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…     

六硫基·二(2-甲基吡啶)合锌的结构表征

标题化合物采用锌粉、硫粉及 2 甲基吡啶直接反应 ,最后得到金黄色晶体 ,其结构由X 射线结晶学分析得到晶体数据。晶体属单斜晶系 ,空间群Cc,Z =4,Mr=,a =7.5 10 (2 ) ,b =17.2 95 (5 ) ,c=13.6 85 (1) ,β =94.6 0 (1)° ,V =1771.7 3,Dc=1.6 6 g/cm3,μ(MoKα) =2 0 .9cm- 1,F(0 0 0 ) =90 4。利用 2 389个独立观察点修正到R =0 .0 5 1,Rw =0 .0 6 1。标题化合物是 1个中性分子 ,分子中有 1个扭曲ZnS2 N2 四面体核心。     

氨基多羧酸锗（Ⅳ）螯合物［Ge（OH）（Hpdta）］和［Ge（OH）（H_2dtpa）］·H_2O的合成与结构

由二氧化锗与丙二胺四乙酸（Ｈ_４ｐｄｔａ）和二乙三胺五乙酸（Ｈ_５ｄｔｐａ）直接制备［Ｇｅ－（ＯＨ）（Ｈｐｔｄａ）］（Ⅰ）和［Ｇｅ（ＯＨ）（Ｈ_２ｄｔｐａ）］·Ｈ_２Ｏ（Ⅱ）。Ｘ－射线单晶结构分析证明，在这两个螯合物中，与Ｇｅ（Ⅳ）螯合的氨基多羧酸均呈五齿，由ＯＨ－占据畸变八面体的第六个配位位置。未参与配位的一个羧基形成分子间氢键，而在（Ⅱ）中还有一个自由羧基形成内盐，并与水分子共同形成分子内氢键。晶体参数：［Ｇｅ（ＯＨ）（Ｈｎｄｔａ）］（Ⅰ），Ｍ_γ＝３９２．８５，正交晶系，空间群Ｐｃａ２_１，ａ＝１５．２４８（２），ｂ＝７．０２９（２），ｃ＝１３．３８４（２），Ｖ＝１４３４．５，Ｚ＝４，Ｄ_ｃ＝１．８１９ｇ／ｃｍ~３，μ（ＭｏＫａ）＝２１．５５ｃｍ~（－１），Ｆ（０００）＝８００．用１１７２个Ｉ＞３σ（Ｉ）的独立衍射精修结构，最终偏差因子Ｒ＝０．０３３；［Ｇｅ（ＵＨ）（Ｈ_２ｄｔｐａ）］·Ｈ_２Ｏ（Ⅱ），Ｍ_γ＝４９７．９４，三斜晶系，空间群Ｐ１，ａ＝７．２３１（２），ｂ＝１０．４０７（１），ｃ＝１３．２８６（２），α＝７４．４２（１），β＝７５．３０（１），γ＝８８．１５（１）°，Ｖ＝９３０．９，Ｚ＝２，Ｄ_ｃ＝１     

Crystal Structure of 2-Amino-5,10-dioxo-4-aryl-5,10-dihydro-4H-naphtho [2,3-b]pyran-3-carboxylic Acid Ethyl Ester

The title compounds have been synthesized via a three-component reaction and their structures were characterized by IR, ^1H NMR, ^13C NMR and X-ray single-crystal diffraction. The crystal of compound 4a belongs to monoclinic, space group P121/c1 with a = 8.575（3）, b = 9.590（3）, c = 21.431（6）A, β = 91.172（3）°, V = 1762.1（9）A^3, Mr = 393.36, Z = 4, Dc= 1.483 g/cm^3, μ（MoKα） = 0.113 mm^-1, F（000） = 816, the final R = 0.0366 and wR = 0.0941. The crystal of compound 4b is of triclinic, space group P-1 with a = 8.6420（17）, b = 9.761（2）, c = 11.132（2） A, α = 97.51（3）, β = 97.86（3）, γ = 92.85（3）°, V = 920.1（3） A^3, Mr = 393.36, Z = 2, Dc = 1.420 g/cm^3, μ（MoKα） = 0.108 mm^-1, F（000） = 408, the final R = 0.0612 and wR = 0.1781. In each molecular structure, the naphthalene rings and pyran rings are almost coplanar with the latter in an envelope conformation. The rings formed by the N-H…O intramolecular hydrogen bonds are almost planar in these compounds. Their crystal packing is stabilized by intermolecular hydrogen bonds together with C-H…π and π-π stacking interactions.     

