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.

Synthesis of a highly reactive form of WO2Cl2, its conversion into nanocrystalline mono-hydrated WO3and coordination compounds with tetramethylurea

PICCINELLI, FABIO;
2016-01-01

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.
Nanocrystals; Transmission electron microscopy; X ray diffraction
File in questo prodotto:
File Dimensione Formato  
Dalton(2016)2.pdf

solo utenti autorizzati

Licenza: Accesso ristretto
Dimensione 1.4 MB
Formato Adobe PDF
1.4 MB Adobe PDF   Visualizza/Apri   Richiedi una copia

I documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.

Utilizza questo identificativo per citare o creare un link a questo documento: https://hdl.handle.net/11562/955450
Citazioni
  • ???jsp.display-item.citation.pmc??? ND
  • Scopus 7
  • ???jsp.display-item.citation.isi??? 6
social impact