Crystallization Features of LiI-CrIII Coordination Compounds with Cyclobutane-1,1-Dicarboxylic Acid Anions

• Published in: Journal of structural chemistry Vol. 64; no. 4; pp. 550 - 562
• Main Authors: Bazhina, E. S., Shmelev, M. A., Kiskin, M. A., Eremenko, I. L.
• Format: Journal Article
• Language: English
• Published: Moscow Pleiades Publishing 2023; Springer Nature B.V
• Subjects: Aqueous solutions; Atomic; Atomic/Molecular Structure and Spectra; Calcium ions; Chemistry; Chemistry and Materials Science; Chromium; Coordination compounds; Crystallization; Cyclobutane; Dicarboxylic acids; Inorganic Chemistry; Lithium ions; Methanol; Molecular; Optical and Plasma Physics; Physical Chemistry; Single crystals; Solid State Physics; cyclobutane-1,1-dicarboxylic acid; lithium; 3; calcium; chromium(III) complexes; heterometallic compounds; X-ray diffraction analysis
• ISSN: 0022-4766; 1573-8779
• DOI: 10.1134/S0022476623040030

For the goal of preparing Li I –Cr III heterometallic coordination compounds, we studied the reaction of Cr(NO 3 ) 3 ·9H 2 O and Li 2 (cbdc) (obtained by the neutralization of LiOH·H 2 O and cyclobutane-1,1-dicarboxylic acid (H 2 cbdc)) interacting in the 1:3 ratio in aqueous and methanol solutions. It was found that synthesis in the aqueous medium and subsequent crystallization of the reaction solution results in a low yield (9%) of crystalline 2D polymeric compound {[CaLi 6 Cr 4 (OH) 4 (cbdc) 8 (H 2 O) 16 ]·7H 2 O} n ( 1 ) formed due to the hydrolysis of a chromium(III) carboxylate complex and the introduction of Ca 2+ ions penetrating into the structure as impurities in the initial LiOH·H 2 O compound. The use of methanol as a solvent in a similar reaction and subsequent long-term aging leads to the formation of crystals of [Li 5 Cr(cbdc) 4 (H 2 O) 5 ] n ( 2 , yield: 55%) whose 3D polymeric structure contains independent fragments with five Li + ions and does not contain Ca 2+ ions. The crystal structures of 1 and 2 are determined by single-crystal XRD (CCDC No. 2161744 ( 1 ), No. 2161745 ( 2 )).