Rhenium(I) tricarbonyl complexes with poly(azolyl)borates generated in situ from an organometallic precursor containing the B-H...Re coordination motif.
Complex fac-[Re(kappa(3)-H(mu-H)(2)B(tim(Me)))(CO)(3)] (1) reacts with protic azoles, like 2-mercapto-1-methylimidazole (tim(Me)H), 2-mercaptobenzothiazole (bztH), or pyrazoles (pz*H), to afford fac-[Re(kappa(3)-H(mu-H)B(tim(Me))(2)(CO)(3)] (2), fac-[Re(kappa(3)-H(mu-H)B(tim(Me))(bzt))(CO)(3)] (3), fac-[Re(kappa(3)-H(mu-H)B(tim(Me))(pz))(CO)(3)] (4), fac-[Re(kappa(3)-HB(tim(Me))(pz)(2))(CO)(3)] (5), and fac-[Re(kappa(3)-H(mu-H)B(tim(Me))(3,5-Me(2)-4-EtOOCCH(2)pz))(CO)(3)] (6). Complexes 2-6 are stabilized by tridentate poly(azolyl)borates generated in situ, and their formation involves most probably a metal-assisted process which is considerably faster for the pyrazole derivatives. The characterization of the novel complexes, 3-6, has been done by common analytical techniques, including single crystal X-ray diffraction analysis. The solid state structures confirmed the presence of hybrid heteroscopionates, presenting (kappa(3)-H, S, S'), (kappa(3)-H, S, N), or (kappa(3)-S, N, N) binding motifs. Multinuclear ((1)H, (13)C, and (11)B) NMR studies have also shown that the coordination mode found in the solid state is retained in solution.
Videira
Margarida
M
Departamento de Química, ITN, Estrada Nacional 10, 2686-953 Sacavém Codex, Portugal.
Moura
Carolina
C
Datta
Amitabha
A
Paulo
António
A
Santos
Isabel C
IC
Santos
I
I
D001881:Borates / Q000138:chemical synthesis / Q000737:chemistry*; D018360:Crystallography, X-Ray; D005031:Ethylenethiourea / Q000031:analogs & derivatives* / Q000138:chemical synthesis / Q000737:chemistry; D009682:Magnetic Resonance Spectroscopy; D015394:Molecular Structure; D009942:Organometallic Compounds / Q000138:chemical synthesis* / Q000737:chemistry; D011720:Pyrazoles / Q000138:chemical synthesis / Q000737:chemistry*; D012211:Rhenium / Q000737:chemistry*; D013055:Spectrophotometry, Infrared
D001881:Borates; D009942:Organometallic Compounds; D011720:Pyrazoles; D005031:Ethylenethiourea; C031280:pyrazole; D012211:Rhenium; C077232:2-mercaptoimidazole