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1.
V. V. Semenov N. V. Melenskova N. F. Cherepennikova Yu. A. Kurskii O. V. Kuznetsova M. A. Lopatin 《Russian Journal of Applied Chemistry》2007,80(4):647-653
A mixture of two isomers of organosilicon carbofunctional compounds, 4-(3′-triethoxysilylpropylimino)pent-2-en-2-ol (EtO)3Si-CH2CH2CH2-N=C(Me)-CH=C(Me)-OH (Ia, 83%) and 4-(3′-triethoxysilylpropylamino)pent-3-en-2-one (EtO)3-CH2CH2CH2-NH-C(Me)=CH-C(O)Me (Ib, 17%) was prepared by reaction of 3-aminopropyltriethoxysilane with acetylacetone. The use of trimethylsilyl ether of acetylacetone instead of acetylacetone yields Ia (84%) and silylated derivatives (Me3SiO)n(EtO)3?n Si-CH2CH2CH2-N=C(Me)CH=C(Me)OH (II) (16%). Solid, liquid, or resinous products were prepared by hydrolytic condensation of I and II. Compositions for preparing transparent sol-gel films were developed. 相似文献
2.
L. S. Zakharov G. N. Molchanova T. M. Shcherbina P. V. Petrovskii M. I. Kabachnik 《Russian Chemical Bulletin》1998,47(9):1718-1724
A number of trialkylsilylmethyl diphenyl phosphates MeRR′SiCH2OP(O)(OPh)2 (1a-e: R=Et (a), Pr (b), CF3CH2CH2 (c, e), Me3SiCH2 (d); R′=Me (a-d), Et (e)) were synthesized and their thermal rearrangement, of the 1,2-shift type, was studied. The rearrangement consists of the
migration of an alkyl group from Si atom to the methylene carbon atom and gives the corresponding silyl esters. The rate of
the rearrangement was found to increase in the order1d<1b<1a<1 (R=R′=Me)<1c corresponding to the enhancement of the total inductive effect (−I) of the substituents at the Si atom. The relative migration ability of the substituents at the Si atom, determined by GC/MS
analysis of the disiloxane fraction resulting from hydrolysis of pyrolyzed phosphates1a-e, increases in the order R=Pr<Et<CF3CH2CH2<Me≪Me3SiCH2, which differs substantially from the order in which the rate of the rearrangement of phosphates1a-d changes. The electronegativity of the migrating group affects noticeably the relative ability to migrate.
For Part 4, see Ref. 1.
Deceased.
Translated fromIzvestiya Akademii Nauk, Seriya Khimicheskaya, No. 9, pp. 1767–1772, September, 1998. 相似文献
3.
Aldo Arrais Enrico Boccaleri Enrico Sappa Andrea Secco 《Journal of Sol-Gel Science and Technology》2006,38(3):283-292
Co2(CO)8 has been reacted with but-2-yn-1,4-diol (BUD) and the reactivity of the resulting complex Co2(CO)6(HOCH2C≡CCH2OH) (complex 1) is discussed. Complex 1 has been reacted with all the components used in the synthesis of sol-gel materials based on tetraethyl-orthosilicate (TEOS)
with the aim at obtaining evidences for the processes occurring during the formation of inorganic-organometallic sol-gel materials
containing BUD. Reaction pathways are discussed.
BUD and complex 1 have also been reacted with 3-(triethoxysilyl)propyl isocyanate (TSI); the new ligand [(EtO)3Si(CH2)3NHC(— O)OCH2C≡CCH2OC(—O)NH(C H2)3Si(OEt)3] (TB) and the complex Co2(CO)6[(EtO)3Si(CH2)3NHC(—O)OCH2C≡CCH2OC(—O)NH(CH2)3Si(OEt)3] (11) have been obtained; these were characterized by means of spectroscopic techniques and mass spectrometry. Reactions of ligand
TB and of complex 11 with TEOS have been performed. “Condensation” reactions of ligand TB (with TB) and of complex 11 (with complex 11) have also been attempted. Solid, amorphous materials were obtained: these were characterized by means of IR-Raman, SEM microscopy
and XRD on powders. 相似文献
4.
