Synthesis and Structure of the Disilagermirane R2Ge(SiR2)2 and the Solvent‐Separated Ion Pair [Li([12]crown‐4)2][GeR3]; (R = SiMe3)

General name for these diphosphanes: (S.S)-2.2"-bis[(R)-l -(dialkylphosphino)ethyl]-l .I"-biferrocene. trans-[RhCI(CO)j(K,R)-(S.S)-riBuTRAP)] was prepared from [RhCI(CO),], and (R.R)-(S,S)-nBuTRAP: m.p. 222-225 C (decomp); [ X I ; ' = -760.3 (c = 0.321 in CHCI,): 'H NMR (200 MHr. CDCI,. TMS) 6 = 0.81 -1.00 (m. 12H).1.10-2.38(m.30H).2.8X(quint., J = 7 H z . l H ) , 3 . 0 X ( q u i n t . , J = 7 H z . I H ) , 4.03-4.09 (m, 2H). 4.28 (s, 5H). 4.31 (s, 5H). 4.35-4.45 (m. 4H); "P{'H; NMR (81 MHz, CDCI,. 85% H,PO,) 6 = 27.27 (dd, 'J(P.P) = 341. 'J(P,Rh) = I 1 9 Hr), 32.56 (dd. 'J(P.P) = 341. 'J(P.Rh) =I19 Hr). Orange crystals for the X-ray crystal structure were grown from CHLCI,;EtOH by solvent diffusion techniques: crystal data: orthorhombic. P2,2,2, (no. 19).

[1]  D. Stalke,et al.  Crystal handling at low temperatures , 1993 .

[2]  A. Heine,et al.  Structural characterization of two modifications of tris(tetrahydrofuran)(tris(trimethylsilyl)silyl)lithium: a compound with a silicon-29-lithium-7 NMR coupling , 1993 .

[3]  D. Stalke,et al.  Darstellung und Struktur von zwei hochreaktiven Intermediaten: [Li(thf)4][Cu5Cl4R2] und [Li(thf)4][AICI3R], R = Si(SiMe3)3 , 1993 .

[4]  A. Heine,et al.  Preparation and Structure of Two Highly Reactive Intermediates: [Li(thf)4][Cu5Cl4R2] and [Li(thf)4][AlCl3R], R Si(SiMe3)3 , 1993 .

[5]  J. A. Cooke,et al.  Molecular Structures of a Siladigermirane and a Cyclotrigermane , 1992 .

[6]  D. A. Horner,et al.  Three-membered rings of carbon, silicon, and germanium. An analysis of thermodynamic stability to fragmentation , 1992 .

[7]  D. Stalke,et al.  Observation of a Direct SnLi Bond; The Crystal and Molecular Structure of Monomeric [Ph3SnLi · PMDETA] and the Detection of 119, 117Sn7Li NMR Coupling in Solution , 1991 .

[8]  D. Stalke,et al.  Erster Nachweis einer direkten Sn‐Li‐Bindung und einer direkten 119, 117Sn‐7Li‐NMR‐Kopplung: [Ph3SnLi(PMDETA)], eine monomere Verbindung im Kristall und in Lösung , 1991 .

[9]  J. A. Cooke,et al.  Thermolysis of a siladigermirane: evidence for the formation of a germasilene , 1991 .

[10]  T. Tsumuraya,et al.  Strained‐Ring and Double‐Bond Systems Consisting of the Group 14 Elements Si, Ge, and Sn , 1991 .

[11]  S. Masamune,et al.  Verbindungen mit SiSi‐, GeGe‐ und SnSn‐Doppelbindungen sowie gespannte Ringsysteme mit Si‐, Ge‐ und Sn‐Gerüsten , 1991 .

[12]  P. Jutzi,et al.  Synthesis and solid-state structure of (Me3Si)3CGeCH(SiMe3)2, a monomeric dialkylgermylene , 1991 .

[13]  G. Sheldrick Phase annealing in SHELX-90: direct methods for larger structures , 1990 .

[14]  D. Roddick,et al.  Preparation and characterization of tris(trimethylsilyl)silyl and tris(trimethylsilyl)germyl derivatives of zirconium and hafnium. X-ray crystal structures of (.eta.5-C5Me5)Cl2HfSi(SiMe3)3 and (.eta.5-C5Me5)Cl2HfGe(SiMe3)3 , 1988 .

[15]  H. Schnering,et al.  Hexa-t-butyldigerman und Hexa-t-butylcyclotrigerman: Moleküle mit den derzeit längsten GeGe- und GeC-Bindungen☆ , 1988 .

[16]  M. Weidenbruch,et al.  Siliciumverbindungen mit starken intramolekularen sterischen Wechselwirkungen ☆: XXVIII. Neue Cyclotrisilane und Cyclotetrasilane , 1987 .

[17]  P. Schleyer,et al.  Bond Stretch Isomerism in Bicyclo[1.1.0]tetrasilanes. Contrasts Between Strained Silicon and Carbon Ring Systems , 1987 .

[18]  P. V. R. Schleyer,et al.  Bindungsdehnungsisomerie in Bicyclo[1.1.0]tetrasilanen ― das unterschiedliche Verhalten von gespannten Silicium- und Kohlenstoffringen , 1987 .

[19]  A. Brook,et al.  Synthesis of some tris(trimethylsilyl)germyl compounds , 1986 .

[20]  G. Becker,et al.  Synthese und Struktur von Lithium-tris(trimethylsilyl)-silanid · 1,5 DME , 1985 .

[21]  M. Goto,et al.  Peralkylcyclotrisilane: Crystal and molecular structure of [(t-BuCH2)2Si]3 , 1984 .

[22]  K. Peters,et al.  Hexa‐tert‐butylcyclotrisilane, a Strained Molecule with Unusually Long SiSi and SiC Bonds , 1984 .

[23]  H. Schnering,et al.  Hexa-tert-butylcyclotrisilan, ein gespanntes Molekül mit ungewöhnlich langen Si-Si- und Si-C-Bindungen , 1984 .

[24]  David J. Williams,et al.  Synthesis of a cyclotrigermane and its conversion to a digermene , 1982 .

[25]  T. Bally,et al.  Cyclotrisilane (R2Si)3 and disilene (R2Si:SiR2) system: synthesis and characterization , 1982 .

[26]  H. Gilman,et al.  Tris(trimethylsilyl)silyllithium , 1968 .

[27]  H. Gilman,et al.  Tetrakis(trimethylsilyl)silane , 1964 .