Crystal and Molecular Structure of 3，4－diphenyl－5－ethyl－5－methyl－1，3，4－diazaphospholidin－2－thione－4－oxide

ＣｒｙｓｔａｌａｎｄＭｏｌｅｃｕｌａｒＳｔｒｕｃｔｕｒｅｏｆ３，４－ｄｉｐｈｅｎｙｌ－５－ｅｔｈｙｌ－５－ｍｅｔｈｙｌ－１，３，４－ｄｉａｚａｐｈｏｓｐｈｏｌｉｄｉｎ－２－ｔｈｉｏｎｅ－４－ｏｘｉｄｅ￥ＦｅｎｇＫｅ－Ｓｈｅｎｇ；ＣｈｅｎＲｕ－Ｙｕ（Ｉ...     

Synthesis and Crystal Structure of △~6－4－Amino－5，6－diphenyl－5－hydroxy－1，2，4－triaza－cyclohexene－3－thione－monohydrate

ＳｙｎｔｈｅｓｉｓａｎｄＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆ△~６－４－Ａｍｉｎｏ－５，６－ｄｉｐｈｅｎｙｌ－５－ｈｙｄｒｏｘｙ－１，２，４－ｔｒｉａｚａ－ｃｙｃｌｏｈｅｘｅｎｅ－３－ｔｈｉｏｎｅ－ｍｏｎｏｈｙｄｒａｔｅ￥ＬｉｎＺｈｅｎ－Ｇｕａｎｇ；?..     

Crystal Structure of 3－［（α－Phenyl） triphenyl germylethyl］－4－phenyl－Δ~2－1，2，4－triazoline－5－thione

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆ３－［（α－Ｐｈｅｎｙｌ）ｔｒｉｐｈｅｎｙｌｇｅｒｍｙｌｅｔｈｙｌ］－４－ｐｈｅｎｙｌ－Δ~２－１，２，４－ｔｒｉａｚｏｌｉｎｅ－５－ｔｈｉｏｎｅＣｈｅｎＲｕ－Ｙｕ；ＬｉＦｅｎｇ－Ｆｕ（ＩｎｓｔｉｔｕｔｅｏｆＥｌｅ?..     

Crystal and Molecular Structure of 5，6，7，8，9，10－Hexahydro－3－（4－methylphenylamino）－2－thioxoquinoxaline

ＣｒｙｓｔａｌａｎｄＭｏｌｅｃｕｌａｒＳｔｒｕｃｔｕｒｅｏｆ５，６，７，８，９，１０－Ｈｅｘａｈｙｄｒｏ－３－（４－ｍｅｔｈｙｌｐｈｅｎｙｌａｍｉｎｏ）－２－ｔｈｉｏｘｏｑｕｉｎｏｘａｌｉｎｅＳｕｎＤａ－Ｑｉｎｇ；ＬａｎｇＪｉａｎ－Ｐｉｎｇ；ＬｕＺｈ...     

Crystal Structure of 2－Thio－2－（3＇－methyl－4＇－chloro－oxyphenyl）－1，3，2－benzodioxaphosphole

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆ２－Ｔｈｉｏ－２－（３＇－ｍｅｔｈｙｌ－４＇－ｃｈｌｏｒｏ－ｏｘｙｐｈｅｎｙｌ）－１，３，２－ｂｅｎｚｏｄｉｏｘａｐｈｏｓｐｈｏｌｅＳｕｎＭｉｎｇ；ＬｉｕＸｉａｏ－Ｌａｎ；ＭｉａｏＦａｎｇ－Ｍｉｎｇ（Ｉｎｓｔｉｉｔ...     

Crystal and Molecular Structure of 4-Phenyl-cyclohexanone Semicarbazone

ＣｒｙｓｔａｌａｎｄＭｏｌｅｃｕｌａｒＳｔｒｕｃｔｕｒｅｏｆ４－Ｐｈｅｎｙｌ－ｃｙｃｌｏｈｅｘａｎｏｎｅＳｅｍｉｃａｒｂａｚｏｎｅＺｈｏｕＫａｎｇ－Ｊｉｎｇ（ＦｕｊｉａｎｉｎｓｔｉｔｕｔｅｏｆＲｅｓｅａｒｃｈｏｎｔｈｅＳｔｒｕｃｔｕｒｅｏｆＭａｔｔｅ...     

Synthesis and Structure of 4，5－bis（2，4－Dinitrophenylthio）－1，3－Dithiole－2－Thione

ＳｙｎｔｈｅｓｉｓａｎｄＳｔｒｕｃｔｕｒｅｏｆ４，５－ｂｉｓ（２，４－Ｄｉｎｉｔｒｏｐｈｅｎｙｌｔｈｉｏ）－１，３－Ｄｉｔｈｉｏｌｅ－２－ＴｈｉｏｎｅＱｕＺｈｅｎｇ；ＣａｉＪｉｎｇ－Ｈｕａ；ＦａｎｇＱｉ；ＹｏｕＸｉａｏ－Ｚｅｎｇ（Ｃｏｏｒｄｉｎａｔｉ...     

