关附庚素碘甲烷盐的晶体结构和分子构型

关附庚素是从毛茛科植物黄花乌头块根中分得的一种生物碱。关附庚素碘甲烷盐的晶体属正交晶系;空间群为D_2~4-P2_12_12_1;晶胞中含四个分子;晶胞参数a=16.87A,b=16.93A,c=10.09A。强度数据用PW1100四圆衍射仪收集,采用MoK_a辐射。晶体结构用重原子法导出;碘原子由Patterson法求得;其它卅五个非氢原子的坐标由三维Fourier综合确定。结构用块对角矩阵进行最小二乘修正,然后加卅六个氢原子位置又修正了一轮,最后的R因子为0.0578,并根据反常散射确定绝对构型。     

[Pt(TMCPDA)(Ac-Cl)2]的分子结构和晶体结构

[Pt(TMCPDA)(Ac-Cl)_2]属四方晶系,空间群为P4_32,2,单胞参数为:a=b=14.618(4),c=16.654(2)A,V=3558.9A~3,Z=8,D_c=1.957gcm~(-3).在Enraf-Nonius CAD4衍射仪上用MoK,射线,收集了0(?)2θ(?)44°的独立衍射点2184个。铂原子坐标用直接法解法。非氢原子和部分氢原子的坐标用数轮差富利叶合成得到。部分氢原子坐标用理论计算定出。铂原子各向异性热振动参数和其他原子的各向同性热参数经全矩阵最小二乘法修正。最后偏离因子R=0.065,R_w=0.077.分子的绝对构型已测定,不对称碳原子为1s,3R.     

2-(2′-噻唑偶氮)-5-二乙胺基酚的晶体结构

用 Philips PW-1100型单晶衍射仪收集了2-(2′-噻唑偶氮)-5-二乙胺基酚晶体的三维衍射数据.应用最小函数法和直接法测定了晶体结构.在衍射仪上测得晶胞常数 a=20. 018(±0. 005),b=8. 894(±0. 03) (?),c=7. 658(±0. 002) ,z=4. 空间群为P2_12_12_1. 原子的坐标参数、温度因子参数及非氢原子的各向异性温度因子参数一起进行了全矩阵最小二乘修正,最后 R 因子为0. 072,加权以后 R_W 为0. 051. 晶体结构分析结果表明:二乙胺基有效地参与了共轭体系,使二乙胺基的强助色性能得到了很好的解释.     

正交晶系天花粉蛋白2.4分辨率的晶体结构和分子结构

在酸性条件下(pH=5.4)培养出正交晶系天花粉蛋白晶体。用面探测器收集了X射线衍射强度数据。以C2空间群天花粉蛋白2.6分辨率的晶体结构中的分子模型作为已知结构模型,用分子置换法解出正交晶系P2_12_12_1空间群天花粉蛋白的晶体结构。所得到的初始结构模型先后用模拟退火法和立体化学制约的最小二乘修正技术对原子坐标及温度因子进行修正。最后在2.4分辨率范围内模型的β因子为0.197,键长的均方根误差为0.021,键角距离的均方根误差为0.081。分子结构模型与(2Fo—Fc)为系数的电子云密度图吻合得很好。键长键角合理。结构测定结果表明,P2_12_12_1;空间群天花粉蛋白的分子的空间结构与单斜晶系C2空间群中的分子结构甚为相似。     

柳珊瑚酸的分子结构和绝对构型

本文首次应用X射线单晶衍射法证实了一种新的倍半萜骨架,并测定了柳珊瑚酸的分子结构和绝对构型。柳珊瑚酸的晶体属于正交晶系,空间群:D_2~ -P2_12_12_1,晶胞参数:a=16.135,b=13.189,c=12.901,α=β=γ=90°。单胞中分子数为8,不对称单位含两个分子,用直接法导出全部非氢原子位置,经最小二乘法修正后,最终偏离因子R=0.056。文中还对柳珊瑚酸分子的结构进行了讨论,并对核磁共振溶剂效应有关理论进行了较深入的讨论,初步探讨了分子结构与其毒性之间的关系。     

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。     

十二硼十二氢镍乙二胺晶体结构的研究

Ni(en)_3B_(12)H_(12)晶体属于三方晶系,空间群为R_3,晶胞参数为:a=b=12.890(2),c=23.955(20),α=B=90°,Υ=120°,Z=6。在室温下用CAD-4衍射仪收集单晶衍射强度数据(MOK_α);重原子法和差Fourier法解出全部非氢原子坐标,用加氢程序定出全部氢原子的坐标。各原子坐标及热振动参数经全矩阵最小二乘方修正,对于985个独立衍射点[I≥3σ(I)]最后偏离因子R=0.069。结构分析表明,该化合物属于离子型,Ni(en)_-~(2+)离子和B_(12)H_(12)~(-2)离子间相互以正三角双锥方式配位。Ni(en)~(2+)离子具有D_3对称性,Ni-N平均键长为2.138,B_(12)H_(120~(-2)离子呈正二十面体构型,B-B平均键长为1.786。     

