3,3,6,6-四甲基-9-对氯苯基-1,8-二氧代-2,3,4,5,6,7-六氢氧杂蒽的合成和晶体结构

标题化合物C2 3H2 5O3Cl是由对氯苯甲醛与 5,5 二甲基 1 ,3环己二酮在乙二醇中反应而得。结构通过单晶X 射线衍射法测定 ,其晶体属于单斜晶系 ,空间群P2 1 /n ,a =6.0 4 8(1 ) ,b =1 9.543(3) ,c =1 7.42 0 (3) ,β =97.2 9(1 )° ,V =2 0 4 2 .2 (6) 3,Mr=384.90 ,Dc=1 2 52 g/cm3,Z =4,μ(MoKα) =2 .0 6cm- 1 ,F(0 0 0 ) =81 6。晶体结构用直接法解出 ,经用全矩阵最小二乘法对原子参数进行修正 ,最终的偏离因子为R =0 .0 39,Rw=0 .0 4 7。X 射线衍射分析表明 :平面 1 (C(8) -C(9) -C(1 9) )与平面 2 (C(1 0 ) -C(1 1 ) -C(1 2 ) )之间的两面角为1 6.2 4° ;平面 1与平面 3(C(7) -C(8) -C(9) )之间的两面角为 1 77.37° ;平面 1与平面 4(C(1 )-C(5) -C(6) )之间的两面角为 98.2 1°;平面 2与平面 3之间的两面角为 1 61 .1 2° ;平面 2与平面 4之间的两面角为 81 .98°;平面 3与平面 4之间的两面角为 79.1 5°     

微波辐照下4-苯基-7,7-二甲基-2,5-二氧代-1,2,3,4,5,6,7,8八氢喹啉的合成和晶体结构

标题化合物C1 7H1 9NO2 是由苯甲醛、5,5 二甲基 1 ,3 环己二酮、丙二酸亚异丙酯及醋酸铵在微波辐照下干反应而得。结构通过单晶X 射线衍射法确定 ,其晶体属于单斜晶系 ,空间群P2 1 /a ,a =7.52 4 (2 ) ,b =2 2 .483(3) ,c =9.2 73(2 ) ,β =1 1 3 0 4 (2 )°,V =1 44 3.7(5) 3,Mr=2 69.34,Dc=1 .2 39g/cm3,Z =4,μ(MoKα) =0 81cm- 1 ,F(0 0 0 ) =576,在 6 <2θ <51 0°范围内收集 2 994个独立衍射点 ,其中可观测衍射点 2 0 91个 [I >2 .50σ(I) ]。晶体结构用直接法解出 ,经用全矩阵最小二乘法对原子参数进行修正 ,最后的偏离因子为R =0 .0 4 4 ,Rw=0 .0 58。在晶体结构中 ,O(3) -C(9) -C(4) -C(5) -N(1 )构成一个平面 ,该平面与苯环的二面角为 84.2 5°     

微波辐射下2-氨基-7,7-二甲基-3-乙氧羰基- 4-(2-呋喃)基-5-氧代-5,6,7,8-四氢-4H- 苯并吡喃的合成和晶体结构

标题化合物C18H21NO5是由2-呋喃亚甲叉氰乙酸酯和5,5-二甲基-1,3-环己酮在醋酸铵存在下用微波辐射反应得到,结构通过单晶X-射线衍射法确定,其晶体属三斜晶系,空间群P 睿琈r =332.36,a =11.232(2),b =13.048(2),c =13.274(3),α=105.7(1),β=95.68(2),g =109.56(1)? V=1752.4(6)3,Z=2,Dc=1.276Mg·m-1, =0.093mm-1,F(000)=704, 最终的偏离因子为R=0.0431,wR=0.0973,在分子结构中平面 1 (呋喃环) 与平面2 ((C(5)、 C(6)、C(9)、O(1))之间的二面角为 84.70°, 平面2 与平面 3 (C(1)、C(4)、C(5)、C(6)) 之间的二面角为 2.9°, 平面 1 与平面3 之间的二面角为 85.9°。吡喃环和与吡喃环合的六员环为信封式结构。     

