+ Resolve Article
+ Follow Us
Follow on FacebookFollow on Facebook
Follow on TwitterFollow on Twitter

+ Translate
+ Subscribe to Site Feed
GeoScience Most Shared ContentMost Shared Content

Solid-State NMR Study of Paramagnetic Bis(alaninato-κ(2)N,O)copper(II) and Bis(1-amino(cyclo)alkane-1-carboxylato-κ(2)N,O)copper(II) Complexes: Reflection of Stereoisomerism and Molecular Mobility in (13)C and (2)H Fast Magic Angle Spinning Spectra

, : Solid-State NMR Study of Paramagnetic Bis(alaninato-κ(2)N,O)copper(II) and Bis(1-amino(cyclo)alkane-1-carboxylato-κ(2)N,O)copper(II) Complexes: Reflection of Stereoisomerism and Molecular Mobility in (13)C and (2)H Fast Magic Angle Spinning Spectra. Inorganic Chemistry 54(10): 4663-4677

Solid-state stereochemistry and mobility of paramagnetic copper(II) complexes formed by aliphatic amino acids (l-alanine, d,l-alanine, 1-amino-2-methyl-alanine) and 1-amino(cyclo)alkane-1-carboxylic acids (alkane = propane, butane, pentane, hexane) as bidentate ligands has been studied by (13)C and (2)H solid-state fast magic angle spinning (MAS) NMR spectroscopy. We examined the prospective method to characterize solid-state paramagnetic compounds in a routine way. Both (13)C and (2)H MAS spectra can distinguish d,l and l,l diastereomers of natural and polydeuterated bis([Dn]alaninato)copper(II) (n = 0, 2, 8) complexes with axial and/or equatorial methyl positions (conformations) primarily due to different Fermi-contact (FC) contributions. The three-bond hyperfine couplings clearly show Karplus-like dependence on the torsional angles which turned out to be a useful assignment aid. Density functional theory calculations of the FC term and crystal structures were also used to aid the final assignments. The correlations obtained for bis(alaninato-κ(2)N,O)copper(II) complexes were successfully used to characterize other complexes. The usefulness of the (2)H MAS spectra of the deuterated complexes was underlined. Even the spectra of the easily exchangeable amine protons contained essential stereochemical information. In the case of a dimer structure of bis(1-aminohexane-1-carboxylato-κ(2)N,O)copper(II) both the (13)C and (2)H resolutions were good enough to confirm the presence of the cis and trans forms in the asymmetric unit. With regard to the internal solid-state motions in the crystal lattice, the obtained quadrupolar tensor parameters were similar for the d,l- and l,l-alaninato isomers and also for the cis-trans forms suggesting similar crystal packing effects, static amine deuterons involved in hydrogen bonding, and fast rotating methyl groups.


PMID: 25920900

DOI: 10.1021/ic502987e

Other references

Bakhtin, I., 1979: Main trends in the development of the branch. Ptitsevodstvo (12) 6-9

Spoor, G., 1982: Potential for mole drainage as drainage technique on heavy soils. The implications of recent work at the NCAE are discussed.

Gvozdanovic, V.; Kallai, L., 1962: Three years experience with peroral cholegraph. Tenth International Congress of Radiology Book of Abstracts, Montreal, Quebec, Canada p 329

Arpaci, T.; Kilicarslan Toruner, E., 2016: Assessment of problems and symptoms in survivors of childhood acute lymphoblastic leukaemia. NlmCategory="UNASSIGNED">Significant physical and psychosocial problems and related symptoms are observed in cancer survivors after treatment as well as during the treatment period. This study was aimed to assess problems and symptoms...

Maas J.L.; Galletta G.J.; Ellis M.A., 1989: Cane canker diseases of thornless blackberry in eastern usa. Acta Horticulturae (Wageningen) (262): 205-208

Morfin Otero R.; Diaz T.; Atilano G.; Esparza Ahumada S.; Rodriguez Chagollan J.J.; Rodriguez Noriega E., 1990: Beta lactamases producing bacteria in a developing country. Abstracts of the Annual Meeting of the American Society for Microbiology 90: 15

Spallacci, P.; Lanza, F., 1973: The residual effect of long term manuring and annual application of chemical fertilizers on maize in monoculture. The residual effect of manure + topdressed mineral N applied annually in 1949-1966 on the grain yield obtained in 1967-1969 with annual application of NPK was greater than that of the corresponding residual effect of mineral fertilizers supplying...

Bielinski, K.; Rosinski, A., 1989: Influence of the age of White Italian geese on their reproductive performance. Data on 120 [female] geese and 30 ganders kept on a 12-h light day for 12 yr showed that annual egg production was relatively stable at 50-60 eggs per annum in the first 5-6 yr, and declined thereafter. Egg fertility was maintained at about 90% ti...

Brues, A.M., 1959: Low-level irradiation. A symposium organized by the Section on Zoological Sciences of the American Association for the Advancement of Science, cosponsored bv the United States Atomic Energy Commission and the Division of Biological and Medical Research of the Argonne National Laboratory, and presented at the Indianapolis meeting, December 30, 1957. (American Association for the Advancement of Science. Publication No. 591.). A symposium of papers dealing with the background irradiation of man: it is well produced but a somewhat expensive book for the general reader as well as the scientist. The first part consists of four papers on the scientific background, and deals...

Anonymous, 1996: Cuts hit health visitors hardest. NlmCategory="UNASSIGNED">HEALTH VISITORS are bearing the brunt of cuts to services by cash-strapped trusts, the Health Visitors' Association claimed this week.