E. K. Beloglazkina A. V. Shimorsky A. G. Mazhuga O. V. Shilova V. A. Tafeenko N. V. Zyk 《Russian Journal of General Chemistry》2009,79(7):1504-1508
Cu(ClO4)2·6H2O was shown to react with 2,2′-[propane-1,3-diylbis(thio-2-phenylnemethylidene]-bis(3-pyridylamine) (I) or (5Z)-2-ethoxycarbonylmethyl-(2-pyridylmethylidene)-3,5-dihydro-4H-imidazol-4-one (II) in the presence of CH3CN with the reduction of copper(II) to copper(I) and the formation of the tetrahedral complex CuI(CH3CN)4ClO4 (III). In the course of the reaction the organic ligands I and II were oxidized to the corresponding sulfoxides. 相似文献
5.
A. S. Antsyshkina G. G. Sadikov S. A. Syrbu M. N. Rodnikova M. R. Kiselev V. A. Burmistrov S. A. Kuvshinova A. A. Syrbu 《Russian Journal of Inorganic Chemistry》2011,56(11):1800-1811
The molecular and crystal structures of N≡C-C6H4-C6H4-O-(CH2)8-O-CO-CH=CH2 (4(3-acryloyloxy)octyloxy-4′-cyanobiphenyl) (I) and N≡C-C6H4-C6H4-O-(CH2)6-O-CO-CH=CH2 (4(3-acryloyloxy)hexyloxy-4′-cyanobiphenyl) (II) were determined by X-ray diffraction. The structures of I and II are stereotype. The space group of I and II is C2/c, Z = 8; lattice parameters I: a = 34.677(7)?, b = 9.452(2)?, c = 13.004(3) ?, β = 99.30(3)°; II: a = 30.858(6) ?, b = 9.504(2) ?, c = 13.082(2) ?, β = 92.78(3)°. The planar extended molecules I and II are packed in the unit cell to give clearly differentiated aliphatic and aromatic regions throughout the whole crystal. All
intermolecular contacts are concentrated in the aromatic region. The molecular packing is very loose but the aromatic areas
of I and II fully coincide. The only free parameter of the structure is the length of the aliphatic chain (CH2)n (n = 8 and 6). According to DSC data, compound I possesses enantiotropic mesomorphism and II possesses monotropic mesomorphism. 相似文献
6.
V. V. Semenov N. F. Cherepennikova N. V. Melenskova O. V. Kuznetsova B. A. Bushuk S. B. Bushuk Yu. A. Kal’vinkovskaya W. E. Duglas 《Russian Journal of Coordination Chemistry》2007,33(7):539-545
A reaction of 3-aminopropyl(triethoxy)silane with acetylacetone gave a mixture of two isomeric carbon-functionalized organosilicon compounds capable of complexation and sol-gel polymerization. These were 4-(3′-triethoxysilylpropylimino)-pent-2-en-2-ol (EtO)3Si-CH2CH2CH2-N=C(Me)CH=C(Me)OH (Ia, 83%) and 4-(3′-triethoxysilylpropylamino)-pent-3-en-2-one (EtO)3Si-CH2CH2CH2-NH-C(Me)=CH-C(O)Me (Ib, 17%). With acetylacetone trimethylsilyl ether instead of acetylacetone itself, compound Ia and silylated derivatives (Me3SiO) n (EtO)3 ? n Si-CH2CH2CH2-N=C(Me)CH=C(Me)OH were obtained as admixture in 84 and 16% yields, respectively. Reactions of ligands Ia and Ib with europium and terbium propan-2-olates afforded the corresponding complexes. Formulations of lanthanide complexes, oligodimethylsiloxanediols, and 3-aminopropyl(triethoxy)silane were used to prepare transparent sol-gel films. The photoluminescence spectra of the films show narrow bands due to Eu3+ or Tb3+ emission. Emission from the organosilicon matrix appears as a broad band at 430 to 435 nm. 相似文献
7.