双环[3.3.0]-3,7-辛二烯-2,6-二酮晶体的分子结构

利用 Enraf-Nonius CAD4四圆单晶衍射仪测定了双环[3.3.0]-3,7-辛二烯-2,6-二酮(2)的单晶结构,晶体属三斜晶系,空间群为 PI,晶胞参数为:a=6.596(2)(?),b=7.414(1)(?),c=7.359(1)(?),α=106.64(1)°,β=100.17(1)°,γ=98.44(1)°,ν=331.9((?)~3),Ζ=2。用直接法得到分子的粗结构。对1013个可观察反射点用全矩阵最小二乘法修正,最后得R=0.060,结构测定的结果证实:两个五员环自成一个平面,两平面间夹角为117.3°。     

杂氮三环化合物晶体的X射线衍射研究——Ⅱ.1-氯丙基-2,8,9-三氧杂-5-氮杂-1-硅三环[3,3,3,0~(1.5)]十一碳烷-3-酮的晶体与分子结构

题目所指的化合物(NC_6H_(10)O_4Si-CH_2CH_2CH_2Cl)属正交晶系,所属空间群为P2_12_12_1。晶胞参数:a=12.943,b=11.477,c=8.273。Z=4。取1243个可观测独立反射数据,用直接法和Fourier综合解得粗结构,经最小二乘修正,偏离因子R为0.049。三个五员环(Si,O,C,C,N)都有一个较大的扭角,分别为23.7°,41.6°,42.8°。其中带羰基环的最大扭角相对较小(23.7°)。三环最小二乘平面间夹角接近120°,分子中的氯丙基-CH_2CH_2CH_2C1近乎在一个平面上折叠。     

对苯二甲酸·1,3-二(4-吡啶基)丙烷的水热合成和晶体结构(英文)

用1,3-二(4-吡啶基)丙烷、对苯二甲酸和去离子水在413K下通过水热反应法得到了标题化合物(C13H14N2).(C8H6O4).该化合物晶体属于三斜晶系,空间群为P墿,晶胞参数为a=0.95267(19)nm,b=1.1927(2)nm,c=1.6959(3)nm,α=96.40(3)°,β=98.12(3)°,γ=101.52(3)°,Z=2.单晶衍射结果表明标题化合物由对苯二甲酸分子和1,3-二(4-吡啶基)丙烷通过两种类型的分子间π-π堆积作用以及O—H…N氢键作用构成.同时,还对标题化合物进行了元素分析和红外测试.     

2-氨基-3-氰基-7,7-二甲基-4-苯基-5-氧代-5,6,7,8-四氢-4H-苯并吡喃的合成和晶体结构

标题化合物C18H18N2O2是由亚苄基丙二睛和5,5-二甲基-1,3-环己酮在乙二醇中反应2小时得到,结构通过单晶X-射线衍射法确定,其晶体属单斜晶系,空间群P21/c,Mr=294.34,a = 11.3070(1), b= 9.4750(1),c = 14.919(2) ,β= 99.34(1)埃琕 = 1577.1(3) 3,Z = 4,Dc=1.240Mgm-3,μ=0.082mm-1,F(000)=624, 最终的偏离因子为R=0.0381,wR=0.0961,在分子结构中存在3个环:苯环(A)、吡喃环(B)及与吡喃环稠合的六员环(C)。A与B、A与C及B与C之间的两面角分别为 92.5°、85.7°和8.2°。     

4,4’-一氧二（苯胺灵）的合成和晶体结构

通过4,4’-一氧二（异氰酸苯酯）与异丙醇加成反应，合成标题化合物 4,4’-一氧二（苯胺灵）(Ⅰ) (C20H24N2O5, Mr=372.41)，并用X射线衍射、红外光谱、13C核磁共振、电子轰击质谱和元素分析对标题化合物进行表征. 晶体属于三斜晶系，空间群为P1晶体学参数为: a=0.85107(17), b=0.91164(18), c=1.45701(3) nm, α=80.44(3)°, β=85.25(3)°, γ=62.88(3)°, V=0.9922(3) nm3, Z=2, Dc=1.247 g•cm－3, μ(Mo Kα)=0.90 cm－1, F(000)=396.两个苯环平面之间的夹角为62.06° (0.06°). 晶体结构经全矩阵最小二乘法修正，最终偏离因子R=0.0520, wR=0.1434(对可观察点).此化合物应具有广谱的生物活性.     

