Synthesis and Crystal Structure of Dimethyl-3-（4-bromophenyl）-1-phenyl-4,5-dihydro-1H-pyrazole-4,5-dicarboxylate

The title compound (C19H17BrN2O4) was synthesized via a one-pot procedure starting from 4-bromobenzaldehyde, dimethyl acetylenedicarboxylate (DMAD) and phenylhydrazine with pyridine as the catalyst. Its structure was determined by single-crystal X-ray diffraction analysis. The crystal belongs to the monoclinic system, space group P21/c with a = 11.115(3), b = 8.090(2), c = 20.211(5) , β = 97.032(5)°, V = 1803.7(8) 3, Z = 4, Mr = 417.25, Dc = 1.536 g/cm3, μ = 2.306 mm-1, F(000) = 852, the final R = 0.0403 and wR = 0.0895 for 2215 observed reflections with I 2σ(I).     

Synthesis and Crystal Structure of 3,3＇-（4-Dimethylaminobenzylidene）- bis-（4-hydroxycoumarin）

The title compound 3,3'-(4-dimethylaminobenzylidene)-bis-(4-hydroxycoumarin) 3 was synthesized by the reaction of 4-hydroxycoumarin with 4-dimethylaminobenzaldehyde, and its chemical structure was determined by X-ray single-crystal diffraction. It crystallizes in monoclinic, space group P21/n with a = 11.698(2), b = 10.882(2), c = 16.594(3) , β = 90.69(3)o, V = 2112.1(7) 3, Z = 4, F(000) = 952, Dc = 1.432 Mg/m3, Mr = 455.45, μ = 0.102 mm-1, λ = 0.71073 , the final R = 0.0779 and wR = 0.2143 for 3031 observed reflections with I > 2σ(I).     

Synthesis and Crystal Structure of a Dinuclear Complex： Bis[aqua（phen）（4- aba）copper（Ⅱ）nitrate（4-abaH）dihydrate]

The title complex has been obtained by the reaction of copper nitrate tri-hydrate with 4-abaH (4-abaH=4-aminobenzonic acid) and phenanthroline in ethanol solution,and its structure was determined by X-ray crystallography with the following data: monoclinic,space group C2/c,Mr=1266.13,Cu2C52H54N10O20,a=25.884(5),b=10.205(2),c=20.849(4) ,β=106.34(3)°,Z=4,V=5284.7(18) 3,F(000)=2616,Dc=1.591 g/cm3,μ=0.896 mm-1,the final R=0.0441 and wR=0.1148 for 4200 observed reflections (I > 2σ(I)). In the molecule of the title complex,the asymmetric unit contains one half molecule. The Cu(Ⅱ) atom is five-coordinated by a terminal water molecule,a bidentate phenanthroline and two monodentate 4-aminobenzoate ligands forming a square pyramidal coordination environment. The two bridging 4-aminobenzoate ligands result in a dinuclear copper(Ⅱ) cluster with a short Cu–Cu distance (3.048 ) and a π-π stacking between the adjacent phenanthroline rings (2.96 ).     

Synthesis and Crystal Structure of（3S,4R,Z）-3,6-dimethyl-2-（3-methylbut-2-enylidene）-2,3,3a,4,7,7a-hexahydrobenzofuran-3,4-diol

The title compound of(3S,4R,Z)-3,6-dimethyl-2-(3-methylbut-2-enylidene)-2,3,3a,4,7,7a-hexahydrobenzofuran-3,4-diol,C15H22O3,as a potential gastric cytoprotective agent has been synthesized by the reduction of bisabolangelone in methanol with sodium borohydride.The title compound was characterized by IR and NMR spectra.Meanwhile,the crystal was obtained and determined by X-ray single-crystal diffraction.Crystal data:monoclinic system,space group P21 with a = 6.0692(12),b = 8.9954(18),c = 13.182(3) ,β = 92.59(3)°,V = 718.9(2) 3,Z = 2,F(000) = 272,Dc = 1.156 g/cm3,μ = 0.633 mm-1,R = 0.0362 and wR = 0.1051 for 9490 independent reflections(Rint = 0.0172) and 2461 observed reflections(I > 2σ(I)).Intermolecular O-H…O interactions link the molecules into one-dimensional infinite chains running along the b axis,which contributes to the stability of the crystal structure.     

