Preparation and Crystal Structure of Sodium Hydrogen Epoxysuccinate

C4H3O5Na(0.5H2O) was prepared by the reaction of H2O2 and maleic anhydride. The product was characterized by elemental analysis and IR measurement. The crystal structure was determined by single-crystal diffraction analysis. The crystal belongs to monoclinic, space group C2/c with a = 21.132(3), b = 8.646(2), c = 6.196(1) ?, β = 90.67(1)o, V = 1132.0(4) ?3, Mr = 163.06, Dc = 1.914 g/cm3, Z = 8, F(000) = 664, μ = 0.243 mm-1, the final R = 0.0354 and wR = 0.1151. X-ray analysis reveals that there exists a stable symmetrical structure in the complex, and a network structure is formed via intermolecular hydrogen bonds.

Preparation and Crystal Structure of Paeonol

Paeonol was prepared by the extraction method from Moutan Cortex. Its crystal struc- ture was determined by single-crystal X-ray diffraction.The compound crystallizes in the monoclinic sys- tem, space group P21/c with a = 6.724(4), b = 8.792(6), c = 14.689(10) ?, β = 100.138(11)o, V = 854.8(10) ?3, Mr = 166.17, Z = 4, F(000) = 352, Dc = 1.291 g/cm3, μ = 0.097 mm-1, the final R = 0.0454 and wR = 0.0988 for 845 observed reflections with I > 2σ(I).

Preparation and Crystal Structure of 3-(2-Hydroxyphenyl)-6-(4-nitrophenyl)-7H- 1,2,4-triazolo[3,4-b][1,3,4 ]thiadiazine

3-(2-Hydroxyphenyl)-6-(4-nitrophenyl)-7H-1,2,4-triazolo[3,4-b][1,3,4] thiadiazine, C 16H 11N 5O 3S, was prepared by the cyclization of 3-(2-hydroxyphenyl)-4-amino-5-mercapto-1,2,4-triazole with 2-bromo-4-nitroacetophenone. The compound was characterized by means of elemental analysis, IR, 1H NMR, 13C NMR, mass spectrometry, and X-ray diffraction. The compound crystallizes in a monoclinic system with space group C c, a=2.1853(4) nm, b=2.1192(5) nm, c=1.3526(3) nm, β=95.21(2)°, V=6.238(2) nm3 , D calcd.=1.505 Mg/m3, Z=16, F(000)=2916, R 1=0.0501, wR 2=0.0427. A comparison between the crystal structures of 1,2,4-triazolo[3,4-b] [1,3,4] thiadiazine and 1,2,4-triazolo[3,4-b][1,3,4] thiadiazole was made in the structural view. A two-dimensional network is formed by hydrogen bonds and π-π stacking interactions.

PREPARATION AND X—RAY CRYSTAL STRUCTURE OF [(C_6H_5)_2PCH_2CH-2P(C_6H_5)_2]Fe(NO)_2

The complex [(C_6H_5)_2PCH_2CH_2P(C_6H_5)_2]Fe (NO)_2, was easily synthesized by the reaction of Fe (CO)_5, NaNO_2 and (C_6H_5)_2PCH_2CH_2P(C_6H_5)_2 (dppe) in methanol and determined by X—ray diffraction which denoted that the title complex has two crystallographically independent molecules in its asymmetric unit.

PREPARATION AND CRYSTAL STRUCTURE OF TETRAMETHYLETHENE-BRIDGED DICYCLOPENTADIENYLSAMARIUM (Ⅲ) COMPLEX

(CH_3)_4C_2(C_5H_4)_2Sm(C_5H_5)OC_4H_, Mr=499.4, orthorhombic, Cc2a, a=11.696(6), b=12.539(5), c=29.432(15), V=4316(4)~, Z=8, Dc=1.54g. cm^(-3), μ (MoKα)=27.8cm^(-1), F(000)=2024, R=0.077 for 1833 observed reflections. In the molecule the samarium atom is bonded to three cyclopentadienyl rings and an oxygen of tetrahydrofuran(THF). The three centroids of the cyclopentadienyl rings and the oxygen form a tetrahedral configuration around the Sm(Ⅲ) atom, The average Sm-C(η~) bond distances for the three cyclopentadienyl groups are 2.72(3), 2.76(3), 2.78(8) respectively, and Sm-0 bond is 2.53(1).

