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．     

两种不同构型的吡唑啉酮衍生物的合成与结构

报道了PMBP-PCH(PCH为2-吡啶甲酰肼)和PMBP-INTH(INTH为异烟酰肼)2种化合物的合成与晶体结构分析,PMBP-PCH属三斜晶系,具有P空间群,a=7.783(2),b=10.993(3),c=12.621(3)?=92.96(2),=103.87(2),g=101.54(2),V=1021.5(5)3,Z=2,Dc=1.307g/cm3,m(MoK?=0.088mm-1,F(000)=421,R=0.0436,wR=0.0937.晶体结构表明,在此分子内形成了一个大的共轭体系,由于分子间氢键力的作用,使它们在晶体中以二聚体的形式存在.PMBP-INTH晶体属单斜晶系,具有P21/c空间群,a=14.083(4),b=13.865(3),c=10.609(2)?=101.66(2)o,V=2028.8(8)3,Z=4,Dc=1.301g/cm3,m(MoK?=0.087mm-1,F(000)=832,R=0.0473,wR=0.0898.此化合物在O(1)原子与邻近分子的N(1)原子之间存在较强的氢键,在结晶的过程中,通过分子间质子迁移,使该化合物形成了1个以N(2)为负电荷中心,N(1)为正电荷中心的两性离子结构,且分子通过此氢键形成了一维链状结构,并沿b轴呈层状堆积.     

基于萘基块新型开链冠醚的合成及晶体结构研究

以3,6-二溴-2,7-二羟基萘为起始原料,经与2-溴-N-苯基乙酰胺醚化,再用硼氢化钠和三氟化硼乙醚还原得基于萘基块新型的开链冠醚,两步总收率为96%.利用单晶X衍射研究其结构,晶体为三斜晶系,P-1空间群,a=9.588(3),b=10.898(3),c=13.060(4),α=103.190(4)°,β=93.953(4)°,γ=115.622(5)°,V=1176.0(6)3,Z=2,Dc=1.571 g/cm3,λ=0.71075 nm,μ(Mo Kα)=3.472 mm-1,Mr=353.22,F(000)=560.在晶体结构中,分子中的一个N—H基团与另外一分子形成双分叉氢键N—H…Br和N—H…O,进而组装成二聚体.这些中心对称的二聚体进一步通过C—H…π相互作用叠加成二维层状结构平行于(110)面.     

[Co(Phen)2(H2O)2](HL)NO3·3H2O的合成及晶体结构

在水溶液中,以邻菲咯啉、丁二酸与硝酸钴为原料合成了一个新的超分子化合物[Co(Phen)2(H2O)2].(HL).(NO3).3H2O,并经元素分析、IR、X射线单晶衍射分析进行了结构表征.结构分析表明,晶体属三斜晶系,P1-空间群,a=0.968 0(2)nm,b=1.370(3)nm,c=1.394 9(3)nm,α=61.714(3)°,β=71.495(4)°,γ=79.575(4)°,V=1.543 7 nm3,Z=2,ρ=1.481 g/cm3,C28H31CoN5O12,Mr=688.51,F(000)=714 andμ=0.627 mm-1,7 754个独立衍射点中,5 428个可观察点满足I≥2σ(I),R1=0.074 5,wR2=0.210 7.晶体中[Co(Phen)2(H2O)2]2+通过π-π相互作用堆积成二维层状结构,层间通过氢键作用构成三维超分子.     

一维链状高价锰配合物[Mn_2(C_7H_4O_3)_4(CH_3OH)_2]·4H_2O_2CH_3OH的合成与结构

合成了一维链状高价锰配合物[Mn2(C7H4O3)4(CH3OH)2]4H2O2CH3OH,并对其进行了IR、X-射线衍射、UV-Vis和TG-DSC等表征。单晶衍射结果表明,该配合物晶体属三斜晶型,空间群P?晶胞参数a=7.653(5),b=10.486(7),c=12.943(8),=103.24(1),?=104.55(1),?=110.11(1),V=885.4(9)3,Z=1。UV-Vis光谱在547nm有一个吸收峰,相应于Mn(Ⅳ)的d-d电子跃迁光谱。     

三硫代-α-过萘甲酸基吡啶合铜的二聚体的合成和结构

标题化合物由α-萘荒酸和CuCl~2在吡啶溶剂中反应或由Cu~4(α-C~10H~7CSS~2)~4.1/2CS~2在吡啶和甲醇的混合溶剂中结晶合成得到.此化合的结构由单晶X射线衍射分析测定.晶体属三斜晶系,C~4^1-PI空间群,晶胞参数α=7.085(2),b=8.672(3),c=13.598(5)A,α=92.40(3),β=102.59(4),γ=105.67(4),V=780.6A^3,Z=1.对于2390个衍射点结构修正后,R=0.058.化合物的分子处在对称中心上,Cu-Cu键长(2.616A)表明铜原子之间有一定的相互作用,如果不考虑Cu-Cu的相互作用,周围的S和N原子以变形的四面体构型与Cu配位.     

