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Synthesis and Structural Characterization of Non‐Homoleptic Carbamato Complexes of V V and W VI and Their Facile Implantation onto Silica Surfaces
Author(s) -
Bresciani Giulio,
Bortoluzzi Marco,
Zacchini Stefano,
Gabbani Alessio,
Pineider Francesco,
Marchetti Fabio,
Pampaloni Guido
Publication year - 2018
Publication title -
european journal of inorganic chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.667
H-Index - 136
eISSN - 1099-0682
pISSN - 1434-1948
DOI - 10.1002/ejic.201701260
Subject(s) - chemistry , homoleptic , spectroscopy , nuclear magnetic resonance spectroscopy , diethylamine , inorganic chemistry , infrared spectroscopy , crystallography , vanadium , ionic bonding , reactivity (psychology) , stoichiometry , amide , nuclear chemistry , metal , stereochemistry , organic chemistry , ion , physics , quantum mechanics , medicine , alternative medicine , pathology
The vanadium(V) amido‐carbamato derivatives VO(NR 2 )(O 2 CNR 2 ) 2 (R = Me, 1 ; Et, 2 ) are obtained by the reaction of VOCl 3 with preformed carbamato species (ammonium or sodium carbamates). The synthesis of an ionic ammonium chlorido‐amide of W VI , 3 , is performed using WOCl 4 and diethylamine as precursors. Moreover, the reactivity of 3 with CO 2 is investigated. Mixed W VI chlorido‐carbamato compounds, 4 and 5 , are obtained by the reaction of WOCl 4 with stoichiometric amounts of sodium diethylcarbamate. All of the products are characterized by analytical and spectroscopic methods (IR spectroscopy, multinuclear NMR spectroscopy) and by X‐ray diffraction in the cases of 3 and 4 . DFT calculations are useful to elucidate the structures of the compounds and to give insight into the various reaction pathways. The combination of 2 or 5 with amorphous silica gives solid materials, which are characterized by inductively coupled plasma‐optical emission spectroscopy (ICP‐OES) and energy dispersive X‐ray spectroscopy (EDS) coupled to scanning electron microscopy (SEM).