Synthesis and Crystal Structure of 2-Methoxy-benzoic Acid 2-Oxo-3-（2,4,6-trimethyl-phenyl）-1-oxa-spiro[4.4]non-3-en-4-yl Ester

The new title compound 2-methoxy-benzoic acid 2-oxo-3-(2,4,6-trimethyl-phenyl)-1-oxa-spiro[4.4]non-3-en-4-yl ester(3,C25H26O5) has been synthesized by the condensation reaction of 4-hydroxy-3-(2,4,6-trimethyl-phenyl)-1-oxa-spiro[4.4]non-3-en-2-one(2) with 2-methoxylben-zoyl chloride,and characterized by 1H NMR and MS spectra.Its crystal structure was determined by single-crystal X-ray diffraction.The crystal is of monoclinic,space group P21/c with a = 10.6945(7),b = 12.8176(7),c = 16.4223(10) ,β = 103.5665(17)o,V = 2188.3(2) 3,Z = 4,Dc = 1.234 g/cm3,F(000) = 864.000,μ = 0.085 mm-1,the final R = 0.0520 and wR = 0.1132 for 2732 observed reflections with I 2σ(I).In the crystal structure,the C(1)-C(2)(1.478 ) bond is significantly shorter than the normal single C-C bond(1.53 ),suggesting that the carbonyl group on C(1) has formed a conjugated system with a double bond on C(2) and C(12).     

Formation and Crystal Structure of 1-（N-tert-butyloxycarbonyl-L-prolyl）-1,3-dicyclohexylurea

The title compound 1-(N-tert-butyloxycarbonyl-L-prolyl)-1,3-dicyclohexylurea formed in the coupling reaction of N-Boc-L-proline and n-butyl amine activated by DCC as an unexpected product was characterized through IR,1H NMR,13C NMR and HRMS spectra as well as single-crystal X-ray diffraction analysis.The crystal(C23H39N3O4,Mr = 421.57) belongs to the orthorhombic system,space group P212121,a = 10.8990(5),b = 12.2153(6),c = 18.8102(9) ,V = 2504.3(2) 3,Z = 4,Dc = 1.118 g/cm3,λ(MoKα) = 0.71073 ,μ = 0.076 mm-1,F(000) = 920,the final R = 0.0572 and wR = 0.1521 for 3564 observed reflections with I > 2σ(I).An intramolecular hydrogen bond N(3)-H…O(2) is observed.     

Synthesis and Crystal Structure of 3-（4-Bromobenzyloxy）-6-morpholinopyridazine

The title compound 3-(4-bromobenzyloxy)-6-morpholinopyridazine(C15H16BrN3O2) was synthesized,and its crystal structure was studied.It crystallizes in the triclinic system,space group P with a = 8.3408(17),b = 8.8620(18),c = 10.832(2) ,α = 108.09(3),β = 91.28(3),γ = 100.90(3)°,Dc = 1.562 g/cm3,Z = 2,λ = 0.71073 ,μ(MoKα) = 2.769 mm-1,Mr = 350.22,V = 744.5(3) 3,F(000) = 356,the final R = 0.0522 and wR = 0.1366 for 2016 observed reflections with I > 2σ(I).In the crystal structure,the morpholine ring adopts a chair conformation with O(2) and N(3) atoms at the flap positions-0.656(7) and 0.622(6)  out of the mean plane formed by the other four C atoms,respectively.These molecules generate centro-symmetric dimers through intermolecular π-π interaction.     

A New Heteropolyoxotungstate with a Three-dimensional All-inorganic Framework [（C2H4N2）4（P4Co3W4O（28）H6）（H2C2O4）]n

A new heteropolyoxotungstate [(C2H4N2)4(P4Co3W4O28H6)(H2C2O4)]n with a three-dimensional framework was hydrothermally synthesized.The compound crystallizes in a tetragonal system,space group I41/a with a = 17.1006(17),b = 17.1006(7),c = 10.7525(5),V = 3144.2(2)3,Z = 4,Dc = 3.795 g·cm-3,F(000) = 3300,MoKα(λ = 0.71073 ),μ = 16.460 mm-1,the final R = 0.0335 and wR = 0.0776.In the heteropolyoxotungstate,tungsten-oxygen octahedra are linked by sharing two cis-vertexes into an infinite helical chain extending along the c axis.Cobalt atoms in the octahedral geometry act as the linkers of these chains,forming a three-dimensional framework.The cobalt and phosphorus atoms in the tetrahedral geometry play a role in stabilizing the three-dimensional framework.Ethylenediamine molecules are polymerized into organic chains which locate in the interspaces of the framework in the way of interwinding with the W-O chains.     

