.93(2)°,Z=4。在CAD—4四圆衍射仪上,用MoKα射线收录了3576个独立衍射数据(I≥3σ(I))。晶体结构用直接法解出,经Fourier合成和全矩阵最小二乘方修正,最后偏离因子R=0.045。结构分析表明,晶体中Mo—Mo间距为3.421,二钼原子间未成键。Mo原子周围呈近似五角双锥的七配位构型。本结构的特征在于二Mo原子间除双硫桥外还存在氧桥。     

[Hg(C5H4S5)I2]2的合成与晶体结构(C5H4S5 = 4,5-亚乙基二硫杂-1,3-二硫杂-2-硫酮)

用 HgI2 和 4,5-亚乙基二硫杂-1,3-二硫杂-2-硫酮 (C5H4S5)反应,合成一种二核汞配合物[Hg(C5H4S5)I2]2 1。X 射线衍射结果表明,晶体属于单斜晶系,C2/c 空间群,晶胞参数 a =21.6847(1),b = 8.5125(4),c = 15.6699(8),a=112.7850(1)°,V=2666.8(2) ?3。Mr = 1357.54,Z = 4,Dx = 3.381 g/cm3,ì = 16.913 cm–1,F(000) = 2400,R=0.0639,wR=0.1711,S=1.052。配合物 1 具有二聚体结构,2 个汞原子通过 2 个碘原子桥联,形成 1 个 Hg2I2菱形平面,汞原子周围的配位是四面体结构,通过分子间的硫…硫作用和碘…硫作用,形成准二维超分子网络。 S S S H g I I S S S S I I H g S     

鹤草酚的晶体结构和分子结构

鹤草酚晶体属三斜晶系,空间群为PI,晶胞参数为a=9.901(3),b=11.195(4),c=11.752(4)Å,α=80.74(3),α=75.66(3),γ=76.46(3)°,晶胞内分子数Z=2.用SyntexP3/R3型四圆衍射仪收集到2891个独立衍射强度.以直接法SHELXTL解出晶体结构.结构参数的修正采用了块对角矩阵最小二乘法,最后得偏离因子R=5.7%.晶胞中含有d-,l-两种对映体分子,它们彼此以I连系组成外消旋体.每分子中的两个六环分别同相邻的氧共面,其双面角为14.2°.两个六环通过碳(sp³)桥相连,并由于形成分子内氢键O-H…O(分别为2.705Å和2.745Å)而限制了自由转动.     

草药牛筋果化学成分的研究IV牛晶V的分子晶体结构

用SYNTEX R_3型四圆衍射仪收集了牛晶V的三维衍射数据,晶体空间群为P2_1/c;a=9.620(6),b=14.660(8),c=10.709(6),β=101.12°;Z=4。分子式为C_(16)H_(14)O_6·H_2O。利用直接法和差值Fourier法解出了晶体结构。经位置坐标参教,各向异性温度因子和比例因子,块矩阵最小二乘修正,R值为0.0522。 结构分析表明,苯环处在分子的中心位置,苯环两侧是两个六员杂环。除个别原子外,大部分非氢原子都处在同一个平面上。分子内存在着一个较大的共轭体系。所有的极性基团都分布在分子的外侧,这种结构可能与抗癌机理有密切的关系。     

双聚α-联呋喃二甲酰肟二氯化铜(Ⅱ)配合物[(α-FDO)CuCl_2]_2·C_2H_5OH的分子结构及化学键研究

本文报道了[(α-FDO)CuCl_2]_2·C_2H_5OH的制备和晶体结构.晶体属于三斜晶系,空间群P1,晶胞参数α=6.038(1),b=10.912(2),c=12.167(2)A;α=114.13°,β=96.23°,γ=98.08°;V=712.1(4)A~3,Z=1;D_m=1.73,D_c=1.75g·cm~(-3),R=0.070.在晶体中,分子通过Cl桥形成双聚体.利用晶体结构数据,进行了EHMO计算,并对分子的成键情况进行了讨论.指出了二甲酰肟与金属Cu(II)形成的五员螯合环呈平面构型的原因.主要是与环上的N=C双键的存在有关,而并不是由于形成了环型π-轨道.     

