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Synthesis and Characterization of [Mo 3 S 4 (NDABu)(HNDABu) 2 ] 3– and [Mo 3 S 4 (HNDAPr) 3 ] 2– Anions as Building Blocks for Organic–Inorganic Hybrid Solids
Author(s) -
Duval Sylvain,
Dumur Frédéric,
Guénée Laure,
Marrot Jérôme,
SimonnetJégat Corine,
Cadot Emmanuel
Publication year - 2013
Publication title -
european journal of inorganic chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.667
H-Index - 136
eISSN - 1099-0682
pISSN - 1434-1948
DOI - 10.1002/ejic.201201253
Subject(s) - iminodiacetic acid , chemistry , polyoxometalate , crystallography , infrared spectroscopy , ligand (biochemistry) , thermogravimetric analysis , spectroscopy , nuclear magnetic resonance spectroscopy , hybrid material , chalcogenide , gravimetric analysis , coordination complex , inorganic chemistry , stereochemistry , metal , chelation , organic chemistry , catalysis , biochemistry , physics , receptor , quantum mechanics
The polymetallic cation [Mo 3 S 4 (H 2 O) 9 ] 4+ was used as an inorganic precursor to generate new hybrid organic–inorganic chalcogenide clusters. Three organic compounds with flexible and hanging arms were synthesized and investigated as ligands for coordination complexes with the rigid and electroactive inorganic {Mo 3 S 4 } unit. Interestingly, the {Mo 3 S 4 } core formed hybrid structures with the flexible H 3 NDABu [ N ‐(3‐carboxypropyl)iminodiacetic acid] and H 3 NDAPr [ N ‐(2‐carboxyethyl)iminodiacetic acid] ligands, which were characterized by X‐ray crystallography. Surprisingly, no crystals were isolated, when the more rigid H 3 NDABn [ N ‐(4‐methoxycarbonylbenzyl)iminodiacetic acid] ligand was used. The two coordination complexes [Mo 3 S 4 (NDABu)(HNDABu) 2 ] 3– and [Mo 3 S 4 (HNDAPr) 3 ] 2– were characterized by X‐ray diffraction (XRD), IR spectroscopy, thermal gravimetric analysis (TGA), 1 H NMR spectroscopy, elemental analysis, and electrochemistry. The organic ligands H 3 NDABu, H 3 NDAPr, and H 3 NDABn were characterized by XRD, IR, HR mass, and 13 C and 1 H NMR spectroscopy. [Mo 3 S 4 (NDABu)(HNDABu) 2 ] 3– and [Mo 3 S 4 (HNDAPr) 3 ] 2– constitute promising preformed building blocks to generate new organic–inorganic hybrid molecular or extended materials.