Molecular Structure of a D-homoandrostanyl Steroid Derivative:  Single Crystal and Powder Diffraction Analyses

Martinetto, Pauline; Térech, Pierre; A, Grand; Ramasseul, R.; Dooryhée, E.; Anne, M.

doi:10.1021/jp0612681

Cited by 11 publications

(8 citation statements)

References 29 publications

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“…The other possibility of solving the single-crystal structure of gel fibers ab initio from its polycrystalline XRPD data is not routine yet and requires sophisticated and not-so-accessible synchrotron beam line. 34…”

Section: Determination Of Molecular Packing Within Gel Fibersmentioning

confidence: 99%

Supramolecular gelling agents: can they be designed?

2008

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The last two decades have witnessed an upsurge of research activities in the area of supramolecular gelators, especially low molecular mass organic gelators (LMOGs), not only for academic interests but also for their potential applications in materials science. However, most of the gelators are serendipitously obtained; their rational design and synthesis is still a major challenge. Wide structural diversities of the molecules known to act as LMOGs and a dearth of molecular level understanding of gelation mechanisms make it difficult to pin-point a particular strategy to achieve rational design of gelators. Nevertheless, some efforts are being made to achieve this goal. Once a gelling agent is serendipitously obtained, new gelling agents with novel properties may be prepared by modifying the parent gelator molecule following a molecular engineering rationale; however, such approach is limited to the same class of gelling agent generated from the parent gelating scaffold. A crystal engineering approach wherein the single-crystal structure of a molecule is correlated with its gelling/nongelling behaviour (structure-property correlation) allows molecular level understandings of the self-assembly of the gelator and nongelator molecules and therefore, provides new insights into the design aspects of supramolecular gelling agents. This tutorial review aims at highlighting some of the developments covering both molecular and crystal engineering approaches in designing LMOGs.

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Section: Determination Of Molecular Packing Within Gel Fibersmentioning

confidence: 99%

Supramolecular gelling agents: can they be designed?

2008

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“…A reasonably good data set (in favorable cases) may be obtained from a limited source of synchrotron beam lines. 56 Moreover, solving structures from PXRD data has not yet become routine. These considerations left us with the other alternative procedure originally proposed and demonstrated by Weiss et al 57 wherein the PXRD patterns of the xerogel are compared with that of the simulated pattern obtained from the single crystal structure of the gelator molecule.…”

Section: Structure-property Correlationmentioning

confidence: 99%

Ferrocene based organometallic gelators: a supramolecular synthon approach

et al. 2011

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The supramolecular synthon namely primary ammonium dicarboxylate (PAD) synthon has been exploited to generate a new series of salt based low molecular weight gelators (LMWGs) derived from ferrocenedicarboxylic acid (FDCA) and primary amines Me-(CH 2 ) n -NH 2 (n ¼ 3-15). While most of the salts are capable of forming gels with DMSO and DMF, nearly all of them show a tendency to form gels with at least one of the solvents studied. Structure property correlation based on single crystal and powder X-ray diffraction data in combination with optical-, scanning-, and transmission-electron microscopy reveals that the supramolecular synthon approach adopted herein for designing LMWGs is indeed useful and allows one to get an easy access to a new series of organometallic gelators.

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“…To establish the structural properties of such materials, the most direct approach is to use powder XRD, although it is important to emphasize that carrying out structure determination from powder XRD data is significantly more challenging than from single-crystal XRD data. However, the opportunities in this regard have improved significantly in recent years as a consequence of progress in the development of new data analysis techniques − (such as the direct-space strategy for structure solution, which has made a particularly significant impact in the case of structure determination of organic molecular solids from powder XRD data).…”

Section: Introductionmentioning

confidence: 99%

Exploiting the Synergy of Powder X-ray Diffraction and Solid-State NMR Spectroscopy in Structure Determination of Organic Molecular Solids

et al. 2013

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We report a strategy for structure determination of organic materials in which complete solid-state nuclear magnetic resonance (NMR) spectral data is utilized within the context of structure determination from powder X-ray diffraction (XRD) data. Following determination of the crystal structure from powder XRD data, first-principles density functional theory-based techniques within the GIPAW approach are exploited to calculate the solid-state NMR data for the structure, followed by careful scrutiny of the agreement with experimental solid-state NMR data. The successful application of this approach is demonstrated by structure determination of the 1:1 cocrystal of indomethacin and nicotinamide. The 1H and 13C chemical shifts calculated for the crystal structure determined from the powder XRD data are in excellent agreement with those measured experimentally, notably including the two-dimensional correlation of 1H and 13C chemical shifts for directly bonded 13C–1H moieties. The key feature of this combined approach is that the quality of the structure determined is assessed both against experimental powder XRD data and against experimental solid-state NMR data, thus providing a very robust validation of the veracity of the structure.

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Molecular Structure of a D-homoandrostanyl Steroid Derivative: Single Crystal and Powder Diffraction Analyses

Cited by 11 publications

References 29 publications

Supramolecular gelling agents: can they be designed?

Supramolecular gelling agents: can they be designed?

Ferrocene based organometallic gelators: a supramolecular synthon approach

Exploiting the Synergy of Powder X-ray Diffraction and Solid-State NMR Spectroscopy in Structure Determination of Organic Molecular Solids

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