The Crystal Structure of Biphenyltetracarboxylic Dianhydride Isomers

１　ＩＮＴＲＯＤＵＣＴＩＯＮＡｒｏｍａｔｉｃｐｏｌｙｉｍｉｄｅｓａｒｅａｃｌａｓｓｏｆｐｏｌｙｍｅｒｓｋｎｏｗｎｆｏｒｔｈｅｉｒｈｉｇｈｔｅｍｐｅｒａｔｕｒｅｓｔａｂｉｌｉｔｙ,ｅｘｃｅｌｌｅｎｔｅｌｅｃｔｒｉｃａｌａｎｄｍｅｃｈａｎｉｃａｌｐｒｏｐｅｒｔｉｅｓ．Ｔｈｅｓｅｐｒｏｐｅｒｔｉｅｓｍａｋｅｔｈｅｍｈｉｇｈｌｙｄｅｓｉｒａｂｌｅｆｏｒｈｉｇｈｐｅｒｆｏｒｍａｎｃｅａｐｐｌｉｃａｔｉｏｎｓ〔１〕．Ｈｏｗｅｖｅｒ,ｔｒａｄｉｔｉｏｎａｌｐｏｌｙｉｍｉｄｅｓｓｕｃｈａｓＵＰＩＬＥＸＲａｎｄ…     

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.     

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 AND MOLECULAR STRUCTURE OF(μ-PhCH_2S)(μ-CH_3C(0)CH_2S)Fe_2(CO)_6

<正> The crystal and molecular structures of (μ-PhCH2S)(μ-CH3C(O)CH2S)-Fe2(CO)6 have been determined by X-ray diffraction technique. The complex has chemical formula of C16H12O7S2Fe2 and Mr=492.08. The crystals are tri-clinic, space group P1,with a=8.461(5), b=10.937(5), c=ll.419(4)A,α=81.61 (3), β=78.21(4),γ=71.04(4)°,V=974.5A3, Dc=1.68 gcm-3,μ(MoKα)=17.3cm-1, Z=2,F(000)=495.93. The final R was 0.038 for 2874 independent reflections.     

Crystal Structure of Calcium Complex with Cyanuric Acid Ligand［Ca（C_3H_3N_3O_3－O）（H_2O）_6］［（OH）（C_3H_2N_3O_3）］

ＣｒｙｓｔａｌＳｔｒｕｃｔｕｒｅｏｆＣａｌｃｉｕｍＣｏｍｐｌｅｘｗｉｔｈＣｙａｎｕｒｉｃＡｃｉｄＬｉｇａｎｄ［Ｃａ（Ｃ_３Ｈ_３Ｎ_３Ｏ_３－Ｏ）（Ｈ_２Ｏ）_６］［（ＯＨ）（Ｃ_３Ｈ_２Ｎ_３Ｏ_３）］ＬｉｎＺｈｏｕ－Ｂｉｎ；ＣｈｅｎＣｈａｎｇ－Ｚｈａｎｇ；...     

5-L-孟氧基4-苄氨基丁烯内酯的不对称合成和晶体结构研究

温和条件下,苄胺与手性合成子5-(L)-孟氧基3-溴-2(5)呋喃酮通过串联的不对称迈克尔加成/分子内消除反应合成了一种新手性化合物:5-L-孟氧基-4-苄胺基丁烯内酯。产物经过IR、1H-NMR、MS谱学表征,并经X-ray单晶衍射测定了其结构。新化合物属于正交晶系,P212121空间群,a=5.2945(4),b=14.2829(10),c=26.0769(18),Mr=343.45,Z=4,V=1972.0(2)3,Dc=1.157g/cm3,μ(MoKα)=0.076mm-1,F(000)=744,R=0.0387,wR=0.0880。     

