Methylzinn- und Methylindium-bis(trimethylsilyl)amide / Methyltin and Methylindium Bis(trimethylsilyl)amides

1991 ◽  
Vol 46 (4) ◽  
pp. 459-467 ◽  
Author(s):  
Michael Rannenberg ◽  
Johann Weidlein ◽  
Axel Obermeyer
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Homologous Series ◽  
Nmr Spectra ◽  
The Other ◽  
Crystal Structure Determination ◽  
New Compounds

BrSn[N(SiMe3)2]3 and ClIn[N(SiMe3)2]2 react with LiMe · O(C2H5)2 (Me = CH3) in toluene or hexane to give the corresponding amido derivatives MeM[N(SiMe3)2]x (M = Sn, x = 3 and M = In, x = 2). These new compounds and the other members of the homologous series MenM[N(SiMe3)2]4 or 3-n are characterized by their IR, Raman und NMR spectra. In addition, the results of the crystal structure determination of MeSn[N(SiMe3)2]3 are reported.

Synthesis and Coordination Chemistry of Novel Binucleating Macrocyclic Ligands with Amine-thioether and Amine-thiophenolate Donor Functions

2001 ◽  
Vol 56 (9) ◽  
pp. 901-907 ◽  
Author(s):  
Marco H. Klingele ◽  
Gunther Steinfeld ◽  
Berthold Kersting
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Reductive Amination ◽  
Condensation Product ◽  
Macrocyclic Ligands ◽  
Crystal Structure Determination ◽  
Deprotonated Form ◽  
X Ray ◽  
New Compounds

Abstract The ability of the aromatic tetraaldehyde l,2-bis(4-tert-butyl-2,6-diformylphenylsulfanyl)-ethane (1) to function as a precursor in the preparation of binucleating hexaamine-dithiolate ligands has been investigated. Reductive amination of compound 1 with bis(aminoethyl)amine under medium-dilution conditions affords the macrobicyclic hexaamine-dithioether compound L1. Deprotection of the [1+2] condensation product gives the corresponding 24-membered hexa-amine-dithiophenol ligand H2L2. The formulation of L1 as a macrobicyclic amine-thioether was confirmed by an X-ray crystal structure determination of the tetranuclear nickel(II) complex of L1, [{(L1)Ni2Cl2}2(μ-Cl)3](BPh4) (2b). The formulation of the doubly deprotonated form (L2)2- of H2L2 as a 24-membered amine-thiophenolate ligand was confirmed by an X-ray crystal structure determination of the dinuclear cobalt(III) complex, [(L2)CoIII(μ-OH)](ClO4)2 · Cl (3). The preparation and the crystal structures of the new compounds are described.

Offene und geschlossene P-funktionalisierte Diferriophosphonium-Salze des Typs [ { CpFe(CO)2}2P(Ph)R]+ X⁻ bzw. [ {μ-CO(CpFeCO)2} P(Ph)R]+ X⁻ / Open and Closed P-Functionalized Diferriophosphonium Salts of the Type [{CpFe(CO)2}2P(Ph)R]+ X⁻ and [{ μ-CO(CpFeCO)2}P(Ph)R]+ X⁻

1993 ◽  
Vol 48 (6) ◽  
pp. 705-712 ◽  
Author(s):  
Christian Klasen ◽  
Guido Effinger ◽  
Siegbert Schmid ◽  
Ingo-Peter Lorenz
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Nmr Spectra ◽  
Crystal Structure Determination ◽  
Ir And Nmr Spectra ◽  
Deprotonation Reaction ◽  
Alkylating Reagents

The reaction of Ph(R)PSiMe3 with an excess of CpFe(CO)2Cl results in the elimination of Me3SiCl to give the open diferriophosphonium halides [{CpFe(CO)2}2P(Ph)R]Cl (R = H, Ph, CH2SiMe3, Me) (1 a—d). The deprotonation reaction of 1 a with KOBut at —78°C results in the formation of the unstable diferriophosphane {CpFe(CO)2}2PPh (3), which reacts with alkylating reagents RX (R = Me, CH2Ph, CH2COOEt; X = Cl, I) to give the P-functionalized diferriophosphonium halides [{CpFe(CO)2}2P(Ph)R]X (1 d’—f). The light-sensitive compounds 1b—f are found to eliminate readily a CO ligand upon photolysis to give the corresponding closed P-functionalized diferriophosphonium salts [{µ-CO(CpFeCO)2}P(Ph)R]X (2b—f) with a bridging CO ligand and a Fe— Fe bond. The mass, IR and NMR spectra of 1, 2 and the results of a crystal structure determination of [{μ-CO(CpFeCO)2}PPh2]BPh4 (2b’) are reported and discussed.

Two lithium tricyanomethanide compounds: syntheses and single-crystal structure determination of LiK[C(CN)3]2 and Li[C(CN)3]·½ (H3C)2CO

2015 ◽  
Vol 70 (3) ◽  
pp. 191-196 ◽  
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Structure Determination ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Cell Parameters ◽  
New Compounds

AbstractThe new compounds LiK[C(CN)3]2 and Li[C(CN)3]·½ (H3C)2CO were synthesized and their crystal structures were determined. Li[C(CN)3]·½ (H3C)2CO crystallizes in the orthorhombic space group Ima2 (no. 46) with the cell parameters a=794.97(14), b=1165.1(2) and c=1485.4(3) pm, while LiK[C(CN)3]2 adopts the monoclinic space group P21/c (no. 14) with the cell parameters a=1265.7(2), b=1068.0(2) and c=778.36(12) pm and the angle β=95.775(7)°. Single crystals of K[C(CN)3] were also acquired, and the crystal structure was refined more precisely than before corroborating earlier results.

Vom Fluorsilan zum Siloxan — 1,3-Silylgruppenwanderung am Si3CSiO-Gerüst/ From a Fluorosilane to a Siloxane — 1,3-Migration of Silyl Groups in the Si3CSiO System

1985 ◽  
Vol 40 (8) ◽  
pp. 1023-1028 ◽  
Author(s):  
Uwe Klingebiel ◽  
Sabine Pohlmann ◽  
Lutz Skoda ◽  
Cornelia Lensch ◽  
George M. Sheldrick
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Crystal Structure Determination ◽  
Silyl Groups ◽  
Trimethylsilyl Groups

AbstractThe nature of the products which are formed in the reaction of tris(trimethylsilyl)Methylfluorosilanes (Me3Si)3C -SiF2R with KOH depends on the bulkiness of the substituents R. The condensed siloxane is obtained for R = F . The crystal structure determination of this siloxane (Me3Si)3C -SiF2-O -SiF2-C (SiMe3)3 shows that the Si -O - Si unit is linear. A fluorosilanol as well as a siloxane could be isolated for R = Me. 1,3-Migration of one or two trimethylsilyl groups from the carbon to the oxygen takes place for R = phenyl, rm-butyl or silylamine, with formation of siloxanes which are isomeres o f the expected silanols.

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