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…     

Crystal and Molecular Structure of 4-Hydroxy-3-Methoxy-4-N-Methylstilbazonium Iodide C15H16NO2+·I-

The crystal structure of the title compound C15H16NO2+ · I-(Mr=369. 19) has been determined by single crystal X-ray diffraction analysis. The crystal belongs to tbe monoclinic system with space group P21/c, a=8. 957(1), b=21. 8117(2), c=7. 8760(10)A , β=103.94(1)°, V=1493.8(3)A3, Z=4, Dc=1. 642g cm3,μ=2. 141mm-1, F(000)=728, final R=0. 0264, and Rw=0. 0644(I＞2σ(I)) for 2938 independent reflections. The results show that in the crystal structure of the title compound the planar cations have two configurations, and these cations are anti-parallelly packed through the strong π…π interaction.     

Synthesis and Crystal Structure of (Z)-4-(p-Bromo phenylthio)-3-(p-nitrobenzoyloxy)-3-buten-2-one

１　ＩＮＴＲＯＤＵＣＴＩＯＮＩｎｏｒｄｅｒｔｏｅｖａｌｕａｔｅｔｈｅｓｅｌｅｃｔｉｖｉｔｙａｎｄｒｅａｃｔｉｖｉｔｙｏｆｅｎｏｎｅｓａｓｄｉｅｎｏｎｅｐｈｉｌｅｓａｎｄｄｉｅｎｅｓｉｎＤｉｅｌｓＡｌｄｅｒｒｅａｃｔｉｏｎ,Ｐａｒａｌｔａｓｙｎｔｈｅｓｉｚｅｄβｆｕｎｃｔｉｏｎａｌｉｚｅｄｌａｃｅｔｙｌｖｉｎｙｌａｒｅｎｅｃａｒｂｏｘｙｌａｔｅｓａｓａｓｕｂｓｔｒａｔｅｏｆ１,３ｄｉｐｏｌａｒｃｙｃｌｏａｄｄｉｏｎｒｅａｃｔｉｏｎ〔１〕．Ｘｒａｙｃｒｙｓｔａｌｌｏｇｒａｐｈｉｃｓｔｕｄ…     

A New Sandwich Type Transition Metal Substituted Polyoxotungstate under Hydrothermal Conditions:[NH3(CH2)4NH3]6[Co4(HzO)2(B-α-GeW9034)2]}·7H2O

A new sandwich transition metal substituted polyoxotungstate,[NH3(CH2)4NH3]6 [Co4(H2O)2(B-α-GeW9O34)2]·7H2O 1,was hydrothermally synthesized and characterized by IR spectra and single-crystal X-ray diffraction.The single-crystal X-ray analysis reveals that the crystal crystallizes in monoclinic system,space group P21/c with a=16.6073(6),b=15.3333(5),C=19.9869(7)(A),β=103.41(1)°,Mr=5481.38,V=4950.8(3)(A)3,Z=2,Dc=3.677 g/cm3,F(000)=4900,μ(MoKα)=22.165 mm-1,GOOF=1.005,the final R=0.0228 and wR=0.0527.The crystal structure indicates that the[Co4(H2O)2(B-α-GeW9O34)2]12-polyoxoanion contains two trivacant Keggin[B-α-GeW9O34]10-fragments in a staggered fashion linked via a rhomb-like Co4O16 group in a centrosymmetric arrangement(C2h symmetry)leading to a sandwich-type structure.     

2,6-二甲基-4-苯基-1,4-二氢吡啶-3,5-二甲酸乙酯的合成和晶体结构

标题化合物C1 9H2 3NO4由苯甲醛、尿素、乙酰乙酸乙酯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P2 1 /c ,a =9.745(2 ) ,b =7.388(2 ) ,c =2 4 .354(5) ,β =92 .60 (3)°,V =1 751 .6(6) 3,Z =4,Mr=32 9.38,Dc=1 2 4 9g/cm3,μ(MoKα) =0 .0 87mm- 1 ,F(0 0 0 ) =70 4。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 ,最终的偏离因子为R =0 .0 4 1 6,wR =0 .1 1 75。在晶体结构中 ,二氢吡啶环与苯环之间的二面角为 92 .1 4°。     

