The reaction of mononuclear ruthenium precursor [Ru(II)(acac)(2)(CH(3)CN)(2)] (acac = acetylacetonate) with the thiouracil ligand (2-thiouracil, H(2)L(1) or 6-methyl -2-thiouracil, H(2)L(2)) in the presence of NEt(3) as base in ethanol solvent afforded a trinuclear triangular complex Ru(3)(O,O-acetylacetonate)(3)(mu-O,O,gamma-C-acetylacetonate)(3)(mu(3)-sulfido) (1). In 1, each ruthenium center is linked to one usual O,O-bonded terminal acetylacetonate molecule whereas the other three acetylacetonate units act as bridging functions: each bridges two adjacent ruthenium ions through the terminal O,O-donor centers at one end and via the gamma-carbon center at the other end. Moreover, there is a mu(3)-sulfido bridging in the center of the complex unit, which essentially resulted via the selective cleavage of the carbon-sulfur bond of the thiouracil ligand. In diamagnetic complex 1, the ruthenium ions are in mixed valent Ru(III)Ru(III)Ru(II) state, where the paramagnetic ruthenium(III) ions are antiferromagnetically coupled. The single crystal X-ray structure of 1 showed two crystallographically independent C(3)-symmetric molecules, Ru(3)(O,O-acetylacetonate)(3)(mu-O,O,gamma-C-acetylacetonate)(3)(mu(3)-S) (1), in the asymmetric unit. Bond distances of both crystallographically independent molecules are almost identical, but there are some significant differences in bond angles (up to 6 degrees ) and interplanar angles (up to 8 degrees ). Each ruthenium atom exhibits a distorted octahedral environment formed by four oxygen atoms, two from each of the terminal and bridging acetylacetonate units, one gamma-carbon of an adjacent acetylacetonate ligand, and the sulfur atom in the center of the complex. In agreement with the expected 3-fold symmetry of the complex molecule, the (1)H and (13)C NMR spectra of 1 in CDCl(3) displayed signals corresponding to two types of ligand units. In dichloromethane solvent, 1 exhibited three metal center based successive quasireversible redox processes, Ru(III)Ru(III)Ru(III)-Ru(III)Ru(III)Ru(II) (couple I, 0.43 V vs SCE); Ru(III)Ru(III)Ru(IV)-Ru(III)Ru(III)Ru(III) (couple II, 1.12 V); and Ru(III)Ru(III)Ru(II)-Ru(III)Ru(II)Ru(II) (couple III, -1.21 V). However, in acetonitrile solvent, in addition to the three described couples [(couple I), 0.34 V; (couple II), 1.0 V; (couple III), -1.0], one irreversible oxidative response (Ru(III)Ru(III)Ru(IV) --> Ru(III)Ru(IV)Ru(IV) or oxidation of the coordinated sulfide center) appeared at E(pa), 1.50 V. The large differences in potentials between the successive couples are indicative of strong coupling between the ruthenium ions in the mixed-valent states. Compound 1 exhibited a moderately strong charge-transfer (CT) transition at 654 nm and multiple ligand based intense transitions in the UV region. In the Ru(III)Ru(III)Ru(III) (1(+)) state, the CT band was slightly blue shifted to 644 nm; however, the CT band was further blue shifted to 520 nm on two-electron oxidation to the Ru(III)Ru(III)Ru(IV) (1(2+)) state with a reduction in intensity.

First example of mu(3)-sulfido bridged mixed-valent triruthenium complex triangle Ru(III)(2)Ru(II)(O,O-acetylacetonate)(3)(mu-O,O,gamma-C-acetylacetonate)(3)(mu(3)-S) (1) incorporating simultaneous O,O- and gamma-C-bonded bridging acetylacetonate units. Synthesis, crystal structure, and spectral and redox properties.

