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71.
A. A. Koridze A. M. Sheloumov F. M. Dolgushin A. I. Yanovsky P. V. Petrovskii O. L. Tok 《Russian Chemical Bulletin》1998,47(5):995-1000
Reactions of the alkyne cluster Os3(μ-CO)(CO)9(μ3-Me3C2Me) with alkynes Me3SiC≡CR (R=Me, Bun) in refluxing hexane result in the formation of clusters Os3(CO)9{μ3-C(SiMe3)=C(Me)C=C(SiMe3)=C(Me)C=C(SiMe3)R} (2a: R=Me;3a: R=Bun). The dienediyl ligand in these complexes is formed by alkyne-vinylidene coupling, with vinylidene generated in the course of reaction from the alkyne molecule by the acetylene-vinylidene rearrangement involving a 1,2-shift of the Me3Si group. The structure of cluster3a was determined by X-ray structural analysis. The dienediyl ligand is coordinated to three metal atoms of the cluster framework by two π-ethylene bonds with two osmium atoms and two σ-bonds with the third osmium atom with the formation of the osmacyclobutene moiety. The1H and13C NMR study of13CO-enriched samples of clusters2a and3a revealed the stereochemical nonrigidity of these molecules due to the exchange of the hydrocarbon and carbonyl ligands. 相似文献
72.
A. A. Kamyshova A. Z. Kreindlin P. V. Petrovskii A. S. Peregudov Yu. A. Borisov A. A. Koridze 《Russian Chemical Bulletin》2005,54(12):2805-2812
The reaction of [Cp*2RuBr]+Br− with bromine in CH2Cl2 (CD2Cl2) in an inert atmosphere at room temperature produces the complexes [Cp*Ru(Br)C5Me4CH2Br]+Br3
− (syn conformer), [Cp*Ru(Br)C5Me3(CH2Br)2]+ (syn and anti conformers), and [Ru(Br)(C5Me4CH2Br)2]+ (syn conformer). All complexes were characterized by 1H and 13C NMR spectroscopy; the former complex, by elemental analysis. These complexes were also prepared by the reaction of [Cp*RuC5Me4CH2]+BF4
− with bromine in CH2Cl2.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 12, pp. 2712–2718, December, 2005. 相似文献
73.
Several 57Fe-labeled ferrocene derivatives and other cyclopentadienyliron complexes were studied by 57Fe and 13C NMR with respect to isotope-induced chemical shifts 1Delta12/13C(57Fe) and the magnitude and sign of coupling constants 1J(57Fe,13C) and 2J(57Fe,1H). The geometries of the complexes were optimized by DFT methods [B3LYP/6-311+G(d,p)] and chemical shifts (GIAO) and coupling constants were calculated at the same level of theory. The trends in calculated 57Fe nuclear shielding agree well with the experimental data and, in the case of coupling constants 1J(57Fe,13C) and 2J(57Fe,1H), both sign and magnitude are correctly reproduced. 相似文献
74.
O. A. Kizas A. V. Usatov P. V. Petrovskii M. G. Ezernitskaya F. M. Dolgushin A. I. Yanovsky Yu. N. Novikov A. A. Koridze 《Russian Chemical Bulletin》1998,47(9):1797-1804
The reaction of Os3(μ-Cl)2(CO)10 (1) with Ph2PCH2PPh2 (dppm) in a toluene solution at 65°C results in novel osmium complexes [Os3(μ-Cl)2(CO)9]2(dppm) (2) and [Os3(μ-Cl)2(CO)8]2(dppm)2 (3). Compounds 2 and 3 were characterized by1H and31P NMR, and IR spectroscopy and their structures were established by X-ray analysis. In both compounds, dppm is a bridging
ligand between the two cluster units. Molecule3 can be considered as an unusual 12-membered macrocycle containing C, P, Cl, and Os atoms in the ring.
Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 9, pp. 1844–1851, September, 1998. 相似文献
75.
The first (trifluoromethyl)tetramethylruthenocene-based ruthenium pincer complex RuCl(CO)[{2,5-(Bu 2 t PCH2)2C5H2}Ru(C5Me4CF3)] was synthesized by cyclometallation of the bisphosphine ligand {1,3-(Bu 2 t PCH2)2C5H2}Ru(C5Me4CF3) with RuCl2(DMSO)4 in 2-methoxyethanol in the presence of NEt3. The new complex was fully characterized by 1H, 19F, 31P{1H}, 13C{1H} NMR and IR spectroscopy. 相似文献
76.
I. T. Chizhevskii A. A. Koridze P. V. Petrovskii N. E. Kolobova 《Russian Chemical Bulletin》1981,30(5):884-886
Conclusions New rhodium complexes, derivatives of Rh(
4-C7H8)(acac) and Rh(
4-C7H8)(
5-C5H5) with functional groups in the norbornadiene ligand, have been synthesized.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 5, pp. 1124–1127, May, 1981. 相似文献
77.
