Low-Valent Titanium Porphyrin Complexes. Synthesis and Structural Characterization of the First Titanium(II) Porphyrin Complex, (ɳ2-Diphenylacetylene)Oitanium Octaethylporphyrin
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Abstract
The anaerobic reduction of the dlchlorotltanlum( IV) porphyrins (OEP)TICI2 and (TTP)TICI2 (OEP = octaethylporphyrlnato, TTP = meso -tetra-p -tolylporphyrlnato) with LIAIH4 in the presence of diphenylacetylene In toluene produces the 11"-alkyne T~II) aclducts (OEP)TI(172-Phc==cPh) (1) and (TTP)Ti(172-PhC==cPh) (2). The structure of 1 has been determined by single-crystal X-ray diffraction analysis. Complex 1 crystallizes in the centrosymrnetrlc space group C2/c with a= 49.369 (7) A, b = 13.734 (9) A, c = 36.042 (5) A, {3 = 136.62 (1)0 , V = 16784 (9) A3, Z = 16, R = 0.061, and Rw = 0.063. The asymmetric unit of 1 contains two molecules. Alkyne C-C distances and Ti-alkyne distances are 1.30 ( 1) (C27-C28), 2.016 (5) (TI 1-C27), 2.015 (5) (Ti 1-C~8), 1.30 (1) (C81-C62), 2.007 (7) (T12-C61 ), and 2.028 (7) A (Ti2-C62).
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Reprinted (adapted) with permission from Organometallics 10 (1991): 2102, doi:10.1021/om00053a009. Copyright 1991 American Chemical Society.