Synthesis and Crystal Structures of Schiff Bases Bearing Ferrocenylphenyl Groups

The Schiff bases bearing ferrocenylphenyl and diferrocenylphenyl groups were synthesized by the reactions of m-ferrocenylaniline with salicylaldehyde or 1, 4-bis (2′-formyl- phenyl)-1, 4-dioxabutane. The title compounds were characterized by elemental analysis, IR, 1H NMR and X-ray structural determination.

Crystal Type Iof Azilsartan Polymorphs: Preparation and Analysis

Azilsartan (2-ethoxy-1-([2’-(5-oxo-4,5-dihydro-1,2,4-oxadiazol-3-yl)biphenyl-4-yl]methyl)-1H-benzimidazole-7-carboxylic acid) is a new angiotensin II receptor antagonist used in the treatment of hypertension. This paper describes the preparation of type I crystal and its single crystal diffraction data, the comparison of the powder diffraction data for both type I and II crystals as well as their stability and solubility in methanol.

Synthesis, Characterization and Crystal Structure of Bis[1 -meth oxy-2,2,2-tris-（pyrazol-1 -yl-KN2）ethane]-coppe r（Ⅱ） Bis-perchlorate

Bis[1-methoxy-2,2,2-tris-（pyrazol-l-yl-KN2）ethane]-copper（Ⅱ） bis-perchlorate （2） was synthesized by reacting of pyrazole based tripodal scorpionate ligand 1-methoxy-2,2,2-tris（pyrazol-1-yl）ethane （1） with copper（Ⅱ） perchlorate hexahydrate in methanol, acetonitrile and water mixture as solvent. Slow evaporation of the filtered reaction mixture in air produced blue color block crystals suitable for single crystal X-ray diffraction study of the title complex. Compound 2 crystallizes in the monoclinic space group P21/n with unit cell parameters, α = 8.1269（1） ,A, b = 21.8348（2）A, c = 9.1522（1） A, a = γ= 90° , β = 99.7611 （4）°. The structure of the compound was characterized by IR Spectroscopy, elemental analysis and single crystal X-ray diffraction analysis.

Synthesis, characterization, spectroscopic and crystallographic investigation of Cobalt(Ⅲ) schiff base complex with two perpendicular diamine coumarin ligands

New transition metal complex of Cobalt(III) of the ligand (E)-3-(1-(2-aminoethylimino)ethyl)-4-hydroxy-2H-chromen-2-one, derived from condensation of ethylene diamine with 3-acetyl-4-hydroxy-chromene-2-one have been synthesized by reaction of cobalt(III) salt and the ligand, in amounts equal to metal-ligand molar ratio of 1:2. Both the Schiff base and the complex of Co(III) were characterized by IR, UV-Vis, 1H NMR- and 13C NMR-spectroscopy techniques. Single crystal X-ray diffraction investigation, at low temperature T = 120 K, shows that the cobalt complex is triclinic P-1, a = 10.426(5) ?, b = 11.3234(2) ?, c = 15.729(5) ?, α(°) = 70.102(4), β(°) = 86.049(4), γ(°) = 82.497(4), Z = 2, and its structure consists of isolated [Co(III)(C13H13N2O3)2]+ complex cations with distorted octahedral geometry, ClO-4 counter anions, acetone solvent and water molecules. The crystal cohesion is stabilized by hydrogen bonds between ligands and water molecules, and ionic interactions between complex cations and counter anions.

On the Mechanism of Condensation between 5-Amino-4, 6-dichloro- 2-methylpyrimidine and 1-Acetyl-2-imidazolin-2-one

The condensation reaction between 5-amino-4, 6-dichloro-2-methylpyrimidine and 1-acetyl-2-imidazolin-2-one using POCl3 as solvent gave 4, 6-dichloro-2-methyl-5-(1-acetyl-tetra- hydro-imidazo-2-ylidene)-aminopyrimidine predominantly and 4, 6-dichloro-2-methyl-5-{1-[1-(2- oxo-tetrahydro-imidazolyl)]-acetyene}-aminopyrimidine as by-product. No 4, 6-dichloro-2- methyl-5-(1-acetyl-2-imidazolin-2-yl)-aminopyrimidine was found. The result indicated an esterifi- cation-addition-elimination mechanism.

