Content of review 1, reviewed on May 19, 2025

The manuscript by Nicholson, Hanton and Macreadie presents a series of structures using a relatively unusual ligand which incorporates end groups that either chelate or tend towards bridging (and hence towards extended structures). The structures are described in exhaustive detail, perhaps a little too much even (although I am not suggesting they be cut back). The gas sorption results are not spectacular, however, on the basis of ligand novelty, and therefore novelty of the resulting structures, I think that this will be of interest to the readers of CrystEngComm and I recommend acceptance subject to the authors considering the points below.
- "All samples were obtained as bulk crystalline material", although the Cu one is a mixture of polymorphs. Philosophically, is that a bulk sample?
- The Cu structure exhibits deterioration in diffraction with temperature. Two polymorphs exist. What happens to the cells of the alpha/beta polymorphs on cooling, is there any evidence for conversion to explain the poor diffraction rather than invoking disorder?
- I'm not sure why well-ordered solvent would be removed "for consistency". It can be removed for pore space analysis, but in terms of structural analysis should be included if found (it is going into the CSD and should be as correct as possible rather than incorrect for convenience).
- Channel measurements to two decimal places is unusual for this sort of work. Is this atom-atom or does it include vdW surfaces (i.e. geometric measurement or accessible volume)?
- "(Error! Reference source not found.)" is not a standard referencing style but seems to have been referenced a couple of times.
- Reference 22 is simply "Agilent".
- Why only two PXRD patterns if all samples were bulk crystals? I know a couple of PXRD people that would not like to see a comparison, but would rather a fit of the data (although this referee is not insisting, just a comment for future reference having been told off for this myself).

Source

    © 2025 the Reviewer.

References

    J., N. E., R., H. L., K., M. L. 2025. Metal ion influence on paddlewheel SBUs formed from a mixed donor multidentate ligand and the consequences for MOF structures. CrystEngComm.