New Synthesis and Molecular Structure of 2-(4'-Methoxyphenyl)-2,4-dithia-1,3,2-diazaphospholidine-5,1'-spirocyclohexane

1 INTRODUCTION Our continuous efforts to look for biologically active heterocyclic compounds led to a new and efficient synthesis of phosphoroheterocycles 1, 3, 2-diazaphospholidine-4-thione 2-sulfides in good yields by the treatment of Lawesson磗 reagent with various -aminonitriles in one-pot procedure. Many approaches to synthesize such phosphoroheterocycles have been reported[1~4]. The common pathways leading to 1, 3, 2-diazaphospho- lidine-4-thione(one) 2-sulfide(oxide) are using t…     

Synthesis and Crystal Structure of 2-Morpholinylthioformyl-2-phenyl-4-morpholinyl-5-phenyl-1,3-dithiole

1　ＩＮＴＲＯＤＵＣＴＩＯＮα Ｔｈｉｏｃａｒｂｏｎｙｌｔｈｉｏｆｏｒｍａｍｉｄｅｓｗｅｒｅｓｙｎｔｈｅｓｉｚｅｄｉｎ 1 980 [1～ 2 ],ｈｏｗｅｖｅｒ,ｔｈｅｒｅｗａｓｎｏｒｅｐｏｒｔｏｎｔｈｅｉｒｐｒｏｐｅｒｔｉｅｓａｎｄｒｅａｃｔｉｏｎａｃｔｉｖｉｔｉｅｓ[3].Ｗｅｒｅｐｏｒｔｅｄｔｈｅｒｅａｃｔｉｏｎｏｆα ｔｈｉｏｃａｒｂｏｎｙｌｔｈｉｏｆｏｒｍａｍｉｄｅｓｐｒｅｖｉｏｕｓｌｙ[4 ].Ｈｅｒｅ ,ｗｅｒｅｐｏｒｔｔｈｅｓｙｎｔｈｅｓｉｓｏｆ 2 ｍｏｒｐｈｏｌｉｎｙｌｔｈｉｏｆｏｒｍｙｌ 2 ｐｈｅｎｙ…     

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 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.     

Synthesis and Crystal Structure of 1-[(1-Phenyl-4-cyano)pyrazol-5-yliminomethyl]- 2-nitroiminoimidazolidine

1　INTRODUCTIONNeonicotinoids[1～2]areanovelanddistinctclassofinsecticides.Theycombineselectiveactivityagainstinsectswithafavourablesafetyprofile.Neonicotinoidsactatthenicotinicacetylcholinereceptor(nAChR)[3～4].Sincethefirstneonicotinoid,imi-dacloprid(IMI)1wasintroducedtothemarketbyBayerin1991,alotofitsanalogswerereported.Thesecompoundshavethesamestructuralunit,asshowedindashedlineareainIMI.AccordingtothemodelproposedbyYamamotoetal[5],thedistancebetweenthetwonitrogenatomsofIMIisthe…     

Crystal Structure and Conformation of 2''''-C-Ethoxy- 3'''',5''''-O-(tetraisopropyldisiloxane-1,3-diyl)uridine

INTRODUCTION In the past few years many modified nucleosides have been synthesized primarily because of their potential antiviral and anticancer activities. For synthetic purpose, ketonucleosides are very useful intermediates[1], using the reaction of carbonyl group with Wittig reagents[2], cyanide ion[3],organometallic reagents[4] and other nucleophilic reagents[5], some nucleoside derivatives were obtained. Recently, we found some ketonucleosides could react with primary alcohol to form…     

Synthesis and Crystal Structure of 2[1-（1,1-Dimethylethyl）-5-methyl-1-H-pyrazol-4-ylcarbonyl]-N-phenyldrazinecarbothioamide

