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• W2622595890 abstract "There has been significant recent interest in differentiating multicomponent solid forms, such as salts and cocrystals, and, where appropriate, in determining the position of the proton in the X —H... A — Y X − ...H— A + — Y continuum in these systems, owing to the direct relationship of this property to the clinical, regulatory and legal requirements for an active pharmaceutical ingredient (API). In the present study, solid forms of simple cocrystals/salts were investigated by high-field (700 MHz) solid-state NMR (ssNMR) using samples with naturally abundant 15 N nuclei. Four model compounds in a series of prototypical salt/cocrystal/continuum systems exhibiting {PyN...H—O—}/{PyN + —H...O − } hydrogen bonds (Py is pyridine) were selected and prepared. The crystal structures were determined at both low and room temperature using X-ray diffraction. The H-atom positions were determined by measuring the 15 N— 1 H distances through 15 N- 1 H dipolar interactions using two-dimensional inversely proton-detected cross polarization with variable contact-time (invCP-VC) 1 H→ 15 N→ 1 H experiments at ultrafast (ν R ≥ 60–70 kHz) magic angle spinning (MAS) frequency. It is observed that this method is sensitive enough to determine the proton position even in a continuum where an ambiguity of terminology for the solid form often arises. This work, while carried out on simple systems, has implications in the pharmaceutical industry where the salt/cocrystal/continuum condition of APIs is considered seriously." @default.
• W2622595890 created "2017-06-15" @default.
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• W2622595890 date "2017-06-05" @default.
• W2622595890 modified "2023-09-25" @default.
• W2622595890 title "Exploring the salt–cocrystal continuum with solid-state NMR using natural-abundance samples: implications for crystal engineering" @default.
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• W2622595890 doi "https://doi.org/10.1107/s205225251700687x" @default.
• W2622595890 hasPubMedCentralId "https://www.ncbi.nlm.nih.gov/pmc/articles/5571809" @default.
• W2622595890 hasPubMedId "https://pubmed.ncbi.nlm.nih.gov/28875033" @default.
• W2622595890 hasPublicationYear "2017" @default.
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