Synthesis and Crystal Structure Analysis of 2-（3,5-Di-tert-butyl-2-hydroxyphenyl）-2-（3,4- dimethylphenyl） Acetic Acid Dimethylamine Salt

A new compound 2-（3,5-di-tert-butyl-2-hydroxyphenyl）-2-（3,4-dimethylphenyl） acetic acid dimethylamine salt （[NH2（CH3）2][C24H31O3]） was synthesized and structurally determined. It is of monoclinic system, space group P21/c with a = 14.731（2）, b = 10.1185（10）, c = 17.065（2） A^°, β = 98.293（10）° ,Z = 4, V = 2517.0（6）A^°^3, Dc = 1.091 g/cm^3, F（000） = 904 and Mr= 413.58. The dihedral angle defined by two benzene rings is 98.23°.     

Synthesis and Crystal Structure of 3-（2-Hydroxy-phenyl）-5-（2-methylphenyl）-6-thoxycarbonyl-cyclohexen-2-one

1 INTRODUCTION The molecular assembly of one- or multi-dimen-sional aggregation by hydrogen bonds is now an im-portant subject of supramolecular chemistry and crys-tal engineering[1, . Supramolecular structures formed 2]via intermolecular hydrogen bonds X–H…X or C–H…X (X = O, Cl, N, et al.) are very common inorganic compounds[3~12], and they generally possessdifferent properties due to these hydrogen bonds. Concerning about the spectra of benzene-contai-ning…     

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…     

Synthesis and Crystal Structure of（E）-Ethyl 2-（5-（3-methyl-2-butenyloxy）-2-（3-（4-（3-methyl-2-butenyloxy）phenyl）acryloyl）phenoxy）acetate

The title compound,(E)-ethyl 2-(5-(3-methyl-2-butenyloxy)-2-(3-(4-(3-methyl-2-butenyloxy)phenyl) acryloyl) phenoxy)acetate(1),has been synthesized and characterized by FT-IR and 1H-NMR spectroscopy,ESI-MS,and X-ray single-crystal diffraction.FT-IR,1H-NMR and ESI-MS confirm the functional groups,particularly the ethyl groups in the ester moiety,of the compound.The single-crystal X-ray diffraction has revealed a monoclinic structure,space group P21/n with a = 14.6832(14),b = 7.7581(7),c = 23.075(2),β = 101.670(2)o,V = 2574.2(4) ?3,Z = 4,Dc = 1.235 g/cm,μ = 0.085 mm-1,and F(000) = 1024.The skeleton of chalcone in the molecular structure is coplanar.     

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.     

Syntheses and Crystal Structures of Methyl 2-（4,5-Dibromo- 1-methylpyrrole-2-carbonylamino）-3-phenyl propanoate and 4,5-Dibromo-1-methyl-2-trichloroacetylpyrrole

1 INTRODUCTION Pyrrole and its derivatives have attracted much attention due to their chemical properties as well as biological activities[1]. They have been widely used as the materials to produce pharmaceutical, essences, biochemicals, etc. It has been found that a great deal of pyrrole derivatives present bioactivities, such as antitumor and antiviral activities[2~5]. Thus, due to the interest in exploring the syntheses of potential bioactive materials which contain pyrrole ring andna…     

Synthesis and Crystal Structure of (2S,2'S,4'R)-2-(1-Hydroxy-1-ethylpropyl)-1-[(1'-p-tosyl-4'-hydroxypyrrolidin-2'-yl)methyl]pyrrolidine

1 INTRODUCTION In recent years, chiral β-amino alcohols have attracted much attention due to their special bio- logical functions and catalytic activities. Chiral β- amino alcohol moieties are usually found not only in natural products (e.g., cinchona alkaloids, ephe- drine, toxal, etc.) with special biological activities[1, 2], but also critical structural segments of some syn- thesized biologically active compounds, such as adrenergic agonists or antagolist[3, 4] and inhibitors for HI…     

Synthesis and Structure of E-2- (2,4,6-tri-tert-butylphenylphosphinyl ) - 2- [N- (tert-butyldimethylsilyl) - N- (p-chrolophenyl ) ] amino- 1- (2,4,6-tri-tert- butyl-phenyl ) phosphacthylene

