Abstract
New pentanuclear complexes [Cu3M2(CHF2COO)12(H2O)8]·2H2O, where M = Er (I) and Nd (II), were synthesized by reacting individual copper haloacetates and REE in aqueous solution. The molecular structure of complex I was determined by single crystal X-ray diffraction analysis (CIF file CCDC no. 2159724). The structural features of the complexes and the nature of the carboxylate bridges between the metal centers affect the properties of these complexes; therefore, two similar compounds with the monochloroacetate ligand were prepared for comparison: [Cu3M2(СH2ClCOO)12(H2O)8]·2H2O, where M = Er (III) and Nd (IV). Compounds III and IV are isostructural to previously studied complexes of this type with other REE. Compounds I–IV were characterized by X-ray diffraction analysis and IR spectroscopy, and their thermal behavior was studied. To confirm the formation of precursors of molecular species of crystalline compound I, the solute species of the complexes were determined by electrospray ionization mass spectrometry (ESI-MS).
Similar content being viewed by others
REFERENCES
Xu. Can, S. Chen, and L. Jia, Russ. J. Inorg. Chem. 67, 22 (2022). https://doi.org/10.1134/S0036023622601519
Q. Ba, J. Qian, and C. Zhang, J. Clust. Sci. 30, 747 (2019). https://doi.org/10.1007/s10876-019-01534-7
L. Zhong, M. Liu, and B. Zhang, et al., Chem. Res. Chin. Univ. 35, 693 (2019). https://doi.org/10.1007/s40242-019-9058-9
A. Vasil’ev, O. Volkova, E. Zvereva, and M. Markina, Low Dimensional Magnetism (FIZMATLIT, Moscow, 2018) [in Russian].
J. B. Goodenough, Magnetism and the Chemical Bond (John Wiley & Sons, New Jersey, 1963).
F. Chen, W. Lu, Y. Zhu, B. Wu, X. Zheng, J. Coord. Chem. 63, 3599 (2010). https://doi.org/10.1080/00958972.2010.514904
N. Muhammad and M. Ikram, et al., J. Mol. Struct. 1196, 754 (2019). https://doi.org/10.1016/j.molstruc.2019.06.095
A. A. Bovkunova, E. S. Bazhina, I. S. Evstifeev, et al., Dalton Trans. 50, 12275 (2021). https://doi.org/10.1039/d1dt01161h
X.-M. Chen, M.-L. Tong, Y.-L. Wu, and Y.-J. Luo, J. Chem. Soc., Dalton Trans. 10, 2181 (1996). https://doi.org/10.1039/DT9960002181
V. K. Voronkova, R. T. Galeev, S. Shova, et al., Appl. Magn. Reson. 25, 227 (2003). https://doi.org/10.1007/BF03166687
Y. Cui, F. K. Zheng, D. C. Yan, et al., Chin. J. Struct. Chem. 17, 5 (1998).
C.-G. Zhang, D. Yan, Y. Ma, and F. Yang, J. Coord. Chem. 51, 261 (2000). https://doi.org/10.1080/00958970008055132
W. Wojciechowski, J. Legendziewicz, M. Puchalska, and Z. Ciunik, J. Alloys Compd. 380, 285 (2004). https://doi.org/10.1016/j.jallcom.2004.03.056