Crystal Structure and Spectroscopic Properties of[Ni（phen）3]Pic2.2CH3CN

1　ＩＮＴＲＯＤＵＣＴＩＯＮＩｎｔｈｅｐｒｏｃｅｓｓｏｆｔｈｅｐｒｅｐａｒａｔｉｏｎｏｆＮｉ(Ｐｉｃ) 2 Ｌ(Ｌ =1 ,3 ｂｉｓ (2 ｆｏｒｍｙｌｐｈｅｎｏｘｙ) 2 ｈｙｄｒｏｘｙｌ ｐｒｏｐａｎｅｔｈｉｏｓｅｍｉｃａｒｂａｚｏｎｅ )ｍｉｘｅｄｃｏｍｐｌｅｘｗｉｔｈｐｈｅｎ,ａｒｅｄｃｒｙｓｔａｌｗａｓｏｂｔａｉｎｅｄｉｎａｃｅｔｏｎｉｔｒｉｌｅｓｏｌｕｔｉｏｎ .Ｈｏｗｅｖｅｒ,ｔｈｅｅｌｅｍｅｎｔａｌａｎａｌｙｓｉｓｒｅｓｕｌｔｓｏｆｔｈｅｒｅｄｃｒｙｓｔａｌｉｎｄｉｃａｔｅｄｔｈａｔｉｔｉｓｎｏｔｔｈｅ…     

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…     

Crystal Structure of trans－2－（1－Naphthyl）－1－（p－（4＇，4＇，5＇，5＇－tetramethyl－4＇，5＇－dihydro－1＇H－imidazolyl－1＇－oxy－3＇－oxide）－phenyl）－imine，C_（24）H_（24）N_3O_2

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆｔｒａｎｓ－２－（１－Ｎａｐｈｔｈｙｌ）－１－（ｐ－（４＇，４＇，５＇，５＇－ｔｅｔｒａｍｅｔｈｙｌ－４＇，５＇－ｄｉｈｙｄｒｏ－１＇Ｈ－ｉｍｉｄａｚｏｌｙｌ－１＇－ｏｘｙ－３＇－ｏｘｉｄｅ）－ｐｈｅｎｙｌ）－ｉｍ...     

羰基三核钌簇Ru_3（CO）_9（C_6H_5）_2N_2HCS的合成和晶体结构

本文根道了Ｒｕ_３（ＣＯ）_９（Ｃ_６Ｈ_５）_２Ｎ_２ＨＣＳ的合成及晶体结构，晶体属单斜晶系，空间群Ｐ２_１／ｍ，晶胞参数ａ＝９．６０４（２），ｂ＝１４．２７９（５），ｃ＝９．９８６（１），β＝１０３．４５（１）°，Ｖ＝１３３１．９，Ｍ_ｒ＝７８２．６１，Ｚ＝２，Ｄ_ｘ＝１．９５１ｇ／ｃｍ~３，μ（ＭｏＫα）＝１７．７３ｃｍ~（－１），Ｆ（０００）＝７５４，Ｒ＝０．０３８．（Ｃ_６Ｈ_５）_２Ｎ_２ＨＣＳ通过Ｎ和Ｓ原子与３个钌原子成螯合配位，另外还有九个羰基与之配位。整个分子具有Ｃ_Ｓ对称性。     

Synthesis and Crystal Structure of Chiral 4-Hydroxy-4-butyrolactam Fused Aziridine

A novel compound of chiral 4-hydroxy-4-butyrolactam fused aziridine was synthesized via tandem nucleophilic displacement reaction under mild condition. Its structure was determined by IR, 1H NMR, elemental analysis and X-ray diffraction. The crystal of the new compound is of orthorhombic, space group P212121 with a = 6.4246（6）, b = 13.5081（13）, c = 18.6399（18） A, Mr = 278.39, Z = 4, V = 1617.6（3）A^3, Dc = 1.143 g/cm^3, p（MoKa） = 0.075 mm^-1, F（000） = 608, the final R = 0.0297 and wR = 0.0679.     

Hydrothermal Synthesis and Structure of a New Molybdenum Phosphate: (NH_3CH_2CH_2NH_3)_(2.5)[Mo_5O_(15)(PO_4) (HPO_4)]·7.5H_2O

1 INTRODUCTION A new class of materials of metal oxide clusters based on anionic molybdenum phosphate frameworks has received much attention as a consequence of their potential applications in catalysis and materials science [1]. As a result, some molybdenum phosphates have been studied [2,3]. Recently we have studied the structure of NaPMO material[4] and the spectrum of multicomponent compound with Keggin struc- ture [5]. Here we report the synthesis and crystal structure of a new…     

