A low-cost, modular self-driving laboratory platform (RoboChem-Flex) is designed to democratize autonomous chemical experimentation. This platform combines customizable hardware with Python-based control software to make advanced Bayesian optimization more accessible. Photochemical, biocatalytic and thermal processes are demonstrated, showcasing a broad range of potential applications in both fully closed-loop and human-in-the-loop approaches.

An inorganic bicyclo[2.2.0]hex-1(4)-ene featuring a B₂N₂Al₂ scaffold is synthesized and crystallographically characterized, validating a highly strained bridgehead B=B bond between tricoordinate and pentacoordinate boron centres. Structural and computational analyses reveal pronounced geometric strain and distinct electronic distribution. Thermal fragmentation and K⁺ sequestration lead to divergent skeletal transformations.

The on-surface synthesis of two homologues of Clar’s goblet, C₆₂H₂₂ and C₇₆H₂₆, allows structure–property relationships to be established for these nanographenes. This work enables the rational design of spin-entangled polyradical systems with tunable spin numbers and enhanced resilience, opening up new possibilities for both fundamental research and quantum information technologies.

A paired electrolysis strategy enables efficient C–N coupling between lignin and various nitrogen sources (nitroaromatics and nitrogen oxides), paving the way for using renewable lignin to produce high-value nitrogen-containing aromatics.

Decarboxylative functionalization of aliphatic carboxylic acids is a powerful strategy in organic synthesis, yet most methods focus on decarboxylative monofunctionalization. Now, an electrophotocatalytic decarboxylative vicinal dichlorination of aliphatic carboxylic acids has been developed to enable late-stage decarboxylative difunctionalization of bioactive molecules and natural products.

Upgrading biomass-derived carbon-oxygenates into value-added chemicals has emerged as a promising strategy to reduce reliance on crude oil as a carbon source. Here a bioinspired design of molecular catalysts is reported to promote interfacial electron transfer, enabling efficient electrochemical C–C coupling of different aldehydes.

A hierarchically integrated 1D@3D covalent organic framework heterostructure is constructed via a one-pot synthesis, leading to the formation of an S-scheme heterojunction with a built-in electric field. The heterostructure has a photocatalytic H₂ evolution rate of 45.7 mmol g⁻¹ h⁻¹, outperforming both of the constituent single-component COFs.

Unactivated alkanes are difficult to use in enantioselective synthesis. Now a copper-catalysed radical S–C cross-coupling strategy enables their direct conversion into sulfur-stereogenic alkyl sulfilimines with high enantioselectivity. Two complementary methods using photo- and thermal chemistry combine hydrogen atom transfer with enantioselective copper-mediated S-stereocentre formation and chirality-transferring radical substitution.

Two-dimensional high-entropy materials are of interest for diverse applications, but low-temperature synthesis remains challenging. Now a topological anionic confinement strategy is reported in which MoO₄²⁻ tetrahedral scaffolds template two-dimensional high-entropy molybdates at 120 °C. Metastable clusters homogenize via a dissolution–regrowth process and then coalesce into well-defined nanoplates.

A methanol-based circular bioeconomy envisions the conversion of greenhouse gases into one-carbon compounds, which are subsequently utilized to enable sustainable biomanufacturing. Here a carbon metabolism reconfiguration strategy combined with adaptive laboratory evolution is adopted to obtain methylotrophic Saccharomyces cerevisiae capable of producing chondroitin sulfate A.

The combination of biocatalysts with electro- and photocatalysis provides a compelling route towards sustainable chemical and energy production driven by renewable electricity or light. We reflect on the challenges and opportunities associated with combining these technologies.

Sijia Dong, Assistant Professor at Northeastern University, talks to Nature Synthesis about the computational studies and design of photoenzymatic catalysts.

Youn-Suk Choi, Vice President of Technology at Samsung Advanced Institute of Technology, talks to Nature Synthesis about their use of self-driving laboratories for chemical research.