Synthesis and Structure of a Dimolybdenum Carbonyl Compound with Thiolato-Bridges [Et4N] 2 [Mo2 (CO) 8 (SC6H4-Cl -p) 2]

Reaction of Mo (CO)6 with p-Cl-C6H4SNa and Et4NCl · H2O in CH3CN afforded a dinuclear molybdenum (0) compound [Et4N]2 [Mo2 (CO)8 (SC6H4-Cl-p)2] (1). The crystal structure was determined by X-ray diffraction. The crystallographic data: C36H48Cl2Mo2N2O8S2, Mr= 963.71, monoclinie, P21/c, a=9. 269(4),b=13.750(3), c=17.466(6) A ;β=104.84(3)°; V=2151.8(3) A3; Z=2; Dc=1.49 g/cm3; F(000)=984; μ=8.3 cm-1; MoKα radiation (λ=0. 71073A ); Final R = 0. 055 and Rw=0. 065 for 3287 reflections with I＞3. 0σ(I). The X-ray structure analysis revealed that the Mo2S2 core is planar. The geometry around each Mo atom is a distance is 4. 014(2) A , and this obviously indicates the absence of Mo-Mo bond.     

Crystal Structure of cis-2-[(P, P-Diethoxy)phosphono(m-nitro)benzyloxy]-4-Phenyl-5,5-Dimethyl-1,3,2-Dioxaphosphorinane 2-Sulfide

The crystal structure of the title compound cis-2-[(P, P-Diethoxy)phosphono(m-nitro)benzyloxy]-4-Phenyl-5,5-Dimethyl-1,3,2-Dioxaphosphorinane 2-Sulfide, C22H29NO8P2S, was determined by single crystal X-ray diffraction. It crystallizes in the monoclinic system, space group P21/c, with Mr=529.49, a=9.888(2), b=20.831(4), c=12.797(3) , β=94.42(3)°, V=2628(1) 3, Z=4, Dx=1.338 g/cm3, λ=0.71073, μ=0.2796 mm-1 and F(000)=556. The structure was solved by direct methods. The final R factor is 0.052 and Rw is 0.057 for 1793 unique observed reflections [I≥3σ(I)]. A cis-configuration and a preferred chair conformation for the molecule have been established by X-ray diffraction analysis. The results presented also give a good explanation to the correlation between the configurational assignments and the regularity in the chemical shifts of C4-H and 31P NMR.     

Synthesis and Structure of Di［bis（diphenylphosphino）ethane］ Copper（Ⅱ） Dinitrate

ＳｙｎｔｈｅｓｉｓａｎｄＳｔｒｕｃｔｕｒｅｏｆＤｉ［ｂｉｓ（ｄｉｐｈｅｎｙｌｐｈｏｓｐｈｉｎｏ）ｅｔｈａｎｅ］Ｃｏｐｐｅｒ（Ⅱ）ＤｉｎｉｔｒａｔｅＬＩＮＫｕｎ－Ｈｕａ；ＹＡＮＧＲｕｉ－Ｎａ；ＣＡＩＤｏｎｇ－Ｍｅｉ；ＪＩＮＤｏｕ－Ｍａｎ（ＨｅｎａｎＩｎ...     

Synthesis and Crystal Structure of N,N′,N″- Tris-（2-aminophenyltriphenylphosphium）- benzene- 1,3,5-tricarboxamide

A new tripodal P,N ligand （C63H48N3O3P3） was prepared and characterized by elemental analysis, IR and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 13.013（3）, b = 28.406（6）, c = 14.911（3） A^°, β= 111.04（3）°, V= 5144.6（18） A^°^3 Z = 4, Dc = 1.276 g/cm^3, Mr = 987.95, λ（MoKa） = 0.71073 A^°,μ = 0.17 mm^-1, F（000） = 2064, R = 0.0786 and wR = 0.1545. A total of 43260 unique reflections were collected, of which 5112 with I 〉 2σ（I） were observed. The title compound has a central benzene ring, which is linked by -NH-CO- bonds to three 2-aminophenyltriphenylphosphium moieties, of which two with P（1） and P（2） centers are pointing to the same face of the central aryl ring, while the third one directs oppositely, forming a pseudo-propeller. In the crystal structure, there exist face-to-face π-π stacking interactions which increase the stability of the crystal structure.     

