Best practice and pitfalls in absolute structure determination

The absolute structure determination of compounds with axial and planar chirality obtained by recently developed asymmetric syntheses was achieved using the crystalline sponge method without using any reference compounds or synthetic modifications.

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Chiral Crystalline Sponges for the Absolute Structure Determination of Chiral Guests

Journal of the American Chemical Society ◽

10.1021/jacs.7b06607 ◽

2017 ◽

Vol 139 (33) ◽

pp. 11341-11344 ◽

Cited By ~ 21

Author(s):

KaKing Yan ◽

Ritesh Dubey ◽

Tatsuhiko Arai ◽

Yasuhide Inokuma ◽

Makoto Fujita

Keyword(s):

Structure Determination ◽

The Absolute ◽

Absolute Structure

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Precise absolute structure determination for light-atom structures

Acta Crystallographica Section A Foundations of Crystallography ◽

10.1107/s0108767311095249 ◽

2011 ◽

Vol 67 (a1) ◽

pp. C191-C191 ◽

Cited By ~ 1

Author(s):

S. Parsons

Keyword(s):

Structure Determination ◽

Light Atom ◽

Absolute Structure

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Redetermination of β-Ba(PO3)2

Acta Crystallographica Section E Structure Reports Online ◽

10.1107/s1600536814000361 ◽

2014 ◽

Vol 70 (2) ◽

pp. i7-i7 ◽

Cited By ~ 2

Author(s):

Matthias Weil

Keyword(s):

Bond Length ◽

Coordination Polyhedron ◽

Structure Determination ◽

Length Distribution ◽

Anisotropic Displacement Parameters ◽

The Absolute ◽

Bond Length Distribution ◽

Absolute Structure ◽

Atomic Coordinates

In comparison with the previous structure determination of the β-modification of bariumcatena-polyphosphate that was based on Weissenberg film data [Grenieret al.(1967).Bull. Soc. Fr. Minéral. Cristallogr.90, 24–31], the current CCD-data-based redetermination reveals all atoms with anisotropic displacement parameters, standard uncertainties for the atomic coordinates, and the determination of the absolute structure. Moreover, a much higher accuracy in terms of the bond-length distribution for the polyphosphate chain, with two shorter and two longer P—O distances, was achieved. The structure consists of polyphosphate chains extending parallel to [100] with a periodicity of two PO4tetrahedra. The Ba2+cations are located between the chains and are surrounded by ten O atoms in the form of a distorted coordination polyhedron, with Ba—O distances ranging from 2.765 (3) to 3.143 (3) Å, also reflecting the higher precision of the current redetermination.

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The use of Mo Kα radiation in the assignment of the absolute configuration of light-atom molecules; the importance of high-resolution data

Acta Crystallographica Section B Structural Science Crystal Engineering and Materials ◽

10.1107/s2052520614014498 ◽

2014 ◽

Vol 70 (4) ◽

pp. 660-668 ◽

Cited By ~ 22

Author(s):

Eduardo C. Escudero-Adán ◽

Jordi Benet-Buchholz ◽

Pablo Ballester

Keyword(s):

High Resolution ◽

Crystal Structures ◽

Structure Determination ◽

Great Majority ◽

Data Sets ◽

Light Atom ◽

High Resolution Data ◽

The Absolute ◽

Absolute Structure

Recent studies have confirmed the usefulness of the Hooft and Parsons methodologies for determination of the absolute crystal structures of enantiopure light-atom compounds using CuKα radiation. While many single-crystal diffractometers used for small-molecule structure determination are equipped with molybdenum anodes, use of data from such instruments for the absolute structure determination of light-atom crystal structures is rarely documented and has often been found to be unsuccessful. The Hooft and Parsons methodologies have been applied to 44 data sets obtained from single crystals containing light-atom molecules of known chirality using Mo Kαradiation. Several factors influencing the calculation of accurate and precise values for the Hooft and Parsons parameters obtained from these data sets have been identified, the inclusion of high-resolution diffraction data being particularly important. The correct absolute structure was obtained in all cases, with the standard uncertainties of the final absolute structure parameters below 0.1 for the great majority.

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