The title compound E-2-(2, 4, 6-tri-tert-butylphenylphosphinyl)-2-[ N- ( tert-butyldimethylsilyl )-N- ( p-chrolophenyl )] amino-l- ( 2, 4, 6-tri-tert-butylphenyl)phosphacthylene (C49H78NClP2Si, Mr= 806.65) was synthesized and characterized by X-ray diffraction analysis. The crystal is monoclinic, space group P 21 /n with a=10.319(3), b=23.309(5), c=21.41(1) A, β=99.64(5)°, V=5078(3)A3, Z =4, Dc=1. 05g/cm3, F(000)=1760, μ=1. 92cm-1. Due to the steric hindrance from substituents around phosphaethylene, the P = C bond length is significantly longer than those observed in its analogues. The values of the three bond angles involved in the sp2-hybridized carbon atom (C(1)) of the phosphaethylene are 133.4, 115.1 and 111.4° respectively, deviating significantly from the ideal value of 120°. In addition,although 5 sp2- hybridized atoms (C(2), P(1), C(1), N and C(44)) are sequentially bonded in this molecule, no interaction is observed among the remaining pz orbits of these atoms on the string.     

CRYSTAL STRUCTURE OF 2-(PHENYLAMINO THIOFORMYD-3,4,5,6-TETRAHYDROPYRIMIDINE

<正> The title compound 2-(phenylamino thioformyl)-3,4,5,6-tetrahy-dropyrimidine(C11H13N3S,Mr=219)was synthesized by the reaction of N,N'-diphenyl dithiooxamide with 1,3-diamine trimethylene.The crystal is monoclinic,space group P21,with unit cell constants a=6.253(1),b=7.304(1),c=12.027(2)A,β=102.71(1)°,Z=2,V=535.9(2)A3,Dc=1.35.g/cm3.The final deviation factor R=0.025.The result reveals that the dihedral angle between the thio-formyl group [S,C(7),C(8),N(1)]and the phenyl ring is 33.4°,and the thio-formyl group and the mean plane of the atoms [N(3),C(8),N(2),C(9)]are nearly coplanar.     

Synthesis and Molecular Structure of (E)-1-(Morpholino)-2-(thiomethyl)-2-phenylvinylphosphonate

1 INTRODUCTION Phosphorus-containing vinyl compounds havebeen widely studied due to their versatile physiolo-gical activities and applications in transition metalchemistry, asymmetric catalysis and photorearrange-ment[1～4]. In our previous papers, we have reportedthe syntheses of 2,2,4,5-tetrasubstituted-1,3-dithio-les[5] and 2,5-bis(morpholino)-3,4-bis-(p-chloro-phe-nyl)thiophenes[6] by the reactions of α-thioaroyl-thiofor-mamide with trimethyl phosphite at room tempera-ture and in refl…     

Syntheses and Crystal Structures of （S）-Methyl 2-（4-R-phenylsulfonamido）-3-（1H-indol-3-yl）propanoate （R = H （1） and Cl （2））

The title compounds （S）-methyl-2-（4-R-phenylsulfonamido）-3-（1H-indol-3- yl）propanoate （R = H （1）, Cl （2）） have been synthesized and their crystal structures also have been determined by X-ray single-crystal diffraction. Compound 1 （C18H18N2O4S） belongs to orthorhombic, space group P212121 with a = 9.6348（14）, b = 11.1517（17）, c = 16.412（3） A, V = 1763.4（5） A^3, Mr = 358.40, Z = 4, De = 1.350 g/cm^3,/t = 0.209 mm^-1, F（000） = 752, R = 0.0348 and wR = 0.0714. Compound 2 （CI8H17ClN2O4S） crystallizes in orthorhombic, space group P212121 with a = 9.3128（14）, b = 10.9655（16）, c = 17.783（3） A, V = 1815.9（5） A^3, Mr = 392.85, Z = 4, De = 1.437 g/cm^3, p = 0.352 mm^-1, F（000） = 816, R = 0.0389 and wR = 0.0845. The absolute structure Flack parameters X of compounds 1 and 2 are -0.03（8） and -0.06（7）, respectively. X-ray analysis reveals that the crystal structures of these two compounds both involve two intermolecular N-H…O hydrogen bond＇s.     

