期刊
CRYSTALS
卷 11, 期 5, 页码 -出版社
MDPI
DOI: 10.3390/cryst11050517
关键词
rhodium carboxylate; axial ligand; DBU
资金
- University of Tennessee Graduate School's Student Faculty Research Award
This article describes the synthesis and structural characterization of rhodium(II) carboxylate complexes, including two DBU adducts with similar attributes revealed by single-crystal X-ray diffraction analysis. Compound 1 crystallized with solvent molecules showing intermolecular interactions, while compound 2 lacked solvent and exhibited weak intramolecular interactions. UV-vis spectroscopy was conducted on both adducts in various solvents to study band shifts.
In this article, we describe the synthesis of 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU) adducts of rhodium(II) carboxylate complexes, [Rh-2(mu-O2CCR3)(4)(DBU)(2)] (R = H (1), Me (2)). The DBU ligand is coordinated to the axial site in both adducts via the imido-nitrogen atom, and single-crystal X-ray diffraction analysis of 1 and 2 revealed structurally similar attributes between the compounds. The Rh-Rh bond distance is 2.4108(3) angstrom for 1 and 2.4143(2) angstrom for 2. The Rh-N distance is 2.2681(3) angstrom for compound 1 and 2.2587(10) angstrom for compound 2. Compound 1, however, crystallized with solvent molecules in its unit cell, and Hirshfeld surface analysis showed intermolecular C-H center dot center dot center dot O interactions between oxygen atoms of [Rh-2(mu-O2CCH3)(4)] and the hydrogen of the chloroform solvent among other intermolecular close-contact interactions. The crystal structure of compound 2 was found to be devoid of solvent and showed weak intramolecular C-H center dot center dot center dot O interactions from the DBU axial ligand to the oxygens of the bridging acetates. Otherwise, Hirshfeld analysis showed that 2 was dominated by H center dot center dot center dot H interactions. UV-vis spectroscopy of both adducts was also conducted in different solvents to examine shifts attributed to the pi*(Rh-2) to sigma*(Rh-2) band.
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