Hydrothermal Synthesis and Crystal Structure of Inorganic-organic Hybrid Compound [H3NC2H4NH2]VOPO4

An inorganic-organic hybrid compound, [H_3NC_2H_4NH_2]VOPO_4 was synthesized by means of the hydrothermal method. It was crystallized in a monoclinic system, a space group P2_1/c, with the crystal cell parameters: a=0.92285(11) nm, b=0.72994(9) nm, c=0.98495(11) nm, β=101.280(3)°, V=0.65067(13) nm~3, M_r=223.02 g/mol, D_c=2.277 g/cm~3, Z=4, R=0.0315, ωR=0.0865, GOF=1.085. The VO_5N octahedra chains are corner-linked by PO_4 tetrahedra; the VO_5N octahedra are all trans-linked with V—O bonds being alternately short and long. The monoprotonated ethylenediamine was intercalated between the layers with one end coordinating to V and the other end as an H-bond donor interacting with a terminal O atom of PO_4 from a neighboring sheet. The elementary analysis, infrared spectrum characters and thermal stability were also given.     

Synthesis and Crystal Structure of trans(N)-(1,10-Phenanthroline)-bis (DL-Al aninato)-Cobalt( Ⅲ ) Chloridetrihydrate

The title compound was synthesized by the reaction of cis-[Co(phen)2Cl2]Cl·3H2O with DL-alanine at pH = 8, and isolated using a column chromatographic method. Its crystal structure was determined. The crystal structure belongs to mono-clinic system, space group P21/c, with a = 0. 9549(6) nm, b=2.3746(8) nm, c= 1.0782(4) nm, β=114.13(3)°? Z = 4, Dc= 1. 50 g/cm3. The final refinement converged to R = 0. 047 for 3246 independent observed reflections. In the octahedral coordination sphere formed by the cobalt atom and the coordinate atoms, N, O of DL-alan-inato ligands are in the configuration of trans-N ,N form.     

STUDY ON TRINUCLEAR MOLYBDENUM CLUSTER COMPOUNDS——THE CRYSTAL AND MOLECULAR STRUCTURE OF THE TWO TRINUCLEAR MOLYBDENUM CLUSTERS(C_5H_7S_2)[Mo_3(μ_3-O )(μ-X)_3(μ-OAc)_3Cl_3](X=Cl,Br)

The crystal structure of two isomorphic cluster compounds with formula (C_5H_7S_2)-[Mo_3(μ_3-O)(μ-X)_3(μ-OAc)_3Cl_3] (X=Cl for compound (Ⅰ) and compound (Ⅱ)) has been investigated by X-ray diffraction method. The parameters of two crystals are: a=10.423(1),b=17.095(4), c=14.062(7), β=97.54(4)(°); Dc=2.20gcm~(-3), D_o=2.17g cm~(-3) for compound (Ⅰ). and a=10.511(3), b=11.213(2), c=14.053(3), β=96.12(2)(°); D_c=2.52g cm~(-3), D_o=2.53gcm~(-3) for compound (Ⅱ). The space groups are P2_1/C. Z=4. The 2621 and 2548 independent reflections with I>3σ(I) were collected on a CAD-4 four-circle diffractometer by means of MoKα radiation. The crystal structures were solved by heavy atom method and refined by full-matrix least-squares technique to a final discrepancy factors of R=0.061 and 0.051 respectively. The results of investigation show that the molecule consists of the cation (C_5H_7S_2)+ and the trinuclear Mo cluster anion, the configuration of which is similar to that of (Et_4N)_2[Mo_3(μ_3-O)(μ     

Studies on the Synthesis and Structure of Cycl opentadienylruthenium Derivatives——Crystal and Molecular Structure of (η~5-C_5Me_4Et)_2Ru

The title compound was synthesized by refluxing RuCl3 with cyclopentadiene in methanol. It crystallizes in space group C5-Pn with cell dimensions: a=0. 9735(4) nm, b=0. 8604(3) nm, c=1. 2261(6) nm, β=94. 83(3), and Z = 2. Structure was solved by Patterson method and Fourier functions, and was refined to final R value of 0. 0365 based on 1872 observable reflections. In contrast to the staggered conformation of decamethylferrocene, this molecule adopts the eclipsed comformation. The conformation difference was explained by the polarizability and metal atom size.     