杂氮三环化合物X射线研究——Ⅲ.1-氯甲基-2,8,9-三氧杂-5-氮杂-1-硅三环[3,3,3,0~(1.5)]十一烷-3-酮的结构测定

题目所指化合物属单斜晶系,P2_1/c空间群,晶胞参数a=6.751(1),b=11.274(3),c=13.134(4),β=100.390(3)°,晶胞含分子数Z=4.用直接法和Fourier综合解得粗结构,取1490个可观测独立反射数据,经最小二乘修正,偏离因子R为0.056。三个五员环(Si,O,C,C,N)中各最大扭角分别为33.2°,23.0°,35.1°,其中最小者(23.0°)属于含羰基的环。     

Pr(Ⅲ)和5-氨基间苯二甲酸的配位聚合物的水热合成和单晶结构研究

报道了单晶Pr(C8H5NO4) 1 5·H2 O的水热合成和晶体结构。中心离子Pr3 +处于 9配位的环境中。来源于配体的两个羧基螯合Pr3 +形成两个四元环。其它四个羧基通过桥键连接中心离子。晶体数据如下 :正交晶系 ,空间群Pbcn ,a =1 2 2 2 2 8( 7)nm ,b =0 80 2 95 ( 5 )nm ,c =2 5 61 1 1 ( 1 4)nm ,α =90°,β=90°,γ=90°。配体通过螯合和桥键金属离子在ac平面内构成地板形网格。羧基采用 η1,3 方式连接层平面 ,沿着b轴构成一维通道。与金属离子配位的水分子悬挂在隧道中     

微波辐射下4-苯基-5-乙氧羰基-6-甲基-3,4-二氢吡啶-2-酮的合成和晶体结构

标题化合物C1 5H1 6NO3由苯甲醛、醋酸铵、乙酰乙酸乙酯、麦氏酸在微波辐射下干反应而得。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P1 ,a =7.870 (1 ) ,b =9 2 90 (1 ) ,c=1 0 .640 (2 ) ,α =1 0 2 .76(3) ,β =1 1 0 .42 (3) ,γ =96.92 (3)°,V =694.2 (2 ) 3,Z =2 ,Mr=2 59.30 ,Dc=1 .2 4 0 g/cm3,μ(MoKα) =0 .0 86mm- 1 ,F(0 0 0 )=2 76。晶体结构用直接法解出 ,经用全矩阵最小二乘法对原子参数进行修正 ,最终的偏离因子为R =0 0 4 2 3,wR =0 .1 2 57。在晶体结构中 ,吡啶酮环与苯环之间的二面角为 87.31°。     

Synthesis and Structure of 6-(4- Fluorobenzylamino)-3-methylthio-1,5- diphenyl-1H-pyrazolo[3,4-d]pyrimidin-4(5H)-one

1 INTRODUCTION It was reported that the pyrazolopyrimidinone derivatives play a very important role in the bio- chemistry of living cell. Many potential drugs[1～3] and agrochemicals[4, 5] have been modeled on the compound, and the study on derivatives …     

Synthesis and Crystal Structure of Methyl(7,7-Dimethyl-2-amino-4-(4-chlorophenyl)-5-oxo-5,6,7,8-tetrahydro-4H-benzo-[b]-pyran-3-yl)Carboxylate

<正>The title compound methyl (7,7-dimemyl-2-amino-4-(4-chlorophenyl)-5-oxo-5,6,7,8-tetrahydro-4H-benzo-[b]-pyran-3-yl) carboxylate (C19H20ClNO4, Mr = 361.81) was synthesized and crystallized. The crystal belongs to triclinic, space group P 1 with a = 8.519(2), b = 10.346(2), c = 11.481(3) A, α = 108.16(1), β = 107.78(2), γ= 91.83(2)°, Z = 2, V = 906.5(3) A3, Dc = 1.326 g/cm3, μ(MoKα) = 0.234 mm-1, F(000) = 380, R = 0.0467 and wR = 0.1270 for 3142 observed reflections (I > 2σ(I)). X-ray analysis reveals that the C(7), C(8), C(9), O(1), C(10) and C(11) atoms form a six-membered ring which adopts a boat conformation. In the ring, the distances of C(8)-C(9) and C(10)-C(11) are 1.332(3) and 1.357(3) A, respectively, which indicates that they are C=C double bonds. Another six-membered ring (C(8)-C(9)-C(15)-C(14)-C(13)-C(12)) adopts the half-chair confonnation. In addition, there are intermolecular hydrogen bonds in the crystal structure.     

