cas 307531-92-6, 1 3 5 7 9 11 14-HEPTAISOBUTYLTRICYCLO

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Lithium-Templated Formation of Polyhedral Oligomeric Silsesquioxanes (POSS)
A coordination complex, lithium hepta(i-butyl)silsesquioxane trisilanolate (1; Li-T7), a stable intermediate in silsesquioxane (SQ) syntheses, was successfully isolated in 65% yield and found to be highly soluble in nonpolar solvents such as hexane. The structure of Li-T7 was confirmed by NMR, IR spectroscopy, matrix-assisted laser desorption ionization time-of-flight mass spectrometry, electrospray ionization mass spectrometry, and computational simulation, providing detailed elucidation of the intermolecular self-association of the SQ cage with a box-shaped Li6O6 polyhedron through strong coordination bonds. After acid treatment, Li-T7 undergoes lithium-proton cationic exchange, yielding hepta(i-butyl)silsesquioxane trisilanol (2; H-T7) quantitatively. The high yield of H-T7 seems to be influenced by Li-O bonding in the Li-T7 complex that affects the selective formation of hepta(i-butyl)silsesquioxane trisilanolate and the bulky i-butyl groups which may prevent decomposition or SQ cage-rearrangement even at reflux under alkaline conditions. Single-crystal X-ray crystallography confirms the presence of the dumbbell-shaped SQ partial cages through strong intermolecular hydrogen bonds. Interestingly, lowering the polarity of the reaction solution by adding dichloromethane results in formation of the cubic octa(i-butyl)silsesquioxane (3; T8) cage in a good yield (47%), which is isolated by crystallization from the reaction solution.
Prigyai, Nicha,Chanmungkalakul, Supphachok,Ervithayasuporn, Vuthichai,Yodsin, Nuttapon,Jungsuttiwong, Siriporn,Takeda, Nobuhiro,Unno, Masafumi,Boonmak, Jaursup,Kiatkamjornwong, Suda
(2019)
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Synthesis of incompletely caged silsesquioxane (T7-POSS) compounds via a versatile three-step approach
Abstract: Three kinds of incompletely condensed polyhedral oligomeric silsesquioxanes (T7-POSS) with three Si–OH groups: (i-C4H9)7Si7O9(OH)3, (i-C8H17)7Si7O9(OH)3 and (C6H5)7Si7O9(OH)3 were prepared by a versatile three-step approach (hydrolysis, condensation, and neutralization) from i-C4H9Si(OEt)3, i-C8H17Si(OEt)3, and C6H5Si(OEt)3, respectively, with the LiOH·H2O as catalyst. The structures of the three T7-POSS were characterized by FTIR, 1H NMR, 13C NMR, 29Si NMR, MALDI-TOF MS and XRD. The accurate incompletely caged structure of the three T7-POSS indicated that the built-up three-step approach is a versatile and effective way to synthesize T7-POSS with high yield. The best reaction conditions to synthesize the isobutyl-T7, isooctyl-T7 and phenyl-T7 POSS have been suggested, involving acetone and a co-solvent, the molar ratio of the RSi(OEt)3: LiOH·H2O: H2O and the reaction temperature. The thermal stability of the three T7-POSS were characterized by TGA, showing different degradation behaviors. The thermal stability of phenyl-T7 POSS was the highest among the three T7-POSS.
Ye, Miaofen,Wu, Yiwei,Zhang, Wenchao,Yang, Rongjie
p. 4277 - 4294
(2018)
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Photoluminescence of Binary and Ternary Europium-based Polyhedral Oligomeric Silsesquioxane and Sol–Gel Complexes
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Bindu, Pardeshi Hima,Huy, Bui The,Kumar, Avvaru Praveen,Kumar, Begari Prem,Lee, Yong-Ill,Sherial, Raghuveer
(2020)
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Synthesis, thermal stability and photoresponsive behaviors of azobenzene-tethered polyhedral oligomeric silsesquioxanes
A series of azobenzene-tethered polyhedral oligomeric silsesquioxane (POSS) derivatives, i.e. monoazobenzene-substituted POSS (MonoAzo-POSS), bisazobenzene-substituted POSS (BisAzo-POSS) and triazobenzene-substituted POSS (TriAzo-POSS), were synthesized through the amidation acidylation of aminopropylisobutyl POSS and benzoic acid derivatives (AzoMs) with one, two and three azobenzene groups (AzoM1, AzoM2 and AzoM3). Their structures were characterized by FT-IR, 1H NMR, 13C NMR and mass spectra, and their thermal stability and photoresponsive behaviors in DMF solutions were evaluated with TGA, XRD and UV-vis spectra, respectively. The results indicated that the thermal stability and photoisomerization of azobenzenes could be effectively controlled by their molecular structure. In MonoAzo-POSS, the large steric hindrance of POSS destroys the molecular ordering and limits the molecular packing, contributing to its poor thermal stability. And the low molecular ordering of MonoAzo-POSS offers an azo group with large free space, and its trans-cis photoisomerization rate increases accordingly. But, in BisAzo-POSS and TriAzo-POSS, the incorporation of POSS units does not impact on the regularity of azobenzenes obviously, and the hindrance effect of nanosize POSS on the molecular motion plays a primary role in increasing their high thermal stability. Their photoisomerization rates decrease due to the steric hindrance of POSS and the unfolding structure of the azo moieties in BisAzo-POSS and TriAzo-POSS.
Zhou, Jinlan,Zhao, Yongchen,Yu, Kaichao,Zhou, Xingping,Xie, Xiaolin
experimental part
p. 2781 - 2792
(2012/01/14)

