[C(6)H(6)NO](+) ions, in two isomeric forms involved as key intermediates in the aromatic nitrosation reaction, have been produced in the gas phase and analyzed by IR multiple photon dissociation (IRMPD) spectroscopy in the 800-2200 cm(-)(1) fingerprint wavenumber range, exploiting the high fluence and wide tunability of a free electron laser (FEL) source. The IRMPD spectra were compared with the IR absorption spectra calculated for the optimized structures of potential isomers, thus allowing structural information on the absorbing species. [C(6)H(6)NO](+) ions were obtained by two routes, taking advantage of the FEL coupling to two different ion traps. In the first one, an FT-ICR mass spectrometer, a sequence of ion-molecule reactions was allowed to occur, ultimately leading to an NO(+) transfer process to benzene. The so-formed ions displayed IRMPD features characteristic of a [benzene,NO](+) pi-complex structure, including a prominent band at 1963 cm(-)(1), within the range for the N-O bond stretching vibration of NO (1876 cm(-)(1)) and NO(+) (2344 cm(-)(1)). A quite distinct species is formed by electrospray ionization (ESI) of a methanol solution of nitrosobenzene. The ions transferred and stored in a Paul ion trap showed the IRMPD features of substituent protonated nitrosobenzene, the most stable among conceivable [C(6)H(6)NO](+) isomers according to computations. It is noteworthy that IRMPD is successful in allowing a discrimination between isomeric [C(6)H(6)NO](+) species, whereas high-energy collision-induced dissociation fails in this task. The [benzene,NO](+) pi-complex is characterized by IRMPD spectroscopy as an exemplary noncovalent ionic adduct between two important biomolecular moieties.
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http://dx.doi.org/10.1021/ja0637548 | DOI Listing |
Molecules
October 2024
Chemistry Research Laboratory, Department of Chemistry, University of Oxford, 12 Mansfield Road, Oxford OX1 3TA, UK.
Imidazo-fused diazaborines, which serve as intermediary structures somewhat alongside benzene and borazine, had been of particular interest to Dewar and Snyder more than 60 years ago. To this end, Dewar utilised his 'π-'so as to represent ''as a '' species; however, sadly, modern representations have deviated and leapt into '' counterparts. Bonding in boron species has never been straightforward, to such an extent that the orthodox '' like diborane, , HB-BH, which conformed to the paradigmatic rules of molecular structure, in particular, hybridisation and electronegativity, was later evolved to a more realistic '' bonding so as to give the lie to the purported diborane structures of X-ray diffractors.
View Article and Find Full Text PDFAngew Chem Int Ed Engl
December 2024
Krupp-Chair for General and Inorganic Chemistry, Saarland University, 66123, Saarbrücken, Germany.
Unlike cyclopropanes, the analogous BC species (diboriranes) tend to adopt non-classical Hückel-aromatic structures with bridging moieties R between the boron atoms. The coordination of the thus generated cyclic 2e π-system to transition metals is completely unexplored. We here report that complexation of non-classical diboriranes cyclo-μ-RBDurCPh (R=H, SnMe; Dur=2,3,5,6-tetramethylphenyl) to Fe(CO) fragments allows for the carbonylative ring expansion of the BC ring to either four- or five-membered rings depending on the nature of the BRB 3-center-2-electron bond (3c2e): The H-bridged diborirane (R=H) initially reacts with Fe(CO) to the allylic π-complex with an agostic BH/Fe interaction.
View Article and Find Full Text PDFChem Sci
September 2024
Institute for Integrated Catalysis, Pacific Northwest National Laboratory Richland WA 99352 USA
β-Carbon eliminations of aryl, allylic, and propargylic alkoxides of Rh(i), Pd(ii), and Cu(i) are key elementary reactions in the proposed mechanisms of homogeneously catalysed cross-coupling, group transfer, and annulation. Besides the handful of studies with isolable Rh(i)-alkoxides, β-carbon eliminations of Pd(ii)- and Cu(i)-alkoxides are less definitive. Herein, we provide a comprehensive synthetic, structural, and mechanistic study on the β-alkynyl eliminations of isolable secondary and tertiary propargylic alkoxide Cu(i) complexes, LCuOC(H)(Ph)C[triple bond, length as m-dash]CPh and LCuOC(Ar)C[triple bond, length as m-dash]CPh (L = N-heterocyclic carbene (NHC), dppf, -BINAP), to produce monomeric (NHC)CuC[triple bond, length as m-dash]CPh, dimeric [(diphosphine)CuC[triple bond, length as m-dash]CPh], and the corresponding carbonyl.
View Article and Find Full Text PDFInorg Chem
August 2024
Institute of Chemistry, Humboldt-University Berlin, Brook-Taylor-Str. 2, D-13089 Berlin, Germany.
Nitriles and isonitriles are important σ-donor ligands in coordination chemistry. Isonitriles also function in low-valent complexes as π-acceptor ligands similar to CO. Herein we present the unusual behavior of the highly reducing, high-spin iron(I) complex [Fe(hmds)] toward these compound classes.
View Article and Find Full Text PDFACS Catal
May 2024
Department of Chemistry and Biochemistry, Montana State University, Bozeman, MT 59717, United States.
We describe a detailed investigation into why bulky ligands-those that enable catalysis at "12 " Pd-tend to promote overfunctionalization during Pd-catalyzed cross-couplings of dihalogenated substrates. After one cross-coupling event takes place, PdL initially remains coordinated to the π system of the nascent product. Selectivity for mono- vs.
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