1INTRODUCTIONThiosemicarbazidespossessingNC=Sgroupareanessentialstructurefeatureresponsibleforvariousbiocidalproperties[1～7].Moreover,theyaretheconvenientandkeyintermediatesforthesyn-thesisofheterocycliccompoundssuchas1,3,4-thiadiazoles,1,2,4-triazoleand…     

Synthesis,Structure and Reaction of a New Bitungsten Compound:(Et_4N)_2W_2S_4 (tdt)_2

1INTRODUCTION'TheclusterscontainingMo--SorW--Shavebeenstudiedextensivelyfortheirimportantapplicationsinmanyfieldsll~43.Alongwith.thedevelopmentofrationaldesignedsynthesissuchasthe"UnitConstruction"utilizingwell-definedactivecom-poundsasbuildingblocks,binuclearsulfidecompoundsusedtodesignnewclustershavebeenpaidattentiontots'6itandalotofcompoundscontainingiM,S.O.--.J' (M=MoorW)coreshavebeenprepared['i.Inthispaper,thefirstexamplpofbitung-stencompoundwithtdtZ--ligands(Et.N),W,S.(tdt),,…     

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

1 INTRODUCTION Inorganic solid supports as catalysts resulting in higher selectivity, milder conditions and easier work-up has been reported as useful catalysts for many reactions [1~3]. Recently, we have reported the Knoevenagel condensation and some other reactions[4~6] catalyzed by KF-Al2O3. In this paper, we discussed the crystal structure of the title compound synthesized by the reaction of 2-cyano-3-(3,4-methylenedioxylphenyl)acrylonitrile and 5,5-dimethyl-1,3-cyclohexanedione in…     

Multifunctional Ligands. Phosphinimine-Substituted Cyanofluoroaromatics Including X-ray Molecular Structures of Three Representative Ligands 4,6-(CN)(2)C(6)F(2)-1,3-(N=PPh(3))(2), 4,6-(CN)(2)C(6)F(2)-1,3-(N=PPh(2)Me)(2) and 4,6-(CN)(2)C(6)F(2)-1-(N=PPh(3))-3-(N=PPh(2)Me). Formation of Rhodium(I) Complexes

Reaction of 1,3-dicyanotetrafluorobenzene with 2 equiv of (trimethylsilyl)iminophosphoranes gave the disubstituted derivatives 4,6-(CN)(2)C(6)F(2)-1,3-AB: 1, A = B = (N=PPh(3)); 2, A = B = (N=PPh(2)Me); and 3, A = (N=PPh(3)), B = (N=PPh(2)Me). Monosubstituted compounds of the type 2,4-(CN)(2)C(6)F(3)-1-A; notably 4, A = (N=PPh(3)), and 5, A = (N=PPh(2)Me), were readily obtained by reaction of 1 molar equiv of the silylated iminophosphorane with the cyanofluoro aromatic. Substitution of the fluorine para to the CN group(s) occurs in all cases. Reactions of 1,2- and 1,4-dicyanotetrafluorobenzene with (trimethylsilyl)iminophosphoranes gave only monosubstituted derivatives 3,4-(CN)(2)C(6)F(3)-1-A (6, A = (N=PPh(3)), and 7, A = (N=PPh(2)Me)) and 2,5-(CN)(2)C(6)F(3)-1-A (8, A = (N=PPh(3)), and 9, A = (N=PPh(2)Me)), respectively, as the result of electronic deactivation of the second substitutional point. 1, 4,6-(CN)(2)C(6)F(2)-1,3-(N=PPh(3)), 2, 4,6-(CN)(2)C(6)F(2)-1,3-(N=PPh(2)Me)(2), and 3, 4,6-(CN)(2)C(6)F(2)-1-(N=PPh(3))-3-(N=PPh(2)Me) have been structurally characterized. For 1 (at 21 degrees C), monoclinic, C2/(c) (No. 15), a = 15.289(2) ?, b = 10.196(1) ?, c = 23.491(6) ?, beta = 91.63(2) degrees, V = 3660(2) ?(3), and Z = 4. The P=N bond length is 1.579(2) ? and the P(V)-N-C(phenyl) angle is 134.0(2) degrees. For 2, (at 21 degrees C) monoclinic, C2/(c) (No. 15), a = 18.694(2) ?, b = 8.576(1) ?, c = 40.084(4) ?, beta = 94.00(1) degrees, V = 6411(2) ?(3), and Z = 8. The P(1)=N(1) bond length is 1.570(4) ?, the P(2)=N(2) bond length is 1.589(3) ?, the P(1)-N(1)-C(14) angle is 131.6(3) degrees, and the P(2)-N(2)-C(16) angle is 131.3(3) degrees. For 3, (at -80 degrees C) monoclinic, P2(1)/c (No. 14), a = 9.210(1) ?, b = 18.113(2) ?, c = 20.015(2) ?, beta = 100.07(1) degrees, V = 3287(2) ?(3), and Z = 4. The P(1)=N(1) bond length (PPh(3) group) is 1.567(4) ?, the P(2)=N(2) bond length (PPh(2)Me group) is 1.581(5) ?, the P(1)-N(1)-C(1) angle is 140.4(4) degrees, and the P(2)-N(2)-C(3) angle is 129.4(4) degrees. These new multifunctional chelating ligands readily react with [Rh(cod)Cl](2) and AgClO(4) to give cationic Rh(I) complexes in which the imine and/or the nitrile groups are coordinated to the Rh center.     

