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Synthesis and Crystal Structures of Axially Substituted Titaniumphthalocyanines and Preparation of PcTi@SBA‐15 and PcTi&TiO x @SBA‐15 Materials
Author(s) -
Darwish Wael,
Schlecht Sabine,
Schaper Andreas,
Fröba Michael,
Harms Klaus,
Massa Werner,
Sundermeyer Jörg
Publication year - 2009
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/zaac.200801289
Subject(s) - monoclinic crystal system , triclinic crystal system , chlorobenzene , silanol , crystallography , raman spectroscopy , chemistry , crystal structure , titanium , ligand (biochemistry) , infrared spectroscopy , medicinal chemistry , catalysis , organic chemistry , biochemistry , physics , receptor , optics
Four axially substituted titanium(IV)phthalocyanines of formula trans ‐[PcTi(OSiPh 3 ) 2 ], [PcTi{(NH) 2 C 6 H 4 }], [PcTi(η 2 ‐S 2 )], and [PcTi=S] were prepared starting from the reactive species N,N′‐di‐4‐tolylureato(phthalocyaninato)titanium(IV). The prepared compounds were characterized by using UV/Vis‐spectroscopy, FT‐IR and raman spectroscopy, TGA, elementalanalysis and MALDI‐TOF measurements. The compound trans ‐[PcTi(OSiPh 3 ) 2 ] crystallizes from chlorobenzene in the triclinic space group P $\bar{1}$ with a = 10.4160(8) Å, b = 11.2160(8) Å, c = 13.1495(9) Å, α = 114.124(5)°, β = 99.452(6)°, γ = 96.174(6)°, and Z = 1. [PcTiS 2 ] crystallizes from chlorobenzene in the monoclinic space group P 2 1 / n with a = 13.114(3) Å, b = 9.752(2) Å, c = 20.975(5) Å, β = 100.46(2), and Z = 4. The crystal structures of both compounds are discussed. The reactive ureato complex could also successfully be anchored onto SBA‐15 and TiO x @SBA‐15 materials using the apical ureato ligand as a good leaving group for the reaction with the silanol groups of the host material.