Polynuclear Cu(I) and Ag(I) Complexes of 1,3-Diisobutyl Thiourea, Synthesis, Crystal Structure and Antioxidant Potentials
, Adnan Shahzad 2,3, Ezzat Khan 2,4,*, Muhammad Nawaz Tahir 5, Gul Shahzada Khan 4, Amin ur Rashid 6 and Muhammad Said 2
Round 1
Reviewer 1 Report
After reading the manuscript, I have come to the conclusion that the work was rushed and would need proper attention for it to be resubmitted. The language is in some cases inappropriate and the content in most instances, not enough.
In my opinion this needs to be rejected at this stage
Some major concerns are listed below:
1. Normally when we describe complexes, it is prudent to mention, yes the nuclearity, but also what leads to it!! How many ligands and through what atoms?
2. Paragraph 1 of the introduction is jumbled up with different issues. Please try and keep paragraphs crisp and focused
3. Please give a detailed description of the experimental X-Ray analysis section. This is also seen in the anti-oxidant analysis section. The point of these sections normally is to help readers who would want to repeat such experiments. So much information is left out. What concentrations for example!!?? Also, the description of how Hirshfeld Surface Analyses were done is missing.
4. Is there any reason for not doing other important analyses such as elemental and mass spec? How clean are your samples? Sure you have crystal structure – but that’s just one out of many – it might not be representative of all that you have in the sample.
5. The crystallography section is poorly done. Some chronological ways need to be adopted in the discussion. E.g. coordinations and geometry first, then bond distances and angles then intermolecular interactions, etc.
6. Once again just one paragraph to describe 7 Figures. Does this mean the figures are not important (nothing much to say about them) in which case why have the figures? See some useful descriptions in a paper such as Biometals (2022) 35:363–394, https://doi.org/10.1007/s10534-022-00377-6
Comments for author File: 
Comments.pdf
Author Response
On the basis of reviewers' suggestions and observations, the article is passed through major revision. Pointwise reply to the reviewer comments is listed hereunder and all changes in the main file have been highlighted in yellow. The reply is detailed as below;
- Normally when we describe complexes, it is prudent to mention, yes the nuclearity, but also what leads to it!! How many ligands and through what atoms?
Reply: Discussion section of the paper is modified as suggested by the reviewer.
- Paragraph 1 of the introduction is jumbled up with different issues. Please try and keep paragraphs crisp and focused
Reply: The introduction part has been improved and organized as suggested.
- Please give a detailed description of the experimental X-Ray analysis section. This is also seen in the anti-oxidant analysis section. The point of these sections normally is to help readers who would want to repeat such experiments. So much information is left out. What concentrations for example!!?? Also, the description of how Hirshfeld Surface Analyses were done is missing.
Reply: Details of X-ray, antioxidant and Hirshfeld surface analysis are provided as suggested by the reviewer.
- Is there any reason for not doing other important analyses such as elemental and mass spec? How clean are your samples? Sure you have crystal structure – but that’s just one out of many – it might not be representative of all that you have in the sample.
Reply: The reactions of Ag salts contained some impurities which did not allow for collection of reliable results. The bulk purity was therefore not determined.
- The crystallography section is poorly done. Some chronological ways need to be adopted in the discussion. E.g. coordinations and geometry first, then bond distances and angles then intermolecular interactions, etc.
Reply: We have modified the order of discussion in light of the reviewer's comments.
- Once again just one paragraph to describe 7 Figures. Does this mean the figures are not important (nothing much to say about them) in which case why have the figures? See some useful descriptions in a paper such as Biometals (2022) 35:363–394, https://doi.org/10.1007/s10534-022-00377-6.
Reply: Figures have been described in a section before “Conclusion”, further 6 figures have been merged in to 3, in order to reduce the overall volume of the manuscript.
Reviewer 2 Report
This contribution deals with the preparation, structural characterization and biological study silver and gold coordination polymer.
The work is interesting and consequently, I recommend its publication in Inorganics after major revision.
I have major points that can be easily solved by the authors. They are listed hereunder.
In the experimental part the authors should detailed the synthetic procedure and characterization for the ligand.
The N-H···Cl interactions looks to be too long for this type of noncovalent interactions. The authors should better justify with literature papers.
For the ligand and complex the authors should perform the UV-VIS spectra in solid phase.
The authors should study the luminescence properties of the complexes.
Author Response
Comments of the reviewers were taken off positively and the paper is revised accordingly. All changes and modifications have been yellow highlighted.
They are enlisted as below;
1. In the experimental part the authors should detailed the synthetic procedure and characterization for the ligand.
Reply: Synthetic procedure and characterization of the ligand is included in the relevant part of the manuscript as required.
2. The N-H···Cl interactions look to be too long for this type of noncovalent interaction. The authors should better justify with literature papers.
Reply: We have added a justification and compared it with literature.
3. For the ligand and complex the authors should perform the UV-VIS spectra in solid phase. The authors should study the luminescence properties of the complexes.
Reply: We request the reviewer to relax this condition because these techniques are not available at our institute. We feel that the provided data are sufficient for confirmation of structural features of the complexes.
Thank you
Reviewer 3 Report
The manuscript from the group of Noor reports the preparation and crystal structures of three complexes containing Cu(I) or Ag(I) and diisobutylthiourea ligands. The complexes were prepared by standard methods and all three compounds were studied by X-ray diffraction. The datasets were collected at room temperature however, no checkcif files were included in the submission so that the quality of the structure determinations cannot be assessed. In the case of the Cu(I) complex IR spectroscopic data and a mass spectrum was also recorded. For the other two compounds no such data is given. For a publication in this journal the identity and purity of the bulk material should be established. The authors should obtain at least IR- and elemental analysis data for the three compounds and should include this in a supplementary file. The structure of the Cu(I)-iodo complex with the ligand has previously been reported (E. Kahn, J. Coord. Chem., 73, 2020, p.20). The authors should cite this work and incorporate this in their discussion of the structure of their CuCl-derivative. Overall, the manuscript can only be accepted once the major changes are made.
Author Response
The paper is revised in light of reviewers comments all changes and revisions have been yellow highlighted. Justifications are provided therein, checkcifs are also provided for consideration of the reviewer. In some cases, there are alerts, which have been justified within the file.
The article E. Kahn, J. Coord. Chem., 73, 2020, p.20 was not found however, help has been taken from the ref. E. Khan et al., Crystals 2021, 11, 989 which deals with CuI complex with the same ligand. We request the reviewer to correct us if the given paper is not studied.
Further, we request the reviewer to relax the condition of additional analysis, because purity of our complexes did not allow to collect reliable results for bulk material through these techniques. We feel that the provided data are sufficient for confirmation of structural features of complexes.
Thank you for your time and improving the manuscript.
Author Response File: Author Response.pdf
Round 2
Reviewer 2 Report
The paper can be published in present form.
Reviewer 3 Report
The authors have made a number of corrections and addition to the manuscript. I can therefore recommend acceptance in its present form.