Nitration of 2,2＇-Dinitro-4,4＇-biphenyldicarboxylic Acid at High Concentration of Sulfuric and Nitric Acids

Nitration of 4,4'-biphenyldicarboxylic acid(BPDC) was studied and an aromatic carboxylic acid containing four nitro groups was synthesized and characterized through elemental analysis and IR spectra.Crystal structure of TNBPDC(TNBPDC = 2,2',6,6'-tetranitro-4,4'-biphenyl dicarboxylic acid) was determined by X-ray single-crystal diffraction.The title compound(C20H20N6O14,Mr = 600.42) crystallizes in tetragonal,space group I41/a with a = 9.8774(1),b = 9.8774(1),c = 25.335(7) ,V = 2471.7(8) 3,Z = 4,Dc = 1.613 g/cm3,F(000) = 1240,μ(MoKα) = 0.142 mm-1,T = 294(2) K,the final R = 0.0797 and wR = 0.2177 for 554 observed reflections with I > 2σ(I).In this crystal,there exist a number of H-bonds which link the molecules to form a three-dimensional infinite network structure.The thermal decomposition of the title compound has been carried out through DSC and TG-DTG analyses at a heating rate of 10 ℃/min.The results indicate that the compound has high heat-resistant stability.     

THE STUDY OF SPECTRA AND X-RAY CRYSTAL STRUCTURE OF A NOVEL BIONICS INSECTICIDE——(CH_3)_2NHCH(CH_2S_2O_3)_2Na·H_2O

IR and NMR spectra of novel bionics insecticide—C_5NS_4O_6H_(12)Na·H_2O have been studied. The molecular and crystal structures of the compound also have been determined. The compound crystallizes in the monoclinic space group C_(2h)~5, - P2_1/n with α= 8.0972. (9) , b =16.262(4), c = 10.370(3), β= 94.26(2)° and z = 4.The result shows that N atom in this compound captures a proton to form HN~ group, Na~ is in statistical disorder. Therefore, the structural formula of tho compound is (CH_3)_2HN~ —CH(CH_2S_2O_3~-)_2·1/2 (Na~ )_2·H_2O.     

Synthesis,Structure and Photochromism of a New Diarylethene and Its Ag(Ⅰ) Complex

A new symmetric diarylethene containing cyano group was synthesized and structurally characterized by elemental analysis,IR,1 H NMR and X-ray single-crystal diffraction.It belongs to the monoclinic system,space group C2/c with a = 18.848(6),b = 8.561(2),c = 16.875(5) ?,β = 100.398(6)o,V = 1344.6(11) ?~3,Z = 4,μ = 0.262 mm~(-1),Dc = 1.415 g/cm~3,M_r = 570.56,F(000) = 1160,the final R = 0.0808 and wR = 0.2107 with I 2σ(I).The two thienyls adopt reactive anti-parallel conformation and the carbon distance of photocyclization is 3.57 ?.The neighboring molecules are stacked closely with C–H…F hydrogen bonding.In addition,the photochromism of the new compound was investigated in solvents with different polarity and PMMA film.The alternative photo-irradiation of 254 nm light and ≥550 visible light can induce the reversible photo-cyclization and photo-reversion with the color interconversion between colorlessness and blue.In THF solution,the λ_(max) of diarylethene in PSS in visible band is 585 nm.The diarylethene further reacted with AgBF_4 in benzene to give rise to complex 1,which was structurally characterized by elemental analysis,IR,ESI-MS and TG.1 demonstrated reversible photochromism in both solution and PMMA film.The complexation of metal ions with diarylethene leads to a minor red-shift of the λ_(max) of 1 in THF in PSS to 590 nm.     

Syntheses, Structural Characterization of Fe and Ni Complexes with Polypyrazolyl Borate Ligand ： Fe [ HB （pz） 3 ] 2 and Ni [ HB （pz） 3 ] 2

Fe(Ⅱ) complex Fe[HB(pz)3]2(compound 1, pz=pyrazole) and Ni(Ⅱ) complex Ni[HB(pz)3]2(compound 2) have been obtained by the reaction of MCI2(M=Fe and Ni) with NaHB(pz)3 in MeOH. The two complexes(compounds 1 and 2) were characterized by IR, NMR, elemental analysis and X-ray diffraction. Compound 1 crystallizes in space group P21/c with a=1.224(3) nm, b=1.161(2) nm, c=1.648(3) nm, β=107.62(15)°, V=2.233(8) nm3, Z=2. Compound 2 crystallizes in space group P21/c with a=0.97926(18) nm, b=1.7423(3) nm, c=1.3156(2) nm, β=97.055(16)°, V=2.2277(7) nm3, Z=4. The results of X-ray structural analyses show that both compounds 1 and 2 are monomeric neutral, possessing a similar coordination mode and a similar structure around the metal centers. The related spectral characterizations, steric effects and binding properties are discussed.     

