Combining solid state NMR, powder X-ray diffraction, and DFT calculations for CsSc3F10 structure determination

Abstract

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Polymorphs of Rb3ScF6: X-ray and Neutron Diffraction, Solid-State NMR, and Density Functional Theory Calculations Study

“…The 45 Sc chemical shift values for six-and seven-coordinated Sc environments range from −32 to 14 ppm and from −67 to −40 ppm, respectively. 12,28 To the best of our knowledge, solid-state NMR data of an eightcoordinated Sc environment were not previously reported in the literature. Therefore, from the Sc NMR results, all Sc sites are six-coordinated.…”

“…To determine suitable values of U , a series of calculations were performed using the CASTEP module, implemented in the Materials Studio 7.0 software package. Different U values were used for previously studied fluoroscandates. , The correlations between the calculated isotropic 45 Sc and 19 F magnetic shielding constants (σ iso ) and experimentally determined isotropic (δ iso ) chemical shift values have been plotted and fitted by linear regressions (Figure S1). From these fits, R 2 values were obtained.…”

“…Structural studies on almost all reported lithium, potassium, and sodium fluoroscandates have been performed. Recently, the structures of two members of the CsF-ScF 3 system, CsScF 4 and CsSc 3 F 10 , have been reported. , However, rubidium-containing fluoride compounds have been overlooked. Only the structure of the RT RbSc 3 F 10 polymorph has been reported to date.…”

“…Different U values were used for previously studied fluoroscandates. 12,28 The correlations between the calculated isotropic 45 Sc and 19 F magnetic shielding constants (σ iso ) and experimentally determined isotropic (δ iso ) chemical shift values have been plotted and fitted by linear regressions (Figure S1). From these fits, R 2 values were obtained.…”

Solid-state vibrational circular dichroism for pharmaceutical purposes

“…[6] To obtain accurate knowledge of the structure of a given solid API and thus resolve all pharmacokinetics issues (ADME), the development of reliable analytical techniques for solid-phase structures is needed. [7] Various technologies commonly used to analyze solid-state compounds have improved over time, [8,9] but they retain some significant disadvantages. Thermal methods are commonly incapable of providing accurate atomistic insight into solidstate structures.…”