Synthesis,crystal structures,and catalytic property of dioxomolybdenum(VI) complexes with hydrazones
Two new dioxomolybdenum(VI) complexes, [MoO2(L1)]
n
· 0.5
n
CH3OH (I) and [MoO2(L2)(CH3OH)] (II), where L1 and L2 are the dianionic form of N′-[1-(4-diethylamino-2-hydroxyphenyl)methylidene]isonicotinohydrazide and N′-(2-hydroxy-4-methoxybenzylidene)-3-methylbenzohydrazide, respectively, were prepared and structurally characterized by physicochemical
and spectroscopic methods and single-crystal X-ray determination. For complex I, a polymeric structure is obtained, which is linked by coordination of the pyridine N atoms to the Mo atoms of other [MoO2(L1)] units. Complex II is a mononuclear molybdenum compound. In both complexes, the Mo atoms are in octahedral coordination. The catalytic properties
of the complexes indicate that they are efficient catalysts for sulfoxidation. 相似文献
8.
S. N. Adamovich R. G. Mirskov A. N. Mirskova M. G. Voronkov 《Russian Journal of General Chemistry》2010,80(10):1972-1973
Reaction of tris(2-hydroxyethyl)amine hydrochloride Cl− N+H(CH2CH2OH)3 with zinc diacetate and bis(2-methylphenoxy)acetate in the molar ratio 2: 1 results in complexes 2[Cl− N+H(CH2CH2OH)3]· Zn (OCOR)2 (I, II) R= Me (I), 2-MeC6H4OCH2 (II), which contain two protatrane cations linked with zinc diacylate by two coordination bonds HO → Zn. Complexes I and II are also formed by the reaction of the corresponding tris(2-hydroxyethyl)amine hydrochloride acylate RCOO−N+H(CH2CH2OH)3 with ZnCl2. The structure of complexes I, II is proved by elemental analysis, IR and 1H, 13C, 15N NMR spectroscopy. 相似文献
9.
Giuliana Gervasio Domenica Marabello Enrico Sappa Andrea Secco 《Journal of Cluster Science》2007,18(1):67-85
Ru3(CO)12 has been reacted with the compounds hex-1-en-3-yne [EtC≡CCH=CH2], 2-methyl-hex-1-en-3-yne [EtC≡CC(=CH2)CH3] and with 3(ethoxy-silyl)propyl isocyanate [(EtO)3Si(CH2)3NCO] and the compound tb [(EtO)3Si(CH2)3NHC(=O)OCH2C≡CCH2OC(=O)NH(CH2)3Si(OEt)3] in hydrocarbon solution. Some reactions in CH3OH/KOH solution (followed by acidification) have also been performed.
The main products of the reactions with ene-ynes are the clusters Ru3(CO)6(μ-CO)2L2 (L = C6H8, C7H10) and their demolition products, the “ferrole” Ru2(CO)6L2 complexes. One of the isomers of Ru3(CO)6(μ-CO)2L2, and Ru2(CO)6L2 (L = C7H10) have been reacted with vinyl-triethoxysilane [(EtO)3SiCH=CH2]: these reactions did not afford complexes containing new carbon–carbon bonds or triethoxy-silyl groups. Only polymerization
of vinyl-triethoxysilane occurred.
The reactions of Ru3(CO)12 with triethoxysilyl-propyl-isocyanate and tb (in the presence of Me3NO) lead to the same products, that is the isomeric complexes (μ-H)Ru3(CO)9[C=N(H)(CH2)3Si(OEt)3] with a “perpendicular” ligand (complex 3, as proposed on the basis of spectroscopic results) and (μ-H)Ru3(CO)9[HC=N(CH2)3Si(OEt)3] with a “parallel” ligand (complex 4, as confirmed by a X-ray analysis). The reaction pathways leading to these products are discussed. Complex 4 has been reacted with tetraethyl orthosilicate and the resulting material has been characterized. These reactions are part
of a study on the synthesis of inorganic-organometallic materials through sol–gel techniques.
