Synthesis, structural properties and reactivity of ruthenocene-based pincer Pd(ii) tetrahydroborate

Dalton Transactions : an International Journal of Inorganic Chemistry
Sergey V SafronovElena S Shubina

Abstract

Two novel ruthenocene-based pincer palladium tetrahydroborates were characterized by XRD, NMR and FTIR. The alcoholysis of Pd(ii) tetrahydroborate LPd(BH4) (L = κ3-[{2,5-(tBu2PCH2)2C5H2}Ru(C5H5)]) yields the dinuclear cationic Pd(ii) tetrahydroborate with the bridging BH4- ligand [(LPd)2(μ,η1,2:η1,2-BH4)]+. The bifurcate dihydrogen-bonded complexes are the active intermediates of the first proton transfer in the step-wise alcoholysis of LPd(BH4), yielding eventually [(LPd)2(μ,η1,2:η1,2-BH4)]+. According to the X-ray and DFT/M06 geometry analysis, the BH4- ligand in both palladium tetrahydroborates has a mixed coordination mode η1,2. The possibility of BH3-group abstraction from LPd(BH4) by an excess of organic base (THF, Py) with the formation of hydride LPdIIH is shown. This Pd(ii) hydride is a very reactive compound able to rapidly capture CO2 (ca. 15 min) converting into the formate complex LPdII(η1-OC(O)H). The hydrolysis of LPdH with subsequent CO2 insertion yields a hydrocarbonate complex LPdII(η1-OC(O)OH). The hydrocarbonate complex forms hydrogen-bonded dimers in the crystal due to hydrogen bonds between the OC(O)OH fragments.

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Citations

May 14, 2020·Molecules : a Journal of Synthetic Chemistry and Natural Product Chemistry·Sergey V SafronovElena S Shubina
Jul 8, 2020·Molecules : a Journal of Synthetic Chemistry and Natural Product Chemistry·Igor E GolubElena S Shubina
May 6, 2021·Inorganic Chemistry·Alexander Yu KostyukovichValentine P Ananikov

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