Charakterisierung eines Mehrkomponenten‐Lithiumlithats durch eine Kombination von Röntgenstrukturanalyse, NMR‐Spektroskopie und theoretischen Studien

Pöppler, Ann‐Christin; Granitzka, Markus; Herbst‐Irmer, Regine; Chen, Yu‐Sheng; Iversen, Bo B.; John, Michael; Mata, Ricardo A.

doi:10.1002/ange.201406320

Cited by 7 publications

(5 citation statements)

References 75 publications

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“…Kimura and Brown reported in 1971 that LiHMDS exists as a tetramer-dimer mixture in hydrocarbons and as dimer-monomer mixture in THF and Et2O. [51] Later, especially Collum and Lucht carried out deeply-rooted mechanistic studies to elucidate the aggregation of LiHMDS with various amine and ether ligands by 6 Li, 15 N, and 13 C NMR spectroscopic studies. [52] Williard and Mulvey et al…”

Section: Structure Of Lihmds and Its Havier Analogesmentioning

confidence: 99%

“…[93] The first dimension represents the regular chemical shifts δ and the second dimension gives the diffusion coefficients D of species separated by their particle size (Fig. [1][2][3][4][5][6][7][8][9][10][11][12][13][14][15][16][17]. The authors referred this pseudo 2D experiment as "Diffusion-Ordered NMR Spectroscopy" (DOSY).…”

Section: Extracting Diffusion Coefficientsmentioning

confidence: 99%

“…Chromatography" experiment has gained huge popularity as an advanced tool for identifying individual species in a multicomponent solution (Fig. [1][2][3][4][5][6][7][8][9][10][11][12][13][14][15][16][17][18]. It is essentially important that signals show a desirable distribution, so no signal overlap is present.…”

Section: Extracting Diffusion Coefficientsmentioning

confidence: 99%

“…[81a] A double logarithmic plot of the diffusion coefficients from appropriate standards against their MWs leads to a linear calibration plot (Fig. [1][2][3][4][5][6][7][8][9][10][11][12][13][14][15][16][17][18][19][20] that can be used to calculate molecular masses from diffusion coefficients.…”

Section: Molecular Weights Derived From a Power Lawmentioning

confidence: 99%

“…[12] This is why the knowledge of the structure in the solid state and especially in solution where they operate is extraordinary important to deduce structure-reactivity relationships. [13] In the following chapters a brief synthetical and structural overview of the most important sec-organoamides will be given. Finally, the use of self-diffusion measurements as a valuable tool for the determination of aggregation states will be introduced.…”

Section: Introductionmentioning

confidence: 99%

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DOSY External Calibration Curve Molecular Weight Determination as a Valuable Methodology in Characterizing Reactive Intermediates in Solution

Neufeld¹

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Extracting Diffusion Coefficients 1.2.7 Molecular Weight Determination 1.3 Scope of this Thesis 2 RESULTS AND DISCUSSION 2.1 Development of the DOSY-External Calibration Curve MW-Determination Methodology 2.1.1 Application of a Normalized Reference System with Fixed Diffusion Coefficients 2.1.2 External Calibration Curves (ECC) and Internal References 2.1.3 Quality of TOL-d7 and THF-d7 as Internal Reference 2.1.4 Influence of Shape 2.1.5 Influence of Concentration 2.1.6 Influence of Temperature 2.1.7 Influence of Halides and Molar Density 2.1.8 Influence of Deuterated Compounds 2.2 DOSY-ECC-MW-Determination of Organometallics and Metal Amides 2.2.1 Structure of LDA in THF Solution 2.2.2 Structure of LDA in Toluene Solution 2.2.3 Structure of Na-Indenide in THF Solution 2.2.4 Structure of [t-BuLi]4•4[Me2NC6H4Li]4 in Toluene Solution 2.2.5 Structure of MHMDS with Ammonia as Donorbase in Toluene Solution 2.2.6 Structure of Hauser Base i Pr2NMgCl in THF solution 2.2.7 Structure of Turbo-Hauser Base i Pr2NMgCl•LiCl in THF solution 2.2.8 Structure of Turbo-Hauser Base TMPMgCl•LiCl in THF solution 3 SUMMARY AND OUTLOOK 4 EXPERIMENTAL PART 4.1 Techniques and Experiments 4.1.1 Handling of Air-and Moisture Sensitive Compounds 4.1.2 NMR Experiments 4.1.3 Computational Details 4.2 Synthesis and Crystallization 4.2.1 Donor-Base-Free LDA 4.2.2 Na-Indenide 4.2.3 MHMDS-Ammoniacates (M = Li, Na, K, Rb and Cs) 4.2.4 i Pr2NMgCl 4.2.5 i Pr2NMgCl•LiCl 4.2.6 TMPMgCl•LiCl 4.3 Preparation of DOSY-NMR-Samples 4.3.1 Internal References 4.3.2 LDA 4.3.3 Na-Indenide 4.3.4 MHMDS-Ammoniacates (M = Li, Na and K) 4.3.5 i Pr2NMgCl and i Pr2NMgCl•LiCl 4.3.6 TMPMgCl•LiCl4.4 X-Ray Analysis 4.4.1 [NH3•LiN(SiMe3)2]2•TOL 4.4.2 [NH3•NaN(SiMe3)2]2 4.4.3 [NH3•KN(SiMe3)2]2 4.4.4 [NH3•RbN(SiMe3)2]2 4.4.5 (NH3)4•[NaN(SiMe3)2]2 4.4.6 [(THF)ClMg(μ-i Pr2N)]2

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Section: Structure Of Lihmds and Its Havier Analogesmentioning

confidence: 99%