Synthesis and diverse crystal packing in o-, m- and p-bis(carbonylthioureido)benzenes containing bisferrocenes.

Three bisferrocene-based bis(acylthiourea) positional isomers, namely, 1,2-bis(ferrocenylcarbonylthioureido)benzene (1), 1,3-bis(ferrocenylcarbonylthioureido)benzene (2) and 1,4-bis(ferrocenylcarbonylthioureido)benzene (3), all [Fe(CH)(CHNOS)], have been synthesized via facile nucleophilic addition reactions of 2.3 equivalents of ferrocenoyl isothiocyanate with o-, m- and p-phenylenediamine, respectively. The structures of the three new synthesized isomers were fully characterized by H NMR, C NMR, IR and UV-Vis spectroscopy, elemental analyses and cyclic voltammetry.

Coordination reactions of 2-pyridinecarboxaldehyde-phenylhydrazonatolithium with selected transition metal (Zn, Sn, Fe, Co, Ni and Zr) chlorides and its coupling reaction with dichloromethane.

The reactions of 2-pyridinecarboxaldehyde-phenylhydrazonatolithium C5H4Npy-CH[double bond, length as m-dash]Ni-NaLi(Ph) (abbreviated as Li) with a 1/2 equivalent of anhydrous metal (Zn, Sn, Fe and Co) chlorides or NiCl2(DME) (DME = 1, 2-dimethoxyethane) produced the corresponding mononuclear metal(ii) complexes ( and ), in which each ligand acts as a bidentate ligand and the coordination geometries around the metals are shown to be tetrahedral within the complexes , , and , respectively, and a tetragonal pyramid in the complex . The reaction of Li successively with sodium tert-butoxide and anhydrous ZrCl4 afforded the unanticipated bizirconium complex , in which each monoanionic ligand behaves as a tridentate bridge. Whereas treatment of Li with NiCl2 and then CH2Cl2 led to an interesting methylene-bridged bis(2-pyridyl-phenylhydrazone) compound in moderate yield; a comparative experiment showed that when the Li reacted with CH2Cl2, the coupling compound was also obtained but in very low yield.

Metal (Mg, Fe, Co, Zr and Ti) complexes derived from aminosilyl substituted aminopyridinato ligand: synthesis, structures and ethylene polymerization behaviors of the group 4 complexes.

Lithium N-[(N,N-dimethylamino)dimethylsilyl]-2-pyridylamidate (2) was prepared from the reaction of new compound N-[(N,N-dimethylamino)dimethylsilyl]-2-pyridylamine (1) and LiBu(n). Treatment of the lithium salt (2) with an equal equivalent of MgBr(2)(THF)(2), FeCl(2) and CoCl(2) afforded the corresponding dinuclear complexes , , and , in which metal atoms possess similar trigonal bipyramidal geometries and each ligand functions as a bimetallic bridging binding aminopyridinato moiety with N-donation from the dimethylamino group. While the stoichiometric reaction of with ZrCl(4) gave the mononuclear zirconium complex (6); the seven coordinated zirconium atom adopts a distorted pentagonal bipyramid geometry and the ligand acts as monoanionic η(2)-aminopyridinato moiety with the pendant arm coordinated via N(CH(3))(2).

meso-Bis{η(5)-1-[1-(dimethylamino)ethenyl]-3-(trimethylsilyl)cyclopentadienyl}iron(II) and the cobalt(II) analogue.

The two title crystalline compounds, viz. meso-bis{η(5)-1-[1-(dimethylamino)ethenyl]-3-(trimethylsilyl)cyclopentadienyl}iron(II), [Fe(C(12)H(20)NSi)(2)], (II), and meso-bis{η(5)-1-[1-(dimethylamino)ethenyl]-3-(trimethylsilyl)cyclopentadienyl}cobalt(II), [Co(C(12)H(20)NSi)(2)], (III), were obtained by the reaction of lithium 1-[1-(dimethylamino)ethenyl]-3-(trimethylsilyl)cyclopentadienide with FeCl(2) and CoCl(2), respectively. For (II), the trimethylsilyl- and dimethylaminoethenyl-substituted cyclopentadienyl (Cp) rings present a nearly eclipsed conformation, and the two pairs of trimethylsilyl and dimethylaminoethenyl substituents on the Cp rings are arranged in an interlocked fashion.