2-(2'-吡啶基)-5-甲苯并噻唑及其二氯二乙基锡(Ⅳ)络合物的结构以及抗肿瘤有机锡络合物分子设计的展望

X-射线单晶衍射法测定了2-(2′-吡啶基)-5-甲苯并噻唑(1)及其二氯二乙基锡(Ⅳ)络合物(2)的结构。晶体(1)属单斜晶系,空间群为P2_1/n,晶胞参数a=5.808(2),b=10.283(3),c=18.373(3),β=91.48(2)°,Z=4,D_c=1.370g·cm~(-3),偏离因子R=0.047。晶体(2)属单斜晶系,空间群P2_1/c,晶胞参数a=17.271(2),b=9.411(1),c=14.015(2),β=122.98(1)°,Z=4,D_c=1.648g·cm~(-3),偏离因子R=0.047。络合物中Sn—N平均键长已达2.50。参考顺铂类药物研究经验,展望了抗肿瘤有机锡络合物发展的前景。     

Crystal Structures of (Z)-1-Phenyl-1-phenylseleno-2-(p-tolylsulfonyl)ethene and (Z)-1,3-Diphenyl-3-phenyl-seleno-2-(p-tolylsulfonyl)-2-propen- 1-ol

1 INTRODUCTION The vinyl sulfones are versatile intermediates in organic chemistry and have been extensively stu- died[1]. The available methodology for vinyl sulfone synthesis mainly consists of Horner-Emmons reac- tions of carbonyl compounds with sulf…     

Resolution and Crystal Structure of 9α-(3-Azabicyclo[3,3,1]nonanyl)- 2''-cyclopentyl-2''-hydroxyl-2''-thienylacetate

The crystal structure of 9α-(3-azabicyclo[3,3,1]nonanyl)-2'-cyclopentyl-2'-hydro-xyl-2'-thienylacetate (C16H27NO3S, Mr = 349.48) has been determined by single-crystal X-ray diffraction analysis. The crystal belongs to orthorhombic, space group P212121 with a = 14.937(3), b = 8.1673(16), c = 15.423(3) (A), V = 1881.5(6) (A)3, Z = 4, Dc =1.234 g/cm3, μ = 0.188 mm-1, F(000) = 752, the final R = 0.0468 and wR = 0.1251. The bicyclo[3,3,1]nonane ring system adopts the most favored twin-chair conformation. The crystal structure shows the existence of intramolecular O-H…O hydrogen bonds by which a one-dimensional chain struc- ture is formed.     

Crystal Structure of 2-(4-Fluorophenylamino)-2-thiomethyl acetophenone

1mThODUCTIONThioacetalshavebeenwellstudied,becauseoftheirapplicationsinorganicsyn-thesist1i.However,aketohemithioacetalshaveseldombeeninvestigated.Inthispa-Per,wediscussedthecrystalstructureofthetitlecompoundsynthesizedbythereac-tionofabenzoylhemithioacetal(2-hydroxy-2-thiomethylacetoPhenone)and4-fluthroaniline.Sinceknowledgeofthemolecularandcrystalstructureofthetitlecom-PoundwasconsideredusefulforunderstandingthemechanismofthereactionandchemicalproPertiesofaketohemithioacetal,theX-raycr…     

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?..     

Synthesis and Crystal Structure of 5,5-Dimethyl-2-(4-chlorophenyl)(3-hydroxy-5,5-dimethyl-2-cyclohexen-1-one-2-yl)methyl-3-(4-methoxyphenylamino)-2-cyclohexene-1-one

The title compound 5,5-dimethyl-2-(4-chlorophenyl)(3-hydroxy-5,5-dimethyl-2-cyclohexen-1-one-2-yl)methyl-3-(4-methoxyphenylamino)-2-cyclohexen-1-one has been synthesized,and its crystal structure was characterized by X-ray single-crystal diffraction. The crystal belongs to monoclinic,space group P21/c with a=9.4193(13),b=26.915(4),c=21.188(3),β =101.906(3)°,V =5256.2(13)3,Z =4,C60H68Cl2N2O8,Mr=1016.06,Dc=1.284 g/cm3,F(000)=2160,λ(MoKα)=0.71073,μ=0.182 mm–1,R=0.0530 and wR=0.1131 for 4128 observed reflections (I>2σ(I)). X-ray analysis reveals that there are two independent molecules in the unit and the cyclohexenone rings adopt different conformations. In addition,there are four intramolecular hydrogen bonds in the title molecule.     

