The reaction of benzamidinato silicon trichloride [{PhC(NR)2}SiCl3] [R = Bu(t) (1), SiMe3 (2)] with 2 equiv of potassium in THF afforded mononuclear chlorosilylene [{PhC(NBu(t))2}SiCl] (3) and [{PhC(NSiMe3)2}2SiCl2] (4), respectively. Compound 4 was formed by the disproportionation of unstable [{PhC(NSiMe3)2}SiCl]. The reaction of [{PhC(NBu(t))2}SiCl3] (1) with 1 equiv of LiR (R = NMe2, OBu(t), OPr(i), PPr(i)2) in THF yielded [{PhC(NBu(t))2}SiCl2R] [R = NMe2 (5), OBu(t) (6), OPr(i) (7), PPr(i)2 (8)]. Treatment of 5-8 with 2 equiv of potassium in THF resulted in the novel heteroleptic silylene [{PhC(NBu(t))2}SiR] [R = NMe2 (9), OBu(t) (10), OPr(i) (11), PPr(i)2 (12)]. Compounds 4, 9, and 12 have been analyzed by X-ray crystallography.
The syntheses, spectroscopy and single crystal X-ray structures of the multifunctional acrylamide-derived ligand N-pyrazolylpropanamide (ϭ L) (1), and its complexes [L 2 CuCl 2 ] (2) and [L 4 Co 3 Cl 6 ] (3) with copper(II) and cobalt(II) chlorides, respectively, are described. The ligand 1 is easily obtained in one step by the reaction of pyrazole with acrylamide in a 1:1 molar ratio in the presence of trimethylbenzylammonium hydroxide as a basic catalyst. The reaction of CuCl 2 · 2H 2 O with 1 in a 1:2 metal salt:ligand molar ratio in ethanol/-triethylorthoformate solution gave coordination compound 2. The crystal structure of 2 contains two sevenmembered chelate rings formed by two nitrogen atoms of the pyrazolyl groups and two weakly coordinated carbonyl oxygen atoms Materials. Acrylamide, pyrazole, trimethylbenzylammonium hydroxide (Triton B, 40 % in methanol), copper(II)chloride dihydrate, cobalt(II)chloride hexahydrate, triethylorthoformate (for dehydration), acetonitrile (99 %) and absolute ethanol were all obtained from commercial suppliers and used as received.Physical Methods. Microanalyses of the compounds were performed using a Leco CHNS 923 apparatus. Melting points were
The reaction of base-free Ph 2 Be with 1, in toluene gaVe the carbene adduct Ph 2 Be(i-Pr-carbene) (1) as colorless crystal blocks. For comparison, the di-n-butyl ether adduct Ph 2 -Be(n-Bu 2 O) (2) was prepared from BeCl 2 and PhLi in a mixture of Et 2 O and n-Bu 2 O. Single-crystal X-ray determinations reVeal monomeric solid-state structures for both complexes.
Readily accessible and easy-to-use phenyliodine(III) dichloride, PhICl(2), has been established as an innovative and superior reagent for the one-electron oxidation of cerium(III) complexes, comprising amide, amidinate, and cyclopentadienyl derivatives. Its use allowed the successful synthesis and structural characterization of the first members of three new classes of chloro-functionalized (organo)cerium(IV) compounds, including the long sought-after Cp(3)CeCl.
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