Crystal Structure of 4, 5-trans-2-Amino-1, 3, 3-tricyano-4, 5-di (4-chlorophenyl)cyclopentene. Ethanol. Monohydrate

1mTRODUCT10NSincethetimeKaganhasdem0nstratedasimplepreparationofsamariumdiio-didefromsamariummetaland1,2-diiodoethanet1),SmI2hasbeenwidelyusedinsyntheticreactionst23.Thereactivityofsamariumdiiodidetowardsvariousnitrogen-containingcomP0undshasalreadybeenexamined.Thereare,toourknowledge,noliteratureexamplesforthereductionofcyanogrouptoproduceaminowiththisreagent.Inthispaper,wediscussedthecrystalstructureofthetitlecomP0undsyn-thesizedbythereactionofsamariumdii0didereagentwithp-chloroben-zyli…     

3,3,6,6-四甲基-4a-羟基-9-邻甲氧基苯基-1,8-二氧代-2,3,4,4a,5,6,7,8,9,9a-十氢化-1H-氧杂蒽的合成和晶体结构

标题化合物C24H30O5是由邻甲氧基苯甲醛与5，5-二甲基-1，3-环己二酮在N，N-二甲基甲酰胺中反应而得。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C2／c，a=33．942（6），b=7273（1），c=22667（4）A，β=128．989（9）°，Mr=398．50，V=4349（1）A3，Dc=1．2179·cm-3，Z=8，μ（MoKa）=840mm－1，F（000）=1712。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=0.043，Rw=0．052。在晶体结构中，存在一个分子间氢键。     

4-(2'-羟基苯甲酰肼)苯亚甲基／亚乙基－5－甲基－2－苯基－2，4－二氢－吡唑啉酮－3超分子化合物的合成与晶体结构

报道了4-(2'－羟基苯甲酰肼)苯亚甲基－5－甲基－2－苯基－2，4－二氢－吡 唑啉酮－3（B_1）和4-(2'－羟基苯甲酰肼)亚乙基－5－甲基－2－苯基－2，4－二 氢－吡唑啉酮－3（B_2）的合成、表征及晶体结构分析，B_1晶体属单斜晶系， C2/c空间群，所得晶胞参数为：a = 1.4201(2) nm, b = 1.65542(2) nm, c = 1. 8455(3) nm, β = 101.32(1)°，V = 4.2541(10) nm~3, Z = 8, D_c = 1.344 g/cm~3, μ = 0.094 mm~(-1), F(000) = 1808, R = 0.0442, wR = 0.1037。该 化合物由水分子通过氢键连接成沿ac面无限延伸的二维网络结构的超分子。B_2晶 体属三斜晶系，P1空间群，a = 1.2120(2) nm, b = 1.2223 (2) nm, c = 1.4159 (3) nm, α = 70.38 (1)°, β = 74.91 (1)°, γ = 63.64(1)°, V = 1.7549 (5)° nm~3, Z = 4, D_c = 1.326 g/cm~3, μ = 0.092 mm~(-1), F(000) = 736, R = 0.0436, wR = 0.1076。此化合物通过分子间氢键形成沿α轴无限延伸的一维 链状结构的超分子，由于分子间的作用力使其分子又沿b轴呈层状堆积。     

3,3,6,6-四甲基-9-邻氯苯基-1,8-二氧代-3,4,5,6,7,9-六氧化氧杂蒽的合成和晶体结构

标题化合物C23H25对O3Cl是由邻氯苯甲醛与5，5-二甲基1，3-环己二酮在N，N-二甲基甲酸腹中反应而得。结构通过单晶X-射线衍射法确定，其晶体属于单科晶系，空间群=1632。晶体结构用直接法解出，使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=0．054，Rw一0．063。在晶体结构中，吡喃环与苯环之间的两面角为92．43°。     

Crystal and Molecular Structure of 2-(2, 6-Dinitro-4-Trifluoromethyl) phenylthio-5, 7-Dimethyl-1,2,4-Triazolo [1, 5-a] Pyrimidine