Synthesis and Crystal Structure of Ethyl 4-（2-Chloro-4-fluorophenyl）-6-hydroxy-3-oxo-1,3-dihydro-5-isobenzofurancarboxylate

The crystal structure of the title compound(C17H12ClFO5,Mr=350.72) was determined by single-crystal X-ray diffraction.The crystal belongs to monoclinic,space group P21/c,with a=7.693(1),b=15.767(1),c=12.986(1),β=97.23(1)°,V=1562.6(2)3,Z=4,Dc= 1.491 g/cm3,λ(MoKα)=0.71073,F(000)=720,μ(MoKα)=0.280 mm-1,R=0.0563 and wR=0.1674.A total of 3592 unique reflections were collected,of which 2462 with Ⅰ2σ(Ⅰ) were observed.Five-membered lactone rings and hydroxyl-substituted phenyl rings are approximately coplanar with their dihedral angle of 4.1°.The dihedral angle between two different phenyl rings is 71.3°.To our interest,intramolecular O(1)-H(1)···O(4) hydrogen bonds could be found in each molecule.Intramolecular hydrogen bonds and intermolecular van der Waals force contribute to the stability of the structure.     

Synthesis and Crystal Structure of 4-tert-Butyl-6-（4-chlorophenyl）-3,6- dihydro-2H-1,3-thiazin-2-iminium Chloride

The title compound, 4-tert-butyl-6-（4-chlorophenyl）-3,6-dihydro-2H-1,3-thiazin- 2-iminium chloride （C14H18C12N2S）, has been synthesized by the reaction of 1-（4-chlorophenyl）- 4,4-dimethylpent-1-en-3-one with thiourea, and its crystal structure was determined by single- crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P211c with a = 16.3064（11）, b = 9.4471（6）, c = 11.2626 （8）A, β = 108.400（1）°, Z = 4, V = 1646.28（19） A^3, Mr = 317.26, Dc = 1.280 g/cm^3, S = 1.078,μ = 0.510 mm^-1, F（000） = 664, the final R = 0.0514 and wR = 0.1412 for 3210 observed reflections （I 〉 2σ（I））. The thiazine ring system displays a twisted boat conformation, and three N-H,..Cl hydrogen bonds exist in the crystal. The combination of two N-H...Cl hydrogen bonds generate an R2^1 （6） ring.     

Synthesis and Crystal Structure of 2-Ethoxy-3-n-butyl-benzofuro[2,3-d]pyrimidin-4（3H）-one

The crystal structure of the new title compound 2-ethoxy-3-n-butyl- benzofuro[2,3d]pyrimidin-4（3H）-one （C16H18N2O3, Mr = 286.32） has been prepared and determined by singlecrystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with a = 13.7167（14）, b = 13.113（1）, c = 8.378（1） A, β = 98.992（2）^o, V = 1488.4（3） A^3, Z = 4, Dc = 1.278, F（000） = 608, μ = 0.089 mm^-1, MoKa radiation （2 = 0.71073）, R = 0.0498, wR = 0.1238 for 2336 observed reflections with I 〉 2σ（I）. X-ray diffraction analysis reveals that all ring atoms in the benzo[4, 5]furo [2,3-d] pyrimi- dinone moieties are almost coplanar.     