离子对化合物[(IBz)_2Im](TCNQ)的合成与结构表征(英文)

A novel compound [(IBz)2Im](TCNQ) [(IBz)2Im=1,3-bis(4-iodobenzyl) imidazole cation, TCNQ-=7,7,8,8-tetracyanoquinodimethanide anion] was synthesized by the reaction of [(IBz)2Im]Br and LiTCNQ in CH3OH and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c with a=1.147 35(18) nm, b=2.028 1(3) nm, c=1.264 1(2) nm, β=104.73(0)°, V=2.666(65) nm3, Z=4, C29H19I2N6, Mr= 705.30, Dc=1.757 g·cm-3, R1=0.053 2 and wR2=0.111 2. The structure analysis shows that the anions are stacked into column with isolated π-dimers, and there is one type of TCNQ entries (TCNQ-), in agreement with the IR spectra analysis of the compound. The most prominent structural features are the completely segregated stacking columns of the TCNQ-anions and [(IBz)2Im]+ cations. CCDC: 759523.     

INVESTIGATIONS ON THE CRYSTAL STRUCTURE OF 2-(m-CYANOPHENYL)-5-CYANOBENZOTHIAZOLE AND CONFORMATIONS OF ITS ISOMERS

The crystal structure of 2-(m-cyanophenyl)-5-cyanobenzothiazole has been determined by X-ray single crystal diffraction method and its conformational analysis and its two isomers have been carried out by employing the PCILO method. The crystal of title compound belongs to the monoclinic system, space group P2_1/c, a=23.793(7), b=3.852(1), c=27.004(11), β=98.40°(3), Z=8, D_(calc). =1.42g/cm~3, F(000)=1072, the final β=0.048. The crystals of this molecule and its two isomers belong to a same space group, but the packing schemes of the molecules in the unit cell, the separations and the mutual orientation of-C≡N bonds are not same. From the detailed analysis and comparison of their packing schemes in crystal, it can be considered that they may be possible to polymerize to different extent in the solid state by appropriate energy stimulation.     

STUDY ON SYNTHESIS, STRUCTURE AND COMPLEXATION CHARACTERISTIC OF UO_2Cl_4(DCH 18C6·H_3O)_2*

The title compound was synthesized by extracting nranylchloride in HC1 system using dicyclohexyl-18-crown-6 as extraction agent. The absorption peaks 1090 cm~(-1) and 912 cm~(-1) in IR spectrum result from frequence red-shift of anti-symmetric stretch vibration of C—O—C of crown ring and [OUO] group, respectively.X-ray diffraction analysis results in its crystallographic parameters: triclinic system, space group P; a=10.183(3), b=10.606(3), c=12.850(6), α=72.09(3), β=85.97(4), γ=86.14(2)°, V=1315.7, z=1. The structure was solved by heavy atom method. Structure refinements converged to final R=0.062, R_w=0.061. U atom is situated on the symmetry center and coordinated by four chlorine atoms and two oxygen atoms to form a square bipyramid coordination polyhedron. The H_3O~+ group is embedded in the crown ring and connected with three crown oxygen atoms via hydrogen bonds.     

Synthesis,Structure Characterization and Optical Properties of β Lithium Zinc Phosphate

β-LiZnPO_4 single crystal was successfully synthesized via hydrothermal method. It crystallizes in the trigonal space group R3 with a = b = 13.6490 ?, c = 9.1123 ?, γ = 120.00° and Z = 18. Structure of the crystal is constructed by LiO_4, ZnO_4 and PO_4 tetrahedral units to form a three-dimensional(3 D) framework. The crystal has a high transmission ranging from 350 to 800 nm with UV cut-off edge at 220 nm. The nonlinear optical efficiency of the as-prepared β-LiZnPO_4 is about 1.2 times as large as that of KDP(KH_2PO_4) standard. Additionally, band structure and density of states calculations for β-LiZnPO_4 were performed using the total-energy code CASTEP, based on density functional theory(DFT).     

CRYSTAL AND MOLECULAR STRUCTURE OF 4-CHLORO-5- ETHYL-5-METHYL-3-PHENYL-1, 3, 4-DIAZAPHOSPHOLIDIN-2-THIONE-4-SULFIDE

<正> Crystal of the title compound Mr=304. 80 belongs to the triclinic, space group P1, with a = 7. 282)2), b=9. 064(2), c=11. 737(5) A , α=75. 79 (3), β=78. 70(3), γ=88. 49(2)°, V-736. 21 A3, Z=2, Dx = l. 375 g/cm3. The final refinement is converged with R=0. 062 and Rw= 0. 069.The five-membered heterocycle is in envelope conformation. The P - N bond length (1. 68(1)) indicates that the dπ-Pπ bond between P and N of the title compound is stronger than that of the corresponding 4-phenyl compound.     

