Pub Date : 2018-09-07DOI: 10.1002/9781119477822.CH1
R. Andersen, A. Bryan, Michelle Faust, P. Power
The intention of this chapter is to describe in detail reliable synthetic procedures for the uncomplexed metal bissilylamides M{N(SiMe3)2}2 (M =Mn, Fe, or Co) as well as those of their mono-tetrahydrofuran complexes M{N(SiMe3)2}2(THF). In addition, a synthesis for the bis(THF) complex Mn{N(SiMe3)2}2(THF)2 is given. The bis(trimethylsilyl)amido group {N(SiMe3)2} −1, 2 is one of the simplest, most versatile, and inexpensive bulky monodentate ligands. Its steric properties were first demonstrated by Bürger and Wannagat via the synthesis of several low(i.e. twoor three-) coordinate transition metal derivatives in the early 1960s. They were prepared by the simple reaction of an alkali metal salt of the amide {N(SiMe3)2} − with chromium, manganese, iron, cobalt, nickel, or copper halides. The list of new compounds 4 included the trivalent complexes M{N(SiMe3)2}3 (M = Cr and Fe), the divalent species M{N(SiMe3)2}2 (M =Mn, Co, and Ni (unstable)), and the monovalent Cu{N(SiMe3)2}. 4 The volatility of M(II) and M(III) derivatives supported the notion that the compounds had unassociated molecular structures and were therefore the first stable examples of open-shell (i.e. d–d) transition metal complexes with coordination numbers less than four. The closed-shell (d) Cu(I) derivative, although volatile, proved to be tetrameric {CuN(SiMe3)2}4 with four coppers arranged in a planar array and bridged by silylamido ligands. The trigonal planar coordination of the M(III) species was proven for Fe{N(SiMe3)2}3 via a determination of its crystal
{"title":"DIVALENT MANGANESE, IRON, AND COBALT BIS(TRIMETHYLSILYL)AMIDO DERIVATIVES AND THEIR TETRAHYDROFURAN COMPLEXES","authors":"R. Andersen, A. Bryan, Michelle Faust, P. Power","doi":"10.1002/9781119477822.CH1","DOIUrl":"https://doi.org/10.1002/9781119477822.CH1","url":null,"abstract":"The intention of this chapter is to describe in detail reliable synthetic procedures for the uncomplexed metal bissilylamides M{N(SiMe3)2}2 (M =Mn, Fe, or Co) as well as those of their mono-tetrahydrofuran complexes M{N(SiMe3)2}2(THF). In addition, a synthesis for the bis(THF) complex Mn{N(SiMe3)2}2(THF)2 is given. The bis(trimethylsilyl)amido group {N(SiMe3)2} −1, 2 is one of the simplest, most versatile, and inexpensive bulky monodentate ligands. Its steric properties were first demonstrated by Bürger and Wannagat via the synthesis of several low(i.e. twoor three-) coordinate transition metal derivatives in the early 1960s. They were prepared by the simple reaction of an alkali metal salt of the amide {N(SiMe3)2} − with chromium, manganese, iron, cobalt, nickel, or copper halides. The list of new compounds 4 included the trivalent complexes M{N(SiMe3)2}3 (M = Cr and Fe), the divalent species M{N(SiMe3)2}2 (M =Mn, Co, and Ni (unstable)), and the monovalent Cu{N(SiMe3)2}. 4 The volatility of M(II) and M(III) derivatives supported the notion that the compounds had unassociated molecular structures and were therefore the first stable examples of open-shell (i.e. d–d) transition metal complexes with coordination numbers less than four. The closed-shell (d) Cu(I) derivative, although volatile, proved to be tetrameric {CuN(SiMe3)2}4 with four coppers arranged in a planar array and bridged by silylamido ligands. The trigonal planar coordination of the M(III) species was proven for Fe{N(SiMe3)2}3 via a determination of its crystal","PeriodicalId":13689,"journal":{"name":"Inorganic Syntheses","volume":"os-49 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2018-09-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"87246563","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2018-09-07DOI: 10.1002/9781119477822.CH8
Hanan E. Abdou, A. A. Mohamed, J. Fackler, Mukunda M. Ghimire, M. Omary, D. Schilter, T. Rauchfuss, J. A. Denny, M. Darensbourg, M. Morshedi, P. Simpson, Bandar A. Babgi, Katy A. Green, G. J. Moxey, Mark S. Jennaway, M. Cifuentes, M. Humphrey, Samantha G. Eaves, P. Low, K. J. Nelson, Joel S A Miller, T. Woods, K. Dunbar, T. Johnstone, P. Štarha, A. Habtemariam, Sergey S. Zalesskiy, V. Ananikov, Alan J. Reay, I. Fairlamb, W. Geiger, J. Zink, M. J. Shaw, Jared S. Silvia, C. Cummins, D. Mindiola, P. L. Damon, T. Hayton, Matthias Reiners, Nico Ehrlich, M. Walter, Alexandre Hervé, C. D. Sofield, R. Andersen
{"title":"SYNTHESIS OF SELECTED TRANSITION METAL AND MAIN GROUP COMPOUNDS WITH SYNTHETIC APPLICATIONS","authors":"Hanan E. Abdou, A. A. Mohamed, J. Fackler, Mukunda M. Ghimire, M. Omary, D. Schilter, T. Rauchfuss, J. A. Denny, M. Darensbourg, M. Morshedi, P. Simpson, Bandar A. Babgi, Katy A. Green, G. J. Moxey, Mark S. Jennaway, M. Cifuentes, M. Humphrey, Samantha G. Eaves, P. Low, K. J. Nelson, Joel S A Miller, T. Woods, K. Dunbar, T. Johnstone, P. Štarha, A. Habtemariam, Sergey S. Zalesskiy, V. Ananikov, Alan J. Reay, I. Fairlamb, W. Geiger, J. Zink, M. J. Shaw, Jared S. Silvia, C. Cummins, D. Mindiola, P. L. Damon, T. Hayton, Matthias Reiners, Nico Ehrlich, M. Walter, Alexandre Hervé, C. D. Sofield, R. Andersen","doi":"10.1002/9781119477822.CH8","DOIUrl":"https://doi.org/10.1002/9781119477822.CH8","url":null,"abstract":"","PeriodicalId":13689,"journal":{"name":"Inorganic Syntheses","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2018-09-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"84110206","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2018-09-07DOI: 10.1002/9781119477822.CH6
Chia-Wei Hsu, Y. Tsai, B. Cossairt, C. Camp, J. Arnold, C. Cummins
{"title":"SYNTHETIC ROUTE TO WHITE PHOSPHORUS (P4\u0000) AND ARSENIC TRIPHOSPHIDE (AsP3\u0000)","authors":"Chia-Wei Hsu, Y. Tsai, B. Cossairt, C. Camp, J. Arnold, C. Cummins","doi":"10.1002/9781119477822.CH6","DOIUrl":"https://doi.org/10.1002/9781119477822.CH6","url":null,"abstract":"","PeriodicalId":13689,"journal":{"name":"Inorganic Syntheses","volume":"22 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2018-09-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"81514387","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}