A set of samples C60(cr) was prepared and studied using X-ray diffraction analysis, 1H NMR, differential
scanning calorimetry (DSC), and gas adsorption methods for elucidating the state of residual solvents in C60.
The solvent molecules were found to be adsorbed at interfaces of the microcrystals of C60(cr); “sintering” of
the microcrystals on heating is assumed to be responsible for entrapping some of the solvent molecules in the
sample. This may explain the difficulty of removal of the solvents from fullerene samples. The disappearance
of the orientational phase transition in DSC curves of mechanically treated samples was interpreted in terms
of space defects in the crystals of C60.
Titanium(IV) coordination compounds are effectively used as precatalysts for ethylene polymerization and copolymerization with other olefins. New titanium(IV) complexes 3b-d with ligands containing two diphenylcarbinol fragments linked by the perfluorinated hydrocarbon units-CF 2or-C 2 F 4were synthesized. The structures of complexes 3b and 3d were determined by X-ray diffraction. Titanium atoms in 3b have a distorted trigonal-bipyramidal coordination environment while spiro-complex 3d is characterized by tetrahedral molecular geometry. The catalytic behavior of complexes activated by mixtures of Bu 2 Mg and alkylaluminium chlorides from among Me 2 AlCl, Et 2 AlCl, EtAlCl 2 , and Et 3 Al 2 Cl 3 were studied. The resulting catalytic systems catalyze ethylene polymerization to afford ultra-high molecular weight polyethylene, suitable for modern processing methods, and the solvent-free solid state formation of super high-strength (1.37-2.75 GPa) and high-modulus (up to 138 GPa) oriented film tapes. The same catalytic systems catalyze ethylene copolymerization with 1-hexene to afford high molecular weight semicrystalline elastomeric polymers containing up to 20% of comonomer units.
One or two step reactions of potassium and rubidium fullerides with composition M k C 60 (M = K, Rb; k = 3-6) and K 6 C 60 + m K mixtures (m = 1, 3) with anhydrous salts M´Cl 3 (M´ = La, Pr, Nd, Sm, Gd, Tb, Yb, Lu, Y, Sc) and YbI 2 in a toluene-THF medium afforded heterometallic fullerides M 3-n M´nC 60 (n = 1-3). Among these compounds, substituted fullerides with composition M 2 M´C 60 (M´ = Yb, Lu, Sc) display superconducting properties with critical temperatures of 14-20 K.
Abstract Spin-spin and spin-lattice relaxation times of nuclei 69,71Ga, 27Al, 14N in anions [MClnBr4-n]-and the solvate complexes [M(CH3CN)6]3+, produced from dissolution of MCl3 and MBr3 in the mixture CH3CN + CH3NO2 (M = Ga, Al), are measured in the temperature range from -40 up to + 70 °C. It is shown that nuclear spins of 69,71Ga, 27Al relax in the anionic and cationic complexes by means of the second-kind scalar and quadrupole relaxation mechanisms (due to the relaxation of the nuclei 35,37Cl, 79,81Br, 14N). The complexes [MClnBr4-n]-and [M(CH3CN)6]3+ in the investigated solutions are inert and do not undergo exchange processes in the NMR time scale. The scalar spin coupling constants in [M(CH3CN)6]3+ are determined from the scalar contribution to the relaxation rate of 69,71Ga, 27Al, and the measured relaxation time of 14N in the solvate complex; the results are J(69Ga-14N) = 59 ± 5 Hz, J(71Ga-14N) = 74 ± 6Hz, J(27Al-14N) = 22 ± 2Hz.
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