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…     

Crystal Structure of (1R,4R;1S,4S)2-Amino-3-Cyano-1,4-Diphenyl-2-Cyclopentene-1-ol

1INTRODUCTIONIntheearly1970'sthreegroupsofinvestigatorsL,~,'foundthatlow-valenttita-nium,preparedbythereactionofstrongreducingagentswithtitaniumtrichlorideortitaniumtetrachlorideintetrahydrofuran,canabstractoxygenfromketonesoraldehydes,leadingtotheforma-tionofolefins.Theinterestinthereactioninducedbylow--valenttitaniumreagentsisincreasingandalargenumberoffunctionalgroupscanbereduceds4-6).Recent-ly,wefoundthatthetitlecompoundisObtainedbycy-cllzatlonreactionof(3--oxo-1,3-diphenyl)propyl-pro…     

A NEW NITROGEN-BRIDGED DINUCLEAR COBALT COMPLEX: STRUCTURAL CHARACTERIZATION OF (η~5-C_5H_5Co)_2[(μ-N~tC_4H_9)_2 SO_2]

<正> The title complex Co2 (η5-C5H5 )2 [(μ-NtC4H9 )2SO2 ] (1) was isolated from the reaction of CpCo (COD) with tC4H9N = S = NC4H9t and characterized by mass spectral,IR,1HNMR and X-ray diffraction measurements. Co2SO2N2C18H28 Mr = 454. 4, tetragonal,space group P41212 (#92) ,a=9. 212(1) ,c=22. 899(4) A ,V=1943. 0(8) A3,Z= 4,Dc= 1. 55g/cm3 ,F(000)=944,μ(MoKa) = 18.21cm-1 ,R= 0. 048 and Rw = 0. 055 for 682 (I>3σ(Ⅰ))observed unique reflections. G. O. F. = 1. 25. This molecule contains Co-Co bond (2. 335 (2) A ) with two doubly bridging N atoms of the (tC4H9N)2SO2 ligand.     

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.     