1INTRoDUCTIONItwasreportedthattheheterocycliccompoundscontainingl,2,4-triazolo[1,5-ajpyrimldinyldisplayedpotentialbioIogicalactivities['2i.Howeverltheherbicidalac-tivityofthethio-etherderivativesof1,2,4xtriazolo[1,5-ajpyrimidinewasrarelyre-ported"'.Inourpreviouspaper"',wedesignedandsynthesizedaseriesof2-arylthio-l,2,4-triazolo{l,5-ajpyrimidines,someofwhichdisplayedgoodherbicidalactivity.Inordertostudythestructure-activityrelationshipofthesecompounds,thestructureofthetitlecompound(1)wasan…     

Neue Oxocuprate (I). Über Cs3Cu5O4, Rb2KCu5O4, RbK2Cu5O4 und K3Cu5O4

New Oxocuprates(I). On Cs₃Cu₅O₄, Rb₂KCu₅O₄, RbK₂Cu₅O₄ and K₃Cu₅O₄ Cs₃Cu₅O₄ light yellow, powder as well as single crystals [a = 10.313(9), b = 7.630(1), c = 14.750(4) Å, β = 106.48(6)°], Rb₂KCu₅O₄ [a = 9.724(2), b = 7.443(0), c = 14.246(2) Å, β = 106.78(8)°], RbK₂Cu₅O₄ [a = 9.561(1), b = 7.411(0), c = 14.111(1) Å, β = 106.76(7)°] and K₃Cu₅O₄ [a = 9.422(1), b = 7.364(1), c = 13.995(2) Å, β = 107.00(2)°] are new prepared. The colour of the powders becomes lighter according to the sequence showed above. K₃Cu₅O₄ shows pale yellow. The Madelung Part of Lattice Energy, MAPLE, is calculated and discussed.     

Molecular and crystal structure of 5-phenyl, 5-m-nitrophenyl,and 5-spirocyclopentane derivatives of 3-amino-2,4,4-tricyanobicyclo [4,4,0] deca-2,10-diene

To examine the ability of 3-amino-2,4,4-tricyanobicyclo[4,4,0]deca-2,10-dienes (I) to form dimeric associates, we have investigated molecular and crystal structure of three derivatives of (I): 5-phenyl (II), 5-m-nitrophenyl (III), and 5-spirocyclopentano (IV). Hydrogen bonding via the aminonitrile fragment leads to formation of centrosymmetric dimeric associates in compounds (II, III) and a chain structure in (IV). Crystal data for (II): space group P2₁/c, a=8.726(3), b=15.879(5), c=15.597(5) Å, α=γ=90, β=105.13(2)⁰, V=2086.2 ų, Z=4, R=0.093; for (III): space group C2/c, a=24.725(8), b=9.004(5), c=24.391(8) Å, α=γ=90, β=125.36(2)⁰, V=4428.2ų, Z=8, R=0.080; for (IV): space group C2/c, a=24.443(8), b=10.240(5), c=16.645(6) Å, α=γ=90, β=108.89(2)⁰, V=3941.8 ų, Z=8, R=0.089.     

3,3-二甲基-9-(5,5-二甲基-3-羟基-2-环己烯-1-酮-2-基)-1-氧代-2,3,4,9-四氢化氧杂蒽的合成和晶体结构

标题化合物C23H26O4是由水杨醛与5，5-二甲基-1，3-环己二酮在N，N-二甲基甲酰胺中反应而得．结构通过单晶X-射线行射法确定，其晶体属于单料晶系，空间群P21/c，a=7．056（7），b=20.263（3），c=13．665（2）A，β＝93．32（1）°，V=1950．7（4）A3，Mr=366．46，Dc=1.248g／cm3，Z=4，μ（MoKa）=0．84cm－1，F（000）=784。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，最后的偏离因子R=0．068，Rw=0．075。晶体结构分析结果表明，分子中存在一个共轭的烯醇式结构。     

Beiträge zur Chemie des Schwefels. 114. Kristall- und Molekülstrukturen vom Hexathiepan (S6CH2), Pentathian (S5CH2) und Dibenzylpentathian (S5C(CH2C6H5)2)

