Mechanochemical synthesis and characterization of kinetically and thermodynamically stable polymorphs of a lead(II) coordination polymer

摘要

1 alpha polymorph of [Pb(mu-Cl)(2)(mu-bipy)](infinity) (bipy = 4,4'-bipyridine) was synthesized by branch tube method. It was found that one of the ways to synthesize of 1 beta is grinding of 1 alpha. Mechanochemical reactions of compounds [Pb(NO2)(2)(4,4'-bipy)](n) (2), [Pb(NO3)(SCN)(4,4'-bipy)](n) (3), [Pb-2(NO3)(4)(4,4'-bipy)](n) (4) and [Pb-2(SCN)(4)(4,4'-bipy)](n) (5) with KCl, are other ways to synthesize of 1 beta by solid-state reactions. Synthesis of compounds 2-5 from 1 alpha and 1 beta, was not possible but synthesis of [Pb(Br)(2)(4,4'-bipy)](n) (6) and [Pb(I)(2)(4,4'-bipy)] n (7) from 1 alpha and 1 beta was done successfully. In addition, the morphology of initial precursor has direct influence on morphology of resulting calcined material. (C) 2015 Elsevier B.V. All rights reserved.