Preparation and Crystal Structure of PrNb_5O_(14)

Single crystals of PrNb_5O_(14) were prepared by solid state reaction from PrOBr/Nb_2O_5/NH_4Br system at 950℃. Compound PrNb_5O_(14) (M_r=829. 43) crystallized in orthorhombic Pmmn (No. 59) with cell parameters of a=7. 758 (3), b= 20. 092(6), c=6. 241(1) A, V=972. 8(5) A￣3: Z=4; F(000)=1504; Dc=5. 66 g/cm￣3;μ(MoKa)=104. 39 cm￣(-1).The final structure factors are R=0. 063 and R_w=0. 073 respectively for 1747 observed reflections with I>3σ(I). The structure consists of two types of NbO polyhedra, Nb (1) and Nb (3) pentagonal bipyramids and Nb (2)O6 octahedron. Chains of edge sharing pentagonal NbO_7-bipyramids are connected by corner-sharing NbO_6-octahedra. Tunnels running in a-direction are created by this framework of NbO_6 and NbO_7-polyhedra. Praseodymium atoms are 9-coordinated with tricapped trigonal prism polyhedron, and are located in these tunnels at levels between the niobium atoms.

Synthesis and Crystal Structure of 9-Pyridyl-1,8-dioxo-2,3,4,5,6,7-hexahydroxanthene

9-Pyridyl-1,8-dioxo-2,3,4,5,6,7-hexahydroxanthene 3 (C18H17NO3) was prepared by the reaction of 4-pyridinecarboxaldehyde and 1,3-cyclohexanedione using Nafion-H as catalyst. The crystal and molecular structures were studied. The crystal is of orthorhombic, space group Pbcn with a = 20.369(4), b = 14.528(2), c = 9.747(17) ?, V = 2884.3(9) ?3, Dc = 1.360 g/cm3, Z = 8, F(000) = 1248 and μ(MoKα) = 0.093 mm-1. The final R = 0.0395, wR = 0.1087 for 1458 observed reflections (I > 2σ(I)), and R = 0.1032, wR = 0.1340 for all 2580 reflections. The outer rings of the xanthene groups adopt an almost ideal envelope conformation, and the heterocyclic central ring exhibits a distorted boat conformation. The pyridyl group is rotated with respect to the xanthene system by 87°.

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-isopropenyl 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）A^3, Dc = 1.231 g/cm^3, F（000） = 336 and/μ（MoKα） = 0.082 mm^-1 （λ= 0.71073A）. 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 × 10^4 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 × 10^4 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 and Crystal Structure of N-(5-Phenylseleno)pentyl Succinimide

N-(5-phenylseleno)pentyl succinimide 1, C15H19NO2Se (Mr = 324.27), was prepared by treating Br(CH2)5SePh with potassium succinimide. Its crystal structure has been determined by X-ray single-crystal diffraction. The crystal of 1 belongs to monoclinic system, space group P21/c with the crystal cell parameters: a = 18.018(6), b = 5.980(2), c = 14.682(5) ? = 109.977(6)? V = 1486.7(9) 3, Z = 4, Dc = 1.449 g/cm3, (MoK? = 2.523 mm-1, F(000) = 664,the final R = 0.0302 and wR = 0.0666 for 2623 independent observed reflections with I > 2(I). Structure analyses revealed that there exist strong nonclassical hydrogen bonds (CH…O).

Co Content Dependence of Crystal Structure and Specific Magnetization of Fe_(1-x)Co_x-SiO_2 Granules Prepared by Sol-Gel Method

The Co content dependence of crystal structure and specific magnetization of Fe1-xCox-SiO2granular solid prepared by the sol-gel method have been studied. It is found that the crystal structure, Iattice parameter and specific magnetization of the FeCo alloy particles depend on the Co content.