Crystal Structure of 4—（4—chlorophenyl）—7,7—dimethyl—2,5—dioxo—1,2,3,4,5,6,7,8—octahydroquinoline

1 INTRODUCTION Since the discovery of the pharmacological effects of 1,4-dihydropridines(1,4-DHPs) as calcium channel blocks[1], a great deal of work has been directed towards synthesis of the novel 1,4-DHPs acting as calcium antagonists[2, 3]. In fact, it is well-established that slightly modified structures on the DHP exhibit a calcium agents effect[4, 5] ; however, two fused rings have been less well-studied. By refluxing equivalent amounts of dimedone, aromatic aldehyde Meldrum抯 …     

2,6-二甲基-4-苯基-1,4-二氢吡啶-3,5-二甲酸乙酯的合成和晶体结构

标题化合物C1 9H2 3NO4由苯甲醛、尿素、乙酰乙酸乙酯在微波辐射下干反应而得。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P2 1 /c ,a =9.745(2 ) ,b =7.388(2 ) ,c =2 4 .354(5) ,β =92 .60 (3)°,V =1 751 .6(6) 3,Z =4,Mr=32 9.38,Dc=1 2 4 9g/cm3,μ(MoKα) =0 .0 87mm- 1 ,F(0 0 0 ) =70 4。晶体结构用直接法解出 ,经全矩阵最小二乘法对原子参数进行修正 ,最终的偏离因子为R =0 .0 4 1 6,wR =0 .1 1 75。在晶体结构中 ,二氢吡啶环与苯环之间的二面角为 92 .1 4°。     

Molecular and Crystal Structure of 4-〔2-(4-Dimethy aminophenyl)ethenyl〕-1-methypyridinium tetraphenylborate

1　INTRODUCTIONAccordingtotheorganic“saltmethodology”principle〔1〕,whichsuggeststhatCoulombicinteractionsinorganicsaltscouldoverridedipolarinteractionswhichpro-videastrongdrivingforceforcentrosymmetriccrystallizationindipolarmolecularcrystals,asystematicsearchforSHG(SecondHarmonicGeneration)organiccrys-talswasconducted.AsearchontheCambridgeStructuralDatabase〔2〕(Version5.18)wasdonefororganicsaltshavinganionBPh4-(47cmpoundsintotal)orBF4-(147compoundsintotal)andcationcontainingatle…     

Synthesis,Crystal Structure and Herbicidal Activity of O,O＇-Diethyl-N-[2-（5,7-dimethyl-[1,2,4]triazolo[1,5-a]pyrimidin-2-yloxy）-benzoxyl]-1-amino-benzyl phosphonate

The crystal structure of the title compound (C25H28N5O5P,Mr=509.49) has been determined by single-crystal X-ray diffraction.The crystal is of monoclinic,space group P21/c with a=13.0726(4),b=13.4513(4),c=15.103(1),β=93.650(1)°,V=2650.29(14)3,Z=4,Dc= 1.277 g/cm3,F(000)=1072,μ(MoKα)=0.147 mm-1,the final R=0.0748 and wR=0.1956 for 3186 observed reflections (I 2σ(I)).The fused triazolopyrimidine system ring is coplanar,the dihedral angles between the triazolopyrimidine and C(1)-C(3)-C(5) phenyl,the triazolopyrimidine and C(17)-C(19)-C(21) phenyl,and the two phenyl rings are 66.87,58.79 and 80.11o,respectively.Intramolecular N(5)-H(5A)…O(3) and intermolecular C(2)-H(2)…N(4),C(18)-H(18)…O(3),C(19)-H(19)…O(2) and C(24)-H(24C)…N(4) hydrogen bonds together with C-H…π interactions contribute to the stability of the structure and result in a three-dimensional framework.The preliminary bioassay indicates that the title compound exhibits moderate herbicidal activity against dicotyledonous plants (Brassica campestris L) at the concentration of 100 mg/L.