Two new three-dimensional extended framework complexes [Pb3(µ2-XBPP)3(H2O)] 1 and [Pb5(µ3-O)(µ2-XBPP)4(H2O)] 5 have been synthesized using the linker ligand 4-α,α'-xylendiylbis(phenylphosphinato), XPBB, via pH control of the reaction medium. From single crystals of 1, single crystals of the anhydrous [Pb(µ2-XBPP)] (3), the intermediate quarter rehydrated [Pb4(XBPP)4(H2O)] 3 and the half hydrated [Pb2(XBPP)2(H2O)] 4 have been synthesized and their crystal structures determined. Crystals of 5 have been reversibly be dehydrated to [Pb5(μ3-O)(XBPP)4] 6. The dehydration/rehydration was confirmed with X-ray powder diffraction. Solid state 31P CP-MAS NMR of 1, 3, 5 and 7 have been determined. Theoretical magnetic shielding values calculated based on the crystal structures using the plane wave method were satisfactory. Total chemical shielding constants have good correlation with experimental and the observed number of peaks agreed with the measured in SCXRD. Isothermal gas adsorption studies with N2, CO2 and H2O on 3 and 6 were carried out at low pressure (&lt; 1 atm). The observed adsorption of water agreed with the expected to the expected for reactions of hydration and dehydration. Isotherms of N2 and CO2 did not show significant adsorption until 1 atm. A preliminary powder X-ray diffraction kinetic study of the hydration process from 3 to 1 to 4 was performed.

Water dynamics in three-dimensional extended lead(II) structures: Multiple single-crystal-to-single-crystal transformations

253rd National Meeting (2017)

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