Crystal Structure and Physicochemical Properties of a New Tris (2-Amoniumbenzamide) Sulfate (C₇H₉N₂O)₃HSO₄SO₄

Physicochemical properties of a new hybrid compound (C7H9N2O)3HSO4SO4 are synthesized in aqueous solution and characterized by various physicochemical studies. This compound crystallizes in the monoclinic space group P21/c and a unit cell with a = 10.3028(2)A°, b = 12.4995(2)A°, c = 20.6730(2)A°, V = 2600.61(7)A°3, and Z = 8. The structure has been solved using direct method and refined to a reliability R factor of 4.6%. The atomic arrangement of this compound is built up by (HS2O8)3- anionic pairs interconnected with two types (C7H9N2O)22+ cationic pairs via (N, O)-H...O hydrogen bonds. The characterization of these salts was carried out using X-ray diffraction, IR spectroscopy and thermal analysis.

Crystal structure, thermal analysis and IR spectroscopic investigation of bis (N-methyl anilinium) sulfate

Chemical preparation, X-ray single crystal, thermal analysis and IR spectroscopic investigation of (C7H10N)2 SO4 denoted NMAS are described. The NMAS crystallizes in the triclinic system with P-1 space group. Its unit cell dimensions are a = 9.6150(5) ?, b = 9.9744(3) ?, c = 10.2767(6) ?, α = 68.069(3)°, β = 62.929(2)°, γ = 67.285(3)° with V = 785.72(7) ?3 and Z = 2. The structure has been solved using direct method and refined to a reliability R factor of 3.62%. The NMAS structure is built up from chains containing all the components of the structure and parallel to the b axis, linked via N—H-----···O hydrogen bonds. Stability between successive chains is performed by weak interactions originating from the organic cations.

Synthesis, Magnetic Property and Crystal Structure of a Ytterbium-Copper Mixed Metal Complex:Yb_2Cu_3L_6·6H_2O (L=O(CH_2COO)_2)

Reaction of hydrated ytterbium nitrate and copper nitrate with diglycolic acid at pH= 7 produced a new Yb-Cu mixed metal complex, Yb2Cu3L6. 6H2O(L= O(CH2COO)2). Complex Yb2Cu3O36C2H36 (Mr= 1437. 23) crystallized in hexagonalP6/mcc (No. 192) with cell parameters of a= 14. 344 (3), c= 15. 470(7) A,V= 2757(2) A 3; Z= 2; F(000) = 1390; Dcalc.= 1- 731 g/cm3 μ(MoKa) =45. 8 cm-1. The final agreernent factors are R= 0. 077 and Rw = 0.089 for 867 observed reflections with I>3δ(I). It has been characterized by elemental analysis, IR spectrum, magnetic measurement and X-ray crystallography. In the complex, the Yb3+ ion is 9-coordinated tothree ether oxygen and six carboxylate oxygen atoms from three ligands, the copper ionis coordinated to four oxygen atoms from four carboxylate groups of four ligands andtwo water molecules. The Yb3+ ions and the Cu2+ ions are connected by the carboxylate groups of the ligands, thus resulting in the formation of the complicated networkstructure.

Crystal Structure and Physicochemical Properties of 2-Diisopropylammonium Ethylammonium Sulfate Dihydrate

A new organic sulfate (C8H22N2)SO42H2O denoted DPAES is obtained by interaction of H2SO4 with the organic molecule 2-[Diisopropylamino] ethylamine. We describe its crystallographic and structural features. DPAES is triclinic, Pī, with the lattice parameters a = 6.8841(2)?, b = 8.4966(2)?, c = 12.0804(3)?, = 81.824(1)o, = 88.007(1)o, = 78.649(1)o, V = 685.72(3)?3, and Z = 2. Its atomic arrangement is described as inorganic chains of SO42- units and water molecules, these chains are interconnected by organic groups so as to build layers parallel to the (001) planes. The IR data of DPAES are reported and discussed according to the theoretical group analysis and by comparison with IR results of similar compounds. The coupled TG-DTA thermal study shows the departure of two water molecule, con- firming the hydrated character of this compound.

