Abstract The compound [NH4][(CH3)2NH2]2[Ta(C2O4)4]·2H2O has been synthesized and characterized by elemental and TG/DTA analyses, IR spectroscopy and by the single-crystal X-ray
diffraction study. The structure comprises the [Ta(C2O4)4]3− anion, NH4+ and [(CH3)2NH2]+ cations and crystallization water molecules. The Ta atom is octacoordinated by oxygen atoms from four bidentate oxalate groups
forming a coordination polyhedron close to the triangular dodecahedron. The charge-assisted hydrogen bonds from both cations
connect the [Ta(C2O4)4]3− anions into a three-dimensional framework.
Graphical Abstract The synthesis and properties of [NH4][(CH3)2NH2]2[Ta(C2O4)4]·2H2O, the first structurally characterized compound with the tetra(oxalato)tantalate(V) anion, is reported.
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Nine shikonin pigments: shikonin (S), acetylshikonin (AS), propionylshikonin (PS), isobutyrylshikonin (IBS), tiglylshikonin (TS), 3,3-dimethylacrylshikonin (DAS), angelylshikonin (ANS), 2-methyl-n-butyrylshikonin (MBS) and isovalerylshikonin (IVS) were identified in the root epidermis of Echium italicum L. for the first time. A new thin-layer chromatographic (TLC) method for the separation of enantiomers alkannin and shikonin proved only shikonin after saponification of the root extract, and was afterwards esterified with the corresponding acyl chloride to acquire seven standard compounds (all except ANS). The developed isocratic high-peformance liquid chromatographic (HPLC) methods with VIS and mass spectrometry (MS) detection, allowed for the first time simultaneous separation of all nine compounds with similar structures including positional and geometric isomers in a short time. Structures of the main five compounds (AS, IBS, ANS, MBS, IVS) isolated from the extract by a new semi-preparative HPLC on C18 have additionally been confirmed by 1H and 13C nuclear magnetic resonance spectra, which were reported for AS and MBS for the first time. 相似文献
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