Synthesis and Crystal Structure of 2-(4-Fluoro-2-(4-fluorophenoxy) phenyl)-1-(1H-1,2,4-triazol-l-ylmethyl)-3-methoxy-isopropy Alcohol

The title compound 2-(4-fluoro-2-(4-fluorophenoxy)phenyl)-1-(1H-1,2,4-triazol-z 1-ylmethyl)-3-methoxy-isopropy alcohol has been synthesized by the treatment of 1-[2-(4-fluoro-2-(4-fluorophenoxy)phenyl)-2,3-epoxypropyl]-1H-1,2,4-tdazole with sodium methoxide. It be-longs to orthorhombic, space group P212121, with a=9.7229(19), b=11.516(2), c=16.047(3) A, C18H17F2N3O3, Mr-361.35, V=1796.7(6) A3, Z=4, Dc=1.3359 g/cm3, F(000)=752,μ=0.106 mm-1, the final R=0.0329 and wR=0.0803 for 1821 unique reflections. The dihedral angles made by the triazole ring with two benzene rings are 43.56(3) and 54.78(2)°, respectively. The intermolecular hydrogen bond in the crystal lattice plays an important role in stabilizing the structure.     

Synthesis and Crystal Structure of 1-(2-Methyl-5-formyl-3-thienyl)-2-(2-methoxylphenyl)perfluorocyclopentene

A new family of photochromic diarylethene compounds, 1-(2-methyl-5-formyl-3- thienyl)-2-(2-methoxylphenyl)perfluorocyclopentene (1o) having an unsymmetrically substituted hexafluorocyclopentene unit, was synthesized and its structure was determined. The crystal belongs to the monoclinic system, space group P21/c with a = 15.4866(5), b = 9.0744(9), c = 12.6906(3), β = 90.1480(10)°, Z = 4, V = 1783.4(3)3, Dc = 1.513 mg/m3, μ = 0.25, F(000) = 824, the final R = 0.0579 and wR = 0.1566 for 2584 observed reflections (I > 2σ(I)). Interestingly, a colorless compound 1o undergoes photocyclization upon irradiation of UV light to give the blue isomer diarylethene. Upon irradiation with visible light with wavelength greater than 510 nm, the blue compound can return to its initial colorless state.     

Synthesis,Crystal Structure and Antifungal Activity of N-（Pyridine-2-methyl）-2-（4- chlorophenyl）-3-methylbutanamide

A novel compound N-（pyridine-2-methyl）-2-（4-chlorophenyl）-3-methylbutanamide, a racemic compound, has been synthesized with 2-（4-chlorophenyl）-3-methylbutyric acid and pyridin- 2-methylanamine as the raw materials, and its crystal structure （C17H19C1N2O, Mr = 302.79） was determined by single-crystal X-ray diffraction analysis. The crystal belongs to monoclinic, space group P21/n with a = 9.624（9）, b = 23.14（2）, c = 15.626（15）A, β = 106.199（14）°, V = 3342（5） A^3, Z = 8, Dc = 1.204 g/cm^3,μ = 0.23 mm^-1, F（000） = 1280, S = 1.032, R = 0.0681 and wR = 0.1508 for 6513 unique reflections （Rint = 0.0421） with 3375 observed ones. In the crystal structure, there are some intermolecular hydrogen bonds which stabilize the crystal structure. The preliminary bioassay shows that the title compound exhibits good antifungal activity against Botrytis cinerea, Gibberella zeae, Dothiorella gregaria and Colletotrichum gossypii.