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首页> 外文期刊>Zeitschrift fur Anorganische und Allgemeine Chemie >REACTIONS OF SOME SULFUR-FLUORINE COMPOUNDS WITH COMPOUNDS OF TRANSITION METALS - SYNTHESIS AND SPECTROSCOPIC INVESTIGATION OF SULFITO COMPLEXES, INVOLVING MN-II, MO-0, AND W-0 [German]
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REACTIONS OF SOME SULFUR-FLUORINE COMPOUNDS WITH COMPOUNDS OF TRANSITION METALS - SYNTHESIS AND SPECTROSCOPIC INVESTIGATION OF SULFITO COMPLEXES, INVOLVING MN-II, MO-0, AND W-0 [German]

机译：某些硫-氟化合物与过渡金属化合物的反应-涉及MN-II，MO-0和W-0的硫磺复合物的合成和光谱研究[德语]

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摘要

In the oxidative addition reactions of sulfuryl fluoride (1) and of methanesulphonic acid fluoride (2) with eta(2)-ethylene-bis(triphenylphosphine)plat the novel ionic binuclear tetrakis (triphenylphosphine)-(mu-fluoro)-(mu-peroxo)-platinum(II)-fluorosulfonate and -methylsulfonate complexes 3a and 3b were formed. O,O-Sulfito-manganese(II) tricarbonyl 5 a and the binuclear mu-disulfitodimanganese decacarbonyl complex 6 a were obtained in the reaction of disulfuryl difluoride (4) with the carbonyl metalate complex, Na+[Mn(CO)(5)](-). In this redox reaction several further products (e.g., CO, SO2F2 (1) and Mn-2(CO)(10)) were formed and were determined quantitatively. In the presence of acetonitrile the acetonitrile-O,O-sulfito-manganese (II) tricarbonyl complex 5 b was isolated. The new binuclear complexes, bis(eta(5)-cyclopentadienyl)-mu-disulfito-dimetalhexacarbonyls (6 b: metal = Mo-0 and 6 c: metal = W-0) were obtained in the reaction of 4 with the carbonyl metalates Na+[CpM(CO)(3)](-) (M = Mo-I, W-I; Cp = cyclopentadienyl). Further products (e.g., CO, SO2F2 (1) and [CpM(CO)(3)](2), M = Mo, W) were formed and were determined quantitatively. The validity of the concept of hard and soft acids and bases (HSAB-concept) and of the 18-valence-electron rule (18-VE-rule) could not be confirmed in all cases. The characterization of 3 a, 3 b, 5 b, 6 b and 6 c was based on their IR and NMR spectra, and in one case, on the mass spectra (5b). For 3 a and 3 b the dynamic behaviour at room temperature in CD2Cl2 and CD3OD was studied by P-31-NMR spectroscopy. The results are interpreted in terms of exchange processes in solution between the coordinated mu-fluoride and the solvent ligand or the uncoordinated anion. 5 a and 6 a and the by-products (e.g., CO and SO2F2 (1)), which were formed in the redox reactions, were identified by their infrared spectra. [References: 47]
机译：在硫酰氟（1）和甲磺酰氟（2）与eta（2）-乙烯-双（三苯基膦）的氧化加成反应中，新型离子双核四（三苯基膦）-（μ-氟）-（μ-形成过氧）-铂（II）-氟磺酸盐和-甲基磺酸盐复合物3a和3b。 O，O-磺基锰（II）三羰基化合物5a和双核mu-二硫代二锰十羰基络合物6a是通过二氟化二硫醚（4）与羰基金属酸盐络合物Na + [Mn（CO）（5））反应制得的（-）。在该氧化还原反应中，还形成了几种其他产物（例如，CO，SO2F2（1）和Mn-2（CO）（10））并进行了定量测定。在乙腈的存在下，分离出乙腈-O，O-磺基锰（II）三羰基配合物5b。在4与羰基金属化物的反应中获得了新的双核络合物双（η（5）-环戊二烯基）-mu-二磺基-二金属六羰基化合物（6 b：金属= Mo-0和6 c：金属= W-0） Na + [CpM（CO）（3）]（-）（M = Mo-1，WI; Cp =环戊二烯基）。形成另外的产物（例如，CO，SO 2 F 2（1）和[CpM（CO）（3）]（2），M ＝ Mo，W）并定量测定。并非在所有情况下都证实了硬酸和软酸和碱（HSAB概念）和18价电子规则（18-VE规则）的有效性。 3a，3b，5b，6b和6c的表征基于其IR和NMR光谱，在一种情况下，其基于质谱（5b）。对于3a和3b，通过P-31-NMR光谱研究了室温下CD2Cl2和CD3OD中的动力学行为。用配位的mu-氟化物与溶剂配体或未配位的阴离子之间的溶液交换过程来解释结果。通过它们的红外光谱鉴定了在氧化还原反应中形成的5a和6a以及副产物（例如，CO和SO 2 F 2（1））。 [参考：47]

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