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Deprotonated diindolylmethanes as dianionic analogues of scorpionate bis(pyrazolyl)borate ligands: synthesis and structural characterization of representative titanocene and zirconocene complexes

“…This chemical inequivalence of the cyclopentadienyl groups is due to the methine in the backbone of the diindolylmethane ligands that situates the aryl towards one of the cyclopentadienyl rings on titanium, whereas the other cyclopentadienyl ring is in the vicinity of the methine hydrogen. The 1 H and 13 C NMR resonances for the methoxy group of 2 were observed at 3.69 and 55.17 ppm, respectively, comparable with the chemical shifts of the methoxy resonances for the free ligand (3.73 and 55.87 ppm) [11]. Thus, the methoxy substituent of 2-methoxyphenyldi(3-methylindol-2-yl)methane is not coordinated to the titanium atom in 2.…”

“…(1)). NH resonances for the free di(3-methylindol-2-yl)methane ligands ðL 2 H 2 : 7:56 ppm; L 0 2 H 2 : 7:68 ppmÞ [11] are absent in the 1 H NMR spectra for 1 and 2, verifying that deprotonation was successful and that the di(3-methylindol-2-yl)methanes coordinate as dianions. …”

“…CDCl 3 was dried by storage over activated molecular sieves. Di(3-methylindol-2-yl)phenylmethane (L 2 H 2 ) [10,11] and 2-methoxyphenyldi-ð3-methylindol-2-ylÞmethane ðL 0 2 H 2 Þ [11] were prepared by sulfuric acid-catalyzed reactions of 3-methylindole with benzaldehyde and 2-anisaldehyde, respectively, as previously reported. Dichlorobis(g 5 -cyclopentadienyl)-titanium and dichlorobis(g 5 -cyclopentadienyl)zirconium were obtained from Strem Chemical and used as received.…”

“…Chemical shifts are reported relative to tetramethylsilane. Tentative 13 C NMR assignments are based on previously reported NMR assignments for polyindolylmethanes [11,12] as well as on NMR assignments of indole derivatives reported by Park et al [13]. In the reporting of NMR data, indole carbons are labeled C2-C7 with C3a and C7a indicating ring fusion positions.…”

Fortuitous formation of [(LiCl)6{(Me2NCH2C8H5N)3P}2]: an amine-ligated hexameric lithium chloride aggregate

“…Formation of phosphine 1 and its presence as a component of 2 was suggested by the spectroscopic data [13][14][15][16][17][18]. The crystalline solid exhibited poor solubility, compared with that for other indolyl phosphines [16,19,20], in toluene and other non-polar organic solvents, so NMR data for 2 were obtained in d 6 -DMSO.…”