W. G. Bateman and D. B. Conrad, J. Am. Chem. Soc. 37, 2553 (1915).
M. D. Judd, B. A. Plunkett, and M. Pope, J. Therm. Anal. 9, 83 (1976). https://doi.org/10.1007/BF01909269
E. V. Karpova, A. I. Boltalin, Yu. M. Korenev, and S. I. Troyanov, Russ. J. Coord. Chem. 26, 361 (2000).
G. M. Sheldrick, Acta Crystallogr. A64, 112 (2008). https://doi.org/10.1107/S0108767307043930
G. M. Sheldrick, Acta Crystallogr. A71, 3 (2015). https://doi.org/10.1107/S2053273314026370
G. M. Sheldrick, Acta Crystallogr. C71, 3 (2015). https://doi.org/10.1107/S2053229614024218
K. Brandenburg and M. Berndt, DIAMOND. Version 2.1e. Crystal Impact GbR. Bonn, 2000.
J. N. Niekerk and F. R. L. Schoening, Acta Crystallogr. 6, 227 (1953). https://doi.org/10.1107/S0365110X53000715
S. Jangbo, N. Rongzhi, S. Xin, and P. Bo, SPIE Conf. Proc. 10256, 1046357 (2017). https://doi.org/10.1117/12.2260699
V. Ya. Kavun, T. A. Kaidalova, V. I. Kostin, et al., Koord. Khim. 10, 1502 (1984).
A. S. Antsyshkina, M. A. Porai-Koshits, and V. N. Ostrikova, Zh. Neorg. Khim. 33, 1950 (1988).
Y. Sugita and A. Ouchi, Bull. Chem. Soc. Jpn. 60, 171 (1987). https://doi.org/10.1246/bcsj.60.171
G. Oczko and P. Starynowicz, J. Mol. Struct. 523, 79 (2000). https://doi.org/10.1016/S0022-2860(99)00391-9
B. Cristovao, D. Osypiuk, B. Miroslaw, and A. Bartyzel, Polyhedron 188, 114703 (2020). https://doi.org/10.1016/j.poly.2020.114703
J.-P. Costes, M. Auchel, F. Dahan, et al., Inorg. Chem. 45, 1924 (2006). https://doi.org/10.1021/ic050587o
A. N. Georgopoulou, M. Pissas, V. Psycharis, et al., Molecules 25, 2280 (2020). https://doi.org/10.3390/molecules25102280
C. G. Herbert and R. A. W. Johnstone, Mass Spectro-metry Basics (CRC Press, New York, 2003). https://doi.org/10.1002/aoc.509
O. Schramel, B. Michalke, and A. Kettrup, J. Chromatogr., A 819, 231 (1998). https://doi.org/10.1016/S0021-9673(98)00259-3
W. Henderson and J. S. McIndoe, Mass Spectrometry of Inorganic, Coordination, and Organometallic Compounds (John Wiley & Sons Ltd., New Jersey, 2005). https://doi.org/10.1002/0470014318
G. B. Deacon and R. J. Phillips, Coord. Chem. Rev. 33, 227 (1980). https://doi.org/10.1016/S0010-8545(00)80455-5
The Matheson Company Inc., John Wiley & Sons, New Jersey, 1980.
O. S. Pushikhina, K. R. Volkova, E. V. Karpova, et al., Mendeleev Commun. 32, 208 (2022). https://doi.org/10.1016/j.mencom.2022.03.018
M. D. Judd, B. A. Plunkett, and M. I. Pope, J. Therm. Anal. 6, 555 (1974). https://doi.org/10.1007/BF01911560
ACKNOWLEDGMENTS
The authors are grateful to T.V. Filippova and R.A. Khalaniya for carrying out the X-ray powder diffraction studies, and to I.V. Kolesnik for recording the IR spectra. The work used equipment purchased at the expense of the Development Program of Moscow State University.
Funding
This work was supported by the Russian Science Foundation project No. 22-43-02020.
Author information
Authors and Affiliations
Corresponding authors
Ethics declarations
The authors declare that they have no conflicts of interest.
Additional information
Translated by O. Fedorova
Supplementary Information
File 11502_2023_3120_MOESM1_ESM.pdf contains the following supplementary materials:
Photographic materials for compound I prepared by various methods (Fig. S1. Photographs of (a) single-phase crystals of compound I prepared as described in this paper and (b) a multiphase sample after long-term crystallization of solution with the metal molar ratio Cu : Er = 1 : 2);
The results of full-profile analysis (Fig. S2. Profile analysis of the X-ray diffraction pattern for a compound II sample.; Fig. S3. Profile analysis of the X-ray powder diffraction pattern for a compound I sample.);
Analysis of X-ray diffraction patterns of the decomposition products of compounds I and III (Fig. S4. Comparison of the X-ray diffraction patterns measured for solid residues of compound I after it was decomposed in a platinum crucible (the red line) and an alundum crucible (the blue line) at 270°С and in a platinum crucible at 240°С (the green line) with the PDF cards [S1] of erbium fluoride, copper oxide, and copper metal; Fig. S5. Comparison of the X-ray diffraction patterns measured for solid residues of compound III after it was decomposed in an alundum crucible at 400°С with the PDF cards [S2] of erbium chloride hexahydrate, erbium oxochloride, copper(I) chloride, copper(II) oxide, and copper metal.); and
Detailed TG data for all compounds (Fig. S6. TG results for a sample of compound I; Fig. S7. TG results for a sample of compound II; Fig. S8. TG results for a sample of compound III; and Fig. S9. TG results for a sample of compound IV).
Rights and permissions
About this article
Cite this article
Pushikhina, O.S., Karpova, E.V., Tsarev, D.A. et al. Characterization of New Pentanuclear Copper(II) and REE(III) Carboxylate Complexes. Russ. J. Inorg. Chem. 68, 1313–1324 (2023). https://doi.org/10.1134/S0036023623601678
Received:
Revised:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1134/S0036023623601678