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Paper published in Eur. J. Inorg. Chem.

New Heterobimetallic Alkoxides [CdIIMV(OiPr)7]2 (M = Nb, Ta) as Potential Precursors to Pyrochlore Cd2M2O7

 

Rishabh Garg, Corinna Hegemann, Sanjay Mathur

 

Abstract

Attempts to synthesize Cd-M (M= Nb, Ta) heterobimetallic complexes via salt metathesis reaction resulted in an unexpected structural motif [I2CdII2MV(OiPr)7]2 (M = Nb (2), Ta (3)). 1H NMR and multinuclear NMR analyses revealed the co-existence of multiple products in solution. The donor solvents influenced the formation of different intermediate species in solution that was proven by 113Cd NMR data. The isolation of trimetallic [I2Cd{Ta(OiPr)6}K(HOiPr)2]4 (4) and the adduct [I2CdTa(OiPr)5(THF)]5 provided an insight into the reaction mechanism. By exploiting the Lewis acidic nature of cadmium alkoxide different compounds could be synthesized and thoroughly characterized by spectroscopic methods and single crystal X-ray diffraction studies. New heterobimetallic derivatives with the formula [CdIIMV(OiPr)7]2 (M = Nb (6), Ta (7)) produced pyrochlore phases from an amorphous ceramic homogenate indicating their potential as single-source precursors that was confirmed by TG-DTA analysis, which showed that complexes 6 and 7 undergo facile two step thermal decomposition at 600°C to produce Cd2Nb2O7 and Cd2Ta2O7, respectively. Temperature variable X-ray diffraction analysis of 6 additionally proved the formation of crystalline Cd2Nb2O7 phase.

Eur. J. Inorg. Chem. 2017, accepted.

Öffnet externen Link in neuem FensterDOI: 10.1002/ejic.201700331.

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