Isolation and Crystal Structure of Horminone

1　INTRODUCTIONhorminoneRabdsia serra( Maxim) hara,a tradi-tional Chinese medicine for the treatmentofhepatitis,enteritis,acute cholecystitis anddysentery,is a perennial herb distributedmainly in central and southeastern parts ofChina〔1〕.In previous reports,four diter-penoids,Rabdoserrin A,Rabdoserrin B,Excisanin A and Kamebakaurin which be-long to ent- kaurene diterpenoids have beenisolated from this source〔2 ,3〕.Horminonewhich has the structure of abietane quinonewas once isolate…     

Structure of a Polymeric Mn(Ⅱ) Complex Bridged by Benzenetetracarboxylate

The single crystals of the title compound were obtained from a reaction of MnCO3,benzenetetracarboxylic acid (H4BTC)and imidazole in an aqueous solution.The crystal of Mn(II)complex (C28H34Mn2N12O12(4H2O,Mr=912.62) belongs to tricli nic,space group Pī with a=10.036(1),b=10.650(1),c=11.102(1)A,α=114.72(2),β=95.75(1),γ=108.46(2)°,V=984.2(2)A3,Z=1,Dc=1.540 g/cm3,F(000)=472,μ(MoKα)=0.726 mm-1,R=0.0409 and wR=0.1166 for 3909 observed reflections (I>2σ(I)).The crystal consists of the polymeric Mn(II)complex anions and discrete Mn(II) complex cations,both with normal octahedral coordination geometry.Each BTC bridges two Mn(II) atoms to form the anionic polymeric chain,and the cations distribute be-tween the chains and link them through both classic and weak C-H…O H-bonding.     

Synthesis and Crystal Structur of (4,4''-H2bipy)[CdBr4]·H2O

The title compound (4,4'-H2bipy)[CdBr4]·H2O 1 has been synthesized via hydrothermal reaction and characterized by X-ray diffraction. The crystal belongs to monoelinic,space group P21/c with a=8.260(3), b=23.926(7), c=9.774(2) (A), β=106.777(9)°,C10H12Br4CdN2O, Mr=608.26, V=1849.4(9)(A)3, Z=4, Dc=2.185 g/cm3, S=1.005, μ(MoKα)=9.814 mm-1, F(000)=1128, R=0.0646 and wR=0.0989. The crystal structure analysis of 1reveals that the title compound features an isolated structure, based on discrete 4,4'-H2bipy moieties and lattice water molecules which are linked by hydrogen bonds together with tetrahedral cadmium atoms terminally coordinated by four bromine atoms.     

Synthesis and Crystal Structure of O,O'-Diisopropyl-5-(4-chlorophenyl)-1-hydroxy-2E,4E-pentadienylphosphonate

1　INTRODUCTIONAbscisicacid(ABA)isoneofplanthormoneswhichwasisolatedfromyoungcottonfruitsin1963[1].Itnotonlyinhibitsplantgrowth,butalsoprotectsplantsa-gainstdeprivationofwaterduringdroughtdays[2].Hydroxyalkylphosphonicacidsandtheirderivativesappeartobeveryimportantfortheirwidebiologicalactivitiesintheinhibitionofenzymes,fungicidesandplantgrowthregulation[3].Wedesignedandsynthesizedthetitlecompound4,theunsaturatedphosphonateanaloguesofABA,whichexhibitsplantinhibitoryactivityontheelongati…     

Synthesis and Crystal Structure of Chiral Spiro{1-bromo-4-hydroxy-5-N-cyclohexyl-butyrolactam-6-oxo-dirings[3.1.0]hexane-2,3′-(4′-diphenylcarbinol-5′-menthyloxy-butyrolatone)}

A novel compound of chiral spiro{1-bromo-4-hydroxy-5-N-cyclohexyl-butyro-lactam-6-oxo-dirings3.1.0hexane-2,3′-(4′-diphenylcarbinol-5′-menthyloxy-butyrolatone)} was synthesized via tandem nucleophilic substitution reaction under mild conditions=and its structure was determined by IR =1H NMR=elemental analysis and X-ray diffraction.The crystal structure of this compound is of monoclinic system=space group P21 with a=9.7356(9)=b=12.2760(12)=c=14.9577(14)=β=101.0300(10)°=Mr=680.66=Z=2=V=1754.6(3)3=Dc=1.288 g/cm3=μ(MoKα)=1.216 mm-1=F(000)=716=the final R=0.0434 and wR=0.0996.     

