Synthesis, Structural Characterization, and Biological Activities of Organically Templated Cobalt Phosphite (C4H14N2)[Co(H2PO3)4]∙2H2O

Round 1

Reviewer 1 Report

The paper is well written and relates about a new hybrid phosphide, its structural characterization (X-ray, FTIR, TGA), and biological activity.

There are some issues to be better fixed, mostly regarding X-ray crystal structure.

Figures 1-2-3 are low-quality, as well as Figure 4 needs to be revised.

The atomic labelling of Table 2 needs to be better fixed, according to my notes. Tables 1 and 3 need to be revised.

Once all required changes are made up, I will be able to consider the paper worthy of publication on Sci.

Comments for author File: Comments.pdf

Author Response

The paper is well written and relates about a new hybrid phosphide, its structural characterization (X-ray, FTIR, TGA), and biological activity. There are some issues to be better fixed, mostly regarding X-ray crystal structure. Figures 1-2-3 are low-quality, as well as Figure 4 needs to be revised. The atomic labelling of Table 2 needs to be better fixed, according to my notes. Tables 1 and 3 need to be revised. Once all required changes are made up, I will be able to consider the paper worthy of publication on Sci. Sorry, we did our best to draw the structures with Diamond we currently use in the group. For the tables, they can be found as CIF deposited data with both content and form the most accurate in the database.

Reviewer 2 Report

The manuscript titled Synthesis, Structural Characterization, and Biological Activities of Organically Templated Cobalt Phosphite (C₄N₂H₁₄)Co(H₂PO₃)₄·2H₂O by B. E. Bali et. al. discusses the synthesis, structure and biological activity of hybrid cobalt phosphite compound formed at room temperature.  Below are my specific comments on the manuscript.

There are some minor grammatical errors (number agreement issues and missing articles) that should be corrected before publication.

As the 1,4-butanediammonium cation is not directly bonded to the Co^II center, the authors should strongly consider expressing the formula (both in the title and throughout the manuscript) for the title compound as (C₄N₂H₁₄)[Co(H₂PO₃)₄]·2H₂O.

When referring to the dication, the authors should consider changing the use of 1,4-diaminobutane to 1,4-butanediammonium (or similar).

Throughout the manuscript H₂PO₃ should be changed to H₂PO₃^- to indicate this is an anionic ligand.

Pseudo-tetrahedral geometry could be used to describe the phosphite ligand instead of the more unconventional pseudo-pyramid.

The atom numbering scheme in Tables 2 and 3 need to be corrected.

In Section 3.1, the authors give the P-O bond distance ranges and averages – some of these values are not the same as the ones listed in Table 3 and the average for P(7) is incorrect.  These should be corrected.

Figures 1, 2 and 3 are low-res and need to be remade in a higher resolution.  Also, Figure 2 looks like it has been squeezed, which makes it difficult to discern the structure of the chain.

CIFs:  The refinement of the structure looks fine; however, there are several A level and B level alerts that should either be fixed or addressed within the CIF file.

Overall, the structure and its biological activity are interesting.  If the authors address the above concerns, I believe this manuscript is suitable for publication.

Author Response

As the 1,4-butanediammonium cation is not directly bonded to the CoII center, the authors should strongly consider expressing the formula (both in the title and throughout the manuscript) for the title compound as (C4N2H14)[Co(H2PO3)4]·2H2O. You are right, fixed! When referring to the dication, the authors should consider changing the use of 1,4-diaminobutane to 1,4-butanediammonium (or similar). Fixed! Throughout the manuscript H2PO3 should be changed to H2PO3- to indicate this is an anionic ligand. Fixed! The atom numbering scheme in Tables 2 and 3 need to be corrected. Sorry, these were introduced as edited in the deposited CIF! I made some form corrections in table 3! Pseudo-tetrahedral geometry could be used to describe the phosphite ligand instead of the more unconventional pseudo-pyramid. Fixed! In Section 3.1, the authors give the P-O bond distance ranges and averages – some of these values are not the same as the ones listed in Table 3 and the average for P(7) is incorrect. These should be corrected. You are right, corrected! CIFs: The refinement of the structure looks fine; however, there are several A level and B level alerts that should either be fixed or addressed within the CIF file. # start Validation Reply Form _vrf_PLAT029_127NH17 ; PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.951 Why? RESPONSE: A fraction of about 95% of measured reflections is already enough to solve the crystal structure. ; _vrf_PLAT417_127NH17 ; PROBLEM: Short Inter D-H..H-D H6 ..H13B . 2.05 Ang. RESPONSE: Atom H13B belongs to a solvent water molecule which, in principle, could be partially delocalized in terms of rotation. ; # end Validation Reply Form

Reviewer 3 Report

This article describes the synthesis and structural characterization of a hybrid phosphite compound and the assessment of its efficacy against few bacterial strains. While I am inclined to see that article published in Sci, there are some concerns regarding the crystallography (which is a pivotal part of this article) which needed to be addressed. There are several Alert As on the check CIF report for the deposited structure. These need to be addressed before I can recommend this article for publication. In fact, these Alert As are quite easy to address. These originated from some missing information within the CIF file. For this the authors do not need to re-refine the structure, all of them can be eliminated simply by typing in the missing information in the CIF file. Also, after this modification, the authors must re-deposit the CIF file to CCDC through their website. 