Syntheses, Structures, and Some Properties of Three Vanadium Selenites

Three novel vanadium selenites with the formulae [（VO2）（1,10-phenanthtoline）（SeO3H）]2 1, [（VO2）（2,2′-bipyridine）]2（SeO3） 2 and [（VO）（H2O）（SeO3）2]2（HaEDD） 3 （EDD = N1,N1′-（ethane-1,2-diyl）diethane-1,2-diamine） were hydrothermally synthesized, and characterized with elemental analysis, FT-IR spectrum, Raman spectrum, TG-DTA analysis, EPR spectra, and single-crystal X-ray diffraction analysis. Compound I belongs to the triclinic system, space group P1^- with a = 7.7527（5）, b = 9.5345（10）, c = 9.8192（8） A^°, α = 92.712（3）, β = 105.540（3）, γ = 108.154（4）°, V = 657.66（1） A^°^3, Mr = 782.22, Z = 1, F（000） = 384,μ（MoKa） = 3.544 mm^-1, R = 0.0432 and wR = 0.1142; Compound 2 is of orthorhombic system, space group F212121 with a = 7.6574（15）, b = 14.916（3）, c = 19.085（4） A, V = 2179.8（8） Aa, Mr = 605.21, Z = 4, F（000） = 1200, μ（MoKa） = 2.579 mm^-1, R = 0.0338 and wR = 0.0658; Compound 3 belongs to the triclinic system, space group P1^- with a = 9.247（2）, b = 9.659（2）, c = 7.2651（19） A^°, α = 98.171（7）, β = 103.709（5）, γ = 114.712（13）°, V = 550.9（2） A^°^3, Mr = 828.03, Z = 1, F（000） = 400, μ（MoKa） = 7.537 mm^-1, R = 0.0641 and wR = 0.2118. Compound 1 is constructed from alternating corner-shared [VO4N2] octahedra and SeO3H units, forming a dimeric vanadium unit. These assemblies are further linked into an infinite chain via hydrogen bonds along the a axis. In the structure of 2, two distinct V centers form centrosymmetric [V2O6N4] clusters through edge-sharing, and the SeO3 unit serves as a capping unit to fix the oxovanadate cluster. In the structure of 3, each [VO6] octahedron shares four oxygen atoms with adjacent Se atoms, while every SeO3 unit shares two oxygen atoms with neighboring V atoms. This connectivity of alternating VO6 and SeO3 units results in a joint-like chain. Based on the TGA analysis, these three compounds are thermally stable under 200℃ .     

Synthesis and Crystal Structure of [VO2（C17H11N3O2） ] [VO （C4H13N3）（C6H5N3O） ]（C2H5OH）

The reaction of VO（acac）2 with 2-hydroxyl-1-naphthaldehyde isonicotinyl hydrazone and amines （ethylenediamine or diethylenetriamine） in CH3OH yields crystals of novel vanadium compounds characterized by IR, NMR spectroscopic methods and X-ray single-crystal structure determination. Two different vanadium units exist in the crystal cell of [VO2（C17H11N3O2）][VO- （C4H13N3）（C6H5N3O）]（C2H5OH） which crystallizes in the triclinic system, space group P1 with a = 8.0104（17）, b = 13.898（3）, c = 14.955（3）A, α = 89.103（4）, β = 79.551（4）, γ = 78.352（4）°, V = 1603.3（6）A^3, Mr = 723.54, Dc = 1.499 g/cm^3, Z = 2, λ（MoKα） = 0.71073 ]A,μ= 0.644 mm^-1, F（000） = 748, the final R = 0.0547 and wR = 0.0997 for 8920 observed reflections with I 〉 2σ（I）. According to structure analysis, two different molecules are arranged in the lattice and the two vanadium atoms adopt octahedral and square pyramidal coordination geometries, respectively. The interactions between DNA and vanadium complexes have been investigated by UV-Vis absorption spectro- photometry.     

Synthesis and Crystal Structure of CoCl（ieaa）（C10H7—ieai）（C10H7NH2）

1 INTRODUCTION A number of isonitroso-b-diketones and isonitroso-b-ketoesters such as isonitrosoacetyl- acetone(Hiaa), isonitrosobenzoylacetone(Hiba) and isonitrosoethylacetoacetate (Hieaa) have been employed as reagents in spectrophotometric determination of iron, palladium and ruthenium[1]. Transition metal complexes of such ligands[2] are potential models for metal binding sites in ferroverdin[3]. They were found as dyes and light-absorbing agents for the acceleration of the sol…     

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.     

Synthesis, Characterization and Crystal Structure of [Co2Mo2(μ4-C2HPh)(μ-CO)4(CO)4(η5-C5H4C(O)Me)2]

The reaction of μ-alkyne-bridged dimolybdenum compound [Mo2(μ-C2HPh)(CO)4(η5-C5H4C(O)Me)2] 1 with Co2(CO)8 in refluxing toluene gave a new butterfly compound [Co2Mo2(μ4-C2HPh)(μ-CO)4(CO)4(η5-C5H4C(O)Me)2] 2 which was fully characterized by elemental analysis, IR, 1H NMR and X-ray single crystal diffraction techniques. 2 crystallized in monoclinic system, C30H20Co2Mo2O10, Mr=850.23, space group P21/a(#14), a=14.165(5), b=12.498(2), c=16.204(2)(A), β = 96.50(2)°, V = 2850(1)(A)3, Z = 4, Dc = 1.981 g cm-3, F(000)=1672, μ(MoKα)=20.41 cm-1, final R=0.030, Rw=0.039 for 4831 observable reflections with I>2σ(I). The structure contains a Co2Mo2 butterfly core, and each Mo-Co bond is spanned by an asymmetric semi-bridging carbonyl ligand.     