Synthesis and Crystal Structure of (E)2-(3''''-Bromo-5''''-chloro-salicylidene amino)-4-methyl Pyridine

A new Schiff base compound,2-bromo-4-chloro-6-[(4-methylpyridin-2-ylimino)me-thyl]phenol(C13H10BrClN2O),has been synthesized by the condensation of equimolar 3-bromo-5-chlorosalicylaldehyde and 4-methylpyridin-2-ylamine in a methanol solution.The compound Was characterized by elemental analysis,IR spectra,and single-crystal X-ray diffraction.The crystal belongs to the monoclinic system,space group P21 with a=6.048(3),b=14.063(7),c=7.623(4)(A),β=97.703(7)°,Z=2,V=642.5(6)(A)3,Dc=1.683 g/cm3,Mr=325.59,λ(MoKa)=0.71073(A),μ=3.395 mm-1,F(000)=324,R=0.0370 and wR=0.0662.A total of 3879 reflections were collected,of which 1970 with,I＞2σ(I)were observed.As expected.the molecule adopts a trans configuration about the C=N double bond.The benzene and pyridine rings are nearly coplanar(mean deviation from the combined plane is 0.031(3)(A)),with their dihedral angle of 3.3(3)°.The preliminary biological tests show that the compound has excellent antibacterial activities.     

Crystal Structure of[PrAl(CF3COO)2(CF3CHOO)(C2H5)2(C4H8O)2]2

[PrAl(CF3COO)2(CF3CHOO)(C2H5)2(C4H8O)2]2 Mr=1420.56, monoclinic, P21/n, a=10.651(6), b=24.276(9), c=11.110(5)(), β=107.650(4)°, V=2737.4(1)()3, Z=2, Dc=3.45 g/cm3, F(000)=2816, T=233K, MoKα radiation (λ=0.71069()), μ(MoKα)=38.017 cm-1, R=0.048 for 2847 observed reflections (I≥3σ(I)). It is isostructural with [LnAl(CF3COO)2(CF3CHOO)-R2(C4H8O)2]2 (Ln=Ho, R=Et; Ln=Nd, Y, R=iBu). Pr3+ is coordinated by eight oxygen atoms from five bridging ligands and two THF forming a distorted bicap-prism.     

一种新颖有机-无机杂化配位聚合物[(C10H16N)2（Pb2I6）·2DMF·H2O]n的自组装合成和晶体结构(英)

A novel coordination polymer [(C₁₀H₁₆N)₂（Pb₂I₆）·2DMF·H₂O]_n (C₁₀H₁₆N=N-butyl-2-Methy-Pyridinium) was synthesized by the reaction of Pb(NO₃)₂ with C₆H₁₀NI at room temperature in DMF solvent and structurally characterized by means of X-ray single diffraction. The title compound crystallizes in triclinic system, space group P1 with a=1.1237(2) nm, b=1.25330(16) nm, c=0.808 00(12) nm, α=102.523(4)°, β=92.475(5)°, γ=95.712(10)°, V=1.102 9(3) nm³, Z=1, D_c=2.470 Mg·m^-3, F(000)=738, chemical formula C₂₆H₄₈N₄O₃Pb₂I₆ and M_r=1 640.46, μ（MoKα）=11.849 mm^-1, the final R=0.057 8 and wR=0.166 5 for 3716 observed reflections with I > 2σ(I). The title compound consists of cations ([(C₁₀H₁₆N)⁺] and anion chain(PbI₃^-),they are combined by static attracting forces in the crystal. DMF and H₂O locate between the organic and inorganic moiety. CCDC: 210812.     

Synthesis, characterization, and hydrolytic behavior of mixed-ligand diorganotin esters, [R2Sn(O2CR')OSO2Me]2 (R=n-Pr, n-Bu; R'=C9H6N-2, 4-OMe-C9H5N-2, C9H6N-1)