RESEARCH ON TRINUCLEAR MOLYBDENUM CLUSTER COMPOUNDS——CRYSTAL AND MOLECULAR STRUCTURES OF (Et_4N)_2[Mo_3(μ_3-O)(μ_2-Cl)_3(Oac)_2Cl_5]

The title compound forms black crystals shaped like pseudo-octahedrons, which belong to the orthorhombic system The space group is Pna 2_1 with unit cell parametrs of a=17.815(1), b=16.629(2), c=12.003(1), and with Z=4, D_(obs)=1.80g·cm~(-3), and D_(calc)=1.804g·cm~(-3). The crystal structure was solved by the heavy atom method and refiened by fullmatrix least-squares to a final conventional R factor of 0.048 for 2584 unique reflections with I≥σ(Ⅰ). The investigation confirms that the crystal structure consists of tetraethylammonium cations and trinuclear Mo cluster anions. The anion is a μ_3-O monocapped trinuclear cluster with an average Mo-Mo bond length of 2.60 (2). On the side of the Mo_3 triangular plane opposite to the μ_3-O atom, each two Mo atoms are bridged by a Cl atom with the result that these seven atoms (3 Me, 1 O and 3 Cl atoms)form an apex-deficient quasicubane configuration. In addition, each Mo atom is coordinated to three additional atoms resulting in a pseudo-octahedral geome     

Isolation,Crystal Structure and Cytotoxic Activity of Natural Maistemonine and Comparison with the Synthetic Compound

The title compound maistemonine(1) was isolated from the total alkaloid fraction of the 95% ethanol extract of the roots of Stemona japonica, followed by preparative HPLC and recrystallization from a mixture of n-hexane and ethyl acetate. The crystal structure of 1, C_(23)H_(29)NO)6, was determined by single-crystal X-ray diffraction analysis. The crystal belongs to orthorhombic system, space group P212121 with a = 8.5698(6), b = 14.0460(11), c = 17.8815(17) ?, V = 2152.4(3) ?~3, Z = 4, M_r = 415.47, D_c = 1.282 g/cm~3, λ = 0.71079 ?, μ = 0.092 cm~(–1), F(000) = 888, S = 0.995, R = 0.0535 and wR = 0.1067. A total of 5136 unique reflections were collected, of which 3523 were observed(Ⅰ 2σ(Ⅰ)). The absolute configuration of 1 could be assigned by referring to the conserved configuration of the methyl groups at C(2). Compound 1 shows mild cytotoxic activity against the prostate cancer cells LNCaP and PC3 with the IC_(50) values of 29.4 ± 2.3 and 46.6 ± 3.1 mM, respectively. It is noteworthy that the natural maistemonine(1) is different from the synthetic compound which was a racemic with the triclinic space group P1. The lactone rings E from the natural and synthetic 1 are almost perpendicular to each other when overlapping the remaining parts of the molecules.     

Synthesis, Crystal Structure and DNA Binding Studies of α,α'-Bis(3,5-bismethyl-1-pyrozolyl)- carbene-acetyl-isopropenyl Hydrazine

The title compound α,α'-bis(3,5-bismethyl-pyrozole-N-yl)-carbene-acetyl-isopro-penyl hydrazine (C16H22N6O, Mr = 314.40) has been prepared. It was characterized by elemental analysis as well as IR, MS, 1H-NMR and 13C-NMR spectra. Its crystal structure was determined by single-crystal X-ray diffraction, getting the following data: triclinic, space group P1 with a = 6.9734(16), b = 10.773(3), c = 12.001(3) A, α = 75.311(4), β = 82.695(4), γ = 77.143(4)°, Z = 2, V = 847.9(3) A3, Dc : 1.231 g/cm3, F(000) = 336 and μ(MoKα) = 0.082 mm-1 (λ = 0.71073 A). The results of crystal structure determination show that there exist intermolecular and intramolecular hydrogen bonds, resulting in a two-dimensional supramolecular framework of the title compound. The binding of the title compound to DNA was investigated by absorption, emission, and viscosity measurements. The title compound shows absorption hyperchromicity accompanied by a blue shift at about 254 nm. The binding constant Kb for the title compound has been determined to be 1.89 × 104 M-1 from absorption measurements. The addition of the title compound to DNA pretreated with EB causes appreciable reduction in the emission intensity, indicating that the DNA-bound EB fluorophore is partially replaced by the title compound. The value of K is 3.093 × 104 M-1. The relative viscosity of DNA decreased with the addition of the title compound. Results suggest that the title compound binds to DNA with a non-classical intercalative or groove interaction mode. The observed efficient nuclease activity of the title compound is interesting and may have further influences on the chemistry of DNA minor groove binders.     