Contributions to the Chemistry of Sulfur. 114. Crystal and Molecular Structures of Hexathiepane (S₆CH₂), Pentathiane (S₅CH₂), and Dibenzylpentathiane (S₅C (CH₂C₆H₅)₂) The crystal and molecular structures of hexathiepane 1 , pentathiane 2 and dibenzylpentathiane 3 were determined by single crystal X-ray structure analyses. 1 : Monoclinic space group P2₁/c; a = 7.694(4), b = 7.668(4), c = 12.367(6) Å, β = 108.9(1)°; Z = 4, d_calc. = 1.986 g/cm₃. The seven-membered heterocycle exists in twist-conformation. 2 : Monoclinic space group C2/c; a = 10.990(5), b = 6.872(4), c = 15.507(6) Å, β = 94.1(1)°; Z = 8, d_calc. = 1.982 g/cm₃. The six-membered heterocycle exists in chair-conformation. 3 : Monoclinic space group P2₁/c; a = 12.907(8), b = 13.611(8), c = 9.408(6) Å, β = 98.9(1)°; Z = 4, d_calc. = 1.442 g/cm₃. 3 is analogous to 2 a six-membered heterocycle with chair-conformation. The benzylic groups are distorted to each other. Bond lengths, bond angles, and dihedral angles of the heterocyclic sulfur rings arc discussed, especially with regard to a comparison with cyclohexasulfur, cycloheptasulfur. and cyclooctasulfur.     

Monosubstituted Trinuclear and Tetranuclear VIB Metal Carbonyl Complexes: Syntheses of [{M(CO)5}3(Pf-Pf-Pf)] [Pf-Pf-Pf = PhP(CH2CH2PPh2)2] and [{M(CO)5}4(P-Pf3)] [P-Pf3 = P(CH2CH2PPh2)3] (M = Cr,Mo) and Crystal Structures of the Latter Three

The triligate trimetallic complexes, [{M(CO)₅}₃(Pf-Pf-Pf)] and tetraligate tetrametallic complexes, [{M(CO)₅}₄(P-Pf₃)] (M = Cr and Mo), were prepared from [M(CO) ₆] and the corresponding ligands in MeCN/CH₂Cl₂ promoted by Me₃NO at 0 °C. Crystals of trimer lb are monoclinic, space group P 2₁/n, with a = 13.407(3), b = 15.002(5), c = 26.52(1) Å, β = 90.65(2)°, Z = 4, and R = 0.060 for 2760 observed reflections. Crystals of tetramer 2a are monoclinic, space group P 2₁/c, with a – 14.183(8), b = 29.880(4), c = 16.103(2) Å, β = 94.98(3)°, Z = 4, and R = 0.039 for 5014 observed reflections. Crystals of 2b are monoclinic, space group C 2/c, with a = 42.120(8), b = 13.679(1), c = 23.486(2) Å, β = 92.14(1)°, Z = 8, and R = 0.032 for 6897 observed reflections. Each phosphorus atom of the ligands is coordinated to the M(CO)₅ moiety in each title compounds. The geometry of the four metals is a distorted tetrahedron for the tetramers.     

2,6-二甲基-3-苯基-4a-对甲苯基-7-苯甲酰基-4a,5,6,12-四氢-1H,7H-1,3-噁嗪并[3,2-d][1,5]-苯并二氮杂-1-酮的合成及晶体结构

通过2-甲基-4-对甲苯基-1-苯甲酰基-2，3-二氢-1H－1，5-苯并二氮杂与由不对称1-苯基-2-偶氮-1，3-丁二酮热解产生的a-羰基烯酮的[2＋4]环加成反应制备了标题化合物（C34H30N2O3，Mr=514．62），用X射线衍射测定了其单晶结构。晶体属单斜晶系，空间群为P21／n，a=11．560（1），b=19．058（3），c=13．207（2）A，β=106.82（1）°，V=2785.2（7）A3，Z=4，Dc=1．230g．cm-3，MoKa（λ=0.71073A），μ=0．064mm-1，F（000）=1088，2278个可观测衍子射点，R=0．046，Rw=0．049。分子骨架为由苯环、具有类扭船式构象的七元二氮杂环和略微扭曲的唑酮环构成的三环体系。     