1,1—环丙烷二羧酸根二氨合铂的晶体结构和振动光谱的简正坐标分析

测定了1,1-环丙烷二羧酸根二氨合铂([Pt(NH_3)_2CPrDCA]·H_2O)的晶体结构。晶体属正交晶系,空间群为Pnma,a=6.571(2),b=9.709(3),c=14.205(5)A,Z=4。用Patterson函数导出Pt原子坐标,经差值Fourier合成获得全部非氢原子坐标,用最小二乘法修正,最终R因子为0.058,采用U-B力场进行了[Pt(NH_3)_2CPrDCA]分子的简正坐标分析,振动基频的计算值与观测值符合,两者平均偏差5.63cm~(-1),最大误差15.7cm~(-1),证实了振动光谱的归属。     

鬼灯擎素的结构分析

本文报道了从鬼灯擎(Rodgersid aesculifolia Batal)中提取的鬼灯擎素(Bergenin)晶体的结构研究。鬼灯擎素晶体为正交晶系,C_(14)H_(18)O_(10),M_r=346.28,其晶胞参数a=7.468(9),b=13.899(4),c=14.228(0)A;空间群为P2_12_12_1;晶胞内分子数Z=4,D_c=1.5560g/cm~3,结构模型由SHELXTL程序解出;经Fourier合成和最小二乘修正,最后的偏离因子R=0.028。此外,利用晶体结构分析所得分子中各原子的坐标,以半经验分子轨道法CNDO/2程序计算了分子总能量、净电荷分布以及Wiberg键级等,并以此讨论了分子的反应活性中心。     

十钒酸四氢钠与六次甲基四胺加合物的晶体结构

本文合成的晶体属于空间群C_i~1-Pi。晶胞参数a=9.589五,b=10.486,c=11.139,α=103.2°,β=98.20°,γ=103.16°。由Patterson函数得到诸钒原子坐标参数后,用Fourier法及差值法导出全部非氢及氢原子,最终确定晶胞中所包含的化学物种及确切成分为[Na~ ]_2[H_2V_(10)O_(28)~(4-)]·2[(CH_2)_6N_3N·H~ ]·8H_2O。经块矩阵修正所得一致性因子R=0.0279。     

磺基水杨酸盐的晶体结构和倍频效应

用X射线单晶衍射法测定了三水合二（5－磺基水杨酸）钙（C（14）H1（10）O（12）S2Ca·3H2O，1）和二水合（5－磺基水杨酸）二钾（C7H4O6SK2·2H2O，2）的晶体结构·化合物1属单斜晶系，空间群为Pn。，晶胞参数a＝5．604（1），B＝18．560（4），c＝10．006（2），β＝102．19（3）°，Z＝2，最终R＝0．0244．化合物2属正交晶系，空间群Pbca，晶胞参数a＝25．841（5），b＝12．186（2），c＝7．739（2），Z＝8，最终R＝0．0308．化合物1粉末倍频效应为2．86倍KH2PO4，其厘米级单晶体的紫外端吸收边经在375nm附近     

Synthesis, structure and spectral investigation of hydrogen bonded helical chain in mixed ligand Cu(II) pyrimidone complex

A simple mono-aqua-dichloro copper(II) pyrimidone complex has been synthesized and characterized using various spectral techniques such as Infrared and Raman in addition to the single crystal X-ray diffraction. The single crystal X-ray analysis carried out for the complex under study brings out the fact that there are two molecules in the unit cell with parameters a = 9.657(2); b = 3.857(2); c = 10.781(2); alpha = 90 degrees; beta = 107.781 degrees; gamma = 90 degrees; V = 382.891 and are crystallized in monoclinic crystal system with Pn space group. In solid state the molecules are interconnected through strong hydrogen bonding [O4...H21-O2W = 2.644 angstroms; O4...H21 = 1.853 angstroms; angleO4...H21-O2W = 172.87 degrees;] formed between the coordinated water molecule (O2W) and the exocyclic ketonic oxygen of the pyrimidone ring (O4). This H-bonding interaction causing a twist in the C1=O1...H21 segment [angleC1=O1...H21 = 122.29 degrees] in combination with weak pi-pi stacking interaction (3.857 angstroms) of the adjacent pyrimidone rings brings the single stranded helical chain which possesses both P and M sense of supramolecular helical assembly. The internal and external modes of vibrations of the crystal under study have been estimated and discussed by applying group theoretical methods.     

