Synthesis, structures and characterization of the calcium pyrrolates [Ca{(2-(dimethylaminomethyl)pyrrolyl}2 donorn] (donor = THF and pyridine, n = 2; DME and TMEDA, n = 1) as potential precursors for solid-state applications

Wilda Vargas, Karin Ruhlandt-Senge

Research output: Contribution to journalArticle

9 Scopus citations

Abstract

The synthesis and characterization of novel alkaline earth metal pyrrolyl derivatives is described. The target molecules were synthesized using transamination and metallation protocols, involving either the treatment of calcium bis[bis(trimethylsilyl)amide with two equivalents of 2-(dimethylaminomethyl)pyrrole (2-DMAMP) or the reaction of elemental calcium with two equivalents of 2-DMAMP. Different donors, namely THF, pyridine (py), DME (dimethoxyethane), and TMEDA (N,N,N′,N′ -tetramethylethylenediamine) were utilized to study their influence on the structural chemistry of the target compounds. In order to compare the influence of the metal coordination on the pyrrole ligand, we included the crystal structure of the free 2-DMAMP ligand. All new compounds were characterized using 1H, 13C NMR and IR spectroscopy in addition to X-ray crystallography. Crystal data with Mo-Kα radiation (λ = 0.71073 Å) are as follows: 1: [Ca(2-DMAMP) 2(THF)2], a = 15.440(2) Å, b = 14.992(2) Å, c = 10.175(1) Å, β = 94.9(3)° V = 2346.6(6) Å3, Z = 4, monoclinic, space group P21/c, R1(all data) = 0.0981; 2: [Ca(2-DMAMP)2(py)2], a = 9.168(6) Å, b = 10.418(7) Å, c = 13.329(8) Å, α = 85.9(1)°, β = 72.9(1)°, γ = 86.2(1)°, V = 1212.2(1) Å3, Z = 2, triclinic, space group P1, R1 (all data) = 0.0711; 3: [Ca(2-DMAMP)2(DME)], a = 10.814(1) Å, b = 12.907(1) Å, c = 15.170(1) Å, V = 2117.3(3) Å3, Z = 4, orthorhombic, space group P212 121, R1 (all data) = 0.0729; 4: [Ca(2-DMAMP) 2(TMEDA)], a = 9.403(6) Å, b = 15.810(1) Å, c = 15.417(1) Å, V = 2292.0(3) Å3, Z = 4, orthorhombic, space group Pbcn, R1 (all data) = 0.0997; 5: 2-DMAMP, a = 10.8820(7) Å, b = 15.2186(10) Å, c = 9.7578(6) Å, β = 109.736(2)°, V = 1521.05(17) Å3, Z = 2, monoclinic, space group Cc, R1 (all data) = 0.0382.

Original languageEnglish (US)
Pages (from-to)3472-3479
Number of pages8
JournalEuropean Journal of Inorganic Chemistry
Issue number18
DOIs
StatePublished - Sep 26 2003

Keywords

  • Calcium
  • Chemical vapor deposition
  • Intramolecular donation
  • Metallation
  • N ligands
  • Transamination

ASJC Scopus subject areas

  • Inorganic Chemistry

Fingerprint Dive into the research topics of 'Synthesis, structures and characterization of the calcium pyrrolates [Ca{(2-(dimethylaminomethyl)pyrrolyl}<sub>2</sub> donor<sub>n</sub>] (donor = THF and pyridine, n = 2; DME and TMEDA, n = 1) as potential precursors for solid-state applications'. Together they form a unique fingerprint.

  • Cite this