4.7 Article

Palladium(II) complexes of pyrazolated thio/selenoethers: syntheses, structures, single source precursors of Pd4Se and PdSe nano-particles and potential for catalyzing Suzuki-Miyaura coupling

Journal

DALTON TRANSACTIONS
Volume 42, Issue 11, Pages 3908-3918

Publisher

ROYAL SOC CHEMISTRY
DOI: 10.1039/c2dt31975f

Keywords

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Funding

  1. Council of Scientific and Industrial Research (CSIR), New Delhi, India [01(2421)10/EMR-II]
  2. JRF/SRF
  3. Department of Science and Technology (India) [SR/WOS-A/CS-22/2009, SR/S1/IC-40/2010]
  4. IIT Delhi

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The reactions of 4-bromo-1-(2-chloroethyl)-1H-pyrazole prepared from 4-bromopyrazole with the in situ generated PhSNa, PhSeNa, Na2S and Na2Se have resulted in thio/selenoether ligands L1-L4 respectively. The complexes [PdL1/L2Cl(2)](1-2) and [PdL3/L4Cl]BF4 (3-4) of these ligands have been synthesized by reacting them with [PdCl2(CH3CN)(2)] in CH3CN at 70 degrees C. The L1-L4 and their complexes (1-4) have been characterized with spectroscopic techniques viz. H-1, C-13{H-1} and Se-77{H-1} NMR, IR and HR-MS. Single crystal structures of 1-4 determined by X-ray diffraction reveal nearly square planar geometry around Pd in each case. Thermally stable, moisture/air insensitive complexes 1-4 have been found to be efficient pre-catalysts for Suzuki-Miyaura coupling reactions (yield up to 96% in 2 h). Nano-particles (NPs) (size similar to 3-19 nm) were formed in the beginning of these reactions. They are composed of Pd and S or Se with more % of Pd. These NPs also catalyze Suzuki coupling and appear to play an important role in catalysis. Single source one pot synthesis of Pd4Se and PdSe NPs (size ranges similar to 8-26 nm), capped with trioctylphosphine (TOP), has been developed by thermolysis of 2 and 4 at 200-250 degrees C in TOP. HR-TEM, SEM, SEM-EDX and powder XRD have been used to authenticate these nano-particles. The NPs of PdP2 are formed when attempts were made to prepare nano-sized phases of palladium-sulfide by thermolysis of 1 and 3 in TOP.

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