Arene Ruthenium(II) Complexes Bearing the κ-P or κ-P,κ-S Ph2P(CH2)3SPh Ligand

Neutral [Ru(η6-arene)Cl2{Ph2P(CH2)3SPh-κP}] (arene = benzene, indane, 1,2,3,4-tetrahydronaphthalene: 2a, 2c and 2d) and cationic [Ru(η6-arene)Cl(Ph2P(CH2)3SPh-κP,κS)]X complexes (arene = mesitylene, 1,4-dihydronaphthalene; X = Cl: 3b, 3e; arene = benzene, mesitylene, indane, 1,2,3,4-tetrahydronaphthalene, and 1,4-dihydronaphthalene; X = PF6: 4a–4e) complexes were prepared and characterized by elemental analysis, IR, 1H, 13C and 31P NMR spectroscopy and also by single-crystal X-ray diffraction analyses. The stability of the complexes has been investigated in DMSO. Complexes have been assessed for their cytotoxic activity against 518A2, 8505C, A253, MCF-7 and SW480 cell lines. Generally, complexes exhibited activity in the lower micromolar range; moreover, they are found to be more active than cisplatin. For the most active ruthenium(II) complex, 4b, bearing mesitylene as ligand, the mechanism of action against 8505C cisplatin resistant cell line was determined. Complex 4b induced apoptosis accompanied by caspase activation.

NMR Determination of Free Fatty Acids in Vegetable Oils

The identification and quantification of free fatty acids (FFA) in edible and non-edible vegetable oils, including waste cooking oils, is a crucial index to assess their quality and drives their use in different application fields. NMR spectroscopy represents an alternative tool to conventional methods for the determination of FFA content, providing us with interesting advantages. Here the approaches reported in the literature based on 1H, 13C and 31P NMR are illustrated and compared, highlighting the pros and cons of the suggested strategies.

K2CO3/Al2O3: An Efficient and Recyclable Catalyst for One-Pot, Three Components Synthesis of α-Aminophosphonates and Bioactivity Evaluation

A simple and efficient method has been employed for synthesis of a novel series of biologically active α-aminophosphonates (4a-j) by reacting 1H-benzo[d]imidazole-2-carbaldehyde (1) and various aromatic amines (2a-j) and diethyl/dimethyl phosphite (3) by Kabachnik-Field's reaction in the presence of efficient heterogeneous K2CO3/Al2O3 catalyst under solvent-free conditions at 140 ºC. Structures of all the compounds were confirmed by 1H, 13C and 31P NMR and LC-MS. In addition to this antioxidant activity were also evaluated.

Synthesis and crystallographic structure of nickel(0) carbonyl complex with Bitianp, an atropoisomeric diphosphine

The reaction between an atropoisomeric diphosphine, Bitianp and [Ni(CO)4] was achieved by direct condensation in CH3Cl to afford complexes of general formula [Ni(CO)2(Bitianp)]. This compound was characterized by elemental analysis, IR, 1H-, 13C- and 31P-NMR spectroscopies. The structure of nickel complex has been determined by X-ray crystal-lography. Crystal data for C42H28NiO2P2S2 (M = 749.41 g/mol): triclinic, space group P-1 (no. 2), a = 10.539(2) Å, b = 11.811(2) Å, c = 15.994(3) Å, α = 83.93(3)°, β = 88.18(3)°, γ = 65.24(3)°, V = 1797.6(7) Å3, Z = 2, T = 294(2) K, μ(MoKα) = 0.781 mm-1, Dcalc =1.385 g/cm3, 22744 reflections measured (2.56° ≤ 2Θ ≤ 64.726°), 11837 unique (Rint = 0.0157, Rsigma = 0.0215) which were used in all calculations. The final R1 was 0.0360 (I > 2σ(I)) and wR2 was 0.1088 (all data). The coordination sphere of the Ni center is best described as a tetrahedral geometry.

Synthesis and Characterization of Enantiopure Tribenzotriquinacene Dimers Bearing a Platinum-Diacetylene Unit

A pair of enantiomerically pure metallodimers containing two deeply concave tribenzotriquinacene (TBTQ) units linked by a platinum-diacetylene unit were synthesized. Such linear metal-centered TBTQ dimers are considered as edges of metallosquares and metallocubes that bear four or eight mutually syn-oriented TBTQ bowls at their tips, respectively. The structures of the metallodimers were characterized by 1H, 13C and 31P NMR spectroscopy, ESI mass spectrometry, and circular dichroism. The single X-ray crystal structure of (+)-enantiomer confirmed the absolute configuration of the metallodimers and revealed an edge (tip-to-tip) length of 18.456 Å and an approximated syn-orientation of the two TBTQ bowls in the solid state.

Synthesis, characterization and antimicrobial activity of (5- bromo-5-nitro-2-oxido-1,3,2-dioxaphosphinan-2-yl)amino acid esters

Synthesis of a new series of (5-bromo-5-nitro-2-oxido-1,3,2- dioxaphosphinan-2-yl)amino acid esters (3a-l) was accomplished via a two step process, which involves the prior preparation of the monochloride intermediate (2) and its subsequent reaction with the amino acid esters in dry tetrahydrofuran in the presence of triethylamine at reflux temperature. The title compounds (3a-l) structures were established by analytical, IR, 1H-, 13C- and 31P-NMR, and mass spectral data. They exhibited significant antibacterial and antifungal activity.