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28. Reactions of TaF5 with activated arenes. Synthesis of [4-(OH)-3-(OCH3)C6H3CH( O H)][4-(OH)-3-(OCH3)C6H3CHO][TaF6], a rare example of protonated aldehyde.

Author

Hayatifar, Mohammad, Marchetti, Fabio, Pampaloni, Guido, and Zacchini, Stefano

Subjects
*CHEMICAL reactions, *AROMATIC compounds, *CHEMICAL synthesis, *ALDEHYDES, *SOLID state chemistry, *VANILLIN, *DICHLOROMETHANE, *X-ray diffraction
Abstract

Abstract: The rare example of protonated aldehyde salt [4-(OH)-3-(OCH3)C6H3CH( O H)][4-(OH)-3-(OCH3)C6H3CHO][TaF6], 1, was isolated in the solid state by the reaction of 4-hydroxy-3-methoxybenzaldehyde (vanillin) with TaF5 in dichloromethane. The product 1 was characterized by X-ray diffraction and IR spectroscopy. The 1:1 reaction of TaF5 with N,N-dimethylaniline in CH2Cl2 cleanly afforded [TaF4(NMe2C6H5)2][TaF6], 2, which was identified by NMR spectroscopy. Attempts of crystallization of 2 resulted in the isolation of the ammonium salt [NHMe2C6H5][TaF6], 3. [Copyright &y& Elsevier]

Published
2014
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38. The chemistry of niobium and tantalum halides, MX5, with haloacetic acids and their related anhydrides: Anhydride C–H bond activation promoted by MF5

Author

Marchetti, Fabio, Pampaloni, Guido, and Zacchini, Stefano

Subjects
*NIOBIUM, *TANTALUM, *HALIDES, *ANHYDRIDES
Abstract

Abstract: Niobium and tantalum pentahalides, MX5 (1), react with acetic acid and halo-substituted acetic acids, in 1:1 ratio, to give the dinuclear complexes [MX4(μ-OOCMe)]2 [M=Nb, X=Cl, 2a; M=Ta, X=Cl, 2b; Br, 2c] and [MCl4(μ-OOCR)]2 [M=Nb, R=CH2Cl, 4a; CHCl2, 4c; CCl3, 4e; CF3, 4g; CHBr2, 4i; CH2I, 4j; M=Ta, R=CH2Cl, 4b; CHCl2, 4d; CCl3, 4f; CF3, 4h]. The solid state structures of 2b and 4e have been ascertained by X-ray diffraction studies. The reactions of 1 with acetic anhydride and halo-substituted acetic anhydrides result in C–O bond activation and afford 2 and 4, respectively, with concomitant formation of acetyl halides. Moreover, the complexes MCl5[OC(Cl)Me] [M=Nb, 3a; M=Ta, 3b] have been detected in significant amounts within the mixtures of the reactions of MCl5 with acetic anhydride. TaI5 is unreactive, at room temperature, towards both MeCOOH and (MeCO)2O. MF5 react with RCOOH (R=Me, CH2Cl) in 1:1 molar ratio, to afford the ionic compounds [MF4(RCOOH)2][MF6], 5a–d, in high yields. The additions of (RCO)2O (R=Me, CH2Cl) to MF5 give 5, suggesting that anhydride C–H and C–O bonds activation is operative during the course of these reactions. [Copyright &y& Elsevier]

Published
2008
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39. First-row transition and group 12 element bis[poly[4-methyl-1H-pyrazol-1-yl)borate]] derivatives. X-ray crystal structure of Zn[HB(4-Mepz)3]2·CHCl3

Author

Gioia Lobbia, Giancarlo, Bovio, Bruna, Santini, Carlo, Pettinari, Claudio, and Marchetti, Fabio

Abstract

A series of new metal complexes of general formula M[Tp#]2 (where Tp# =hydridotris(4-methyl-1H-pyrazol-1-yl)borate (Tp4Me) or tetrakis(4-methyl-1H-pyrazol-1-yl)borate (pzTp4Me) and M ]- Mn, Fe, Co, Ni, Cu, Zn, Cd) were synthesized from the appropriate metal chloride and KTp# in aqueous solution. These compounds are air-stable solids, sparingly soluble in most organic solvents; they have been characterized by elemental analysis, conductivity and molecular weight measurements, IR, UV, visible spectra and, in the case of diamagnetic compounds, also with 1H and 13C NMR spectra. The X-ray crystal structure of bis[hydridotris(4-methyl-1H-pyrazol-1-yl)borate]zinc(II)·CHCl3 has been determined. The metal is six-coordinate in a distorted octahedral geometry. The N-Zn-N intraligand bond angles range from 84.3(1) to 86.3(1)°. The Zn-N distances vary from 2.114(3) to 2.205(4)A˚. the geometry around the B atoms is tetrahedral. The angles N-B-N range from 106.8(3) to 111.0(3)°, the B-N bond distances vary from 1.528(6) to 1.564(5)A˚. Comparison is made with some related compounds.

Published
1996
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42. A convenient preparation of La2CuO4 from molecular precursors

Author

Simona Samaritani, Marcello Marelli, Alessio Di Giacomo, Daniela Belli Dell'Amico, Marco Lezzerini, Claudio Evangelisti, Luca Labella, Fabio Marchetti, and Lorenzo Falchi

Subjects
Metal ions in aqueous solution, Inorganic chemistry, chemistry.chemical_element, molecular precursors, mixed metal oxides, dialkylcarbamato complexes, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, Inorganic Chemistry, chemistry.chemical_compound, Pyridine, Materials Chemistry, Lanthanum, Physical and Theoretical Chemistry, dialkylcarbamato complexes, Heptane, Aqueous solution, Hydrolysis, Lanthanum cuprate, 021001 nanoscience & nanotechnology, Toluene, Copper, 0104 chemical sciences, mixed metal oxides, chemistry, molecular precursors, Mixed oxide, 0210 nano-technology
Abstract

Exhaustive hydrolysis of a mixture of [La4(CO3)(O2CNBu2)10] and [Cu(O2CNBu2)(py∗)2] (py∗ = 4-dimethylamino pyridine) in molar ratio 1/2 corresponding to a La/Cu molar ratio 2/1 was carried out in toluene at room temperature. The carbamato derivatives of lanthanum and copper can be easily prepared by extraction of the metal ions from aqueous solution into heptane by the NHBu2/CO2 system, according to a method previously reported. The copper precursor was selected amongst a number of derivatives in respect of its easy tractability. The tetragonal modification T′ of La2CuO4 was obtained by treatment at 600 °C of the intermediate mixed carbonate. The thermal treatment of T′-La2CuO4 at 850 °C, followed by cooling down to room temperature, afforded the orthorhombic modification of the mixed oxide.

Published
2017

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