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.
Departamento de Química, ITN, Estrada Nacional 10, 2686-953 Sacavém Codex, Portugal.
Margarida
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Videira
Carolina
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Moura
Amitabha
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Datta
António
A
Paulo
Isabel C
IC
Santos
I
I
Santos
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