Syntheses, characterization and X-ray structures of the fac-[RuCl3(NO)(dppe)] and the trans-[RuCl(NO)(dppe)2]2+ species.
Trans-[RuCl(NO)(dppe)2]2+ species were prepared. The complexes have been characterized by microanalysis, IR and 31P[1H] NMR spectroscopy and cyclic voltammetry. The trans-[RuCl(NO)(dppe)2](ClO4)2 complex shows a reversible one-electron-reduction process at E(1/2) = 0.200 V and another one-electron-reduction irreversible process at -0.620 V, both centered at the NO+ group. The dissociation of the NO group from the trans-[RuCl(NO)(dppe)2]2+ after two one-electron reductions results in the formation of the trans- and cis-[RuCl2(dppe)2] isomers. The product of an electrolyzed solution of the same complex at -0.300 V shows an EPR signal consistent with the presence of the [RuCl(NO(0))(dppe)2]+ complex. Crystal data for trans-[RuCl(NO)(dppe)2]2+*[RuCl4(NO)(H2O)]*1/2[RuCl6]4-*2[H2O] (I) and trans-[RuCl(NO)(dppe)(2)]2+*2[RuCl4(NO)(CH3O)]-*3[CH3OH] (II) are as follow: (I) Space group P-1, a=10.4040(3) A, b=12.3470(4) A, c=23.5620(8) A, alpha=95.885(2) degrees, beta=99.608(2) degrees, gamma=104.378(2) degrees, R=0.0521; (II) space group P-1, a=10.9769(2) A, b=13.2753(3) A, c=24.0287(4) A, alpha=99.743(1) degrees, beta=95.847(1) degrees, gamma=97.549(1) degrees; R=0.0496. The fac-[RuCl3(NO)(dppe)] (III) complex has been also prepared; its crystal data are: space group P2(1)/n (No. 14), a=11.841(2) A, b=13.775(2) A, c=16.295(4) A, beta=92.81(2) degrees; R1=0.0395.
Zampieri
Renata Christina L
RC
Departamento de Química, Universidade Federal de São Carlos, C.P. 676, São Carlos, Brazil.
Von Poelhsitz
Gustavo
G
Batista
Alzir A
AA
Nascimento
Otaciro R
OR
Ellena
Javier
J
Castellano
Eduardo E
EE
D004578:Electron Spin Resonance Spectroscopy; D015394:Molecular Structure; D009569:Nitric Oxide / Q000378:metabolism; D009942:Organometallic Compounds / Q000138:chemical synthesis* / Q000737:chemistry*; D014961:X-Ray Diffraction
D009942:Organometallic Compounds; C468282:chloronitrosobis(diphenylphosphino)ruthenium(III); C468281:trichloronitroso(diphenylphosphino)ruthenium(III); D009569:Nitric Oxide