Abstract
We report a complex system of heteroleptic coordination cages based on the combination of four bis-monodentate ligands whose backbones only slightly differ in shape and length. cis-[Pd2L2L'2] assemblies cleanly form after addition of PdII cations to a 1 : 1 mixture of two shape-complementary ligands, each. When three or even all four ligands are used in combination, the unambiguous discrimination of all individual species in the product mixture becomes difficult by conventional NMR spectroscopic and mass spectrometric methods. Due to steric constraints, the system is restricted to the formation of ten different coordination cages in total, two of which are isomeric. We show that high-resolution trapped ion mobility mass spectrometry (TIMS) allows the clear differentiation of all ten species. Observed size trends could be readily reproduced by the calculation of theoretical values for collisional cross sections (CCS) from geometry-optimized models.
Highlights
Metal-mediated self-assembly of organic building blocks into larger supramolecules has yielded a plethora of structures over the last decades.[1]
Most reported examples have usually been based on one type of organic ligand, each, reducing synthetic effort, avoiding the formation of complicated reaction mixtures and simplifying analytical characterization
While this approach has produced a large number of systems with unique structures and functions, for example lantern-shaped, tetrahedral, octahedral, cubic cages and large spheres,[3] the restriction to a single ligand component puts a limit on the achievable architectural design and functionality
Summary
Metal-mediated self-assembly of organic building blocks into larger supramolecules has yielded a plethora of structures over the last decades.[1] Amongst these, coordination cages take a special role due to their guest recognition capabilities and potential to serve as nanoscopic reaction containers.[2] Most reported examples have usually been based on one type of organic ligand, each, reducing synthetic effort, avoiding the formation of complicated reaction mixtures and simplifying analytical characterization. Ion mobility spectrometry (IMS), usually coupled with high-resolution mass spectrometry, is gradually turning into a popular addition to the structural analysis toolbox used 11070 | Dalton Trans., 2019, 48, 11070–11075
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