Abstract
Polymeric (CuStBu)∞ (1) undergoes reaction with trialkylphosphines to form the cuprous thiolato phosphine complexes [(CuS tBu)4(PR3)2] (R = Me (2a), Et (2b)) in high yield. In contrast to 2b, in polar solvents (CH2Cl 2, tetrahydrofuran), complex 2a is in equilibrium with the ion pair Cu(PMe3)4 +Cu5(StBu) 6 - (3) and other species such as (CuStBu) x(PMe3)2 (x = 6 (4), 8 (5)). Clusters 2-4 were isolated analytically pure and fully characterized in solution by multinuclear nuclear magnetic resonance (NMR) spectroscopy and in the solid state by single-crystal X-ray diffraction and 31P magic angle spinning NMR spectroscopy, while the structure of compound 5 was determined by single-crystal X-ray diffraction. Thermal analysis (TGA/DTA) and examination of the volatile byproducts suggest stepwise phosphine loss and C-S bond cleavage by isobutene elimination as the predominant thermolysis pathways of this new Cu2S precursor class.
| Original language | English |
|---|---|
| Pages (from-to) | 2768-2779 |
| Number of pages | 12 |
| Journal | Chemistry of Materials |
| Volume | 19 |
| Issue number | 11 |
| DOIs | |
| Publication status | Published - May 29 2007 |
Fingerprint
ASJC Scopus subject areas
- Materials Chemistry
- Materials Science(all)
Cite this
Copper(I) tert-butylthiolato clusters as single-source precursors for high-quality chalcocite thin films : Precursor chemistry in solution and the solid state. / Schneider, Sven; Dzudza, Alma; Raudaschl-Sieber, Gabriele; Marks, Tobin J.
In: Chemistry of Materials, Vol. 19, No. 11, 29.05.2007, p. 2768-2779.Research output: Contribution to journal › Article
}
TY - JOUR
T1 - Copper(I) tert-butylthiolato clusters as single-source precursors for high-quality chalcocite thin films
T2 - Precursor chemistry in solution and the solid state
AU - Schneider, Sven
AU - Dzudza, Alma
AU - Raudaschl-Sieber, Gabriele
AU - Marks, Tobin J
PY - 2007/5/29
Y1 - 2007/5/29
N2 - Polymeric (CuStBu)∞ (1) undergoes reaction with trialkylphosphines to form the cuprous thiolato phosphine complexes [(CuS tBu)4(PR3)2] (R = Me (2a), Et (2b)) in high yield. In contrast to 2b, in polar solvents (CH2Cl 2, tetrahydrofuran), complex 2a is in equilibrium with the ion pair Cu(PMe3)4 +Cu5(StBu) 6 - (3) and other species such as (CuStBu) x(PMe3)2 (x = 6 (4), 8 (5)). Clusters 2-4 were isolated analytically pure and fully characterized in solution by multinuclear nuclear magnetic resonance (NMR) spectroscopy and in the solid state by single-crystal X-ray diffraction and 31P magic angle spinning NMR spectroscopy, while the structure of compound 5 was determined by single-crystal X-ray diffraction. Thermal analysis (TGA/DTA) and examination of the volatile byproducts suggest stepwise phosphine loss and C-S bond cleavage by isobutene elimination as the predominant thermolysis pathways of this new Cu2S precursor class.
AB - Polymeric (CuStBu)∞ (1) undergoes reaction with trialkylphosphines to form the cuprous thiolato phosphine complexes [(CuS tBu)4(PR3)2] (R = Me (2a), Et (2b)) in high yield. In contrast to 2b, in polar solvents (CH2Cl 2, tetrahydrofuran), complex 2a is in equilibrium with the ion pair Cu(PMe3)4 +Cu5(StBu) 6 - (3) and other species such as (CuStBu) x(PMe3)2 (x = 6 (4), 8 (5)). Clusters 2-4 were isolated analytically pure and fully characterized in solution by multinuclear nuclear magnetic resonance (NMR) spectroscopy and in the solid state by single-crystal X-ray diffraction and 31P magic angle spinning NMR spectroscopy, while the structure of compound 5 was determined by single-crystal X-ray diffraction. Thermal analysis (TGA/DTA) and examination of the volatile byproducts suggest stepwise phosphine loss and C-S bond cleavage by isobutene elimination as the predominant thermolysis pathways of this new Cu2S precursor class.
UR - http://www.scopus.com/inward/record.url?scp=34250163945&partnerID=8YFLogxK
UR - http://www.scopus.com/inward/citedby.url?scp=34250163945&partnerID=8YFLogxK
U2 - 10.1021/cm0700504
DO - 10.1021/cm0700504
M3 - Article
VL - 19
SP - 2768
EP - 2779
JO - Chemistry of Materials
JF - Chemistry of Materials
SN - 0897-4756
IS - 11
ER -