Assessment of Additives for Nitrogen, Carbon, Hydrogen and Sulfur Determination by Organic Elemental Analysis

Marcó, Alejandro; Compañó, R.; Rubio, R.; Casals, Isidre

doi:10.1007/s00604-002-0956-y

Cited by 21 publications

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“…Despite multiple attempts on independently prepared batches, samples [Fe I ][B(C 6 F 5 ) 4 ] , [Fe II ][BAr F 4 ] 2 , and [Fe II ][B(C 6 F 5 ) 4 ] 2 were consistently low in carbon by about 2% with consistent and accurate H/N percentages. We attribute this discrepancy to incomplete combustion associated with tetraarylborate anions . Nitrogen values were consistently low for Fe 0 (N 2 ) by about 0.5%, probably due to partial loss of the coordinated N 2 ligand.…”

Section: Methodsmentioning

confidence: 99%

Catalytic N₂ Reduction to Silylamines and Thermodynamics of N₂ Binding at Square Planar Fe

et al. 2017

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The geometric constraints imposed by a tetradentate PN ligand play an essential role in stabilizing square planar Fe complexes with changes in metal oxidation state. The square pyramidal Fe(N)(PN) complex catalyzes the conversion of N to N(SiR) (R = Me, Et) at room temperature, representing the highest turnover number of any Fe-based N silylation catalyst to date (up to 65 equiv N(SiMe) per Fe center). Elevated N pressures (>1 atm) have a dramatic effect on catalysis, increasing N solubility and the thermodynamic N binding affinity at Fe(N)(PN). A combination of high-pressure electrochemistry and variable-temperature UV-vis spectroscopy were used to obtain thermodynamic measurements of N binding. In addition, X-ray crystallography, Fe Mössbauer spectroscopy, and EPR spectroscopy were used to fully characterize these new compounds. Analysis of Fe, Fe, and Fe complexes reveals that the free energy of N binding across three oxidation states spans more than 37 kcal mol.

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Section: Methodsmentioning

confidence: 99%

Catalytic N₂ Reduction to Silylamines and Thermodynamics of N₂ Binding at Square Planar Fe

et al. 2017

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“…X-ray quality crystals were grown from C 6 H 5 Cl/pentane. [20] calcd (%) for C 50 H 64 B 2 N 2 Si: C 80.85, H 8.68, N 3.77; found: C 79.6, H 9.10, N 3.87.…”

Section: Synthesis Of 3 Bmentioning

confidence: 96%

Oxidative Addition at a Carbene Center: Synthesis of an Iminoboryl–CAAC Adduct

Dahcheh

Stephan

Bertrand

2014

Chemistry A European J

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The reaction of a cyclic (alkyl)(amino)carbene (CAAC) with dichloro- and dibromobis(trimethylsilyl)aminoborane results in the formation of haloiminoborane-CAAC adducts. When the iodo analogue is used, an oxidative addition at the carbene center affords a cationic iminoboryl-CAAC adduct, featuring a boron-nitrogen triple bond. Similar salts are also obtained by halide abstraction from the chloro- and bromoiminoborane-CAAC adducts. The reactivity of all of these compounds towards CO2 is discussed.

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“…Found: C, 41.74; H, 3.81; N, 9.99. Unsatisfactory analyses were measured even in the presence of V 2 O 5 because of a combustion problem due to the presence of the hexafluorophosphate anion as previously reported in the literature …”

Section: Methodsmentioning

confidence: 99%

“…Found: C, 45.35; H, 4.23; N, 5.62. Unsatisfactory analyses were measured even in the presence of V 2 O 5 because of a combustion problem …”

Section: Methodsmentioning

confidence: 99%

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Transition Metal Complexes of an (S,S)-1,2-Diphenylethylamine-Functionalized N-Heterocyclic Carbene: A New Member of the Asymmetric NHC Ligand Family

2016

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Assessment of Additives for Nitrogen, Carbon, Hydrogen and Sulfur Determination by Organic Elemental Analysis

Cited by 21 publications

References 0 publications

Catalytic N₂ Reduction to Silylamines and Thermodynamics of N₂ Binding at Square Planar Fe

Catalytic N₂ Reduction to Silylamines and Thermodynamics of N₂ Binding at Square Planar Fe

Oxidative Addition at a Carbene Center: Synthesis of an Iminoboryl–CAAC Adduct

Transition Metal Complexes of an (S,S)-1,2-Diphenylethylamine-Functionalized N-Heterocyclic Carbene: A New Member of the Asymmetric NHC Ligand Family

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Assessment of Additives for Nitrogen, Carbon, Hydrogen and Sulfur Determination by Organic Elemental Analysis

Cited by 21 publications

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Catalytic N2 Reduction to Silylamines and Thermodynamics of N2 Binding at Square Planar Fe

Catalytic N2 Reduction to Silylamines and Thermodynamics of N2 Binding at Square Planar Fe

Oxidative Addition at a Carbene Center: Synthesis of an Iminoboryl–CAAC Adduct

Transition Metal Complexes of an (S,S)-1,2-Diphenylethylamine-Functionalized N-Heterocyclic Carbene: A New Member of the Asymmetric NHC Ligand Family

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Catalytic N₂ Reduction to Silylamines and Thermodynamics of N₂ Binding at Square Planar Fe

Catalytic N₂ Reduction to Silylamines and Thermodynamics of N₂ Binding at Square Planar Fe