POLYEDRIC OLIGOMERIC SILICON/OXYGEN CLUSTER WITH AT LEAST ONE ALDEHYDE GROUP AND METHOD FOR PRODUCTION THEREOF
The invention relates to polyedric oligomeric silicon/oxygen clusters characterised by a structure of formula: [(RaXbArSiO1,5)m (RcXdAsSiO)n (ReXfAtSi2O2,5)o (RgXhAuSi2O2)p] where a, b, c and r = 0-1, d and s = 0-2, e, g, f, and t = 0-3, h and u = 0-4, m+n+o+p = 4-14, a+b+r = 1, c+d+s = 2, e+f+t = 3, g+h+u = 4, r+s+t+u = 1, R = H, alkyl, cycloalkyl, alkinyl, cycloalkinyl, aryl, heteroaryl, or a polymeric group, which is substituted or unsubstituted, an alkenyl or cycloalkenyl group with no hydrogen atoms directly on the double bond, or further functionalised polyedric, oligomeric silicon/oxygen cluster units bonded by means of a polymeric unit or a bridging unit, X = oxy, hydroxy, alkoxy, carboxy, silyl, alkylsilyl, alkoxysilyl, siloxy, alkylsiloxy, alkoxysiloxy, silylalkyl, alkoxysilylalkyl, alkylsilylalkyl, halogen, epoxy, ester, fluoroalkyl, isocyanate, protected isocyanate, acrylate, methacrylate, mercapto, nitrile, amino, phosphine group or at least one such group from the substituents of type R comprising type X, A = a substituent with at least one aldehyde group, whereby substituents of type R, type A and also type X are the same or different and comprising at least one substituent, preferably of type A and method for production thereof.
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Page/Page column 13-14

(2008/06/13)

NCO-containing compounds with covalent bound polyhedral oligomeric silicon-oxygen clusters
Functional isocyanate compounds obtained by reacting polyisocyanates with polyhedral, oligomeric silicon-oxygen cluster compounds containing groups which react with isocyanate, so that 1-20 mol% of the original isocyanate groups undergo conversion (or 80-99 mol% if a blocking agent is used). NCO-containing compounds (I) with covalently-bonded, polyhedral, oligomeric silicon-oxygen cluster units (POSO) formed by the reaction of (A) aromatic, aliphatic and/or cycloaliphatic polyisocyanate(s) with an NCO functionality of 2-6 with (B) 0.001-20.0 wt.% POSO units containing NCO-reactive functional groups, with 1-20 mol% conversion based on originally-present free NCO groups and optionally (C) a blocking agent, with 80-99 mol% conversion of NCO groups. Independent claims are also included for: (1) paint containing (I) as crosslinker, with at least one polyol component (2) coatings obtained with this paint.
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(2008/06/13)

OLIGOMER SILASESQUIOXANES, METHOD FOR THE PRODUCTION THEREOF, AND USE OF THE SAME
The invention relates to a method for producing fully condensed oligomer silasesquioxanes of formula R1aR2bR3cR4dR5eR6fR7gR8hSi8O12 wherein R1, R2, R3, R4, R5, R6, R7, R8 represent substituted or unsubstituted alkyl, cycloalkyl, alkenyl, cycloalkenyl, alkinyl, cycloalkinyl, aryl, heteroaryl radicals or hydrogen which are the same or different, and a + b + c + d + e + f + g + h = 8, said compounds having the structure (1). The invention also relates to the use of said compounds for the synthesis of partially condensed silasesquioxanes, functionalised silasesquioxanes, catalysts, and the parent compounds thereof, and for the synthesis and modification of polymers.
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Page/Page column 13-14

(2008/06/13)