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Synthesis, Structures and Characterization of the Calcium Pyrrolates [Ca{(2‐(dimethylaminomethyl)pyrrolyl} 2 donor n ] (donor = THF and pyridine, n = 2; DME and TMEDA, n = 1) as Potential Precursors for Solid‐State Applications
Author(s) -
Vargas Wilda,
RuhlandtSenge Karin
Publication year - 2003
Publication title -
european journal of inorganic chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.667
H-Index - 136
eISSN - 1099-0682
pISSN - 1434-1948
DOI - 10.1002/ejic.200300311
Subject(s) - chemistry , triclinic crystal system , monoclinic crystal system , orthorhombic crystal system , pyridine , ligand (biochemistry) , crystal structure , stereochemistry , tetramethylethylenediamine , trimethylsilyl , denticity , amide , molecule , crystallography , medicinal chemistry , organic chemistry , biochemistry , receptor
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 1 H, 13 C NMR and IR spectroscopy in addition to X‐ray crystallography . Crystal data with Mo‐ K α 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) Å 3 , Z = 4, monoclinic, space group P 2 1 / c , R 1(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) Å 3 , Z = 2, triclinic, space group P $\bar 1$ , R 1 (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) Å 3 , Z = 4, orthorhombic, space group P 2 1 2 1 2 1 , R 1 (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) Å 3 , Z = 4, orthorhombic, space group Pbcn , R 1 (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) Å 3 , Z = 2, monoclinic, space group Cc , R 1 (all data) = 0.0382. (© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2003)