This work presents the first-ever structure of an ion-beam milled MOF determined by MicroED. It demonstrates that ion beam milling can be effectively used together with MicroED on small molecules and MOFs. By employing thin lamellae extracted from microcrystals that are conventionally challenging to study-either too small for X-ray diffraction or too thick for traditional electron diffraction-this approach promises to overcome existing methodological constraints when using electron diffraction for structure determination in the field of chemical crystallography and facilitate structure determination across a wider range of materials and sizes.