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Hydrolyses of HCCSO3SiMe3 (1) and CH3CCSO3SiMe3 (2) lead to the formation of acetylenic sulfonic acids HCCSO3H⋅2.33 H2O (3) and CH3CCSO3H⋅1.88 H2O (4). These acids were reacted with guanidinium carbonate to yield [+C(NH2)3][HCCSO3−] (5) and [+C(NH2)3][CH3CCSO3−] (6). Compounds 1–6 were characterized by spectroscopic methods, and the X‐ray crystal structures of the guanidinium salts were determined...
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