Synthesis and Uncommon Structural Characterization of Novel Zinc and Cadmium Complexes with Imino Nitroxide Radical

Two novel complexes {[Zn(IM4py)2(tp)(H2O)]·2H2O}n 1 and {[Cd(IM4py)2(tp)- (H2O)]·1.25H2O}n 2 (IM4py = 2-(4'-pyridinyl)-4,4,5,5-tetramethylimidazoline-1-oxyl and tp = terephthalate dianion) have been synthesized and characterized by elemental analyses, IR spectrum and single-crystal X-ray diffraction. Crystal data for complex 1: monoclinic, space group C2/c, a = 20.648(7), b = 12.130(4), c = 14.036(4) , β = 106.351(5)o, C32H42N6O9Zn, Mr = 720.09, V = 3373.3(2) 3, Z = 4, Dc = 1.418 g/cm3, μ(MoKα) = 0.790 mm-1, F(000) = 1512, the final R = 0.0407 and wR = 0.0894 for 3480 independent reflections with Rint = 0.0432. Crystal data for complex 2: monoclinic, space group C2/c, a = 21.332(6), b = 12.063(3), c = 14.246(4) , β = 106.704(4)o, C32H40.50N6O8.25Cd, Mr = 753.60, V = 3511.2(2) 3, Z = 4, Dc = 1.426 g/cm3, μ(MoKα) = 0.679 mm-1, F(000) = 1554, the final R = 0.0419 and wR = 0.0961 for 3627 independent reflections with Rint = 0.0440. The framework structures of complexes 1 and 2 are 3-D networks via the hydrogen bonds among 1-D chains. The notable characteristics of the two complexes are that the coordination polyhedron of Zn(II) adopts a rare distorted five-coordinate square pyramidal geometry in 1, and the Cd(II) complex exhibits an unusual distorted seven-coordinate pentagonal bipyramid in 2.     

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.     

Synthesis,Crystal Structure and Photoluminescence of [Gd(C_6NO_2H_5)_3-(H_2O)_2]_(2n)·(nH_5O_2)(nHgCl_5)(2nHgCl_4)·(2nH_2O)

A heterometallic 4f-5d inorganic-organic metal-isonicotinato hybrid Gd(C6NO2H5)3-(H2O)22n·(nH5O2)(nHgCl5)(2nHgCl4)·(2nH2O) 1 has been synthesized via hydrothermal reaction and structurally characterized.Complex 1 crystallizes in the space group C2/c of monoclinic system with four formula units in a cell:a=24.234(8)=b=20.816(7)=c=15.333(3)=β=128.091(8)°=V=6088(3)3=C36H47Cl13Gd2Hg3N6O20=Mr=2260.92=Dc=2.467 g/cm3=S=0.896=μ(MoKα)=10.331 mm-1=F(000)=4216=R=0.0344 and wR=0.0629.The crystal structure analysis reveals that the title complex is characteristic of a one-dimensional chain-like structure.Photoluminescent investigation reveals that the title complex displays a broad and intense emission in the green region.     

Synthesis, Structure and Spectral Characterization of a Discrete Binuclear Copper (II) Complex

1　ＩＮＴＲＯＤＵＣＴＩＯＮＲｅｃｅｎｔｌｙ,ｂｒｉｄｇｅｄｂｉｎｕｃｌｅａｒｃｏｍｐｌｅｘｅｓｏｆｆｉｒｓｔｒｏｗｔｒａｎｓｉｔｉｏｎｍｅｔａｌｓｈａｖｅｒｅｃｅｉｖｅｄｍｕｃｈａｔｔｅｎｔｉｏｎｏｎａｃｃｏｕｎｔｏｆｔｈｅｉｒｂｉｏｌｏｇｉｃａｌｒｅｌｅｖａｎｃｅａｎｄｃｏｎｄｅｎｓｅｄｐｈａｓｅｍａｇｎｅｔｉｃｐｒｏｐｅｒｔｉｅｓ[1,2].Ｉｎｔｈｅｓｅｒｅｓｅａｒｃｈｅｓ,ｍａｎｙｂｒｉｄｇｅｄｌｉｇａｎｄｓｗｈｉｃｈｐｌａｙｉｍｐｏｒｔａｎｔｒｏｌｅｓｈａｖｅｂｅｅｎｕｓｅｄａｓｕｓｅｆｕｌ…     

