he structure of the ionic product [Ti(eta(6)-Me(6)C(6))Cl-3]AlCl4 I has been determined by an X-ray diffraction experiment: orthorhombic; a = 12.890(4), b = 8.609(2), c = 9.168(3) Angstrom; V = 1017.4(6) Angstrom(3), Z = 2; d(calc) = 1.584 g cm(-3). Tetrachlorogallates of titanium(IV) of general formula [Ti(eta(6)-arene)Cl-3]GaCl4 (arene = 1,2,4,5-Me(4)C(6)H(2), Me(6)C(6)), have been obtained by reaction of TiCl4 with the appropriate arene in the presence of GaCl3 in toluene, Formation of complexes with less methyl-substituted arene ligands (MeC(6)H(5), 1,4-Me(2)C(6)H(4) and 1,3,5-Me(3)C(6)H(3)) has been established by C-13-NMR spectroscopy. The MCl(4)/Me(6)C(6)/benzene system gives, either in the presence or in the absence of aluminium trichloride, covalent (M = Zr) or ionic (M = Hf) compounds of Formula Zr(eta(6)-Me(6)C(6))Cl-2(mu-Cl)(3)ZrCl3 4 and [Hf(eta(6)-Me(6)C(6))Cl-3]Hf2Cl9 5. Compounds 4 and 5 have been Fully characterized by conventional methods including X-ray crystallography, Compound 5: orthorhombic; a = 17.662(6), b = 8.960(3), c = 17.683(6) Angstrom; V = 2798.4(16) Angstrom(3), Z = 4; d(calc) = 2.666 g cm(-3).
eta(6)-arene derivatives of titanium(IV), zirconium(IV) and hafnium(IV)
CALDERAZZO, FAUSTO;PAMPALONI, GUIDO;
1996-01-01
Abstract
he structure of the ionic product [Ti(eta(6)-Me(6)C(6))Cl-3]AlCl4 I has been determined by an X-ray diffraction experiment: orthorhombic; a = 12.890(4), b = 8.609(2), c = 9.168(3) Angstrom; V = 1017.4(6) Angstrom(3), Z = 2; d(calc) = 1.584 g cm(-3). Tetrachlorogallates of titanium(IV) of general formula [Ti(eta(6)-arene)Cl-3]GaCl4 (arene = 1,2,4,5-Me(4)C(6)H(2), Me(6)C(6)), have been obtained by reaction of TiCl4 with the appropriate arene in the presence of GaCl3 in toluene, Formation of complexes with less methyl-substituted arene ligands (MeC(6)H(5), 1,4-Me(2)C(6)H(4) and 1,3,5-Me(3)C(6)H(3)) has been established by C-13-NMR spectroscopy. The MCl(4)/Me(6)C(6)/benzene system gives, either in the presence or in the absence of aluminium trichloride, covalent (M = Zr) or ionic (M = Hf) compounds of Formula Zr(eta(6)-Me(6)C(6))Cl-2(mu-Cl)(3)ZrCl3 4 and [Hf(eta(6)-Me(6)C(6))Cl-3]Hf2Cl9 5. Compounds 4 and 5 have been Fully characterized by conventional methods including X-ray crystallography, Compound 5: orthorhombic; a = 17.662(6), b = 8.960(3), c = 17.683(6) Angstrom; V = 2798.4(16) Angstrom(3), Z = 4; d(calc) = 2.666 g cm(-3).I documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.
