Katrin Eppers, Alisha Mertens, Jan Chrubasik, Mathias S. Wickleder, Jan Langwald
{"title":"The Versatile Structural World of Methanedi- and Trisulfonic Acid and Their Salts","authors":"Katrin Eppers, Alisha Mertens, Jan Chrubasik, Mathias S. Wickleder, Jan Langwald","doi":"10.1002/open.70247","DOIUrl":null,"url":null,"abstract":"<p>The syntheses and structural elucidations of 16 novel compounds, derived from methane(poly-)sulfonic acids are presented. The anhydrous acids, that is, methanedisulfonic acid (MDSA—(H<sub>2</sub>C(SO<sub>3</sub>H)<sub>2</sub>, <b>1</b>) and methanetrisulfonic acid (MTSA), the latter as two polymorphic structures (HC(SO<sub>3</sub>H)<sub>3</sub>-I (<i>P</i>3<i>c</i>1, <b>2</b>) and HC(SO<sub>3</sub>H)<sub>3</sub>-II (<i>P</i>2<sub>1</sub>/<i>n</i>, <b>3</b>)) have been crystallized and structurally elucidated. Methanedisulfonic acid was subsequently used to prepare four group I methanedisulfonates (AM<sub>2</sub>[(H<sub>2</sub>C(SO<sub>3</sub>)<sub>2</sub>], AM = Li (<b>6)</b>, K (<b>7</b>)·H<sub>2</sub>O, Rb (<b>8</b>) and Cs (<b>10</b>)) as well as the strontium dihydrate Sr[H<sub>2</sub>C(SO<sub>3</sub>)<sub>2</sub>](H<sub>2</sub>O)<sub>2</sub> (<b>9</b>) and the ternary salt BaK<sub>2</sub>[(H<sub>2</sub>C(SO<sub>3</sub>)<sub>2</sub>]<sub>2</sub> (<b>11</b>). The known trisulfonate K<sub>3</sub>[HC(SO<sub>3</sub>)<sub>3</sub>](H<sub>2</sub>O) was used for the preparation of the oxonium salt [H<sub>3</sub>O]<sub>3</sub>[HC(SO<sub>3</sub>)<sub>3</sub>] (<b>4</b>), which was isolated as a new polymorph (<i>R</i>3<i>c</i>). Subsequent neutralization led to isolation of the compounds AM<sub>3</sub>[HC(SO<sub>3</sub>)<sub>3</sub>] (AM = Li (<b>12</b>)·(H<sub>2</sub>O)<sub>4</sub>, K (<b>13</b>), Rb (<b>14</b>)·H<sub>2</sub>O, as well as the two ternary salts Rb<sub>3</sub>Ag<sub>3</sub>[HC(SO<sub>3</sub>)<sub>3</sub>]<sub>2</sub> (<b>15</b>) and Rb<sub>5</sub>Ag[HC(SO<sub>3</sub>)<sub>3</sub>]<sub>2</sub>(H<sub>2</sub>O)<sub>2</sub> (<b>16</b>). For a structural comparison between a mono-, di-, and trisulfonate, we also prepared the still elusive rubidium methanesulfonate, which crystallizes as the hydrate Rb[H<sub>3</sub>C(SO<sub>3</sub>)](H<sub>2</sub>O) (<b>5</b>). Different synthetic approaches, as well as an in-depth structural analysis of all compounds, are presented. Furthermore, compound <b>8</b> and the oxonium salt of compound <b>1</b> were investigated concerning their thermal decomposition.</p>","PeriodicalId":9831,"journal":{"name":"ChemistryOpen","volume":"15 7","pages":""},"PeriodicalIF":3.0000,"publicationDate":"2026-06-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/open.70247","citationCount":"0","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"ChemistryOpen","FirstCategoryId":"92","ListUrlMain":"https://onlinelibrary.wiley.com/doi/10.1002/open.70247","RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q2","JCRName":"CHEMISTRY, MULTIDISCIPLINARY","Score":null,"Total":0}
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Abstract
The syntheses and structural elucidations of 16 novel compounds, derived from methane(poly-)sulfonic acids are presented. The anhydrous acids, that is, methanedisulfonic acid (MDSA—(H2C(SO3H)2, 1) and methanetrisulfonic acid (MTSA), the latter as two polymorphic structures (HC(SO3H)3-I (P3c1, 2) and HC(SO3H)3-II (P21/n, 3)) have been crystallized and structurally elucidated. Methanedisulfonic acid was subsequently used to prepare four group I methanedisulfonates (AM2[(H2C(SO3)2], AM = Li (6), K (7)·H2O, Rb (8) and Cs (10)) as well as the strontium dihydrate Sr[H2C(SO3)2](H2O)2 (9) and the ternary salt BaK2[(H2C(SO3)2]2 (11). The known trisulfonate K3[HC(SO3)3](H2O) was used for the preparation of the oxonium salt [H3O]3[HC(SO3)3] (4), which was isolated as a new polymorph (R3c). Subsequent neutralization led to isolation of the compounds AM3[HC(SO3)3] (AM = Li (12)·(H2O)4, K (13), Rb (14)·H2O, as well as the two ternary salts Rb3Ag3[HC(SO3)3]2 (15) and Rb5Ag[HC(SO3)3]2(H2O)2 (16). For a structural comparison between a mono-, di-, and trisulfonate, we also prepared the still elusive rubidium methanesulfonate, which crystallizes as the hydrate Rb[H3C(SO3)](H2O) (5). Different synthetic approaches, as well as an in-depth structural analysis of all compounds, are presented. Furthermore, compound 8 and the oxonium salt of compound 1 were investigated concerning their thermal decomposition.
本文报道了由甲烷（聚）磺酸衍生的16个新化合物的合成和结构解析。无水酸，即甲烷二磺酸(MDSA-(H2C(SO3H) 2,1)和甲烷三磺酸（MTSA），后者为两种多晶结构(HC(SO3H)3- i （P3c1, 2）和HC（SO3H)3- ii (P21/n, 3)）的结晶和结构解析。随后用甲烷二磺酸制备了四种I族甲烷二磺酸盐(AM2[(H2C(SO3)2], AM = Li (6)， K(7)·H2O, Rb（8)和Cs(10)）以及二水合锶Sr[H2C(SO3)2](H2O)2(9)和三元盐BaK2[(H2C(SO3)2]2（11）。利用已知的三磺酸盐K3[HC(SO3)3]（H2O）制备了氧鎓盐[h30]3[HC(SO3)3](4)，分离得到了新的多晶（R3c）。随后的中和分离得到化合物AM3[HC(SO3)3] (AM = Li（12）·（H2O）4, K (13), Rb（14）·H2O)，以及两种三元盐Rb3Ag3[HC(SO3)3]2（15）和Rb5Ag[HC(SO3)3]2(H2O)2（16）。为了比较单磺酸盐、二磺酸盐和三磺酸盐的结构，我们还制备了仍然难以捉摸的甲烷磺酸铷，它结晶为水合物Rb[H3C(SO3)](H2O)(5)。不同的合成方法，以及深入的结构分析的所有化合物，提出。此外，还对化合物8和化合物1的氧鎓盐进行了热分解研究。
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