Isolation and Crystal Structure of Stigmast-4-ene-3β,6β-diol

The title compound (C29H50O2, Mr = 430.69) was isolated from the algae Halimeda xishaensis collected from the South China Sea. Its crystal structure was determined by single-crystal X-ray diffraction for the first time. The crystal belongs to orthorhombic, space group P212121 with a = 8.1560(13), b = 10.7861 (18), c = 29.973(5) A, V = 2636.8(8)A3, Z = 4, Dc = 1.085 g/cm3, F(000)= 960, μ(Mo-Ka) = 4.533 mm-1, λ = 0.71073 A, S = 1.061, (△ρ)max= 0.382 and (△ρ)min= -0.244e/A3. The structure was refined to R = 0.0561 and wR = O. 1553 for 2711 observed reflections with I ＞ 2σ(I). X-ray diffraction analysis reveals that the title compound has two β-OH groups, and the side chain is saturated. There exist two intermolecular hydrogen bonds between three molecules.     

含吡嗪甲酸配体的双核铬配合物的水热合成、晶体结构及荧光性质

通过水热法合成了1个双核铬配合物[Cr2(OH)2(2-pca)4].3H2O(2-Hpca=2-吡嗪甲酸),并对其进行了X-射线单晶衍射、红外光谱、元素分析、荧光和热的表征及研究。该配合物属于单斜晶系,P21/c空间群。晶体学数据:a=1.566 35(15),b=0.847 70(6),c=1.974 60(18)nm,β=90.645 0(10)°,C20H20Cr2N8O13,Mr=684.44,V=2.621 7(4)nm3,Dc=1.734 g.cm-3,F(000)=1 392,μ=0.913 cm-1,Z=4,最终R=0.044 7,wR=0.112 0用于3 251个可观测点。在晶体结构中,每个铬原子均为六配位,其中来自两分子2-吡嗪甲酸的2个氮原子、2个羧酸基氧原子和2个桥连羟基上的氧原子,呈现畸变的八面体几何构型。     

Synthesis,Crystal Structure and Herbicidal Activity of O,O＇-Diethyl-N-[2-（5,7-dimethyl-[1,2,4]triazolo[1,5-a]pyrimidin-2-yloxy）-benzoxyl]-1-amino-benzyl phosphonate

The crystal structure of the title compound (C25H28N5O5P,Mr=509.49) has been determined by single-crystal X-ray diffraction.The crystal is of monoclinic,space group P21/c with a=13.0726(4),b=13.4513(4),c=15.103(1),β=93.650(1)°,V=2650.29(14)3,Z=4,Dc= 1.277 g/cm3,F(000)=1072,μ(MoKα)=0.147 mm-1,the final R=0.0748 and wR=0.1956 for 3186 observed reflections (I 2σ(I)).The fused triazolopyrimidine system ring is coplanar,the dihedral angles between the triazolopyrimidine and C(1)-C(3)-C(5) phenyl,the triazolopyrimidine and C(17)-C(19)-C(21) phenyl,and the two phenyl rings are 66.87,58.79 and 80.11o,respectively.Intramolecular N(5)-H(5A)…O(3) and intermolecular C(2)-H(2)…N(4),C(18)-H(18)…O(3),C(19)-H(19)…O(2) and C(24)-H(24C)…N(4) hydrogen bonds together with C-H…π interactions contribute to the stability of the structure and result in a three-dimensional framework.The preliminary bioassay indicates that the title compound exhibits moderate herbicidal activity against dicotyledonous plants (Brassica campestris L) at the concentration of 100 mg/L.     

含有Mo--Mo四重键的双钼络合物Mo_2(C_8H_8)_3的合成和晶体结构

Mo_2(C_8H_8)_3是由Mo(CO)_6和环辛四烯在正癸烷中回流而制得。它的晶体属单斜晶系,空间群为P2_1,单胞参数为:a=7.772(3),b=11.964(5),c=10.445(2),β=100.33(2)°,V=955(1)~3,根据Z=2和fw=504.31计算密度Dc=1.75g/cm~3。在Enraf-Nonius CAD4衍射仪上用MoKα射线收集了I>2σ(I)的独立衍射点2393个。晶体结构用直接法(MULTAN)程序解出,所有非氢原子的位置参数和各向异性热振动参数经全矩阵最小二乘法修正,最后的偏离因子R_1(F)=0.030,R_2(F)=0.035。分子中钼—钼的距离为2.293(1),形成了Mo-Mo四重键。Mo_2(C_8H_8)_3存在两种晶型;一是与W_2(C_8H_8)_3同晶;另一是与Cr_2(C_8H_8)_3同晶。     

