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Synthesis, Characterization, and X‐ray Structures of Ru 3 (CO) 9 (dotpm)(L) Complexes [L = PPh 3 , P(C 6 H 4 Cl‐ p ) 3 , and PPh 2 (C 6 H 4 Br‐ p )]
Author(s) -
Sirat Siti Syaida,
Khan Imthyaz Ahmed,
Shawkataly Omar Bin,
Rosli Mohd Mustaqim
Publication year - 2014
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.201400164
Subject(s) - denticity , phosphine , chemistry , yield (engineering) , crystallography , crystal structure , bond length , nuclear magnetic resonance spectroscopy , x ray crystallography , single crystal , ruthenium , stereochemistry , diffraction , catalysis , materials science , organic chemistry , physics , metallurgy , optics
The reaction of Ru 3 (CO) 10 (dotpm) ( 1 ) [dotpm = (bis(di‐ ortho ‐tolylphosphanyl)methane)] and one equivalent of L [L = PPh 3 , P(C 6 H 4 Cl‐ p ) 3 and PPh 2 (C 6 H 4 Br‐ p )] in refluxing n ‐hexane afforded a series of derivatives [Ru 3 (CO) 9 (dotpm)L] ( 2 – 4 ), respectively, in ca. 67–70 % yield. Complexes 2 – 4 were characterized by elemental analysis (CHN), IR, 1 H NMR, 13 C{ 1 H} NMR and 31 P{ 1 H} NMR spectroscopy. The molecular structures of 2 , 3 , and 4 were established by single‐crystal X‐ray diffraction. The bidentate dotpm and monodentate phosphine ligands occupy equatorial positions with respect to the Ru triangle. The effect of substitution resulted in significant differences in the Ru–Ru and Ru–P bond lengths.