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Synthesis and Crystal Structure Analysis of NH4[Zn(cma)(H2O)2]·H2O Using IAM and HAR Approaches

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Abstract

The crystal structure of NH4[Zn(cma)(H2O)2]·H2O (cma3– = N-carboxymethylaspartate(3–)) is determined by single crystal X-ray structure analysis. The orthorombic crystals (P212121, a = 7.7901(4) Å, b = 11.2368(4) Å, c = 13.2048(5) Å, α = β = γ = 90°, Z = 4) were obtained from the reaction mixture in the form of racemic conglomerate. The single crystal X-ray structure analysis revealed the maximum deviation of bond angles around the Zn atom from an ideal octahedral geometry 14.09° with ∑ = 67.23° and Θ = 236.69°. Intermolecular interactions are based mainly on a moderate N–H⋯O and O–H⋯O hydrogen bonds. The structure shares similar structural features with other structures containing aspartates and their derivatives as a ligands. The results of using different HAR methods based on semi-empirical (B3LYP) and non-empirical (PBE0) global hybrid GGA DFT functionals were compared.

Graphical Abstract

The crystal structure of NH4[Zn(cma)(H2O)2]·H2O (cma3– = N-carboxymethylaspartate(3–)) is determined by single crystal X-ray structure analysis. The orthorombic crystals (P212121, a = 7.7901(4) Å, b = 11.2368(4) Å, c = 13.2048(5) Å, α = β = γ = 90°, Z = 4) were obtained from the reaction mixture in the form of racemic conglomerate.

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Data Availability

The deposition numbers CCDC 2152269–2152272 contain the supplementary crystallographic data for this paper (including structure factors). These data can be obtained free of charge via http://www.ccdc.cam.ac.uk/data_request/cif or Cambridge Crystallographic Data Centre, 12 Union Road, Cambridge CB2 1EZ, UK; fax: + 44 1223 336033. Crystallographic data can be also obtained from Crystallography Open Database (COD) via https://www.crystallography.net/384cod/search.html under the COD ID 3000339–3000342.

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Acknowledgements

This work was supported by the Scientific Grant Agency of the Ministry of Education of Slovak Republic and of Slovak Academy of Sciences VEGA 2/0019/19 and by the Operation Program of Integrated Infrastructure for the project, UpScale of Comenius University Capacities and Competence in Research, Development and Innovation, ITMS2014+: 313021BUZ3, co-financed by the European Regional Development Fund. The authors thank to prof. František Pavelčík for supplying development version of his XFPB software and Mgr. Ivana Božeková for her vast amount of work during preliminary testing phase.

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Authors and Affiliations

  1. Department of Inorganic Chemistry, Faculty of Natural Sciences, Comenius University in Bratislava, Ilkovičova 6, 842 15, Bratislava, Slovakia

    Jana Chrappová, Yogeswara Rao Pateda & Erik Rakovský

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  1. Jana Chrappová
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  2. Yogeswara Rao Pateda
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Contributions

YPR refined and described the synthesis of the ligand. JC and YPR prepared the title compound. ER with YPR did the X-ray structure determination and prepared the figures. All authors contributed to the main manuscript text and reviewed the manuscript.

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Correspondence to Erik Rakovský.

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Chrappová, J., Pateda, Y.R. & Rakovský, E. Synthesis and Crystal Structure Analysis of NH4[Zn(cma)(H2O)2]·H2O Using IAM and HAR Approaches. J Chem Crystallogr 53, 228–235 (2023). https://doi.org/10.1007/s10870-022-00961-1

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