Crystal Structure of C_(19)H_(22)N_2O_3 and Synthesis of Two Potential Schiff-base Ligands

１ＩＮＴＲＯＤＵＣＴＩＯＮＳｉｎｃｅＲｏｂｓｏｎｈａｓｐｕｔｆｏｒｗａｒｄｔｈｅｃｏｎｃｅｐｔｉｏｎｏｆｄｉｎｕｃｌｅａｔｉｎｇｌｉｇａｎｄｉｎ１９７０〔１〕，ｄｉｎｕｃｌｅａｒｃｏｍｐｌｅｘｅｓｈａｖｅｒｅｃｅｉｖｅｄｍｕｃｈａｔｅｎｔｉｏｎｆｏｒ...     

Two-dimensional Supramolecular Structure of a Mercury（Ⅱ） Iodide Complex with Organosulfide

A mercury（Ⅱ） iodide complex with organosulfide [Hg（pymt）（pymtH）I] 1 （pymt = the anion of pyrimidine-2-thiolate） has been synthesized by slow evaporation of the solution at room temperature and structurally characterized by single-crystal X-ray diffraction. Basic ideas and data collected are given. X-ray diffraction analysis reveals that complex 1 is mononuclear. Crystallographic data： C8H7HgIN4S2, Mr = 550.79, monoclinic system, space group P21/c, a = 11.218（4）, b = 9.551（3）, c = 15.877（4） A^°, β = 129.697（15）°, V = 1308.9（7） A^°^3, Z = 4, Mr = 550.79, Dc = 2.795 g/cm^3, F（000） = 995, μ（MoKa） = 14.415 mm^-1, 2（MoKa） = 0.71073 A^°, T= 293（2） K, 2θmax = 54.9°, GOOF= 1.053, the final R = 0.0310 and wR = 0.0742 for 2547 observed reflections with I 〉 2σ（I） （refinement on F^2）. Complex 1 is connected through hydrogen bonds to give a one-dimensional supramolecular chain structure. Furthermore, π-π interactions are also found between the pyrimidine rings with the center-to-center distances of 3.439（4） and 3.603（4） A^°, so complex 1 expands the chains into a two-dimensional network.     

Crystal and Molecular Structure of 1-Methyl-4-(2-( 3,4-dimethoxyphenyl) vinyl) pyridinium 4-Tolylsulfonate Dihydrate C_(16)H_(18)NO_2~+·C_7H_7SO_3~-·2H_2O

1 INTRODUCTIONAs a useful nonlinear optical material, the molecule must have a large second-order hyperpolarizability (β), and also must crystallize in a non-centrosymmetric structure to have a large ((2). Organic conjugated molecules with electronic donors and acceptors possibly have quite strong second-order NLO property. However, only a small percentage of the molecules with large β crystal-lize in useful non-centrosymmetric crystals. Marder and his co-worker carried out a simple an…     

Hydrothermal Synthesis and Crystal Structure of a Cadmium（Ⅱ） Polymer with a Two-dimensional Network Structure： [ Cd（pzdc）（2,2＇-bipy） ]n·nH2O

A metal-organic coordination compound formulated as [Cd（pzdc）（2,2＇-bipy）]n·nH2O 1 （Hzpzdc = pyrazine-2,3-dicarboxylic acid, 2,2＇-bipy = 2,2＇-bipyridine） has been hydrothermally synthesized and structurally characterized by elemental analysis, IR, TG fluorescence spectrum and single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group P2 1/c with a = 10.8081（13）, b = 14.4328（17）, c = 10.2530（12） A, β = 98.504（2）°, V= 1581.8（3） ]A3, C16H14CdN4O5, Mr= 454.71, Dc = 1.909 g/cm^3, μ（MoKa） = 1.420 mm^-1, F（000） = 904, Z = 4, the final R = 0.0230 and wR = 0.0554 for 2901 observed reflections （I 〉 2σ（I））. It exhibits an interesting two-dimensional network structure and shows yellow photoluminescent property at room temperature.