Also, I feel Table 2 within the manuscript is unnecessary so the authors might consider deleting it.

After the above corrections, this manuscript might be suitable for publication in Sci. 

Author Response

This article describes the synthesis and structural characterization of a hybrid phosphite compound and the assessment of its efficacy against few bacterial strains. While I am inclined to see that article published in Sci, there are some concerns regarding the crystallography (which is a pivotal part of this article) which needed to be addressed. There are several Alert As on the check CIF report for the deposited structure. These need to be addressed before I can recommend this article for publication. In fact, these Alert As are quite easy to address. These originated from some missing information within the CIF file. For this the authors do not need to re-refine the structure, all of them can be eliminated simply by typing in the missing information in the CIF file. Also, after this modification, the authors must re-deposit the CIF file to CCDC through their website. Also, I feel Table 2 within the manuscript is unnecessary so the authors might consider deleting it. I sent the revised CIF and manuscript according to your recommendations. I also deleted Table 3 which I judge not too necessary for this publication.

Round 2

Reviewer 1 Report

Dear Authors,

I carefully read the current version of your manuscript, and unfortunately I realized that the manuscript was not revised as I suggested some months ago.

Sorry, I cannot approve this new version of the manuscript.

Best wishes  

Author Response

Dear Authors, I carefully read the current version of your manuscript, and unfortunately I realized that the manuscript was not revised as I suggested some months ago. Reviewer's Comment 1 The paper is well written and relates about a new hybrid phosphide, its structural characterization (X-ray, FTIR, TGA), and biological activity. There are some issues to be better fixed, mostly regarding X-ray crystal structure. Figures 1-2-3 are low-quality, as well as Figure 4 needs to be revised. The atomic labelling of Table 2 needs to be better fixed, according to my notes. Tables 1 and 3 need to be revised. Once all required changes are made up, I will be able to consider the paper worthy of publication on Sci. Your Response 1 We reconsidered the crystal structures figures. For the tables, the crystallographer already deposited the CIF as it is. #################################### Reviewer's Comment 1 As the 1,4-butanediammonium cation is not directly bonded to the CoII center, the authors should strongly consider expressing the formula (both in the title and throughout the manuscript) for the title compound as (C4N2H14)[Co(H2PO3)4]·2H2O. Your Response 1 You are right, fixed! Reviewer's Comment 2 When referring to the dication, the authors should consider changing the use of 1,4-diaminobutane to 1,4-butanediammonium (or similar). Your Response 2 Fixed! Reviewer's Comment 3 Throughout the manuscript H2PO3 should be changed to H2PO3- to indicate this is an anionic ligand. Your Response 3 Fixed! Reviewer's Comment 4 The atom numbering scheme in Tables 2 and 3 need to be corrected. Your Response 4 Sorry, these were introduced as edited in the deposited CIF! I made some form corrections in table3! Reviewer's Comment 5 Pseudo-tetrahedral geometry could be used to describe the phosphite ligand instead of the more unconventional pseudo-pyramid. Your Response 5 Fixed! Reviewer's Comment 6 In Section 3.1, the authors give the P-O bond distance ranges and averages – some of these values are not the same as the ones listed in Table 3 and the average for P(7) is incorrect. These should be corrected. Your Response 6 You are right, corrected! Reviewer's Comment 7 CIFs: The refinement of the structure looks fine; however, there are several A level and B level alerts that should either be fixed or addressed within the CIF file. Your Response 7 # start Validation Reply Form _vrf_PLAT029_127NH17 ; PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.951 Why? RESPONSE: A fraction of about 95% of measured reflections is already enough to solve the crystal structure. ; _vrf_PLAT417_127NH17 ; PROBLEM: Short Inter D-H..H-D H6 ..H13B . 2.05 Ang. RESPONSE: Atom H13B belongs to a solvent water molecule which, in principle, could be partially delocalized in terms of rotation. ; # end Validation Reply Form

Reviewer 2 Report

The third line of the abstract has the space group listed as P\-1.  This is incorrect; in text it should be written as P-1.

1,4-butanediammonium should be referred to as an "ion" not a "molecule."

Author Response

The third line of the abstract has the space group listed as P\-1. This is incorrect; in text it should be written as P-1. 1,4-butanediammonium should be referred to as an "ion" not a "molecule." You are right, both can be considered errors!

Reviewer 3 Report

Seems like the authors have addressed all my concerns so in this form I recommend publication of this article.

Round 3

Reviewer 2 Report

There are several instances where the formula for the title compound is not properly formatted, including in the title.  Please revisit the manuscript (Version 3) to correct the formula.

 

As of 01/14/2020 the deposited CIF downloaded from the CCDC website is still problematic.  It still contains several alerts due to missing/incomplete information.  Please fix these and re-upload the corrected CIF file.