Issue 39, 2016

Synthesis of a highly reactive form of WO2Cl2, its conversion into nanocrystalline mono-hydrated WO3 and coordination compounds with tetramethylurea

Abstract

A new form of WO2Cl2 was obtained by modification of a literature procedure. Both the newly prepared WO2Cl2 and the commercial yellow WO2Cl2 exhibited an orthorhombic structure (powder X-ray diffraction, P-XRD), and their air exposure at room temperature afforded light green and lemon yellow WO3·H2O (orthorhombic phase), respectively. These materials were characterized by P-XRD, high-resolution transmission electron microscopy (HR-TEM) and scanning transmission electron microscopy (S-TEM). The analyses revealed the nanocrystalline nature of light green WO3·H2O, and the prevalent amorphism of lemon yellow WO3·H2O. The reactions of grey WO2Cl2 with one and two equivalents of tetramethylurea (tmu), in CH2Cl2 at room temperature, led to the isolation of the trinuclear complex [WO2Cl2(tmu)]3, 1 (45% yield), and the mononuclear one WO2Cl2(tmu)2, 2 (64%), respectively. Compounds 1 and 2 were fully characterized by analytical and spectroscopic methods, single crystal X-ray diffraction (SC-XRD) and DFT calculations.

Graphical abstract: Synthesis of a highly reactive form of WO2Cl2, its conversion into nanocrystalline mono-hydrated WO3 and coordination compounds with tetramethylurea

Supplementary files

Article information

Article type
Paper
Submitted
28 Jul 2016
Accepted
19 Aug 2016
First published
06 Sep 2016

Dalton Trans., 2016,45, 15342-15349

Synthesis of a highly reactive form of WO2Cl2, its conversion into nanocrystalline mono-hydrated WO3 and coordination compounds with tetramethylurea

M. Bortoluzzi, C. Evangelisti, F. Marchetti, G. Pampaloni, F. Piccinelli and S. Zacchini, Dalton Trans., 2016, 45, 15342 DOI: 10.1039/C6DT02997C

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