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A comprehensive educational strategy designed to make small-molecule crystallography more accessible for students at various academic levels is described. By integrating hands-on laboratory visits, structured courses and advanced application training, we cultivate a deep understanding of fundamental crystallographic concepts while fostering practical skills. This strategy also aims to inspire novice learners, building their confidence and interest in structural science. Our approach demystifies complex concepts through real-world examples and interactive case-learning modules, enabling students to proficiently apply crystallography in their research. The resulting educational impact is evident in numerous publications from undergraduates, scholarship awards to graduates and successful independent research projects, highlighting the effectiveness of our programme in inspiring the next generation of chemical crystallographers. 

Abstract Metalation of the polynucleating ligand^F,tbsLH₆(1,3,5‐C₆H₉(NC₆H₃−4‐F−2‐NSiMe₂^tBu)₃) with two equivalents of Zn(N(SiMe₃)₂)₂affords the dinuclear product (^F,tbsLH₂)Zn₂(1), which can be further deprotonated to yield (^F,tbsL)Zn₂Li₂(OEt₂)₄(2). Transmetalation of2with NiCl₂(py)₂yields the heterometallic, trinuclear cluster (^F,tbsL)Zn₂Ni(py) (3). Reduction of3with KC₈affords [KC₂₂₂][(^F,tbsL)Zn₂Ni] (4) which features a monovalent Ni centre. Addition of 1‐adamantyl azide to4generates the bridging μ³‐nitrenoid adduct [K(THF)₃][(^F,tbsL)Zn₂Ni(μ³‐NAd)] (5). EPR spectroscopy reveals that the anionic cluster possesses a doublet ground state (S=). Cyclic voltammetry of5reveals two fully reversible redox events. The dianionic nitrenoid [K₂(THF)₉][(^F,tbsL)Zn₂Ni(μ³‐NAd)] (6) was isolated and characterized while the neutral redox isomer was observed to undergo both intra‐ and intermolecular H‐atom abstraction processes. Ni K‐edge XAS studies suggest a divalent oxidation state for the Ni centres in both the monoanionic and dianionic [Zn₂Ni] nitrenoid complexes. However, DFT analysis suggests Ni‐borne oxidation for5.