[Li(THF)_4][GdCl_4(THF)_2]的晶体结构

氯化钆与对-甲基苯基锂在四氢呋喃中反应得到产物之一为[Li(THF)_4][GdCl_4-(THF)_2],(M_r=738.2),在-70℃下进行X-射线衍射研究。其晶体属单斜晶系,P2/n空间群。晶体学参数为a=13.263(2),b=8.474(1),c=14.961(0);β=99.72(1)°,V=1657.23(?)~3,Z=2,D_c=1.48g/cm~3,F(000)=750,μ_c=24.2cm~(-1),最终偏离子为R=0.0614。研究结果表明,本题晶体是离子型晶体,围绕Gd~(3+)的四个Cl~-离子和两个THF分子的氧原子构成畸变的八面体。Li~+周围的四个THF分子的氧原子构成一个近似的四面体。     

α'-(BEDT-TTF)_2C_6H_4(SO_3)_2的合成、结构与导电性

用恒电流电化学结晶法合成了一种新的基于BEDT-TIF的电荷转移盐α'-(BEDT- TIF)_2C_6H_4(SO_3)_2 [BEDT-TIF = 双亚乙基二硫四硫富瓦烯,C_6H_4(SO_3) _2~(2-) = 对苯二磺酸根]。通过四圆X射线衍射方法测定了α'-(BEDT-TTF) _2C_6H_4-(SO_3)_2的结构。晶体属于单斜晶系,P2/n空间群;晶胞参数：a = 0. 77937(17)nm, b = 0.66989(11) nm, c = 3.4422 (7) nm, β = 91.135(12) °, V = 1.7968(6) nm~3。该晶体中BEDT-TTF~+自由基沿a轴方向形成具有二聚体结构 的交错排列型柱状堆积,沿b轴方向由户并户强分子间相互作用形成一维分子链。 电荷补偿阴离子C_6H_4(SO_3)_2~(2-)则在a方向存在较强的作用。沿c轴方向, BEDT-TTF~+自由基层和阴离子层交替排列形成夹心式结构。α'-(BEDT-TTF) _2C_6H_4-(SO_3)_2在ab面的某方向的室温电导率为0.5913 Ω~(-1)·m~(-1),电 阻率-温度测定曲线表明它具有半导体导电行为。在150K附近,晶体发生了某种相 变。     

新磺酰脲类化合物N-[2-(4-甲基)嘧啶基]-N''''-2-甲氧羰基苯磺酰脲的合成及其二聚体结构

合成并用X-射线晶体衍射法测定了标题化合物 (C14H14N4O5S, Mr = 350.35)的结构。晶体属正交晶系, 空间群为Pna21, 晶胞参数a = 13.242(4), b = 9.478(3), c = 24.889(8) ? V = 3123.7(17) 3, Z = 8, Dc = 1.490 g/cm3, m = 0.241 mm-1, F(000) = 1456。独立可观测点数为3268。最终偏离因子R = 0.0592, wR = 0.1217 (I > 2s(I) 2153), S = 1.122。X-射线衍射证实标题化合物分子晶体中存在2种构型, 分子中苯环所在的位置同嘧啶磺酰脲平面的取向相反。每种构型中嘧啶磺酰脲、苯环及甲氧羰基分别形成3个独立的平面共轭体系。除此之外, 经由O(1)N(6)和N(2)O(6)形成的分子间氢键以及苯环平面间的p-p 相互作用将2个分子结合在一起从而形成二聚结构。     

[(O)MoCu_3(μ_3-S)_3(μ_3-Cl)(PPh_3)_3]·2THF的合成及其晶体结构

固体化合物(NH_4)_6Mo_7O_(24)·4H_2O和(PPh_3)_2CuCl与饱和液体NH_4HS反应获得桔红针状标题晶体。晶体空间群为P2_1/c,晶胞参数a=11.742(2),b=28.186(7),c=19.304(3),β=100.57(2)°,V=6280.4(?)~3,D_c=1.46g/cm~3,Z=4,F(000)=2816。在3≤2θ≤45°范围内收集到8414个独立衍射强度数据,其中3856个I≥1.5σ(I)强度数据参加结构计算。标题化合物分子是以{MoCu_3S_3Cl}类立方烷型簇为核心的分子,Mo—Cu的平均距离为2.716。     

Synthesis and Crystal Structure of Pd(AETYF)Cl_2CH_2Cl_2 [AETYF = 4''''5''''Diaza-9'''' (4,5-bis(ethylthio)-1,3-dithiole-2-ylidene)-fluorene]

1 INTRODUCTION Over the past decades, extensive work has been carried out to study palladium complexes in organic synthesis, structural analysis, chemical reactivity, catalytic process, spectroscopy and functional mate- rials[1]. Especially the anti…     