Synthesis, Structure and Third-order Non-linear Optical Properties of Tungsten Dioxo Complex with 8-Hydroxyquinoline Ligand WO2 （C9H6NO）2

Tungsten dioxo complex WO2(C9H6NO)2 was obtained via the low temperature solid-state reaction of(NH4)2WS4, 8-hydroxyquinoline(8-hq) and(CH3)4NI, and it was characterized by means of elemental analyses, IR spectroscopy and X-ray diffraction analysis. The crystal of the title compound belongs to monoclinic, space group C2/c, with the crystal cell parameters: a=1.3316(3) nm, b=0.94444(19) nm, c=1.3485(3) nm, β=109.66(3)°, V=1.5970(6) nm3, Z=6. The title compound possesses a supramolecular structure formed through hydrogen bonds and π-π stacking interactions. The third-order non-linear optical(NLO) properties of the title compound were also investigated. The third-order non-linear absorption coefficient α2 and refractive index n2 are 0.85×10-11 m/W-1 and -1.5×10-19 m2/W, respectively. The third-order non-linear susceptibility χ(3) is 3.03×10-13 esu for 3.8×10-5 mol/L sample concentration.     

Solvent-free Michael addition reaction of fluorene with chalcon

A series of novel Michael addition products of fluorene to chalcone were obtained in the presence of sodium hydroxide under solvent-free condition.The advantages of this procedure were mild reaction conditions,simple protocol,and high yields.The structures of the products were characterized by IR,~1H NMR,MS and X-ray diffraction.The crystal of the new compound 3 h is Triclinic,space group P-1 with a = 0.97352(6) nm,b = 1.08918(7) nm,c = 2.58418(16) nm,α= 80.1400(10)°,β= 79.5490(10)°,γ= 64.2440(10)°,V = 2...     

Synthesis,Crystal Structure and Catalytic Activity of a Dinuclear Aluminum Alkyl Complex

Treatment of indolyl-3-aldimines(3-~tBuN=CH)C_8H_5NH with AlMe_3 afforded the deprotonated indolyl aluminum complex cis-[(μ-η~1:η~1-3-~tBuN=CH)C_8H_5NAlMe_2]_2,and its crystal structure was determined by X-ray single-crystal diffraction.The crystal belongs to the orthorhombic system,space group P2_12_12 with a = 14.590(9),b = 15.860(2),c = 13.266(8) A,μ=0.118 mm~(-1),M_r = 512.64,V= 3069.5(3) A~3,Z = 4,D_c= 1.109 g/cm~3,F(000) = 1104,R= 0.0451 and wR = 0.0937 for 4978 observed reflections with I 2σ(I).In addition,the title compound exhibited a high catalytic activity toward the addition of amines to carbodiimide to form guanidines.     

Synthesis, crystal structure and forming mechanism of two novel copper (Ⅱ) α-methacrylate complexes with benzimidazole

Two copper (Ⅱ) a-methacrylate complexes with benzimidazole, Cu [CH_2=C( CH_3)-COO]_2(C_7H_6N_2)_2(1) and Cu_2 [CH_2=C(CH_3)-COO]_4(C_7H_6N_2)_2 (2), have been prepared and characterized by elemental analyses, IR and electronic reflectance spectroscopies. The single crystal X-ray diffraction study of the two complexes shows that complex 1 has a square planar configuration, while complex 2 has a binuclear cage structure. The crystal structural analyses show that both complexes 1 and 2 are monoclinic, with space group P2_1/c, a=0.924 16(8) nm, b=1.233 02(13) nm, c =0.989 1(3) nm, β=91.912(13)°, D_c=1.386 g/cm~3, Z=2, R=0.033 9 for the former; and a=0.905 7(2) nm, b=2.252 1(5) nm, c=1.623 5(4) nm, β=90.11(2)°, D_c =1.411 g/cm~3 , Z=4, R=0.056 8, Cu-Cu=0.266 21 nm for the latter. Different structural types of complexes 1 and 2 were produced simultaneously in the reaction of copper (Ⅱ) α-methacrylate with benzimidazole in methanol solution. The forming mechanism of the complexes has been summarized.