Crystal Structure of 1,3-Dibenzyl-2-benzylaminothiocarbonyl-1,3,4- diazaphospholidin-5-thione-4-sulfide

1 INTRODUCTION Lawesson抯 reagent, 2,4-bis(4-methoxyphenyl)- 1,3,2,4-dithiadiphosphetane-2,4-disulfide, can react with certain substrates to give phosphorus heterocycle compounds. These compounds have some potential biological activities as herbicides, fungicides and insecticides[1,2]. By refluxing the Lawesson抯 reagent with benzylisonitrile in benzene, the title compound, 1,3-dibenzyl-2- benzylaminothio- carbonyl-1,3,4-diazaphospholidin-5-thione-4-sulfide was obtained. In the previous …     

Synthesis and Crystal Structure of 1-(o-methylphenyl)-2-(p-methoxyphenyl)-1,3,2-diazaphospholidin-4-thione-2-sulfide

11NTRODUCTIoNThederivativesofdiazaphospholidinoneorthecorrespondingthionesareknowntopossessinterestingbiologicalproperties,suchasherbicidalactivity"'2i.Inrecentyears,itwasreportedthatthel,4,2-diazaphospholindine-5-thione-2havegoodselectiveherbicidalactivity"'41.Tolookformoreeffectiveherbicideswithlowtoxicity,aseriesofnovel1-(o-methylphenyl)-2-(p-methoxyphenyl)-phospholidin-4-thione-sulfideshavebeensynthesizedandtheirmolecularstructuresstudied.PreliminarybioassaysshowthatthesecomPoundshaveg…     

3,4-二苯基-4-氧(硫)代-1,3,4-二氮磷杂环戊-2-硫酮的合成、结构及其反应机理研究

本文研究了苯基硫脲、苯基二氯化膦与脂肪醛(酮)在无水苯中进行的类Mannich反应,在分离产物时发现,除了生成3,4-二苯基-4-氧代-1,3,4-二氮磷杂环戊-2-硫酮(Ⅰ)外,还得到了少量3,4-二苯基-4硫代-1,3,4-二氮磷杂环戊-2-硫酮(Ⅱ).根据化合物Ⅱ的生成及³¹PNMR跟踪反应的结果,得出反应机理为P-H键对亚胺衍生物的加成.通过X射线衍射分析发现,化合物Ⅰ和Ⅱ的五元杂环均为平面结构,其平面性受4位氧代或硫代的影响较大.     

Molecular and crystalline structure of 2-methyl-4,4-diphenyl-5-phenylazo-2-thia-3-aza-4-phosphahepta-2,4-diene-6-one-2-oxide

The molecular structure of 2-methyl-4,4-diphenyl-5-phenylazo-2-thia-3-aza-4-phosphahepta-2,4-diene-6-one-2-oxide has been determined by x-ray crystallography. The sulfur and phosphorus atoms exhibited distorted tetrahedral coordination. The P-N and P=C bond lengths are intnermediate between single and double bond lengths. Delocalization of -electron density was observed in the flattened molecular fragment Ph–N=N–C(=P)–C(=O)–CH₃.Institute of Physiologically Active Substances, Russian Academy of Sciences, 142432 Chernogolovka. Translated fromIzvestiya Akademii Nauk, Seriya Khimicheskaya, No. 12, pp. 2737–2741, December, 1992.     

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°。     

4-苯基-2-苯偶氮基-1-硫代-3,4-二氮唑硫酮-5的合成和晶体结构

4-苯基-2-苯偶氮基-1-硫代-3,4-二氮唑硫酮-5(C14H10N4S2)是双硫腙与二硫化碳发生加成闭环反应时获得。结构通过单晶X-射线衍射法确定,标题化合物是单斜晶系, 空间群为C2/c,晶胞参数a = 25.169(5), b = 3.9690(8), c = 30.130(6) ?,β= 113.79(3)°, V = 2754.0(1)?3, Mr =298.38, Dc =1.439 g/cm3 , Z = 8, μ(MoKα)=3.80cm－1, F(000)=1232 。最终偏差因子为R = 0.0335, wR = 0.0861。分子结构中硫代二氮唑五员杂环显示出共平面结构,最大偏差0.010(1)?。C=S键长1.634(2)     

3,4-二氨基呋咱基氧化呋咱的合成及其晶体结构

通过3-氨基-4-氯肟基呋咱在稀碱作用下发生脱HC l,1,3-偶极反应制备了新型呋咱(氧化呋咱)类含能化合物3,4-二氨基呋咱基氧化呋咱(DAFF),产率70%。其结构经NMR,IR,四圆单晶X-射线衍射仪和元素分析表征。DAFF晶体属单斜晶系,空间群P21/c,a=0.8255(3)nm,b=0.9731(3)nm,c=1.1958(4)nm,β=91.93(3)°,Z=4,Dc=1.745 g.cm-3。DAFF分子不共面,三个环面扭曲。晶体中存在分子内和分子间氢键。     

1-苯基-3-甲基-4-(6-氢-4-甲基氨基-5-硫杂-2,3-吡嗪)-吡唑啉酮的合成与晶体结构

通过1-苯基-3-甲基-4-氯乙酰基-吡唑啉酮-5 (PMCP) 和4-甲基氨基硫脲 (MTSC) 缩合, 形成了一种新的双杂环化合物 (PMCP-MTSC)。利用元素分析与单晶X-射线衍射进行了表征。 该化合物(C14H15N5OS)属单斜晶系, P21 空间群, 晶体学参数为 a = 7.634(1), b = 11.639(2), c = 8.150(2) ? ?= 98.13(1), V = 716.9(2) ?, Z = 2, Dc = 1.396 g/cm3, (MoKa) = 0.232 mm-1, F(000) = 316, Mr = 301.37。结构由直接法解出,共收集3114个衍射点,其中I > 2(I)的独立衍射点有2453个,用全矩阵最小二乘法修正,最终偏离因子:R = 0.0294, wR = 0.0738。结构分析表明: 该化合物以酮式存在,分子间通过氢键作用(N(5)H…O)连接起来并形成一维链状结构。