3,6-二甲基-9-对硝基苯基-1,8-二氧代-2,7,10-三氧杂蒽的合成和晶体结构

标题化合物C19H13NO7 是由对硝基苯甲醛, 6-甲基吡喃酮在微波辐射下反应而得, 反应在五分钟内完成。结构通过单晶 X-射线衍射法测定, 其晶体属单斜晶系,空间群P21/c, a = 10.669(1), b = 11.544(1), c = 14.045(2) ? b = 105.98(1) , V = 1663.0(3) ?, Mr = 367.30, Z = 4, Dc = 1.467g/cm3, l = 0.71073 ? m(MoKa) = 0.114 mm-1, F(000) = 760, R = 0.0380, wR = 0.0944。在分子结构中存在一个大的共轭体系。     

Synthesis and Crystal Structure of 1-(1''''- t- Butyl-5''''-methyl-4-pyrazolyl-carbonyl)- 3,5-dimethyl-1H-yl-pyrazole

1 INTRODUCTION Pyrazole and its derivatives represent one of the most active classes of compounds possessing a wide spectrum of biological activities. During the past years considerable evidence has been accumulated to demonstrate the efficacy of pyra- …     

Crystal and Molecular Structure ofN—（Pyridin—2—yl—carbonyl）—2—ethoxycarbonyl—benzene sulfonamide

1 INTRODUCTION The sulfonylurea herbicides have been well known for their exceptional low dosage, good crop selectivity and low mammalian toxicity. They can block the biosynthesis of branched amino acids by inhibiting ALS enzyme in plants so as to inhibit weeds. Levitt G. divided the structure of sulfonylurea into three parts: (1) aryl group, (2) bridge and (3) heterocycle[1]. Later Ort et al. modified the bridge by omitting moiety NH in the bridge, synthesized N-(substituted pyrimid…     

4-[2-(4,6-二甲氧基-2-嘧啶氧基)苄胺基]苯甲酸正丙酯的合成和晶体结构

2-甲砜基-4,6二甲氧基嘧啶和N-(4-丙氧羰基苯基)-2-羟基苄胺在四氢呋喃溶液中反应, 生成标题化合物4-[2-(4,6-二甲氧基-2-嘧啶氧基)苄胺基]苯甲酸正丙酯,并测定了其晶体结构。该化合物分子式为C23H25N3O5,晶体属单斜晶系,空间群为P2/n,晶胞参数为a = 14.8504(8),b = 9.4420(4),c = 16.3129(9) 牛 = 104.881(1)埃琕 = 2210.6(2) 3,Z = 4,Dc = 1.272 g/cm3,F(000) = 896.00,(MoK? = 0.91 cm-1,R = 0.051,wR = 0.118,获得19761衍射数据,其中独立衍射点5004个。经元素分析、IR、MS和HNMR等对化合物的结构进行了表征。在分子结构中,各有3个不同的共轭平面。嘧啶环和苯环(C(7) C(12)),及苯环(C(14) C(19))的夹角分别为99.18 , 164.15埃?个苯环之间的夹角为94.93啊;衔锍世啻焦瓜蟆?     

Synthesis and Crystal Structure of 3,3′-(Hexane-1,6-diyl)bis(1-acetyl-5,5-dimethylhydantoin),a New Inducer of Differentiation

1 INTRODUCTION Hexamethylenebis[acetamide] (HMBA) is an effective agent in phaseⅡclinical trial[1] that induces differentiation of certain types of tumors to nonmalignant phenotypes. In an attempt to discover more efficient inducers, a number of derivatives of HMBA have been synthesized and evaluated in vitro[2, 3]. The results proved that increasing the number of functional groups could enhance the anticancer activity. In addition, it was evident that compounds with six methylene i…     

Syntheses and Crystal Structures of Two New Compounds Containing Triarylamine and Benzoic Hydrazide Units

1 INTRODUCTION The design and fabrication of efficient light emitting devices based on organic materials has been an active research area due to their possible application in display technology[1～5]. One of the most fascinating advantages in using th…     

Synthesis and Crystal Structure Analysis of 5?-O-Tosyl-2,3?-anhydrothymidine

In this paper, 5?-O-tosyl-2,3?-anhydrothymidine has been synthesized and its crystal structure was analyzed. The crystal belongs to the triclinic system, space group P1, with a = 5.397(2), b = 6.1886(18), c = 3.507(5) ?, α ?= 87.74(2), β ?= 89.84(4), γ ?= 73.79(2)°, C17H18N2O6S, Mr = 378.39, Z = 1, V = 432.8(3) ?3, Dc = 1.452 g/cm3, F(000) = 198 and Flack = -0.11(14). No intermolecular hydrogen bonds exist in the crystal, and the angle between benzene ring and pyrimidine planes is 32.23°.     

Synthesis and Crystal Structure of Copper(II) Complex with Mixed Bipyridine and 2-Hydroxy-1-naphthaldehyde Ligands

1 INTRODUCTION Galactose oxidase is a monomeric enzyme that catalyzes the stereospecific oxidation of a broad range of primary alcohol substrates and possesses a unique mononuclear copper site essential for catalyzing a two-electron transfer reaction during the oxidation of primary alcohol to corresponding aldehydes[1]. The catalytic reaction is shown in Eq. 1. RCH2OH + O2 RCHO + H2O2 (1) A recent report on the crystal structure of galactose oxidase reveals a unique mo…