Synthesis and Crystal Structure of a [Cu(HTren)Cl_2]ClO_4·H_2O Complex (Tren = Tris(2-aminoethyl)amine)

1INTRODUCTION Investigation of the coordination chemistry of copper(II)continues to be stimulated by interest in developing modes for copper proteins and in under-standing the factors which give rise to the seemingly infinite variety of distortions from regular stereo-chemistry observed in Cu(II)complexes[1,2].For more than decades,due to the unique coordination polyhedra and their easy preparation,tripodal copper complexes have attracted much attention in addition to their special chemi…     

CRYSTAL AND MOLECULAR STRUCTURE OF [K(18-CROWN-6)][Bi(SCN)Cl_3]

<正> The crystal and Molecular structure of [K(18-crown-6)](Bi(SCN)Cl3] has been deterained by X-ray diffraction Method. Its crystal is triclinic, space group Pl,with a = 9.233(4), b = 11.661(5), c=11.738(5)A,a= 81.82(4)° ,β=71.47(4)°,γ=75.55(4)°, and Z = 2. The final structural refine-ment converged with unweighted and weighted R factors of 0.051 and 0.047 for 2924 observed reflections. Results of the structure analysis indicate that the K+ ion enters the cavity of the 18-crown-6 to form the complex cation and one Bi(Ⅲ) atom, one SCN ligand and three Cl atoms fora the anion. Each Bi(Ⅲ) atoa is coordinated by four Cl atoas, of which two are shared with other Bi(Ⅲ) atom, one N atom and one S atoa from two SCN ligands respectively shared with a third Bi(Ⅲ) atoa, forming octahedral geometry.     

四氮杂环十二烷铒配合物的合成及其晶体结构

氮气保护下, 在无水乙腈中合成了1, 4, 7, 10-四氮杂环十二烷(Cyclen)与稀土铒的配合物并得到浅红色棱柱状晶体。元素分析结果表明该配合物的组成为Er(Cyclen)(CF3SO3)3(CH3CN)。用X射线衍射方法研究了其单晶结构。晶体属单斜晶系, P21/a空间群。晶胞参数为a=1.7335(4), b=1.8027(4),c=0.8772(3)nm, β=97.64(3)°, V=2.7171(2)nm^3, Z=4。其中铒为八配位,形成四方反棱柱型配位多面体。     

[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+)。     

CRYSTAL STRUCTURE OF MIXED METAL CLUSTER Co2Nb2Te4 OBTAINED BY SOLID STATE REACTION

<正> Compound Co2Nb2Te4 obtained by heating the elements Co2 Nb anc Te at 1000℃ in a evacuated silica tube, crystallizes in nonoclinic, space group P21/c with a = 8.197(2), b = 6,258(1), c = 7.816(3) A,β=118.48(2)° Z=2, X-ray structural determination shows non-molecular 2-dimensional character of its crystal structure. In the structural unit, two Co and two Nb atoms form a rhombic plane with four Co-Nb bonds (average 2.744A) and one Co-Co bond (2.514A) and there exists no Nb-Nb interaction. The distorted tetrahedral coordination of each metal atom is completed by four Te atoms. The average distances are 2.799A for Nb-Te bonds and 2.545A for Co-Te bonds.     

The crystal structure of Bi14I4 condensed bismuth clusters

The crystal structure of Bi₁₄I₄ — the final known member of binary bismuth halides — was determined by the single crystal X-ray diffractometer technique (P2₁/m, Z = 1, a = 13.309(3) Å, b = 11.447 (3) å, c = 4.342(1) å, γ = 92.08(3)°, R/R_w = 0.060/0.060 for 369 reflections, sinθ/λ≤ 0.593, MoKγ). The structure consists of condensed bismuth clusters and is build up from infinite one-dimensional bismuth nets running along the c-axis and limited by iodine atoms in another direction. The common structural features of bismuth subhalides containing condensed clusters are also considered based on the analysis of interatomic distances and bond angles. The influence of the lone pair of electrons of the bismuth atom on the geometry of bismuth coordination polyhedra, and the connection between bismuth atoms coordination and the formal oxidation state of these atoms is discussed.     