Rudovský J Botta M Hermann P Koridze A Aime S 《Dalton transactions (Cambridge, England : 2003)》2006,(19):2323-2333
A novel "ditopic" ligand containing two monophosphinate triacetate DOTA-like units linked by a thiourea bridge has been synthesized and its complexes with Ln3+ ions (Ln = Y, Eu, Gd, Dy) investigated by NMR spectroscopy and relaxometry. The presence of one water molecule in the first coordination sphere has been determined by the measurement of the dysprosium(III)-induced 17O NMR shifts. The 1H and 31P NMR spectra of the Eu(III) derivative indicate a higher abundance of the fast-exchanging twisted square antiprismatic (m) isomer than the isomeric square antiprismatic (M; m/M = 3:2) complex. The analysis of the 89Y and 13C T1 NMR relaxation times in the Gd(III)/Y(III) mixed complex have provided useful structural information. Values of ca. 6.3 and 8.2 A for the Gd...Y and Gd...C distances, respectively, have been estimated which indicate a rather compact solution structure. This result finds support in the value of the relaxivity whose increase (at 20 MHz and 298 K) on passing from the monomeric (5.7 s(-1) mM(-1)) to the ditopic complex (8.2 s(-1) mM(-1)) can be attributed to the doubling of the inner-sphere term following the doubling of the molecular size. The structural and dynamic relaxivity-controlling parameters were assessed by a simultaneous fitting of the variable temperature 17O NMR and 1H NMRD relaxometric data. The mean water residence lifetime (298tauM) has been found to be 53 ns, one of the shortest values reported for ditopic complexes. The reorientational correlation time is two times longer (298tauR = 183 ps) than the corresponding value of the parent monomeric Gd(III) complex, thus supporting the view of a limited degree of internal rotation. The possible influence of magnetic Gd-Gd coupling has been excluded by a comparison of the 1H NMRD profiles of the homodinuclear Gd(III)/Gd(III) and the heterodinuclear Gd(III)/Y(III) complexes. 相似文献
78.
Polukeev AV Kuklin SA Petrovskii PV Peregudova SM Smol'yakov AF Dolgushin FM Koridze AA 《Dalton transactions (Cambridge, England : 2003)》2011,40(27):7201-7209
Palladium fluorophenyl complexes with different pincer ligands Pd(Ar)[2,6-(tBu(2)PCH(2))(2)C(6)H(3)] (13), Pd(Ar)[2,6-(tBu(2)PO)(2)C(6)H(3)] (14), Pd(Ar)[{2,5-(tBu(2)PCH(2))(2)C(5)H(2)}Fe(C(5)H(5))] (15), and Pd(Ar)[{2,5-(tBu(2)PCH(2))(2)C(5)H(2)}Ru(C(5)H(5))] (16) were synthesized by the reaction of LiAr (Ar = C(6)H(4)F-4) with the respective trifluoroacetate palladium pincer complexes 9-12. The molecular structures of 14 and 16 were determined by an X-ray crystallographic method. Complexes 13-16 and {Pd(Ar)[{2,5-(tBu(2)PCH(2))(2)C(5)H(2)}Fe(C(5)H(5))]}PF(6) (17) were studied by multinuclear NMR spectroscopy and cyclic voltammetry. On the basis of (19)F NMR chemical shifts and (1)J((13)C-(19)F) coupling constants, as well as Pd(II)/Pd(IV) oxidation potentials, electronic characteristics of the corresponding pincer ligands were elucidated. 相似文献
79.
80.
Ivanov D. M. Kuklin S. A. Polezhaev A. V. Petrovskii P. V. Smol’yakov A. F. Dolgushin F. M. Ezernitskaya M. G. Peregudov A. S. Koridze A. A. 《Russian Chemical Bulletin》2009,58(8):1701-1706
Resorcinol-based ruthenium bis(phosphinite) complexes were synthesized. Complexes RuCl(CO)[2,6-(But
2PO)2C6H3] (9) and RuH(CO)[2,6-(But
2PO)2C6H3] (10) were obtained by cyclometallation of 1,3-(But
2PO)2C6H3 with RuCl2(DMSO)4 in 2-methoxyethanol in the presence of Hünig’s base. The interconversion of complexes 9 and 10 was studied. The addition of carbon monoxide to complexes 9 and 10 yielded 18e adducts, RuCl(CO)2[2,6-(But
2PO)2C6H3] (11) and RuH(CO)2[2,6-(But
2PO)2C6H3] (12), respectively. In the case of complex 9, this reaction is reversible. Reaction of complex 10 with trifluoroacetic acid resulted in complex Ru(CF3COO)(CO)[2,6-(But
2PO)2C6H3] (13), which reacted with carbon monoxide to give complex Ru(CF3COO)(CO)2[2,6-(But
2PO)2C6H3] (14). Based on the IR spectral data, the TFA ligand in complexes 13 and 14 is bound in a bi- and monodentate fashion, respectively. The structure of compound 9 was determined by X-ray diffraction analysis. 相似文献