Erratum: Corrigendum: X-ray analysis on the nanogram to microgram scale using porous complexes

Abstract

Previously unnoticed ambiguities in the crystallographic data in our Article (specifically, non-negligible disorder of the miyakosyne A molecule), along with further work by three of the authors (Y.H., K.T. and S.M.) have revealed that the stereochemistry we assigned at C14 of miyakosyne A is incorrect. Our new investigations confirm that we can indeed determine the molecular skeleton of miyakosyne A. However, we can only tentatively and not unambiguously identify all of the stereochemistry of miyakosyne A based on the data included in the original paper. A future publication will confirm the stereochemistry at the C14 moiety of miyakosyne A. The other conclusions of our paper are not affected by this correction.

Analysis of rapidly synthesized guest-filled porous complexes with synchrotron radiation: practical guidelines for the crystalline sponge method

“…With excessive disorder, poor data, over-modeling and/or making erroneous assumptions based upon misguided optimism, the disastrous outcome of drawing incorrect conclusions is very real (Inokuma et al, 2013b;Dauter et al, 2014). Great care must be taken in interpreting the residual electron density for the guest molecules, especially in cases where the structure is not completely known, or if it exhibits conformational flexibility and thus disorder.…”

“…The crystal sponge employed most frequently in their studies is {[(ZnI 2 ) 3 (tris(4-pyridyl)-1,3,5-triazene) 2 ]Áx(solvent)} n (Biradha & Fujita, 2002). However, as time progressed, it became evident that data quality was an issue for this method and eventually a correction for the original report was published that pertained to the incorrect stereochemical determination of miyakosyne A (Inokuma et al, 2013b). As an aside, the study of guests enclatherated in host networks is not novel and was performed over two decades ago where guest molecules were cocrystallized within porphyrin networks, and it is of interest to note that the authors explicitly call these systems 'sponges' within the article's title (Byrn et al, 1993).…”

Materials science: The hole story

“…Crystallographers found the MOF's performance hard to reproduce, and then Fujita's team found an error 10 in its structure of miyakosyne A, making others wary of the technique. Since then, however, Fujita and others have produced detailed instructions 11 that are winning over sceptics.…”

X‐ray Structure Analysis of N‐Containing Nucleophilic Compounds by the Crystalline Sponge Method

“…This demonstrates that the CS method is now ap racticalt ool for drug-discoveryr esearch in pharmaceuticali ndustries.Crystalline sponge (CS) methods are emerging technologiesi n X-ray crystallography facilitatingt he crystal structure determination of non-crystalline (or hard-to-crystallize)c ompounds, withoutt raditional crystallization, on am icrogram scale. [1][2][3][4][5][6] The method uses the porous complex [(ZnI 2 ) 3 ·(tpt) 2 ·x(solvent)] n (1a;t pt = 2,4,6-tris(4-pyridyl)-1,3,5-triazine) [7] as aC St hat can absorb small-to-medium-sized organic molecules,o rient them uniformly in their pores, and make them observable by conventional single crystal X-ray crystallography. Since our earlier publications, the CS method has attracted considerable interest from pharmaceutical industries because they often have situations to urgently determine the structure of trace amountso fc ompounds,s uch as metabolites or impurities derived from their drugs of interest.…”