Nitrogen-Phosphorus(III)-Chalcogen Macrocycles for the Synthesis of Polynuclear Silver(I) Sandwich Complexes.
Nitrogen-Phosphorus(III)-Chalcogen Macrocycles for the Synthesis of Polynuclear Silver(I) Sandwich Complexes.
复制标题
DOI：
10.1021/acs.inorgchem.7b00141
复制
发表时间：
2017-03
影响因子：
4.6
通讯作者：
Sivathmeehan Yogendra;Felix Hennersdorf;J. Weigand
中科院分区：
文献类型：
--
作者：
Sivathmeehan Yogendra;Felix Hennersdorf;J. Weigand
采用两个氮原子、两个硫原子和四个磷原子合成了无机N-P(III)-Ch基大环[- php - nme - pph -Ch-]2 （8Ch; Ch = S, Se）。通过Na2Ch （Ch = S, Se）与无环二氯二磷烷clph - nme - pclph(9)的环缩合反应，方便地得到了大环。用单质硫（S8）或灰色硒（Segray）处理会导致氧化环收缩，分别得到1,3,2,4-噻氮二磷酸丁2,4-二硫（10S）和1,3,2,4-硒氮二磷酸丁2,4-二硒（10Se）。大环8Ch是过渡金属络合的优秀多齿配体，可以分离出单核、二核、三核和四核银夹层配合物。对多核银配合物进行了全面的表征，包括详细的核磁共振和x射线分析。
The synthesis of inorganic N-P(III)-Ch-based macrocycles [-PhP-NMe-PPh-Ch-]2 (8Ch; Ch = S, Se) is presented by incorporating two nitrogen, two chalcogen, and four phosphorus atoms. The macrocycles are conveniently obtained via the cyclocondensation reaction of Na2Ch (Ch = S, Se) with the acyclic dichlorodiphosphazane ClPhP-NMe-PClPh (9). Treatment with elemental sulfur (S8) or gray selenium (Segray) results in an oxidative ring contraction to give 1,3,2,4-thiazadiphosphetidine 2,4-disulfide (10S) and 1,3,2,4-selenazadiphosphetidine 2,4-diselenide (10Se), respectively. Macrocycles 8Ch are excellent multidentate ligands for transition metal complexation, as demonstrated by the isolation of mono-, di- tri-, and tetranuclear silver sandwich complexes. The polynuclear silver complexes are comprehensively characterized, including detailed NMR and X-ray analysis.