Referee: 2
6. There are major issues with the crystal structure of each compound. As can be seen in the checkcif reports, data completeness for 1 and 3 is only 86% and that for 2 is 92%, which is not acceptable. In order to get this number close to 99%, authors need to refine the structures with theta-max to 25 degree. Furthermore, the structure of 3 is not completely solved with so high residual electron densities. In case of compound 2, moiety formula includes the lattice water molecule; should this not be shown as a separate entity based on the formula written for it? For 2, Alert levels B and C should have author responses. Also, in Table S8, Z is shown different from what is correct in cif file (4). For 3, the calculated moiety and sum formula are shown without the hydrogens in cations. Authors must explain the reasons for not including such hydrogens in the refinement. Authors should have seen this disaster in Alerts B and C.

Referee: 3

Recommendation: Major Revision

Comments:
There are 3 Structures in this paper. We examined this file: 1949330-1949332

**exp_20383** (CCDC 1949330)

There is a large residual L.S. shift of 0.213 -- why? There appears to be no reason, other than that not enough cycles of L.S. have been run -- 6 cycles will do the trick.

**exp_15991** (CCDC 1949331)

This structure reports spurious bonds:

Distance (K1-C2): 3.465(7)

It also reports strangely long O-H bond distances:

    Distance (O1W-H1WB): 1.0846
    Distance (O1W-H1WA): 1.0824

If these are adjusted for neutron distances, then *all* X-H distances should be adjusted, but they are not.

**exp_20567** (CCDC 1949332)

There are two cyanide ions in the solvent sphere -- but these are not mentioned in the text. Where do they come from?

If you are not particularly interested in the solvent sphere, I recommend using a solvent mask for these moieties and concentrate on getting the best model of the main molecule.

I attach a refinement with an R1 of 4.17% (down from 8.22%). I have masked everything in the solvent sphere (and assumed it is all water) and have modelled the disorder that is obvious in one part of the main molecule. Please have a look at this structure and take it from there.

Please consider our comments carefully.

Please make sure that all cited geometrical parameters (bond lengths, bond angles, distances between planes etc) are quoted with their e.s.d. values. This also includes any values printed on images.

In the MS, please provide at least one structural drawing showing ADPs of each structure. From these images, any disorder should be visible -- and the nature of the actual molecule must be easily discernible.

Please use CheckCif as a guide in the final preparation of these structures. There should be no CheckCif A or B alerts remaining, and if any of them do, you must provide relevant and meaningful vrf entries.

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