Synthetic and structural chemistry of nickel(Ⅱ) complexes containing dithiolato and phosphine ligands Ⅰ. Preparation and crystal structure of Ni_2(PPh_3)_2(edt)_2

A nickel(Ⅱ) complex containing both dithiolato and phosphine ligands, Ni_2(PPh_3)_2(edt)_2 (edt = SCH_2CH_2S^(2-)), has been prepared and characterized by X-ray diffration. The complex crystallizes in the triclinic system, space group P-1, with a = 10.693(3), b = 17.457 (6), c = 10.606 (3)A, α= 102.84(2), β = 96.49 (2), γ = 82.56(3)°; V = 1906.8 A^3; D_c = 1.439g.cm^(-3) for Z=2; the final con- ventional R was 0.052 based on 3338 observed reflections. Nickel atoms are linked by two sulfur atoms from two edt ligands with the Ni--Ni distance of 2.893 A, and each Ni atom is coordinated by one phosphorus atom and three sulfur atoms with a square-planar geometry, where the average: length of Ni--S bond is 2.180 A and Ni--P bond 2.188 A. The UV-Vis and ~1H NMR spectra have also been recorded.

Preparation, Crystal Structure and Theoretical Calculation of 4-（4,6-Dimethylpyrimidin-2-yl）-3-thio-allophanic Acid Methyl Ester

4-（4,6-Dimethylpyrimidin-2-yl）-3-thio-allophanic acid methyl ester was synthesized with mixing 2-amino-4,6- dimethylpyrimidine, potassium thiocyanate and methyl chloroformate in ethyl acetate. Single crystals suitable for X-ray diffraction measurement were obtained by recrystallization from dimethylformamide at room temperature. The crystal belongs to monoclinic symmetry with space group C2/m, and crystal parameters of a= 1.7537（5） nm, b= 0.6759（2） nm, c=1.1148（3） nm, β=118.557（4）°, V=1.1605（6） nm^3, Z=4, De= 1.375 g/cm^3,μ=0.271 mm^-1, F（000）=504, and 1519 [1〉2σ（I）] observable independent reflections were used for the determination and refmement of the crystal structures with final R1 of 0.0372 and wR2 of 0.0992. The theoretical investigation of the title compound was carried out with DRT-B3LYP/6-311G, HF/6-311G and MP2/6-311G methods, and the atomic net charges and the population were discussed.

Preparation,Crystal Structure and Fungicidal Activity of N-(5-(benzofuranol-7-oxymethyl)-1,3,4-thiadiazol-2-yl)amide Compounds

A variety of new N-(5-(benzofuranol-7-oxymethyl)-1,3,4-thiadiazol-2-yl)amide compounds(8a-i)were synthesized through four steps from benzofuranol as raw materials.The crystal structure of compound 8a(C17H21N3O3S,Mr=347.43)was measured by X-ray diffraction,which was classified as monoclinic system,Z=4,V=1742.72(8)Å3,Dc=1.324 Mg/m3,F(000)=736,S=1.03,μ=0.21 mm-1,space group P21 with a=9.9177(3),b=8.9519(2),c=19.8679(5)Å,the final R=0.035 and wR=0.105 for 3873 observed reflections(I>2σ(I)).The X-ray structure presented N(3)-H(3)···N(2)and C(6)-H(6)···O(3)intermolecular hydrogen bonds,which acted as an important role in stabilizing the crystal structure.Additionally,preliminary biological assay on compound 8a showed good fungicidal activity in vivo,with the inhibition of 75%against Pseudoperonospora cu-bensis at 200 mg/L.