Reactions of the tin precursors, R2Sn(OMe)OSO2Me (R=n-Pr, n-Bu), with an equimolar quantity of 2-quinoline/4-methoxy-2-quinoline/1-isoquinoline carboxylic acid in acetonitrile proceed under mild conditions (rt,12-15 h) via selective Sn-OMe bond cleavage to afford the corresponding mixed-ligand diorganotin derivatives [R2Sn(O2CR')OSO2Me]2 [R'=C9H6N-2, R=n-Pr (1), n-Bu (2); R'=4-OMe-C9H5N-2, R=n-Pr (3), n-Bu (4); R'=C9H6N-1, R=n-Pr (5), n-Bu (6)]. These have been characterized by FAB mass, IR, and multinuclear (1H, 13C, 119Sn) NMR spectral data and X-ray crystallography (for 4 and 6). The molecular structure of 4 (C20H29NO6SSn, monoclinic, P2(1)/n, a=14.1(13) A, b=16.7(18) A, c=20.3(19) A, beta=107(4) degrees, Z=8) comprises distorted octahedral geometry around each tin atom by virtue of weakly bridging methanesulfonate [Sn(1A)-O(3B)=3.010, Sn(1B)-O(3A)=2.984 A] and (N,O) chelation of the carboxylate ligands. The spectral data of 1-4 suggest a similar structural motif in solution. The molecular structure of 6 (C38H53N2O10S2Sn2, monoclinic, P2(1)/c, a=11.339(2) A, b=14.806(3) A, c=24.929(5) A, beta=100.537(3) degrees, Z=4) reveals varying bonding preferences with monomeric units being held together by a bridging methanesulfonate [Sn(2)-O(5)=2.312(2) A] and a carboxylate group bonded to Sn(1) and Sn(2) atoms, respectively. Slow hydrolysis of compound 2 derived from 2-quinoline carboxylic acid in moist CH3CN affords the asymmetric distannoxane, [Bu2Sn(O2CC9H6N-2)-O-Sn(OSO2Me)Bu2]2 (7) (C27H45NO6SSn2, monoclinic, C2/c, a=21.152(3) A, b=13.307(2) A, c=26.060(4) A, beta=110.02(10) degrees, Z=8) featuring ladder type structural motif by virtue of unique mu2-coordination of covalently bonded oxygen atoms [O(6), O(6)#1] of the methanesulfonate groups.     

丙酰皮考林酰肼(C_9H_(11)N_3O_2 )的合成和晶体结构

合成了标题化合物(C9H11N3O2,Mr=193.21),晶体属于单斜晶系,空间群为C2/c, a=13.703(1),b = 9.142(1), c = 16.437(2)?, ( = 105.547(3)(,V = 1983.8(4)?,Z = 8, Dc=1.294g/cm3, F(000)= 816,(??o?α)=0.094 mm-1,R=0.0527, wR=0.1517,I(2((I)的可观察衍射点1596个。有机分子间以氢键相联并形成网状结构,N(2)-H...N(1a)(a: -x+1, y, -z+1/2)和N(3)-H…O(2b)(b: -x+1/2, y-1/2, -z+1/2)键键长分别为3.007(2)和2.786(2)?。     

Synthesis, Crystal Structure and Fungicidal Activity of (E)-2-[(4-tert-Butyl-5- (4-methoxybenzyl)thiazol-2-ylimino)methyl]phenol

The title compound(E)-2-(4-tert-butyl-5-(4-methoxybenzyl)thiazol-2-ylimino)me-thylphenol was synthesized by the reaction of 5-(4-methoxybenzyl)-4-tert-butylthiazol-2-amine with salicylaldehyde=and its crystal structure was determined by single-crystal X-ray diffraction.The crystal belongs to the monoclinic system=space group P21/c with a=5.9362(8)=b=11.5070(15)=c=29.460(4)=β=97.326(3)°=V=1995.9(5)3=Z=4=F(000)=808=C22H24N2O2S=Mr=380.49=Dc=1.266 g/cm3=S=1.031=μ=0.181 mm--1=the final R=0.0474 and wR=0.1441 for 4327 observed reflections(I > 2σ(I)).Intramolecular O-H…N hydrogen bond is observed in the crystal.The preliminary bioassay showed that the title compound exhibits 95% inhibition rate against Rhizoctonia solani at the test concentration of 500 mg/L.