Synthesis and Crystal Structure of （Z）-Methyl-3-methoxy-2-{2-[（4-（E-3-p-tolylacryloyl）phenoxy）methyl]phenyl}acrylate

The title compound,(Z)-methyl-3-methoxy-2-{2-[(4-(E-3-p-tolylacryloyl)phenoxy)-methyl]phenyl}acrylate,was synthesized and determined by X-ray single-crystal diffraction. The crystal belongs to the triclinic system,space group P1 with a = 8.0157(8),b = 12.5748(13),c = 13.3768(14) ,α = 64.770(2),β = 75.720 (2),γ = 89.784(2)°,μ = 0.085 mm-1,Mr = 442.49,V = 1174.1(2) 3,Z = 2,Dc = 1.252 g/cm3,F(000) = 468,T = 294(2) K,R = 0.0603 and wR = 0.1498 for 2644 observed reflections with I 2σ(I). X-ray diffraction analysis reveals that the single crystal contains strong non-classical hydrogen bonds. The preliminary bioassay showed that the title compound exhibits inhibitory activity against the Pseudoperoniospora cubensis and Rhizoctonia solani at the test concentration of 200 mg/L.     

Synthesis and Crystal Structure of Ethyl 1-（2-bromoethyl）-3-（4-meth-oxyphenyl）-1H-pyrazole-5-carboxylate

The title compound ethyl 1-(2-bromoethyl)-3-(4-methoxyphenyl)-1H-pyrazole-5-carboxylate 1 has been synthesized and structurally characterized by single-crystal X-ray diffraction.The crystal is of monoclinic(C15H17BrN2O3,Mr = 353.22),space group C21 with a = 24.691(7),b = 6.7678(17),c = 17.884(5) ,β = 97.184(5)o,V = 2965.1(13) 3,Z = 8,Dc = 1.583 g.cm-3,F(000) = 1440,μ = 2.784 mm-1,the final R = 0.0260 and wR = 0.0596 for 2684 observed reflections with I > 2σ(I).All the carbon atoms in the molecule are nearly coplanar except C(15),with a large conjugated system among the carbonyl group,pyrazole ring and the benzene ring.Three non-classical intermolecular hydrogen bonds help to stabilize the crystal lattice.The regioselectivity was rationalized based on the coordination of potassium ion with the N-anion and the carbonyl oxygen atom.     

A New 3D Supramolecular Network Formed by [Zn_3（2,6-Pyridinedicarboxylate）_3Cl_4]~（4-）and 4-Carboxypyridinium

A new compound [Zn3(C7NO4H3)3Cl4]·[C6NO2H6]4·4H2O (I) has been synthesized and structurally characterized by X-ray crystallography.It crystallizes in monoclinic,space group C2/c with a=16.9018(14),b=12.6902(10),c=25.1170(2),β=90.54°,V=5387.0(8)3,Z=4,Zn3C45H41Cl4N7O24,Mr=1401.76,Dc=1.728 g/cm3,F(000)=2840,μ(MoKa)=1.615 mm-1,the R= 0.0758 and wR=0.2060 for 3468 observed reflections (I 2σ(I)).Analysis of single-crystal X-ray diffraction data shows that compound I displays an interesting example of 3D supramolecular networks with perfect neutral and ionic hydrogen bonding array.     

Syntheses and Crystal Structures of 4-Amino-3- （3-hyd roxyp ropyl）- 1H-1,2,4-triazole-5（4H）-thione and 6-（4-Biphenylyl）-3-（3-hydroxypropyl）-7H-1,2,4-triazolo[3,4-b][1,3,4]thiadiazine

1INTRODUCTION It has been reported that3,6-disubstituted-7H-1,2,4-triazolo[3,4-b][1,3,4]thiadiazines have a broad spec-trum of bioactivities,such as antimicrobial[1],antibac-terial,antifungal[2],anti-inflammatory[3],diuretic[4],an-thelmintic and analgesic[5].They can also be used as plant-growth regulating agents[6],photographic coup-lers,dyes for improved preservability and absorption characteristics,and inhibitors of malignant cellularZOU K.H.et al.:Syntheses and Crystal Structures o…     

Synthesis and Crystal Structure of 1＇-Methyl-4＇-（4-chlorophenyl）-1H-indole-3-spiro-2＇-pyrrolidine-3＇-spiro-4＂-（2＂-phenyloxazole）-2,5＂（3H,4＂H）-dione

