Unprecedented calcium metalla-macrocycle having phosphinoselenoic amide and diphenylphosphinate in the coordination sphere

Naktode, K and Bhattacharjee, J and Das Gupta, S and Pada Nayek, H and Mallik, Bhabani Shankar and Panda, Tarun K (2014) Unprecedented calcium metalla-macrocycle having phosphinoselenoic amide and diphenylphosphinate in the coordination sphere. Journal of Inorganic and General Chemistry, 640 (5). pp. 994-999. ISSN 0044-2313

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An eight-membered calcium metalla-macrocycle of the composition [Ca{Ph 2P(Se)N(Ar)}{Ph2P(O)O}(THF)2]2 (2) (Ar = 2, 6-dimethylphenyl) can be isolated with a good yield by the reaction of neutral phosphinoselenoic amide [Ph2P(Se)NH(Ar)] (1) and calcium bis(trimethylsilyl)amides [Ca{N(SiMe3)2} 2(THF)2] in toluene followed by crystallization in air. The homoleptic calcium phosphinoselenoic amido complex of the composition [Ca{Ph2P(Se)N(Ar)}2(THF)2] (3) can also be obtained through two synthetic routes. In the first route, [Ca{N(SiMe 3)2}2(THF)2] is treated with phosphinoselenoic amide [Ph2P(Se)NH(Ar)] (1) at an ambient temperature followed by re-crystallization in an inert atmosphere to give complex 3 of high purity. In the second route, a one-pot reaction is carried out involving 1, calcium diiodide, CaI2, and potassium bis(trimethylsilyl)amide [K{N(SiMe3)2}] in toluene in an inert atmosphere. When complex 3 is treated with diphenylphosphinic acid in THF, compound 2 is also obtained with a good yield. Both complexes are confirmed using single-crystal X-ray diffraction analysis. The solid-state structure of complex 2 reveals an eight-membered macrocycle formed by two diphenylphosphinate groups and two calcium ions. In addition, a four-membered calcium metallacycle around each calcium atom is formed by the phosphinoselenoic amido ligand through coordination between the nitrogen and selenium atoms. In complex 3, the calcium atom is coordinated by two phosphinoselenoic amido groups and a direct metal selenium bond is observed

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IITH Creators:
IITH CreatorsORCiD
Panda, Tarun Khttp://orcid.org/0000-0003-0975-0118
Mallik, Bhabani Shankarhttp://orcid.org/0000-0001-9657-1497
Item Type: Article
Uncontrolled Keywords: Calcium; Chelating ligand; Macrocycle; N Se donor; Selenium
Subjects: Chemistry
Divisions: Department of Chemistry
Depositing User: Team Library
Date Deposited: 17 Dec 2014 04:02
Last Modified: 22 Jan 2019 10:21
URI: http://raiith.iith.ac.in/id/eprint/1161
Publisher URL: https://doi.org/10.1002/zaac.201300492
OA policy: http://www.sherpa.ac.uk/romeo/issn/0044-2313/
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