Synthesis, X-ray crystal structure and X-band EPR of [Cu(H(2)O)(2)(imH)(4)] x Sq single crystals

The copper salt [Cu(H(2)O)(2)(imH)(4)] x Sq has been synthesized at room temperature. Crystal structure of the [Cu(H(2)O)(2)(imH)(4)] x Sq (Sq is squarete dianion (C(4)O(4)(2-)) and imH is imidazole (C(3)H(4)N(2))) complexes has been investigated by single-crystal X-ray diffraction analyses and the environment of copper ion has been identified by EPR. The single crystal is triclinic with the space group P1. The unit cell dimensions of the crystals are a=9.317 Angstrom, b=9.958 Angstrom, c=12.130 Angstrom, alpha=69.99 degrees , beta=76.61 degrees and gamma=78.13 degrees . The unit cell contains two molecules. The Cu(II) atom has an octahedral arrangement in which the Cu(II) ion lies on the inversion canter and is coordinated by four imidazole ligands with the equatorial plane and two water molecules with the octahedral axial. The complex shows a normal magnetic moment and the single crystal EPR spectra consist of two sets of four hyperfine lines of copper. The ground wave function of the hole of the Cu(2+) is an admixture of d(x(2) - y(2)) and d(z(2)) states.     

Two-dimensional coordination polymers of copper(II) with oxalate: lattice water control of structure

Three oxalate copper(II) complexes, [Cu(bipy)(C(2)O(4))(H(2)O)].2H(2)O (1), [Cu(nphen)(C(2)O(4))(H(2)O)].2H(2)O (2), and [Cu(phen)(C(2)O(4))(H(2)O)].H(2)O (3) (bipy = 2,2'-bipyridine, nphen = 5-nitro-1,10-phenanthroline and phen = 1,10-phenanthroline), have been synthesized and their crystal structures have been determined. Compound 1 crystallizes in the triclinic space group P1 with a = 7.2554(10) A, b = 10.5712(14) A, c = 10.8178(15) A, alpha = 62.086(2) degrees, beta = 77.478(3) degrees, gamma = 81.773(3) degrees, and Z = 2. Compound 2 crystallizes in the triclinic space group P1 with a = 9.582(2) A, b = 10.086(2) A, c = 10.592(2) A, alpha = 64.18(3) degrees, beta = 79.47(3) degrees, gamma = 60.06(3) degrees, and Z = 2. Compound 3 crystallizes in the monoclinic space group P2(1)/n with a = 8.4655(7) A, b = 9.7057(8) A, c = 17.4572(14) A; beta = 103.865(2) degrees, and Z = 4. The crystal structures of all complexes consist of neutral [Cu(L)(C(2)O(4))(H(2)O)] (L = bipy, nphen, and phen) units and one or two lattice water molecules in the unit cell. Each copper atom in 1, 2, and 3 involves a five-coordinate CuN(2)O(2)O' environment, with a distorted square-pyramidal structure. In 1 and 2, two lattice water molecules are around each unit of [CuL(C(2)O(4))(H(2)O)] (L = bipy and nphen) and form two-dimensional networks. Only one lattice water molecule is found in the unit cell of 3 and the two-dimensional structure is different from 1 and 2. The extended three-dimensional structure is formed through pi-pi interactions between layers. The influences of hydrogen bonds and the sizes and Lewis basicity of ligands to the structures were discussed.     

Synthesis and Crystal Structure of 3-(Pyrrole-2''-carboxamido)propanoic Acid·(1/2)H2O

3-(Pyrrole-2'-carboxamido)propanoic acid I has been synthesized from the reaction of β-alanine methyl ester with 2-trichloroacetylpyrrole followed by saponifying and acidating in 85.4% yield, and the crystal structure of 3-(pyrrole-2'-carboxamido)propanoic acid· (1/2)H2O (C8H11N2O3.5, Mr = 191.19) was obtained and determined by X-ray diffraction method. The crystal is of monoclinic, space group C2/c with a = 19.010(4), b = 8.3515(17), c = 13.788(3) (A), β = 125.88(3)°, V = 1773.6(6) (A)3, Z = 8, Dc = 1.432 g/cm3, λ = 0.71073 (A), μ-MoKα) = 0.114 mm-1 and F(000) = 768. The structure was refined to R = 0.0354 and wR = 0.0942 for 1642 observed reflections with I > 2σ(I). It is revealed that the title compound has one pyrrole ring and one propionic acid subchain linked by an amido bond at C(4), and there are 8 molecules of com- pound I and 4 crystal water molecules in each unit cell. The supramolecular layers are stabilized by the hydrogen bonds of N(2) H…O(2), N(1) H…O(4), O(4) H(1W)…O(2) and O(3) H…O(1).     