钼簇合物反应性能的研究: {Mo3S4[S2P(OEt)2]4H2O}的加硫反应以及产物{Mo3(μ3-S)(μ-S2)3[S2P(OEt2]3I}的晶体结构

由贫硫化合物{Mo_3S_4[S_2P(OEt)_2]_4·H_2O}通过加硫获得了富硫化合物{Mo_3S_7[S_2P(OEt)_2]_3·I}(CH_8C_6H_5).化合物属三斜晶系,空间群PI,晶胞参数为a=10.350(1)A,b=13.931(4)A,c=16.369(3)A,α=103.69(2),β=86.62(1),γ=111.99(2)°,V=2183A~3;z=2,D_c=1.817g·cm~(-3).最终结构偏离因子R为0.042. 簇分子{Mo_3(μ_3-S)(μ-S_2)_3[S_2P(OEt)_2]3·I}属{Mo_3(μ3一Y)(μ-S_2)_3[S_2P(OEt)_2]_3·X}(Y=O,S;X=Cl,I)系列构型.{Mo_3}基本上是一个正三角形,Mo—Mo键长分别为2.721(1),2.724(1),2.725(1)A,Mo的配位多面体为七个硫原子组成的畸变五角双锥,有一个I原子联结着三个(S_2)~(2-)桥基的三个不与Mo共平面的S原子,I—S距离平均为3.169A,比相应的Van der Waals距离(～4.00A)明显地短,显示一定程度的成键作用,簇分子的这一构型是一种较为稳定的结构类型.     

Preparation and Crystal Structure of Bis（2－thenoyltrifluoroacetone）Copper（Ⅱ）

ＰｒｅｐａｒａｔｉｏｎａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＢｉｓ（２－ｔｈｅｎｏｙｌｔｒｉｆｌｕｏｒｏａｃｅｔｏｎｅ）Ｃｏｐｐｅｒ（Ⅱ）ＷａｎｇＤｏｎｇ－Ｍｅｉ；ＹａｎｇＲｕｉ－Ｎａ；ＨｕＹｉ－Ｍｉｎ；ＪｉｎＤｏｕ－Ｍａｎ（ＨｅｎａｎＩｎｓｔｉ...     

Die Kristall- und MolekülStruktur von Jodo- bis- [2-(diphenylphosphinomethyl)pyridin]nickel(II)-jodid,einem diamagnetischen,quadratisch-pyramidalen Komplex mit d8-Konfiguration

The Crystal and Molecular Structure of Jodo-bis-[2-(diphenylphosphinomethyl)pyridine]nickel(II)-jodide, which is a Diamagnetic, Square-pyramidal Complex with d⁸-Configuration The crystal and molecular structure of the title compound has been determined by single-crystal X-ray methods with 5119 independent reflextions and refined to R = 0.061 for 4321 observed reflections. The crystals are monoclinic, space group P2₁/n, a = 9.016 ± 0.005, b = 21.612 ± 0.012, c = 17.871 ± 0.010 Å, with and β = 96.32 ± 0.15°; Z = 4. The structure was solved by PATTERSON and FOURIER methods and refined by least squares. The molecule cation has approximate C_s-symmetry. The co-ordination around the nickel atom is approximate square pyramidal with two nitrogen and two phosphorus atoms in the basal plane and the jodine atom in the apex. The Ni? J-distance with 3.047(3) Å is very long. In the basal plane, the nitrogen and phosphorus atoms have cis configuration and the geometric arrangements by the two chelate-5-rings are different. The mean Ni? N(1.963(13)Å) and Ni? P(2.166(5)Å) bond lengths are considerably 0.05 longer and 0.10 Å shorter respectively than the corresponding covalent bonding values, derived from the sum of the covalent radii.     

[ReCl3(NSCl)2(CH3CN)]. Synthese,IR-Spektrum und Kristallstruktur

[ReCl₃(NSCl)₂(CH₃CN)]. Synthesis, I. R. Spectrum, and Crystal Structure Black, moisture sensitive crystals of the title compound are obtained from [ReCl₃(NSCl)₂]₂ and acetonitrile in dichloromethane. The complex is characterized by its i.r. spectrum and an X-ray crystal structure determination (2483 observed independent reflexions, R = 0.035). Crystal data: triclinic, space group P1 , Z = 2, a = 681.8, b = 899.9, c = 1104.0 pm, α = 110.50, β = 97.90 and γ = 101.34°. In the monomeric [ReCl₃(NSCl)₂(CH₃CN)] molecule the Re atom has a distorted octahedral coordination with meridional arrangement of the Cl atoms. The chlorothionitrene ligands have nearly linear ReNS groups with bond lengths that correspond to double bonds (ReN 178 and 179 pm); this agrees with the NReN bond angle of 100°.