The title compound （C26H20ClN3O3） has been synthesized by 1,3-dipolar cycloaddition reaction from isatin, sarcosine and （Z）-4-（4-chlorobenzylidene）-2-phenyloxazol-5（4H）-one through a one-pot procedure, and its structure was confirmed by IR, IH NMR, elemental analysis and single-crystal X-ray diffraction analysis. The crystal belongs to the triclinic system, space group PI, with a = 9.3903（19）, b = 11.398（2）, c = 12.603（3） A, α = 83.495（3）, β = 68.988（3）, γ = 67.178（3）^o, V= 1160.1（4）A^3 Z = 2, Mr= 457.90, Dc= 1.311 g/cm^3, p = 0.198 mm ^-1, F（000） = 476, the final R = 0.0489 and wR = 0.1144 for 3109 observed reflections with I 〉 2σ（I）.     

Crystal Structure of 3-Methyl-4-methoxy-3-(3-methyl-4- methoxy-2-benzofuranyl) -2-H-benzofuranyl

1　ＩＮＴＲＯＤＵＣＴＩＯＮ3ｍｅｔｈｙｌ4ｈｙｄｒｏｘｙｂｅｎｚｏｆｕｒａｎｉｓａｎｉｎｔｅｒｍｅｄｉａｔｅｕｓｅｄｆｏｒｔｈｅｓｙｎｔｈｅｓｉｓｏｆｎａｔｕｒｅｐｒｏｄｕｃｔｓ[1].Ｉｔｈａｓｂｅｅｎｓｙｎｔｈｅｓｉｚｅｄｆｒｏｍ1,3ｄｉｈｙｄｒｏｘｙｂｅｎｚｅｎｅ[2-3].Ｔｏｓｙｎｔｈｅｓｉｚｅａｂｉｅｔａｎｅｑｕｉｎｏｎｅｄｉｔｅｒｐｅｎｏｉｄｓｗｉｔｈｉｔ[4,5],ｗｅｉｎｔｅｎｄｅｄｔｏｐｒｏｔｅｃｔｔｈｅｈｙｄｒｏｘｙａｔｔａｃｈｅｄｔｏｉｔｗｉｔｈＭｅ2ＳＯ4.Ｆｉｎａｌｌｙ,ｔｗｏｃｏｍｐｏｕ…     

Synthesis and Crystal Structure of N-[1-(4-Chlorophenyl)- 1,4-dihydro-4-oxe-6-methylpyridazine-3-carbonyl]- N'-benzoylhydrazine

1 INTRODUCTION Pyridazinone derivatives represent one of the most active classes of compounds possessing a wide spectrum of biological activity. It was widely used in pharmaceuticals and agrochemicals[1, 2]. Rohm Haas Company had reported that pyridazinones exhibit useful plant growth regulating effects [3,4]. It was also reported that diacylhydrazines exhibit excellent insecticides [5~7]. In view of these facts, it was contemplated to synthesize compounds con- taining both pyridazinone …     

Synthesis and Crystal Structure of (E)-2-(1-(2-Hydroxy-4-methoxyphenyl)ethylideneamino)-3-(4-hydroxyphenyl)methyl Propionate

(E)-2-(1-(2-Hydroxy-4-methoxyphenyl)ethylideneamino)-3-(4-hydroxyphenyl)methyl propionate (C22H27O6N, Mr = 401.45) has been synthesized by a condensation reaction of paeonol with tyrosin methyl ester hydrochloride, and its structure was determined by IR, NMR, HR MS and X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P21/c, with a = 11.91291(15), b = 9.49947(12), c = 19.8727(3) , β = 106.1104(15)°, V = 2160.60(5)3, Z = 4, Dc = 1.234 g/cm3, μ = 0.739 mm-1, F(000) = 856, R = 0.0466 and wR = 0.1461 for 3859 observed reflections with (Ⅰ> 2σ(Ⅰ)). In the crystal structure, the title compound is constructed by a centrosymmetric dimmer unit composed of a pair of π-π stacking enantiomers, and such units are linked by intermolecular O(5)-H(5)…O(1) and intramolecular N(1)-H(1)…O(1) hydrogen bonds.     