CRYSTAL STRUCTURES OF [Bu4N]2[M2Ag3（ μ3—S）2（μ—S）4S2Et2dtc]（M=W,Mo）

<正> The title compounds were prepared from the reation of (NH4)2MS4 (M=W,Mo),AgNO3,NadtcEt2 and Et4NBr in CH3CN-H2O solution. The isomorphous compounds [Bu4N]2[W2Ag3S8Et2du] ( I ) and [Bu4N]2[Mo2Ag3S8Et2dtc] (Ⅱ) crystallize in triclinic space qroup Pi with the following crystal parameters:α=13. 043(4),b = 21. 640(6),c=10. 757(6)A ,α=95. 09(5),β = 91. 90(4),γ = 98. 57(3)°,Z = 2,V = 2987A3,Dc=1. 76g/cm3 for I 5;a= 12. 989(2) ,b=21. 574 (9) ,c= 10. 7/1(1) A .α= 95. 06(7), β=91. 61(4), γ=98. 52(2)°, Z = 2,V = 2961 A3.Dc= 1. 58g/cm3 for Ⅱ . The final R and Rw values are 0. 061 and 0. 072 for Ⅰ ,and 0. 062 and 0. 076 for Ⅱ The M2Ag3 (M = W, Mo) unit in anion M2Ag3S8Et2dtc forms a five-membered ring.     

Crystal and Molecular Structure of Bis(η5-methylcyclopentadienyl)titana(IV)-cyclohexasulfane Ti(η5-C5H4CH3)2S5

The crystal and molecular structure of Ti(n⁵-C₅H₄CH₃)₂S₅has been determined by X-ray diffraction studies. The substance crystallizes in the monoclinic crystal system [a = 6.8642(5), b = 16.507(1), c = 13.074(1) Å, β = 82.407(3)°, space group P2₁/n, Z = 4]. The geometry about the titanium atom is a distorted tetrahedron, with a (centroid)-Ti-(centroid) angle of 131.29° and a S? Ti? S angle of 93.38°. The six-membered ring TiS₅ has a cyclohexane-like chair configuration. The structural results are compared to those for similar type titanium complexes.     

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 4-CHLORO-5- ETHYL-5-METHYL-3-PHENYL-1, 3, 4-DIAZAPHOSPHOLIDIN-2-THIONE-4-SULFIDE

<正> Crystal of the title compound Mr=304. 80 belongs to the triclinic, space group P1, with a = 7. 282)2), b=9. 064(2), c=11. 737(5) A , α=75. 79 (3), β=78. 70(3), γ=88. 49(2)°, V-736. 21 A3, Z=2, Dx = l. 375 g/cm3. The final refinement is converged with R=0. 062 and Rw= 0. 069.The five-membered heterocycle is in envelope conformation. The P - N bond length (1. 68(1)) indicates that the dπ-Pπ bond between P and N of the title compound is stronger than that of the corresponding 4-phenyl compound.     

The Crystal Structure of 1, 4, 7, 10- Tetraazacyclododecane Hydrate Triperchlorate

1=mTRODUCTIONMacroazacyclicligandisofwideinterestbecauseofitsstructuralsimilaritywiththeskeletonofPOrphyrinringinsomebibectivesubstancessuchaschlorophyllandhemeetc.tl1.Asametalsimulationenzyme,macroazacyclicligandcoordinatedwithtransitionmetalhasbeeninvestigatedthoroghlyinkinetic,dynamicandstructuralcharactert2.3).Butthere'isnorePOrtaboutthecrystalstructureof1,4,7,1o-tetraaza-cyclododecanehydratetriperchlorate.2EXPERIMENTAL2-lSynthesisoftheTitleComplexTetraazacycldodecanewassynthes…     