Synthesis and Crystal Structure of 3-(Pyrrole-2′-carboxamido)propanoic Acid·(1/2)H_2O

1 INTRODUCTION Pyrrole and its derivatives have attracted much attention due to their chemical properties as well as biological activities[1]. They have been widely used to produce pharmaceutical, essences, biochemicals, etc. It has been found that a great number of pyrrole derivatives present antitumor and antiviral activi- ties[2 ~ 5]. During our searches for bioactive com- pounds, a series of pyrrole derivatives were synthe- sized[6, 7]. We report here the synthesis of 3-(pyrrole- 2?-…     

Synthesis and Crystal Structure of Mn（phen）（PhCOO）2（H2O）

1 INTRODUCTION During the last decade the manganese che- mistry has aroused great interest due to its diverse redox functions of enzymes in photosystem Ⅱ and its specially structural, magnetic and spectroscopic properties[1, 2]. A lot of manganese complexes involving carboxylate ligands have been reported, and their properties been fully explored[3, 4]. The coordination environment of the manganese site in biosystem often consists of oxygen and nitrogen atoms from the carboxylate groups…     

新型—维锯齿链状聚金属氧酸盐配位聚合物［｛La(DMSO)_6(H_2O)}·(PMo_(12)O_(40))·H_2O］_n的合成、结构及表征

以a-H_3PMo_(12)O_(40)·nH_2O, La_2O_3和二甲基亚砜（DMSO）为原料，在 乙腈和水的混合溶剂中制得了一维锯齿链状配位聚合物［｛La(DMSO)_6(H_2O)}· (PMo_(12)O_(40))·H_2O］_n,X射线单晶衍射结果表明，聚合物中金属配阳离子与 杂多阴离子骨架通过Mo-O_d-La-O_d-Mo相连并形成一维无限链，每一个不对称结构 单元中含一个结晶水，La~(3+)的配位数为九，三帽三棱柱构型，配位氧原子分别 来自6个DMSO分子，1个H_2O分子和2个相邻杂多阴离子的端氧，晶体氧于单斜晶系 ，P2_1/c空间群，a=1.3916(3)nm,b=1.7058(3)nm,c=2.4750(5)nm,β=99.16(3)~° ,Z=4,V=5.800(2)nm~3,D_c=2.825g/cm~3,R_1=0.0446,wR_2=0.0871,IR光谱和X射线 单晶衍射结果一致表明，在固态条件下配阳离子和杂多阴离子之间存在相互作用， UV光谱表明，在稀的水溶液中，由于溶剂化作用，杂多阴离子与配阳离子处于解离 状态，热性质研究表明，形成标题化合物后，杂多阴离子的热稳定性与磷钼酸相比 明显增强。     

有机锡配合物{[(n-C8H17)2Sn(O2CCH2CS2NC4H8O)]2O}2的合成，表征及晶体结构

The title complex {[(n-C₈H₁₇)₂Sn(O₂CCH₂CS₂NC₄H₈O)]₂O}₂ has been synthesized by the reaction of (morpholinylthiocarbamoylthio)acetic acid with the di-n-octyltin oxide in 1∶1 molar ratio. The complex was characterized by elemental analysis, IR and ¹H NMR. The crystal and molecular structure of complex was determined by X-ray single crystal diffraction. The crystal belongs to triclinic system with space group P1 and unit cell dimensions: a=1.201 5(9) nm, b=1.481 8(11) nm, c=1.894 1(14) nm, α=72.485(10)°, β=88.586(10)°, γ=66.893(9)°, and Z=1, μ=1.034 mm^-1, V=2.941(4) nm³, D_c=1.295 g·cm^-3, F(000)=1 196, R₁=0.058 8, wR₂=0.155 8. The complex is a centrosymmetric structure with a four-membered central endo-cyclic Sn₂O₂ unit in which two bridged oxygen atoms both connect with an exo-cyclic tin atom. The endo-cyclic tin atoms and the exo-cyclic tin atom are all five-coordinate and have coordination geometry of distorted trigonal bipyramid with an additional weak coordination carboxylate oxygen. Four carboxylate ligands are divided into two types. And two of them are monodentate and connecting to each of exo-cyclic tin atoms by using one oxygen atom, whereas the others bridge to each pair of exo-and endo-cyclic tin atoms utilizing one oxygen atom. CCDC: 277048.     

沙蚕磷草酸盐的合成与晶体结构

合成了一种新的有机磷杀虫剂沙蚕磷[O,O,O',O'-四甲基－S,S'-(2-N,N-二甲氨基-1,3-亚丙基)-双-二硫代磷酸酯],并制备了它的草酸盐。测定了沙蚕磷草酸盐的晶体结构,结果表明,该晶体属三斜晶系,P1空间群,晶胞参数为:a=0.74342(5)nm,b=1.1057(4)nm,c=1.45295(11)nm,α=98.018(11)°,β=101.012(4)°,γ=96.224(10)°,Z=2。通过元素分析,MS、IR及^1H,^1^3CNMR表征了该化合物的结构。