This paper is dedicated to Prof. Gunther Schmid in the occasion of his 70th birthday. 相似文献
10.
The reaction of aminomethylated polystyrene (PSCH2-NH2) and 2-hydroxyacetanilide in DMF results in the formation of polystyrene-anchored monobasic bidentate Schiff base, PSCH2-LH (I). On the other hand, the reaction of chloromethylated polystyrene (PSCH2-Cl), 3-formylsalicylic acid, ethylenediamine and acetylacetone in DMF in presence of ethyl acetate (EA) and triethylamine
(TEA) produces another polystyrene-anchored dibasic tetradentate Schiff base, PSCH2-L′H2 (II). BothI andII react with a number of di-, tri-and hexavalent metal ions like Co, Ni, Cu, Zn and Cd to form polystyreneanchored coordination
compounds, and these have been characterized and discussed. 相似文献
11.
S. A. Adonin A. V. Virovets M. N. Sokolov V. P. Fedin 《Russian Journal of Coordination Chemistry》2010,36(10):734-738
New cluster complexes [W3S4(Acac)3(PPh3)3]PF6 · 0.5CHCl3 (Acac = CH3C(O)CHC(O)CH3) (I) and [W3S4(Hfac)3(PPh3)2Br] · 2CHCl3 (Hfac = CF3C(O)CHC(O)CF3) (II) were synthesized. Their molecular and crystal structures were determined by X-ray diffraction. The cis-cis type of coordination of acetylacetonate and hexafluoroacetylacetonate ligands in I and II, respectively, was established, and the PPh3 ligands were found in the trans-positions with respect to the “capping” sulfide ligand (μ3-S). 相似文献
12.
E. V. Osintseva L. K. Neudachina Yu. G. Yatluk 《Russian Journal of Inorganic Chemistry》2010,55(10):1644-1650
The azo coupling reaction of N-(2-carboxyethyl)anthranilic acid and N,N,N′,N′-tetrabis(2-carboxyethyl)-1,3-phenylenediamine with diazosulfanilic acid yielded the complexones sodium 4-N-(2-carboxyethyl)amino-5-carboxyazobenzene-4′-sulfonate
(I) and 2,4-N,N,N′,N′-tetrabis(2-carboxyethyl)diaminoazobenzene-4′-sulfonic acid (II), respectively. The acidity constants of I and II (20°C, μ = 0.1M KCl) were determined to be as follows: for I, pK
00 = 1.29 ± 0.13, pK
0 = 2.92 ± 0.07, pK
1 = 3.92 ± 0.05, pK
2 = 5.16 ± 0.03; for II, pK
00 = 2.35 ± 0.06, pK
0 = 2.81 ± 0.09, pK
1 = 3.21 ± 0.11, pK
2 = 3.81 ± 0.09, pK
3 = 4.34 ± 0.04, pK
4 = 5.03 ± 0.06, pK
5 = 6.67 ± 0.07. The electronic absorption spectra of I and II were measured, and acid-base equilibrium scheme for I and II in aqueous solutions were suggested. The complexation constants of I and II with copper(II) ions were determined to be logK
CuQI= 5.47 ± 0.06 and logK
CuQII= 5.72 ± 0.13 (20°C, μ = 0.1 M KCl). 相似文献
13.