Preparation and Molecular Structure of (SCZ)(TNPG)·2H_2O

The （SCZ）（TNPG）.2H2O prepared by mixing semicarbazide （SCZ） and trinitrophloroglucinol （TNPG） was characterized by elemental analysis and IR measurement, and its crystal structure was determined by X-ray single-crystal diffraction analysis. The crystal belongs to triclinic,space group P1, （NH2CONHNH3）^＋（C6H2N3O9）^-·2H2O, Mr = 372.23, a = 0.68853（14）, b =0.93966（19）, c = 1.1925（2） nm, α = 67.48（3）, β = 77.56（3）, γ = 78.93（3）°, V = 0.6908（2） nm^3, Z = 2,Dc = 1.789 g/cm^3, Mr = 373.23, F（000） = 384, S = 0.999 and μ（MoKa） = 0.172 mm^-1. The final R and wR are 0.0394 and 0.1057 for 1724 observed reflections with I 〉 2σ（I）. It is concluded that （SCZ）（TNPG） 2H2O is an ionic compound composed of a cation SCZ^＋, an anion TNPG- and two water molecules. The TNPG anion and SCZ^＋ cation are bonded together by electrostatic attraction and hydrogen bonds, and the compound structure is stable. The thermal decomposition of （SCZ）（TNPG） 2H2O was studied by using TG-DTG and DSC techniques with a heating rate of 10 ℃/min, showing the compound contains one endothermic process of dehydrating stage and two intensive exothermic decomposition stages. The enthalpy of exothermic decomposition reaction is 452.31 kJ/mol.

Crystal structures and fluorescence properties of lanthanide complexes prepared with 2,2'-biphenyldicarboxylic acid and 2,2':6',2''-terpyridine

Five lanthanide complexes of Ln2（dpdc）2（tpy）2（NO3）2（H2O）2 [Ln=La （1）, Ce （2）, Pr （3）, Sm （4）, Gd （5）, H2dpdc=2,2’-biphenyldicarboxylic acid and tpy=2,2’：6’,2’’-terpyridine] were prepared at room temperature and characterized by X-ray diffraction, FT-IR and thermo-gravimetric analysis. The results showed that complexes 1–5 were isostructural and consisted of dinuclear units [Ln2（dpdc）2（tpy）2（NO3）（H2O）2] bridged by two dpdc2？ ligands. The dinuclear units with strong intramolecular hydrogen bonds were assembled into 2D supramolecular layers by the weak π？？？π staking interactions between pyridine rings of tpy. The TG analysis showed that the complexes 1–5 behaved higher thermal stability with no mass loss at 〈 320 °C. The lanthanide contraction effect and the solid state luminescence properties of complexes 1–5 were also investigated. The luminescence emission spectra of complexes 1–5 exhibited ligands emission bands and complex 3 and 4 had no typical emission in the visible region.

Crystal structure and quantum chemical investigation of [Cd(NTO)_(4)Cd(H_(2)O)_(6)]·4H_(2)O

[Cd(NTO)4Cd(H2O)6] ?4H2O was synthesized by mixing the aqueous solution of 3-nitro-1, 2,4-triazol-5-one (NTO) and cadmium carbonate. The single crystal structure was determined by a four-circle X-ray diffractometer. The crystal is monoclinic, space group C2/c with crystal parameters of a = 2.1229(3) nm, b = 0.6261(8) nm, = 2.1165(3) nm, β= 90.602 (3)°, V= 2.977(6) nm3, Z = 4, Dc = 2.055 g ? cm-3, μ = 15.45 cm-1 and F(000) = 1824. 2523 observable independent reflections with F04σ(F0) were used for the determination and refinement of the crystal structure. Lorentz-polarization and absorption correction were applied. The final R is 0.0282 and wR = 0.0792. The analytical results show that the Cd+2 has two kinds of coordinate bonds in one crystal. One Cd+2 coordinates with 4 NTO anions and another coordinates with 6 water molecules to form a binucleate complex with a structure of tetrahedron and tetragonal bipyramid, respectively. By using SCF-PM3-MO method, the electron structure of cadmium complex of NTO has been calculated. The analysis of the calculated results shows that when [Cd(NTO)4Cd(H2O)6] ? 4H2O is heated, the crystallization waters will be dissociated first and the ligand waters second and NO2 group has priority of leaving when NTO? is decomposed. Analysis of the energy level and composition of localized molecular orbitals indicates that both the two Cd2+ bond to the coordinating atom with 5s