Acetylenic derivatives of metal carbonyls of the triad Fe, Ru, Os—XI Mass spectra of some binuclear complexes

Abstract

The mass spectra of the following acetylenic derivatives of iron,

Alkyne-substituted homo- and heterometallic carbonyl clusters of the iron, cobalt and nickel triads

“…2 Dependence of the results from the characteristics of the instrument271 or from the experimental conditions. 47,272 Finally, in the working conditions, especially when the temperature increase in the introduction systems is not rigorously controlled, deposition of metal in the instrument can occur, resulting in gradual loss of sensitivity and reduced machine lifetime, and frequent maintenance operations. In particular, instruments with sealed-glass connections must be avoided for these analyses.…”

Isolation of intermediates in the dicobalt octacarbonyl-catalyzed cyclotrimerization of cyclooctyne. Crystal and molecular structure of a cobaltacyclopentadiene complex

“…Evaporation of the more slowly moving orange band gave air-stable, orange crystals of dicarbonyI[2-5-q-2,3:4,5-bis(hexamethylene)(tricarbonylcobalta)cyclopentadiene]cobalt (Co-Co), Co2(CO)5(C8H12)2: mp 101-103 °C (0.36 g, 66%); IR (cm"1) (C6H14) 2070 (m), 2014 (vs), 2006 (m), 1966 (vs); mass spectrum m/e (relative intensity) 474 (6), 446 (8), 418 (10), 390 (8), 388 (15), 362 (6), 360 (14), 332 (18), 244 (42), 216 (100), 201 (20), 173 (55), 159 (65), 145 (87), 131 (95), 117 (off scale), 105 (off scale), 91 (off scale), 79 (96), 77 (95); NMR (C6D6) The most slowly moving band eluted with n-pentane gave on evaporation and recrystallization from n-pentane colorless needles of Tris(hexamethylene)benzene, ,C24H36 (0.45 g, 59% or ca. 90% of available excess of cyclooctyne): mp 199-200 °C (lit.16 mp 197-198 °C); mass spectrum m/e (relative intensity) 324 (100), 281 (98), 253 (23) , 241 (15), 239 (18), 211 (34), 199 (21), 185 (37), 171 (28), 157 (24) , 155 (26), 143 (31), 141 (27), 129 (26), 128 (25), 91 (26), 79 (16), 77 (19). Anal.…”

Dinuclear and Polynuclear Ruthenium Non-cluster Compounds

“…Intense doubly-and triply-charged ions are also found. 57 In hexane, [Ru 3 (CO)i 2 ] reacts with 1,4-dibromocyclooctatetraene to form a related complex, the pale yellow ruthenaindenyl derivative (35; 18%). 58 A probable route to (35) is via the i7 4 -benzocyclobutadiene complex, which was not detected, however.…”