M. Trivedi et al. / Inorganic Chemistry Communications 14 (2011) 920–924
923
We also thank the Heads, Department of Chemistry, University of Delhi
and University of Lucknow, India for their support.
Appendix A. Supplementary material
The crystallographic data in CIF format has been deposited with
CCDC (CCDC deposition number is 806962). This data can be obtained
the Cambridge Crystallographic Data Centre, 12, Union Road, Cambridge
CB2 1EZ, UK; fax: (internet.) +44-1223/336-033; E-mail: deposit@ccdc.
Supplementary data associated with this article can be found, in
the online version, at doi:10.1016/j.inoche.2011.03.031.
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Fig. 4. TGA and DSC profiles of [Cu(O2CCH3)2(CH3CONH2)]2 recorded under an air flow.
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[12] [Cu(O2CCH3)2(CH3CONH2)]2 (1): CuCN (1 mmol), ammonia solution (15 mL), few
drops of glacial acetic acid and 1, 3, 5-Trizine (1 mmol) were taken in a hydrogen
bomb and hydrothermally heated at 180°C for 3 days. The bomb was then slowly
cooled at a rate of 5°C at room temperature to obtain green coloured crystal. Yield:
(0.385 g, 80%). Anal. Calc. for C12H22N2O10Cu2: C, 29.94; H, 4.57; N, 5.82. Found: C,
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and acetamide was reacted in equimolar ratio in methanol.
Fig. 5. Powder X-ray diffractogram of Tetrakis-μ-acetato-bis(acetamido)dicopper(II)
[Cu(O2CCH3)2(CH3CONH2)]2 (1): (a) Simulated; (b) at 210 °C for 6 h; (c) at 500 °C for
15 h.
This indicates that complex have lost the axial acetamide ligand which
seems to be reasonable. The pattern recorded for product obtained at
500 °C (Fig. 5c) matches with CuO, having lattice parameters a=4.561
(5) Å, b=3.379(1) Å and c=5.1183(4) Å (PDF 892530) quite well.
In this work we have presented physico-chemical properties of the
Tetrakis-μ-acetato-bis(acetamido)dicopper(II) [Cu(O2CCH3)2(CH3-
CONH2)]2 (1) by experimental–computational approach. The complex
was volatile and could be sublimed at T=180 ° C. In addition, TGA/DSC
analyses and PXRD data evidenced the occurrence of a clean vaporization
process without premature side decompositions, and of clear PXRD
pattern dominated by the loss of the acetamido ligands. A key point of the
present investigation was the integrated use of a theoretical and
experimental approach, enabling us to validate and integrate the obtained
results and to gain a detailed insight into the structure, bonding and
chemical behavior of the target compound. Taken together, these results
make the [Cu(O2CCH3)2CH3CONH2]2 complex an attractive candidate for a
CVD precursor for copper based thin films and nanosystems. The results of
such investigations will be the focus for our future studies.
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(NBO) wavefunction analysis for the optimized structures was performed with NBO
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Acknowledgements
M.T. acknowledges the financial support from University Grants
Commission, New Delhi (Grant No. F.4-2/2006(BSR)/13-76/2008(BSR)).