A bulky silyl shift-directed synthesis of a silyl-linked amidinate-amidine and its Zr(IV) complex.

A novel silyl-linked amidinate-amidine monoanionic ligand 3 was synthesized by double additions of PhCN starting from silyl-linked bis(amino) monoanion 2, which underwent an intramolecular Li/H metathesis and double silyl shift. The related Zr(IV) complex 4 was prepared and confirmed by X-ray diffraction revealing a structural rearrangement from its precursor. The mechanisms for the reaction processes have been proposed.

The ansa-bridged cyclo-penta-dienyl titanium complex [{η-C(5)Me(4)CH(2)-C(NMe(2))=N}TiCl(2)].

The title complex, dichlorido[N,N-di-methyl-2-(η(5)-tetra-methyl-cyclo-penta-dien-yl)acetamidinido-κN']titanium(IV), [Ti(C(13)H(20)N(2))Cl(2)], exhibits an unusual ansa-bridged conformation. The cyclo-penta-dienyl ring and the mean plane of the Ti-N=C-C-C fragment form a dihedral angle of 88.08 (11)°.

[μ-Bis(trimethyl-silyl)amido]bis-[μ-N,N-dimethyl-N',N''-bis-(trimethyl-silyl)guanidinato]-triangulo-tricopper(I).

The title compound, [Cu(3)(C(6)H(18)NSi(2))(C(9)H(24)N(3)Si(2))(2)], is a trinuclear Cu(I) complex. A crystallographic twofold axis passes through one Cu(I) atom and the N atom of the bis-(trimethyl-silyl)amide ligand that bridges between the other two Cu(I) atoms. The Cu-Cu bonds bridged by the guanadinate ligands [2.

2-Chloro-pyridine-3-carboxamide.

In the crystal structure of the title compound, C(6)H(5)ClN(2)O, the dihedral angle between the pyridine ring and the carboxamine group is 63.88 (8)°. Inter-molecular N-H⋯N and N-H⋯O hydrogen bonds link the mol-ecules into a two-dimensional network.

N-o-Tolyl-benzamidine.

The asymmetric unit of the title compound, C(14)H(14)N(2), contains two independent mol-ecules with slightly different conformations; the dihedral angles formed by aromatic rings in the two mol-ecules are 73.2 (1) and 75.0 (1)°.

Preparation and characterization of inclusion complexes of pefloxacin mesylate with three kinds of cyclodextrins.

The ability of alpha-cyclodextrin, beta-cyclodextrin and hydroxypropyl-beta-cyclodextrin (alpha-CD, beta-CD and HP-beta-CD) to break pefloxacin mesylate (PM) aggregates by forming inclusion complexes has been studied using 1H NMR (nuclear magnetic resonance spectroscopy), 13C NMR and fluorescence spectra. The inclusion constants are determined to compare the corresponding inclusion capacity. Solid-inclusion complexes of PM with CDs are synthesized by coprecipitation method, and all the inclusion ratios are found to be 1:1.

(1R,2R)-(-)-Bis[mu4-1-[[1,1-dimethyl-2-(trimethylsilyl)amidino]amino]-2-([1,1-dimethyl-2-[1,1-dimethyl-2-(trimethylsilyl)amidino]amidino]amino)cyclohexane]tetralithium(I).

The title compound, [Li(4)(C(21)H(46)N(8)Si(2))(2)], has been prepared and its structure determined. The whole molecule can be regarded as a molecular cage made up of the central eight-membered ring and six contiguous rings of three types. As the first example of a bridged amidinate-dicyanamide framework, this noteworthy structure and its electronic features are presented.

Preparation and study on the solid inclusion complex of sparfloxacin with beta-cyclodextrin.

The interaction of sparfloxacin with beta-cyclodextrin (beta-CD) has been studied by several analytical techniques, including 1H-NMR, 13C-NMR, fluorescence spectroscopy, infrared spectroscopy, thermal analysis, and scanning electron microscope. In this paper, solid inclusion complex of sparfloxacin with beta-CD was synthesized by the coprecipitation method. In addition, the characterization of the inclusion complex has been proved by fluorimetry, Infrared, differential scanning calorimetry and 1D, 2D NMR.