A Reflectron Time-of-Flight Mass Spectrometer with a Nano-Electrospray Ionization Source for Study of Metal Cluster Compounds

An experiment facility has been set up for the study of metal cluster compounds in our laboratory, which consists of a nano-electrospray ionization source, an ion transmission and focus system, and a reflectron time-of-fight mass spectrometer. Taking advantage of the nano-electrospray ionization source, polyvalent ions are usually produced in the ＂ionization＂ process and the obtained mass resolution of the equipment is over 8000. The molecular ion peaks of metal cluster compounds [Au20（PPhpy2）10Cl2]（SbF6）4, where PPhpy2=bis（2- pyridyl）phenylphosphine, and [AuaAg2（C）L6]（BF4）4, where L=2-（diphenylphosphino）-5- methylpyridine, are distinguished in the respective mass spectrum, accompanied by some fragment ion peaks. In addition, the mass-to-charge ratios of the parent ions are determi- nated. Preliminary results suggest that the device is a powerful tool for the study of metal cluster compounds. It turns out that the information obtained by the instrumentation serves as an essential supplement to single crystal X-ray diffraction for structure characterization of metal cluster compounds.

New Iboga‑Type Indole Alkaloids from Tabernaemontana divaricata

Two hitherto unknown iboga-type indole alkaloids,namely(3R)-7,19-di-epi-3-methoxytabernoxidine(1)and(3R,19R)-19-hydroxy-3-(2-oxopropyl)voacangine(2),together with eight known alkaloids(3-10),were isolated from the twigs and leaves of Tabernaemontana divaricata.Their structures were established on the basis of spectroscopic data interpretation,single crystal X-ray diffraction analysis and circular dichroism spectrum.

Synthesis and Properties of a Heteronuclear Ag(Ⅰ)/Ni(Ⅱ) Complex

A complex, Ni （en）2Ag3 （CN） s （ en =ethylenediamine）, was obtained through the reaction of [ Ag （ CN ）2 ]^- units with Ni II -diamine cation C Ni （en）2]^2＋, and the structure was determined by single crystal X-ray diffraction. It is indicated that the complex has a 3D architecture through the silver-silver interactions and the bridging eyano groups. This complex displays interesting luminescent properties caused by argentophilieity at room temperature in solid state.

Synthesis and Structure of Dibenzoyl-bissemicarbazone Neodymium(Ⅲ) Perchlorate

A new Schiff base Dibenzoyl-bissemicarbazone C15H16N6O2(L) and its complex with neodymium(Ⅲ ) perchlorate [NdL2(H2O)2](ClO4)3 were synthesized. The crystal and molecular structure of the title complex were determined by single crystal X-ray diffraction. The crystal is monoclinic and conforms to space group P. with cell constants a=10. 893(2) A, b= 12. 118(3) A , c=22. 494(5) A , β=89. 86(3)% V = 2969.19A3. The final standard deviation R=0. 0919. In the complex Nd is coordinated by four nitrogen and six oxygen atoms, of which four nitrogen and four oxygen atoms are provided by two neutral ligands L, and the other two oxygen atoms are provided by two water molecules, forming a ten-coordinated complex cation, which the perchlorate groups exist in the outer sphere. The coordination polyhedron takes a bicapped anti-square prism arrangement. That the average bond length of Nd-N is 2. 735 A indicates that the coordination of N in groups to Nd( Ⅲ ) is very weak.

Synthesis, crystal structure and thermal analysis of a new stilbazolium salt crystal

A new organic crystal of 4-N, N-dimethylamino-4＇-N＇-methyl-stilbazolium benzene sulfonate （DASBS） was synthesized and characterized for the first time. It is a derivative of 4-N, N-dimethylamino-4＇-N＇-methyl-stilbazolium tosylate （DAST） with the benzene sulfonate replacing p-toluenesulfonate. Single crystal XRD demonstrated that the crystal structure of DASBS. H20 was triclinic. The thermal analysis of this new crystal was also conducted, and the melting point was obtained to be 232℃.

Siderochelins with anti-mycobacterial activity from Amycolatopsis sp. LZ149

Three new compounds, namely siderochelins D （2）, E （3）, and F （4）, together with one known siderochelin A （1）, were isolated from Amycolatopsis sp. LZ149 and elucidated by spectroscopic analyses includinglD- and 2D-NMR and X-ray single crystal diffraction. Compounds 1-3 showed antibacterial activity against Mycobacterium smegmatis.