Hydrothermal Synthesis, Crystal Structure and Fluorescence Properties of a Three-dimensional Triply-bridged Binuclear Zinc（Ⅱ） Complex [Zn2（Mba）3（Phen）2EtOH）]·ClO4

The novel complex [Zn2(Mba)3(Phen)2EtOH)]·ClO4 (Hmba=methoxybenzoic acid, Phen=1,10-phenanthroline, EtOH=ethanol) was synthesized by hydrothermal reactions, and its structure was determined by X-ray diffraction. The crystal belongs to the triclinic system, space group P with a=1.15362(1), b=1.3655(3), c=1.61451(1) nm, α=72.842(2), β=83.259(3), γ=72.083(2)°, V=2.3112(6) nm3, Z=2, μ(MoKα)=11.71 cm-1, F(000)=1120, R=0.0552 and wR=0.1157 (I > 2·(I)). The two centric zinc(Ⅱ) ions in the complex locate in a distorted octahedral coordination geometry and a distorted trigonal bipyramid coordination geometry, respectively. Two bridging bidentate carboxyl groups and a μ2-O carboxyl group from three methoxybenzoic acids act as the bridge to link two Zn(Ⅱ) ions. The asymmetric units are connected by π-π packing interactions between aromatic rings to form a three-dimensional supramolecular network. The experimental results show a good fluorescence property for the complex.     

Syntheses and Characterizations of （CH3CH2CH2CH2NH3）6（BiI6）（I）2I3 and （NH3CH2CH2NH3）2Bi2I10

The title compounds have been respectively synthesized by solution process and solvothermal reaction, and their crystal structures were determined by X-ray diffraction method. For （CH3CH2CH2CH2NH3）6（BiI6）（I）2I3 1, it crystallizes in tficlinic, space group P1^- with Mr = 2049.76, a = 8.5719（1）, b = 11.7461（3）, c = 15.700（1）A, V = 1451.4（1）A^3, Z = 1, Dc = 2.345 g/cm^3, F（000） = 924, μ（MoKα） = 8.907 mm^-1, T = 293（2） K, the final R = 0.0655 and wR = 0.0804 for 2399 observed reflections with I 〉 2σ（I）. For （NH3CH2CH2NH3）2Bi2I10 2, it crystallizes in monoclinic, space group P21/n with Mr= 1811.20, a = 8.434（4）, b = 13.862（6）, c = 13.362（6）A, V = 1499.9（12）A^3, Z = 2, Dc = 4.010 g/cm^3, F（000） = 1536,μ（MoKα） = 22.007 mm^-1, T = 293（2） K, the final R = 0.0584 and wR = 0.1451 for 1798 observed reflections with I 〉 2σ（I）. The structures of 1 and 2 contain halobismuthate monomer and dimers, respectively. It is noteworthy that the dimers and their organic counters in 2 connect each other by N…I hydrogen bonds to form a layered structure, and the electrostatic interactions and crystal packing forces between layers give rise to the packing of the crystal. The optical absorption spectra of 1 and 2 reveal the appearance of sharp optical gaps of 2.13 and 2.01 eV, respectively.     

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°。     

Hydrothermal Synthesis and Structure of a Novel Molybdenum Phosphate: Na4(H3O) [Na(HPO4)2(PO4)4Mo18O49]·16H2O①

The title compound Na5H37P6Mo18O90 1 (Mr=1658) was synthesized under hydrothermal condition and its crystal structure was determined by X-ray diffraction. It crystallized in the monoclinic system, space group P21 with a =14.957(1), b =16.535(1), c = 16.159(1)?,β=108.586(2)°, V=3787.85?3, Dc =3.040g/cm3, Z=2,μ(MoKα)=3.17mm－1, F(000)=3242. The final R and wR are 0.0500 and 0.1535 for 6643 observable reflections with I≥2σ(I), respectively. The result of structure analysis indicates that [Na(HPO4)2(PO4)4－Mo18 O49]5－anions 2 in 1 has the symmetry of C2V, in which each MoVIO6 octahedron is connected to adjacent PO4 tetrahedra through corner-sharing and to adjacent octahedra through edge-sharing or corner-sharing.     

一种具有超结构的[Zn(C_2H_8N_2)_3]Cl_2·2H_2O晶体

试图在Eu2O3、Zn粉、HCl、H_2S、Me4NCl、H_2O、CH_3COOH等起始物参加的反应系统中,合成某种二价铕配合物时得到一棱柱状透明[Zn(C2H8N2)3]Cl2 · 2H_2O晶体, 其主要晶体学参数如下：Mr = 350.60,单斜, C2/c, a = 26.3749(7), b =13.9613(5), c =12.9565(4) ?, β = 93.285(1) o, V = 4763.1 ?3, Z = 12, Dx = 1.467g·cm－3, μ(MoKα) = 1.885 mm－1, F(000) = 2208, R = 0.0552。单晶结构分析结果表明本文标题配合物具有一种超结构形式。