Synthese und Kristallstruktur von Dinatrium-di-μ/-oxo-bis[trihydroxo-methylantimonat(V)] / Synthesis and Crystal Structure of Disodium-di-μ-oxo-bis[trihydroxo-methylantimonate(V)]

1991 ◽  
Vol 46 (2) ◽  
pp. 139-142 ◽  
Author(s):  
Markus Wieber ◽  
Udo Simonis ◽  
Dieter Kraft

The oxidation of dialkoxymethylstibine with hydrogen peroxide in the presence of sodium hydroxide leads to the formation of disodium-di-μ-oxo-bis[trihydroxo-methylantimonate(V)]. The salt can be synthesized also by dissolving methanestibonic acid in an aqueous solution of sodium hydroxide. The crystal structure has been determined; it shows a dimeric molecule containing a four-membered ring with Sb -O -Sb linkages. Thermal decomposition and spectroscopic properties o f the com pound are discussed.

1996 ◽  
Vol 51 (8) ◽  
pp. 1141-1144 ◽  
Author(s):  
R. Buheitel ◽  
W. Milius ◽  
W. Schnick

Cl3Ti[N(SiMe2Cl)(SiMe2NH2)] is yielded by reaction of TiCl4 with two molecules ClMe2SiNHSiMe3. A single crystal structure determination (P 21/n, a = 747.12(2), b = 1294.1(3), c = 1496.7(3) pm, β = 90.30(3)°, Z = 4) shows a planar four-membered ring Ti-N-Si-N as the central feature of the monomers formed by a weak coordinative bond of the NH2 group to the Ti atoms. The monomers are connected to give dimers via two Cl bridges linked to the Ti atoms.


Author(s):  
Е.А. Максимова ◽  
А.В. Васильев

Проведено бензилирование арабиногалактана путем его реакции с бензилхлоридом в присутствии гидроксида натрия. Получено бензилированное производное арабиногалактана с выходом 90%. Бензилированное производное представляет собой гидрофобный клееподобный невысыхающий материал. В спектре ЯМР 13С бензилированного производного арабиногалактана содержатся сигналы в областях 130,0–143,3 м.д., отвечающие ароматическим атомам углерода бензильной группы. Осуществлено окисление арабиногалактана путем его реакции с перекисью водорода в присутствии хлорида железа (III) в водном растворе. Окисленное производное представляет собой маслообразное вещество. В спектре ЯМР 13С окисленного арабиногалактана присутствуют сигналы в области 158–173 м.д., соответствующие карбоксильным группам. Benzylation of arabinogalactan was carried by reaction with benzyl chloride in the presence of sodium hydroxide. The benzylated derivative was obtained in a yield of 90%. Benzylated arabinogalactan is hydrophobic, glue-like, non-drying material. 13C NMR spectrum of benzylated arabinogalactan contains signals in the range of 130.0–143.2 ppm. corresponding to the aromatic carbon atoms of the benzyl group. The oxidation of arabinogalactan by reaction with hydrogen peroxide in the presence of ferric chloride (III) in aqueous solution was done. The oxidized arabinogalactan is an oilish material. 13C NMR spectrum of oxidized arabinogalactan contains signals at 158–173 ppm corresponding to carboxyl groups.


Author(s):  
Dennis Mo ◽  
Walter Frank

The chemical reaction of dilithiumN,N′-di(tbutyl)-Si,Si-diphenylsilanediamide and PCl3yielded an off-white solid. Sublimation of the crude product under reduced pressure at elevated temperature gave colourless prismatic crystals of the title compound, C20H28ClN2PSi, which crystallizes in the non-centrosymmetric monoclinic space groupCc.The asymmetric unit of the crystal structure contains one molecule and it is dominated by the central SiN2P four-membered ring, which is almost planar with a mean deviation of the atoms from the best plane of 0.014 Å. The angles between the plane defined by the silicon atom and the two nitrogen atoms and the best planes of theSi-phenyl groups are 85.1 (2) and 77.4 (2)°, with the tilt of the phenyl rings in the opposite direction. Bothtert-butyl groups suffer from a two-position rotational disorder with site occupancies of 0.752 (6)/0.248 (6) and 0.878 (9)/0.122 (9). The P—Cl bond [2.2078 (17) Å] is remarkably elongated compared to the P—Cl distance in PCl3[2.034 Å; Galy & Enjalbert (1982).J. Solid State Chem.44, 1–23].


2018 ◽  
Vol 47 (25) ◽  
pp. 8209-8220 ◽  
Author(s):  
Sebastian Bette ◽  
Reinhard K. Kremer ◽  
Gerhard Eggert ◽  
Robert E. Dinnebier

Long-term crystallisation led to the formation of the 2-1-5 verdigris phase (Cu3(CH3COO)4(OH)2·5H2O). The crystal structure, as well as magnetic, thermal and spectroscopic properties, was investigated.


1998 ◽  
Vol 53 (5-6) ◽  
pp. 569-572 ◽  
Author(s):  
J.-G. Uttecht ◽  
W. Preetz

Abstract By treatment of [Pt(ox)2]2- with hydrogen peroxide the octahedral trans-[Pt(OH)2(ox)2]2- is formed. From the saturated aqueous solution in the presence of dipyridiniomethane dications single crystals of the double complex salt trans-(py2CH2)[Pt(OH)2(ox)2] trans-(py2CH2)[Pt(OH)(ox)2(H2O)]2 · 4H2O were grown and an X-ray structure determination (tricli­nic, space group P1̄, a = 8.649(1), b = 11.189(3), c = 12.731 (2) Å, α = 79.075(12), β = 80.725(8), γ= 73.932(13)°, Z = 1) has been performed. The centrosymmetric trans-[Pt(OH)2(ox)2]2- is connected via hydrogen bonds between its hydroxide groups and the aqua ligands of two protonated complex anions trans-[Pt(OH)(ox)2(H2O)]- .


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