A modular programmable inorganic cluster discovery robot for the discovery and synthesis of polyoxometalates

DOI: 10.1021/acscentsci.0c00415

Authors: Daniel S. Salley (The University of Glasgow) , Graham Keenan (The University of Glasgow) , De-liang Long (The University of Glasgow) , Nicola L. Bell (The University of Glasgow) , Leroy Cronin (The University of Glasgow)
Co-authored by industrial partner: No

Type: Journal Paper
Journal: Acs Central Science

State: Published (Approved)
Published: August 2020
Diamond Proposal Number(s): 22214

Abstract: The exploration of complex multicomponent chemical reactions leading to new clusters, where discovery requires both molecular self-assembly and crystallization, is a major challenge. This is because the systematic approach required for an experimental search is limited when the number of parameters in a chemical space becomes too large, restricting both exploration and reproducibility. Herein, we present a synthetic strategy to systematically search a very large set of potential reactions, using an inexpensive, high-throughput platform that is modular in terms of both hardware and software and is capable of running multiple reactions with in-line analysis, for the automation of inorganic and materials chemistry. The platform has been used to explore several inorganic chemical spaces to discover new and reproduce known tungsten-based, mixed transition-metal polyoxometalate clusters, giving a digital code that allows the easy repeat synthesis of the clusters. Among the many species identified in this work, the most significant is the discovery of a novel, purely inorganic W24FeIII–superoxide cluster formed under ambient conditions. The modular wheel platform was employed to undertake two chemical space explorations, producing compounds 1–4: (C2H8N)10Na2[H6Fe(O2)W24O82] (1, {W24Fe}), (C2H8N)72Na16[H16Co8W200O660(H2O)40] (2, {W200Co8}), (C2H8N)72Na16[H16Ni8W200O660(H2O)40] (3, {W200Ni8}), and (C2H8N)14[H26W34V4O130] (4, {W34V4}), along with many other known species, such as simple Keggin clusters and 1D {W11M2+} chains.

Journal Keywords: Crystals; Crystallization; Anions; Cluster chemistry; Software

Subject Areas: Information and Communication Technology, Chemistry


Instruments: I19-Small Molecule Single Crystal Diffraction