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Open AccessArticlePost Publication Peer ReviewVersion 3, Revised

Synthesis, Structural Characterization, and Biological Activities of Organically Templated Cobalt Phosphite (C4H14N2)[Co(H2PO3)4]∙2H2O (Version 3, Revised)

Engineering Laboratory of Organometallic and Molecular Materials, Faculty of Sciences, University Sidi Mohamed Ben Abdellah, P.O. Box 1796 (Atlas), 30000 Fez, Morocco
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Author to whom correspondence should be addressed.
Received: 12 March 2019 / Accepted: 24 January 2019 / Published: 15 November 2019
Peer review status: 2nd round review Read review reports
Version 3, Revised
Published: 15 November 2019
DOI: 10.3390/sci1030064
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Version 2, Revised
Published: 25 July 2019
DOI: 10.3390/sci1020041
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Version 1, Original
Published: 12 March 2019
DOI: 10.3390/sci1010013.v1
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A novel hybrid phosphite (C4H14N2)[Co(H2PO3)4]∙2H2O was synthesized with 1,4-diaminobutane (dabn) as a structure-directing agent using slow evaporation method. Single crystal
X-ray diraction analysis showed that it crystallizes in the P-1 triclinic space group, with the following unit cell parameters (Å, °) a = 5.4814 (3), b = 7.5515 (4), c = 10.8548 (6), α = 88.001 (4), β = 88.707 (5), = 85.126 (5), and V= 447.33 (4) Å3. The crystal structure was built up from corner-sharing [CoO6]octahedrons, forming chains parallel to [001], which are interconnected by H2PO3-pseudo-tetrahedral units. The diprotonated 1,4-butanediammonium molecules, residing between the parallel chains, interacted with the inorganic moiety via hydrogen bonds leading thus to the formation of the 3D crystal structure. The Fourier transform infrared spectrum showed characteristic bands corresponding to the phosphite group and the organic molecule. The thermal decomposition of the compound consisted mainly of the loss of the organic moiety and the water molecules. The biological tests exhibited significant activity against Candida albicans and Escherichia coli strains in all used concentrations, while less activity was pronounced when tested against Staphylococcus epidermidis and Saccharomyces
cerevisiae, while there was no activity against the nematode model Steinernema feltiae. View Full-Text
Keywords: hybrid phosphite; X-Ray crystal structure; FTIR; thermal behavior; biological activities; antimicrobial; micro-organisms hybrid phosphite; X-Ray crystal structure; FTIR; thermal behavior; biological activities; antimicrobial; micro-organisms
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MDPI and ACS Style

Hamdi, N.; Chaouch, S.; da Silva, I.; Ezahri, M.; Lachkar, M.; Alhasan, R.; Yaman Abdin, A.; Jacob, C.; El Bali, B. Synthesis, Structural Characterization, and Biological Activities of Organically Templated Cobalt Phosphite (C4H14N2)[Co(H2PO3)4]∙2H2O. Sci 2019, 1, 64.

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Reviewer 1

Sent on 24 Mar 2019 by Francesco Capitelli | Approved with revisions
Institute of Crystallography - CNR

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.


Response to Reviewer 1

Sent on 11 Jul 2020 by Najlae Hamdi, Souad Chaouch, Ivan da Silva, Mohamed Ezahri, Mohammed Lachkar, Rama Alhasan, Ahmad Yaman Abdin, Claus Jacob, Brahim El Bali

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

Sent on 26 Jun 2019 by Eric M. Villa | Approved with revisions
Creighton University

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 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.

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.

Response to Reviewer 2

Sent on 11 Jul 2020 by Najlae Hamdi, Souad Chaouch, Ivan da Silva, Mohamed Ezahri, Mohammed Lachkar, Rama Alhasan, Ahmad Yaman Abdin, Claus Jacob, Brahim El Bali

You are right, fixed!

Fixed!

Fixed!

Sorry, these were introduced as edited in the deposited CIF! I made some form corrections in table 3!

Fixed!

You are right, corrected!

# 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

Sent on 27 Sep 2019 by Indranil Chakraborty | Approved with revisions
University of California Santa Cruz

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. 

Response to Reviewer 3

Sent on 11 Jul 2020 by Najlae Hamdi, Souad Chaouch, Ivan da Silva, Mohamed Ezahri, Mohammed Lachkar, Rama Alhasan, Ahmad Yaman Abdin, Claus Jacob, Brahim El Bali

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.

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