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Wilhelm Maximilian Hützler Ernst Egert Michael Bolte 《Acta Crystallographica. Section C, Structural Chemistry》2016,72(9):705-715
A path to new synthons for application in crystal engineering is the replacement of a strong hydrogen‐bond acceptor, like a C=O group, with a weaker acceptor, like a C=S group, in doubly or triply hydrogen‐bonded synthons. For instance, if the C=O group at the 2‐position of barbituric acid is changed into a C=S group, 2‐thiobarbituric acid is obtained. Each of the compounds comprises two ADA hydrogen‐bonding sites (D = donor and A = acceptor). We report the results of cocrystallization experiments of barbituric acid and 2‐thiobarbituric acid, respectively, with 2,4‐diaminopyrimidine, which contains a complementary DAD hydrogen‐bonding site and is therefore capable of forming an ADA/DAD synthon with barbituric acid and 2‐thiobarbituric acid. In addition, pure 2,4‐diaminopyrimidine was crystallized in order to study its preferred hydrogen‐bonding motifs. The experiments yielded one ansolvate of 2,4‐diaminopyrimidine (pyrimidine‐2,4‐diamine, DAPY), C4H6N4, (I), three solvates of DAPY, namely 2,4‐diaminopyrimidine–1,4‐dioxane (2/1), 2C4H6N4·C4H8O2, (II), 2,4‐diaminopyrimidine–N,N‐dimethylacetamide (1/1), C4H6N4·C4H9NO, (III), and 2,4‐diaminopyrimidine–1‐methylpyrrolidin‐2‐one (1/1), C4H6N4·C5H9NO, (IV), one salt of barbituric acid, viz. 2,4‐diaminopyrimidinium barbiturate (barbiturate is 2,4,6‐trioxopyrimidin‐5‐ide), C4H7N4+·C4H3N2O3−, (V), and two solvated salts of 2‐thiobarbituric acid, viz. 2,4‐diaminopyrimidinium 2‐thiobarbiturate–N,N‐dimethylformamide (1/2) (2‐thiobarbiturate is 4,6‐dioxo‐2‐sulfanylidenepyrimidin‐5‐ide), C4H7N4+·C4H3N2O2S−·2C3H7NO, (VI), and 2,4‐diaminopyrimidinium 2‐thiobarbiturate–N,N‐dimethylacetamide (1/2), C4H7N4+·C4H3N2O2S−·2C4H9NO, (VII). The ADA/DAD synthon was succesfully formed in the salt of barbituric acid, i.e. (V), as well as in the salts of 2‐thiobarbituric acid, i.e. (VI) and (VII). In the crystal structures of 2,4‐diaminopyrimidine, i.e. (I)–(IV), R22(8) N—H…N hydrogen‐bond motifs are preferred and, in two structures, additional R32(8) patterns were observed. 相似文献
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Thomas Prenveille Cyrielle Garreau Mathias Matner Dirk Dijkstra Wilhelm Oppermann Diethelm Johannsmann 《Journal of polymer science. Part A, Polymer chemistry》2019,57(5):621-629
The reactivity of urethanes based on 1,6‐hexamethylene diisocyanate (HDI) and 4,4′‐methylene diphenyl diisocyanate (MDI) was investigated at temperatures between 190 °C and 235 °C. Diurethane model compounds end‐capped with either 1‐dodecanol (D‐core‐D) or 1‐hexadecanol (H‐core‐H) were mixed and annealed at high temperature. The core was either MDI or HDI. The transurethanization reaction was followed based on the formation of the compounds (H‐core‐D). The amount of H‐core‐D and of side products, which had formed after variable annealing times, were identified with 1H NMR, FTIR, SEC, and MALDI‐TOF. Transurethanization was considerably faster for MDI‐based urethanes than for HDI‐based urethanes. Only traces of side products were formed during annealing of MDI‐based urethanes, whereas a significant amount of allophanates was formed from HDI‐based urethanes under the same conditions. © 2018 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2019 , 57, 621–629 相似文献
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Dr. Miguel Cortijo Dr. Ángela Valentín-Pérez Dr. Andrei Rogalev Dr. Fabrice Wilhelm Dr. Philippe Sainctavit Dr. Patrick Rosa Dr. Elizabeth A. Hillard 《Chemistry (Weinheim an der Bergstrasse, Germany)》2020,26(59):13363-13366
An original method for determining the handedness of individual non-centrosymmetric crystals in a mixture using a tightly-focused, circularly polarized X-ray beam is presented. The X-ray natural circular dichroism (XNCD) spectra recorded at the metal K-edge on selected crystals of [Δ-M(en)3](NO3)2 and [Λ-M(en)3](NO3)2 (M=CoII, NiII) show extrema at the metal pre-edge (7712 eV for Co, 8335 eV for Ni). A mapping of a collection of some 220 crystals was performed at the respective energies by using left and right circular polarizations. The difference in absorption for the two polarizations, being either negative or positive, directly yielded the handedness of the crystal volume probed by the beam. By using this technique, it was found that the addition of l -ascorbic acid during the synthesis of [Co(en)3](NO3)2 resulted in an enantiomeric enrichment of the Λ-isomer of 67±13 %, whereas the Ni analogue was similarly, but conversely, enriched in the Δ-isomer (65±22 %). 相似文献
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Reassessment of the NH4NO3 thermal decomposition technique for calibration of the N2O isotopic composition
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