Title

Establishing Accurate High-Resolution Crystal Structures in the Absence of Diffraction Data and Single Crystals-An NMR Approach

Authors

Authors

K. Kalakewich; R. Iuliucci;J. K. Harper

Comments

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Abbreviated Journal Title

Cryst. Growth Des.

Keywords

SOLID-STATE NMR; SMALL ORGANIC-MOLECULES; CHEMICAL-SHIFT TENSORS; STRUCTURE PREDICTION; BLIND TEST; NEUTRON-DIFFRACTION; CRYSTALLOGRAPHY; REFINEMENT; POWDER; SPECTROSCOPY; Chemistry, Multidisciplinary; Crystallography; Materials Science, ; Multidisciplinary

Abstract

Predicting accurate crystal structures from theoretical consideration has proven to be remarkably challenging. Although significant progress has been made and numerous approaches have now been investigated, selection of the correct structure as the first choice in blind studies is still rarely achieved. Here a process is described that consistently identifies the correct structure from the myriad candidates created from typical crystal structure prediction software. This approach relies on C-13 solid-state NMR data and a secondary refinement process that includes lattice fields. Four structures are considered, and in all cases the correct structure is selected as the first choice and the only statistically feasible candidate. Data from C-13 chemical shift tensor principal values are found to provide better selectivity, but C-13 isotropic shifts also consistently identify the correct structure. This process involves only experimental NMR data and computer-generated structures, yet the structures created appear to rival the accuracy of structures derived from single crystal diffraction methods including single crystal neutron diffraction.

Journal Title

Crystal Growth & Design

Volume

13

Issue/Number

12

Publication Date

1-1-2013

Document Type

Article

Language

English

First Page

5391

Last Page

5396

WOS Identifier

WOS:000328100400030

ISSN

1528-7483

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