N-(Chalcogen)phosphorylated (chalcogen)ureas of zinc and cadmium(ii): SSPs for group 12-16 thin filmsElectronic supplementary information (ESI) available: TGA/DSC analyses of all complexes (Fig. S6). CCDC 986590-986594 for 1, 7, 8, 11 and 15. Details of the X-ray structure analyses (Table S1). XRPD patterns of ZnO obtained from pyrolysis of 8 (Fig. S2) and of the CdO and CdS mixture obtained from pyrolysis of 13 (Fig. S3). GAXRD pattern of CdS film obtained from 13 (Fig. S4). SEM images of CdS t
The bis-chelates of zinc ( 7-11 ) and cadmium ( 12-17 ) with general formula [M{R 2 P(X)NC(Y)NR′-η 2 -X,Y} 2 ] were obtained from ligands 1-6 ( i Pr 2 P(X)NHC(Y)NC 4 H 8 : 1 : X = S, Y = S; 2 : X = S, Y = O; 3 : X = O, Y = S; 4 : X = S, Y = Se, 5 : X = Se, Y = S; Ph 2 P(X)NC(Y)NC 5 H 10 : 6 : X = S,...
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| Main Authors | , , , , |
|---|---|
| Format | Journal Article |
| Language | English |
| Published |
16.09.2014
|
| Online Access | Get full text |
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| Summary: | The bis-chelates of zinc (
7-11
) and cadmium (
12-17
) with general formula [M{R
2
P(X)NC(Y)NR′-η
2
-X,Y}
2
] were obtained from ligands
1-6
(
i
Pr
2
P(X)NHC(Y)NC
4
H
8
:
1
: X = S, Y = S;
2
: X = S, Y = O;
3
: X = O, Y = S;
4
: X = S, Y = Se,
5
: X = Se, Y = S; Ph
2
P(X)NC(Y)NC
5
H
10
:
6
: X = S, Y = S).
4
and cadmium complex
15
are the first examples of this ligand system with carbon-bonded selenium as a donor atom. All the compounds were characterized by FTIR and multi-nuclear NMR spectroscopies, and microanalysis. The molecular structures of complexes
1
,
7
,
8
,
11
, and
15
were elucidated by single crystal X-ray diffraction. Thermal gravimetric analysis (TGA) and thermolysis experiments were carried out for the metal complexes. Selected pyrolysis residues were analyzed by scanning electron microscopy-energy dispersive spectroscopy (SEM-EDS) and X-ray powder diffraction (XRPD). Remarkably, cadmium complex
13
gave a few crystals of CdS encrusted on the surface of CdO. Preliminary studies using the O,S-mixed cadmium complexes (
13
and
14
) as single source precursors (SSPs) were carried out for the deposition of thin films
via
AA-CVD. The results show that CdS films are obtained from both complexes, and in the case of
14
(the complex containing a P&z.dbd;O fragment), persistent high carbon content was detected.
The bis-chelates [M{R
2
P(X)NC(Y)NR′-η
2
-X,Y}
2
] were evaluated as suitable SSPs for the synthesis of metal chalcogenide thin films by AA-CVD. |
|---|---|
| Bibliography: | 11 10.1039/c4nj00482e 13 14 (Fig. S5a and b). For ESI and crystallographic data in CIF or other electronic format see DOI 15 for 986590-986594 , (Fig. S2) and of the CdO and CdS mixture obtained from pyrolysis of 1 Electronic supplementary information (ESI) available: TGA/DSC analyses of all complexes (Fig. S6). CCDC (Fig. S3). GAXRD pattern of CdS film obtained from and 7 8 (Fig. S4). SEM images of CdS thin film obtained from Details of the X-ray structure analyses (Table S1). XRPD patterns of ZnO obtained from pyrolysis of |
| ISSN: | 1144-0546 1369-9261 |
| DOI: | 10.1039/c4nj00482e |