E. Yu. Ladilina V. V. Semenov Yu. A. Kurskii O. V. Kuznetsova M. A. Lopatin B. A. Bushuk S. B. Bushuk W. E. Douglas 《Russian Chemical Bulletin》2005,54(5):1160-1168
Novel fluorine-containing carbofunctional organosilicon monomers were synthesized: 3-pentafluorobenzylideneaminopropylethoxysilane
(EtO)3Si(CH2)3N=CH-C6F5, N-3-methoxydiethoxysilylpropyltrifluoroacetamide (EtO)2(MeO)Si(CH2)3NHC(O)CF3, and 1,1,5-trihydrooctafluoroamyl N-3-triethoxysilylpropylaminopropanoate (EtO)3Si(CH2)3NH(CH2)2C(O)OCH2(CF2)3CHF2. Compositions for the formation of transparent thermally stable films were prepared from these monomers. The films have low
absorbance intensity near 1550 nm, i.e., in the region of photosignal transmission of modern optical communication systems. The compositions can dissolve complexes
with organofluorine ligands and produce transparent homogeneous films doped with rare-earth metals. The concentrations of
the complexes in the matrices are 3.7–21.4 wt.% (metal concentrations are 0.6–3.7%). Fluorescence and fluorescence excitation
spectra of the matrices and electronic absorption spectra of the doped films were studied.
__________
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 5, pp. 1131–1138, May, 2005. 相似文献
14.
Prithwiraj Byabartta 《Russian Journal of General Chemistry》2009,79(6):1214-1217
The reaction of [Ni(dppa)(Cl)2] or [Ni(dppa)(Br)2] with AgOTf gives [Ni(dppa)(OTf)2], which then form [Ni(dppa)(RaaiR)](OSO2CF3)2 under the action of arylazoimidazole(RaaiR) in a dichloromethane medium [RaaiR′ = p-R-C6H4-N=N-C3H2-NN-1-R′, (I–III), abbreviated as N,N′-chelating agent, where N(imidazole) and N(azo) represent N and N’, respectively; R = H (a), Me (b), Cl (c) and R′ = Me (I), CH2CH3 (II), CH2Ph (III), OSO2CF3 is the triflate anion]. The 1H NMR spectral measurements suggest that a bound azoimine is responsible for a number of signals of phenyl protons in the
aromatic region. The molecules of the complexes contain a number of different carbon atoms which gives a number of different
peaks in the 13C (1H) NMR spectrum. The text was submitted by the author in English.
The text was submitted by the author in English. 相似文献
15.
V. F. Shul’gin E. A. Sarnit O. V. Konnik E. B. Rusanov A. S. Bogomyakov V. I. Ovcharenko V. V. Minin 《Russian Journal of Coordination Chemistry》2012,38(1):44-49
The structures and results of the static magnetic susceptibility investigation of the copper(II) binuclear complex with salicylic
acid diacyl hydrazide (H2L), [Cu2(L)(Py)4] (I), and the copper(II) trinuclear complex with diacyl dihydrazide of salicylic and glutaric acids (H6L′), [Cu3(L′)(Py)4] · 2Py (II), are described. The exchange antiferromagnetic interactions between the paramagnetic centers with the exchange interaction
parameter −2J = 119 cm−1 for dimer I and 14 cm−1 for trinuclear complex II are detected. 相似文献
16.
S. P. Khranenko P. E. Plusnin L. A. Sheludyakova Yu. V. Gerasimova I. V. Korol’kov S. V. Korenev 《Russian Journal of Coordination Chemistry》2009,35(9):681-686
Complexation between crystalline trans-[Pd(H2O)2(NO3)2] and acetylacetone was studied. The complexes Pd2(Acac)2(μ-NO3)2(I) and Pd2(Acac)2(μ-Acac)(μ-NO3)(II) were obtained and examined by elemental analysis, X-ray powder diffraction analysis, differential scanning calorimetry,
simultaneous thermal analysis, mass spectrometry, and vibrational spectroscopy. 相似文献
17.