CRYSTAL AND MOLECULAR STRUCTURES OF 2-ACETYLDIFER-ROCENYLMETHANE AND 3'''' - ACETYLDIFERROCENYLMETHANE

<正> 2 - acetyldiferrocenylmethane, C5H5FeC5H4CH2C5H3 (COCH3) FeC5H5 ( I ),Mr=426. 1,violet-red prism-like crystal,m. p. 163. 7~166. 3℃,obtained from benzene-ligroin solution (benzene : ligroin=1 : 3). A crystal of approximate dimensions 0. 20×0. 40×0. 45 mm was selected for data collection from a CAD4 diffractometer with graphite monochromated MoKa radiation (λ=0. 71069A). Compound Ⅰ crystallized in the triclinic space group P1 with unit cell dimensions;a = 9. 597(2),b=9. 768 (2),c=11.540(1) A ,α= 111-93(1),β=111. 42(1),γ= 92. 46(2)°,V = 913. 9 A3, Z= 2, and Dc= 1. 548 g/cm3. 3' - Acetyldiferrocenylmethane, C5H5FeC5H4CH2C5H4FeC5 H4-COCH3(Ⅱ) ,is an isomer of compound Ⅰ ,yellow needle-like crystal,m. p. 110. 5~ 111. 0℃ ,obtained by the same method. A crystal of approximate dimensions 0. 025×0. 01×0. 45 mm was selected for data collection. Compound Ⅱ crystallized in monoclinic space group P21/c with a = 10. 930 (2), b= 5. 907(6) ,c= 27. 729(5) A ,β= 92. 64 (1)°,V=1788. 4A3,Z=4,Dc=1. 583 g/cm3.     

CRYSTAL STRUCTURE OF 2, 4-DITHIONE-3-AMINO-1, 3, 2-OX-AZAPHOSPHORINEBENZO-2-THIONO PYRIDINIUM

<正> The structure of title compound [C7H6N2OPS3]-·[HNC5H5]+ was determined by x-ray diffraction. It belongs to monoclinic system with space group P21/a, a = 16.745(2), b= 8.563(2), c=21. 050(5)(?), β=93.32(1)°, V= 3013. 6(?)3, Z = 8, Mr = 341. 4, F (000) = 1536, Dc=1. 504 g. cm-3,μ= 53. 0 cm-1. The crystal is composed of discrete cations C5H5NH+ and anions CrH6N2OPS3-. There are two pairs of the cations and the anions in each asymmetric unit. The stability of the anion is increased by the formation of (d-p)π bonding involving the 3d orbital of the P atom and the lone electron pairs of the S atoms.     

［La（EO_3）_3（H_2O）］（ClO_4）_3·H_2O的晶体结构

稀土高氯酸盐开环冠醚三缩乙二醇（ＥＯ_３）［Ｌａ（Ｃ_６Ｈ_（１４）Ｏ_４）_３（Ｈ_２Ｏ）］（ＣｌＯ_４）_３·Ｈ_２Ｏ，单斜晶系，Ｐ２_１／ｃ空间群。晶胞参数为：ａ＝１５．４７４（２），ｂ＝１１．３８６（１），ｃ＝２０．８４１（４），β＝９９．８２（１）°，Ｖ＝３６１８（１），ＭｏＫα，Ｚ＝４，Ｄ_ｃ＝１．７１８ｇ／ｃｍ３，μ＝１．４９９ｍｍ￣（－１）。全矩阵最小二乘精细修正，结构因子Ｒ＝０．０５６，Ｒ_ｗ＝０．０８３。中心原子Ｌａ与开环冠醚醚链上的Ｏ（１）～Ｏ（９）及一个水分子形成１０配位双帽四方反棱柱结构。弱配体高氯酸根不参加配位。     

4-(4-N,N-二甲胺基)苯基-7,7-二甲基-5-氧代-3,4,5,6,7,8-六氢香豆素酮的合成和晶体结构

标题化合物C19H23NO3由4-N,N-二甲胺基苯甲醛、5,5-二甲基-1,3-环己二酮、麦氏酸在乙二醇中于80℃反应2.5小时而得。结构通过单晶X-射线衍射法确定,其晶体属单斜晶系, C19H23NO3,空间群P21, a = 9.364(2), b = 5.974(1), c = 15.731(3)?, b = 102.87(3)°, V = 857.9(3)?3, Z = 2, Dc = 1.213Mg/m3, μ(MoKa) = 0.082mm-1, F(000)=336。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=0.0521, wR=0.1392。在分子结构中,存在3个平面, C(10)~C(15)构成平面1,C(5)-C6)-C(8)-C(9)-O(2)构成平面2,C(1)-C(2)- C(4)-C(5)-C(9)构成平面3,平面1与平面2的最小二乘面的两面角为88.77°,平面1与平面3的最小二乘面的两面角为86.58°,平面2与平面3的最小二乘面的两面角为1.86°.