Combined Approach of Mechanochemistry and Electron Crystallography for the Discovery of 1D and 2D Coordination Polymers

Danilo Marchetti,Enrico Dalcanale,Chiara Massera,Mauro Gemmi,Arianna E. Lanza,Alessandro Pedrini,Lara Righi,Francesca Guagnini

doi:10.1021/acs.cgd.1c01058

Abstract

Mechanochemical synthesis is an attractive preparative method that combines a green approach with versatility, efficiency, and rapidity of reaction. However, it often yields microcrystalline materials, and their small crystal size is a major hindrance to structure elucidation with conventional single-crystal or powder X-ray diffraction methods. This work presents the novel approach of combining mechanochemistry with electron diffraction techniques to elucidate the crystal structure of metal–organic compounds of zinc(II) and copper(II) with 2,6-pyridinedicarboxylic acid and 4,4′-bipyridine.

Highlights

It often yields microcrystalline materials, and their small crystal size is a major hindrance to structure elucidation with conventional single-crystal or powder X-ray diffraction methods
Mechanochemical synthesis can promote the formation of products, polymorphs, and topologies different from what is obtained with solution methods.[7,8]
Conventional single-crystal X-ray diffraction (SCXRD) on the crude product is not applicable, and powder X-ray diffraction (PXRD) methods are the characterization of choice

Summary

Introduction

It often yields microcrystalline materials, and their small crystal size is a major hindrance to structure elucidation with conventional single-crystal or powder X-ray diffraction methods. We have applied this novel combined strategy for the synthesis and characterization of metal−organic compounds, featuring zinc(II) and copper(II) as metal centers and 2,6pyridinedicarboxylic acid (H2PDC) and 4,4′-bipyridine (bipy) as organic ligands.

Results

Conclusion