L. B. Serezhkina E. V. Peresypkina A. V. Virovets N. A. Neklyudova 《Russian Journal of Inorganic Chemistry》2010,55(7):1020-1025
Single crystals of (H3O)[UO2(CH3COO)3] (I) and (NH(C2H5)3)[UO2(CH3COO)3] (II) are synthesized, and their structures are studied by X-ray crystallography. Compound I crystallizes in the tetragonal crystal system with the unit cell parameters a = 13.70640(10) ?, c = 27.5258(5) ?, V = 5171.14(11) ?3, space group I41/a, Z = 16, R = 0.0238. The crystals of compound II are orthorhombic with the parameters a = 13.3685(3) ?, b = 10.6990(3) ?, c = 12.2616(3) ?, V = 1753.77(8) ?3, space group Pna21, Z = 4, R = 0.0228. The uranium-containing structural units of crystals I and II are [UO2(CH3COO)3]− island mononuclear groups belonging to the A B301(A = UO22+, B01 = CH3COO−) crystal-chemical group of uranyl complexes. [UO2(CH3COO)3]− complexes are linked into a three-dimensional framework by electrostatic interactions with the outer-sphere cations and by
hydrogen bonds involving the hydrogen atoms of hydroxonium (I) or triethylammonium (II) with the oxygen atoms of the acetato groups. 相似文献
18.
C. I. Ratcliffe S. K. Garg D. W. Davidson 《Journal of inclusion phenomena and macrocyclic chemistry》1990,8(1-2):159-175
Polycrystalline (CH3)4NOH·5 H2O (I) and (CH3)4NOD·5D2O (II) have been studied by1H NMR lineshapes, second moments and spin-lattice relaxation times and by2H NMR lineshapes as a function of temperature. From low temperatures the first motion to occur is reorientation of the internally rigid (CH3)4N+ ion about a uniqueC
3
axis (E
ta
= 8.37 kJ/mol forI,E
a
= 9.00 kJ/mole forII), followed closely by pseudo isotropic reorientation of the whole ion (E
a
= 18.10 kJ/mol). Motion of the cage molecules (water and hydroxide ion) occurs at higher temperatures with an apparentE
a
= 11.30 kJ/mol. There is some evidence of a phase transition inII but notI in the 220–230 K region.2H NMR lineshapes ofII below 220 K indicate static cage molecules. Some of the2H quadrupole coupling constants derived from these spectra correspond to O·O hydrogen-bond distances which are incompatible with the known room temperature structure ofI. Above the possible transition inII the anisotropic2H lineshapes indicate rapid motion of2H among all possible hydrogen-bond sites via transfer along the bonds and molecular reorientation. This motion persists in the high temperature phase but the lineshape becomes isotropic due to the cubic symmetry of this phase. It is possible that1H or2H tunnelling plays an important part in the motion of the cage molecules and the different phase behaviour ofI andII.Dedicated to Dr D. W. Davidson in honor of his great contributions to the sciences of inclusion phenomena. 相似文献
19.
S. A. Adonin A. V. Virovets M. N. Sokolov V. P. Fedin 《Russian Journal of Coordination Chemistry》2010,36(12):871-875
The crystal structure of the new cluster complex (Et4N)2[Mo3S7Cl6] · CH3CN · H2O (I) was determined. Heating of a solution of I in CH3CN under solvothermal conditions (120°C) induces replacement of one Cl− ligand by CH3CN to give (Et4N)[Mo3S7Cl5(CH3CN)] (II). The product was also studied by X-ray diffraction analysis. 相似文献
20.
S. P. Petrosyants A. B. Ilyukhin V. A. Ketsko 《Russian Journal of Inorganic Chemistry》2008,53(6):879-883
The reaction of indium thiocyanate with bipyridine (4,4-Bipy) and urotropine (Ur) gave [H2(4,4′-Bipy)][In(H2O)2(NCS)4]2 (I) and [HUr]2[In(H2O)(NCS)5] · 2H2O (II), which were identified using elemental analysis, IR spectra, and thermogravimetric analysis. The thermal decomposition of
compound I and II ends at 650 and 640°C, respectively, and gives In2O3. X-Ray diffraction analysis of compound I showed that complex anions in the crystal form chains through O-H…S hydrogen bonds. The anion chains form a close packing
of columns with bipyridine cations located in the voids.
Original Russian Text ? S.P. Petrosyants, A.B. Ilyukhin, V.A. Ketsko, 2008, published in Zhurnal Neorganicheskoi Khimii, 2008,
Vol. 53, No. 6, pp. 951–955. 相似文献