Crystal Structure and Magnetic Properties of the Oxamidato-bridged Cu3 Complex Containing Macrocyclic Ligands

One novel oxamido-bridged trinuclear complex [Cu(CuL)2(ClO4)2] has been syn-thesized and structurally determined.It crystallizes in the monoclinic system,space group P21/n with a = 10.636(4),b = 11.645(4),c = 16.038(6) ,β = 91.029(5)°,V = 1986.2(12) 3,C38H32Cl2Cu3N8O12,Mr = 1054.24,Dc = 1.763 Mg/m3,μ(MoKα) = 1.802 mm-1,F(000) = 1066,Z = 2,the final R = 0.0328 and wR = 0.0882 for 3152 observed reflections.The crystal structure is a trinuclear complex in which the CuII ions are bridged by macrocyclic oxamide groups.C-H···O hydrogen bonding interactions link the trinuclear fragment to form a 2D supramolecular architecture.Magnetic measurements indicate that the compound is moderately antiferromagnetically coupled.     

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.     

Synthesis and Crystal Structure of N-[(3aR,4R,4aR,5aS,6S,6aS)-1,3-Dioxooctahydro-4,6-ethenocyclopropa[f]isoindol-2(1H)yl]-4-(trifiuoromethyl)phenylmethanimine Monohydrate

The crystal structure of the title compound (C19H17F3N2O4,Mr=394.35) was determined by single-crystal X-ray diffraction.The crystal belongs to monoclinic,space group C2/c with a=28.383(6),b=10.355(2),c=12.799(3)(A),β=111.74(3)°,V=3493.8(12)(A)3,Z=8,De=1.499 g/cm3,λ(MoKα)=0.71073,F(000)=1632,μ= 0.127 mm-1,R=0.0412 and wR=0.1019.In the title compound,there exist three intennolecular hydrogen interactions (O(4)...O(1),O(4)...O(3) and O(4)...N(1)) between water.The neighboring molecules are linked to each other generating a two-dimensional network structure via the three intermolecular hydrogen bonds and π-π interactions shaped by phen-phen with centroid distance of 4.049 (A).     

Synthesis and Crystal Structure of 3,3-Dimethyl-7,11-di（thiophene- 2-yl）-2,4-dioxyspiro[5. 5]undecane- 1,5,9-trione

The title compound （C19H18O5S2） has been synthesized by the reaction of thio- phene-2-carboxaldehyde, isopropylidene malonate and 4-chloroaniline using [bmim]Br as solvent, and characterized by IR, ^1H NMR and X-ray single-crystal diffraction. The crystal belongs to monoclinic, space group P21/n with a = 9.4872（15）, b = 9.5148（13）, c = 20.634（3）A, β= 92.209（2）°, V= 1861.2（4）A^3, Mr= 390.45, Z = 4, Dc = 1.393 g/cm^3,μ（MoKα） = 0.313 mm^-1, F（000） = 816, the final R = 0.0685 and wR = 0.1685. X-ray analysis reveals that two six-membered rings adopt chair and planar conformations, respectively.     

Synthesis and Crystal Structure of a New Cadmium（Ⅱ） Complex with 3,4-Pyridinedicarboxylic Acid and 1,4-Bis（imidazol-1-ylmethyl）-butane Ligands

A metal-organic coordination polymer [Cd(PDB)(bimb)]n (H2PDB=3,4-pyridine- dicarboxylic acid, bimb=1,4-bis(imidazol-1-ylmethyl)-butane) 1 has been hydrothermally synthesi- zed and characterized by elemental analysis, IR, TG, fluorescence spectrum and single-crystal X-ray diffraction. Yellow crystals crystallize in the monoclinic system, space group Cc with a=19.001(5), b=7.948(2), c=13.392(4) , β=120.803(3)o, V=1737.0(8)3, C17H17CdN5O4, Mr=467.76, Dc=1.789 g/cm3, F(000)=936, Z=4, μ(MoKα)=1.293 mm-1, the final R=0.0266 and wR=0.0534 for 2707 observed reflections (I > 2?(I)). The structure of 1 exhibits a three-dimensional network structure.