Reactions of divalent metal salts of Co, Ni and Zn with 1,2-di(salicylaldimino-o-phenylthio)ethane (H2L1) and 1,2-di(naphthaldimino-o-phenylthio)ethane (H2L2), having N2O2S2 cores, and 1,2-di(O-salicylaldimino-o-hydroxyphenyl)ethane (H2L3), having a N2O4 core, have been explored. Out of the three ligands and the nine products obtained from the corresponding reactions, two ligands and seven products were crystallographically characterized. However, all the ligands and the products were characterized by analytical and spectral methods. Reaction of H2L1 and H2L2 with Co(II) salts results in oxidative cleavage of the C–S bond to produce a Co(III) product bound to two dissimilar tridentate ligands formed as a result of the cleavage. The reaction of H2L1 and H2L2 with Co(III)acac in the presence of methanolic NaOH also shows cleavage of the C–S bond to give compounds similar to those obtained by reacting H2L1 and H2L2 with Co(II) salts in the absence of additional external base. However, the reaction of Co(II) salt with H2L3 did not lead to any C–O bond cleavage; rather it produced an octahedral Co(II) complex of the hexadentate H2L3. Reactions of all these three ligands with Ni(II) salt resulted in octahedral complexes of the corresponding hexadentate ligands. In the case of Zn(II), while H2L3 with a N2O4 core resulted in an octahedral complex, H2L1 and H2L2, both with a N2O2S2 core, produced pseudo-octahedral complexes whose Zn–S bond lengths are rather long. The conformations of both the 5-membered and 6-membered chelate rings formed in the products were evaluated. The extent of distortion exhibited in the geometry of these octahedral complexes was computed and appropriately compared.

Complexation behaviour of hexadentate ligands possessing N2O4 and N2O2S2 cores: differential reactivity towards Co(II), Ni(II) and Zn(II) salts and structures of the products

Aminocarbyne ligands in organometallic chemistry

The reactions of different transition metals with the multidentate ligand N,N′-bis(1,3,4-thiadiazol-2-yl)-2,6-pyridinedicarboxamide (btapca) afford six new polynuclear complexes: the hexanuclear complexes [{Zn6(O)2(btapca)4}·3DMF·2H2O] (1) and [{Zn6(O)2(btapca)4}·DMF·MeOH·H2O] (2); the pentanuclear complexes [{Zn5(OH)2(btapca)4}·4DMF·H2O] (3), [{Co5(OH)2(btapca)4}·4DMF·MeOH·H2O] (4) and [{Ni5(OH)2(btapca)4}·4DMF·MeOH] (5); and the trinuclear complex [{Fe3(OH)(btapca)3}·2DMF·2MeOH] (6). The dominant characteristic of these polynuclear complexes is that there are μ3- or μ4-oxygen atoms in the metal polyhedrons. The hexanuclear complexes 1 and 2 show similar octahedral features based on zinc centers. The five metal centers in complexes 3, 4 and 5 arrange into two triangles with one common vertex. As for complex 6, three iron(II)/iron(III) atoms form a plane with a μ3-OH− in the center. We also report the magnetic properties of complexes 4, 5 and 6. Complex 4 exhibits intramolecular antiferromagnetic exchange, while the analogous complex 5 is dominated by very strong intramolecular ferromagnetic coupling. The trinuclear complex [{Fe3(OH)(btapca)3}·2DMF·2MeOH] (6) shows comparable weak antiferromagnetic coupling. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2004)

Transition Metal Ion Directed Self‐Assembly of Polynuclear Coordination Complexes: Structural Characterization and Magnetic Properties

Organometallic radical-initiated carbon-sulfur bond cleavage and carbon-carbon coupling in dithiocarbamate and thiocarbenoid cyclopentadienylchromium complexes

A trinuclear cobalt complex, [Co3(μ3-S)(μ-CNEt2)(μ-SCNEt2)2(PPh3)2Cl]·2CH3CN, comprising moieties derived from single and double C–S bond cleavage of diethyldithiocarbamate was isolated and characterized by X-ray structural analysis.

A novel trinuclear cobalt complex comprising moieties derived from single and double C–S bond cleavage of diethyldithiocarbamate

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A novel trinuclear cobalt complex comprising moieties derived from single and double C–S bond cleavage of diethyldithiocarbamate