Synthesis and Crystal Structure of Chloro(p-toluidine)[4-(p-tolyl)imino-2-pentanone-3-oximato]- palladium(Ⅱ), PdCl(p-CH_3C_6H_4NH_2)(p-CH_3C_6H_4-iai)

1 INTRODUCTION Transition metal complexes of N-R-isonitroso- b-ketoimine have received considerable interest, because the isonitroso (oximo) group can coordinate to metal atoms through its oxygen and/or nitrogen atoms to form several geometrical isomers[1～4]. Some palladium(Ⅱ) complexes with N-R-isonitro- soacetylacetoneimine (abbreviated to R-Hiai)[4] and N-R-isonitrosoethylacetoacetate (abbreviated to R- Hieai)[5] have been reported. Here we will report the structure of a palladi…     

Synthesis and Crystal Structure of 2-Amino-4- chloro-5-（4-methylbenzyl）-6-methylpyrimidine

The title compound 2-amino-4-chloro-5-(4-methylbenzyl)-6-methylpyrimidine (C26H28Cl2N6, Mr = 495.44) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. The crystal belongs to monoclinic, space group P21/c with a = 14.892(7), b = 6.129(3), c = 14.889(7) , β = 109.795(8)°, V = 1278.7(10) 3, Z = 2, F(000) = 520, Dc = 1.287 g/cm3, μ = 0.280 mm-1, the final R = 0.0577 and wR = 0.1589 for 1357 observed reflections with I > 2σ(I). A total of 6091 reflections were collected, of which 2257 were independent (Rint = 0.033). The X-ray analysis reveals that the chlorine atom and methyl of the title compound are disordered.     

混合三烃基锡有机酸酯化合物构效关系 （Ⅰ）二环己基－甲基－2，4－二溴－β－甲基苯氧乙酸锡酯 及二环己基－甲基－2－甲氧基－4－丙烯基苯氧乙酸锡酯的晶体结构和分子结构

报道２，４－Ｂｒ２Ｃ６Ｈ３ＯＣＨ（ＣＮ３）ＣＯ２Ｓｎ（Ｃ６Ｈ１１）２ＣＵ３（１）和２－ＯＣＨ３－４－ＣＨ３ＣＨ＝ＣＨＣ６Ｈ３ＯＣＨ２ＣＯ２Ｓｎ（Ｃ６Ｈ１１）２ＣＨ３（Ｈ２Ｏ）（Ⅱ）的晶体结构和分子结构。（Ⅰ）单斜晶系，空间群Ｐ２１／ｃ，ａ＝１３．０６７（３），ｂ＝１０．５９４（３），ｃ＝１８．１５７（４），β＝１０６．９９（２）°，Ｚ＝４，Ｄｃ＝１．６７２ｇ／ｃｍ３，Ｖ＝２４０３．７３，μ＝４３．７３１ｃｍ－１，Ｍｒ＝６２２．９９，Ｆ（０００）＝１２３２；（Ⅱ）单斜晶系，空间群Ｐ２１／ｎ，ａ＝１０．４０９（１），ｂ＝　１２．５７０（２），ｃ＝２０．６６４（２），β＝８３．５１（１）°，Ｚ＝４，Ｄｃ＝１．２８１ｇ／ｃｍ３，Ｖ＝２６８６．４Ａ３，μ＝９．７６１ｃｍ－１，Ｍｒ＝５３９．２８，Ｆ（０００）＝１１２０．最后的偏离因子，化合物（Ⅰ）Ｒ＝０．０４６，Ｒω＝０．０４６；化合物（Ⅱ）Ｒ＝０．０４９，Ｒω＝０．０４７。晶体结构解析表明，化合物（Ⅰ）和（Ⅱ）中的锡均被配体的３个碳和２个氧原子配位，配位原子呈畸变三角双锥构型；化合物中的环己基均为椅式构象；化合物（Ⅱ）中，配位水分子和另一分子的羰基氧与芳环上的甲基氧?     

Synthesis and Crystal Structure of {4-[2-（9- Hexyl-9H-carbazol-3-yl）vinyl]phenyl} Dimethylamine

The title compound {4-[2-(9-hexyl-9H-carbazol-3-yl)vinyl]phenyl} dimethylamine has been synthesized by the well known Wittig reaction, and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in monoclinic, space group P21/c with a = 47.87(2), b = 10.222(4), c = 9.612(4) , β = 92.401(9)o, V = 4699(3) 3, Z = 8, C28H32N2, Mr = 396.56, Dc = 1.121 g/cm3, F(000) = 1712 and μ(MoKa) = 0.065 mm-1. The final R and wR are 0.0793 and 0.1983, respectively for 3524 observed reflections with I > 2σ(I). In the title compound, the bond lengths are normal, and the crystal is stabilized by Van der Waals’ forces.