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91.
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Muthukumaran K Loewe RS Ambroise A Tamaru S Li Q Mathur G Bocian DF Misra V Lindsey JS 《The Journal of organic chemistry》2004,69(5):1444-1452
Synthetic molecules bearing phosphonic acid groups can be readily attached to oxide surfaces. As part of a program in molecular-based information storage, we have developed routes for the synthesis of diverse porphyrinic compounds bearing phenylphosphonic acid tethers. The routes enable (1) incorporation of masked phosphonic acid groups in precursors for use in the rational synthesis of porphyrinic compounds and (2) derivatization of porphyrins with masked phosphonic acid groups. The precursors include dipyrromethanes, monoacyldipyrromethanes, and diacyldipyrromethanes. The tert-butyl group has been used to mask the dihydroxyphosphoryl substituent. The di-tert-butyloxyphosphoryl unit is stable to the range of conditions employed in syntheses of porphyrins and multiporphyrin arrays yet can be deprotected under mild conditions (TMS-Cl/TEA or TMS-Br/TEA in refluxing CHCl(3)) that do not cause demetalation of zinc or magnesium porphyrins. The porphyrinic compounds that have been prepared include (1) A(3)B-, trans-AB(2)C-, and ABCD-porphyrins that bear a single phenylphosphonic acid group, (2) a trans-A(2)B(2)-porphyrin bearing two phenylphosphonic acid groups, (3) a chlorin that bears a single phenylphosphonic acid group, and (4) a porphyrin dyad bearing a single phenylphosphonic acid group. For selected porphyrin-phosphonic acids, the electrochemical characteristics have been investigated for molecules tethered to SiO(2) surfaces grown on doped Si. The voltammetric behavior indicates that the porphyrin-phosphonic acids form robust, electrically well-behaved monolayers on the oxide surface. 相似文献
94.
Laser Raman spectroscopy was employed as a non-destructive probe for the detection and monitoring of crystalline arsenic in
the native oxide films formed during heating of GaAs in air at various temperatures. Spectroscopy of oxide films formed after
successive heating and etching treatments could confirm the location of arsenic to be near the top of the GaAs: native oxide
overlayer. 相似文献
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Evaluation of phase transitions in a series of hydrogen sulfates (Rb3H(SO4)2, (NH4)3H(SO4)2, K3 H(SO4)2, and Na3H(SO4)2) based on the single-crystal structure analysis has revealed the exact nature of such transitions and has sorted out the various ambiguities involved in earlier literature. Rb3H(SO4)2 at 293 K is C2/c. It is isostructural to its ammonium analogue, (NH4)3H(SO4)2, at room temperature. However, the variable temperature single-crystal diffraction studies indicate that the phase transition mechanism is different. When cooled to 100 K, the structure of Rb3H(SO4)2 remains C2/c. When heated to 350 K, it transforms to C2/m (with double the volume at room temperature), which changes to C2/c (with 4 times the volume at room temperature) at 425 K. The high-temperature (420 K) structural phase transition in (NH4)3H(SO4)2 is shown to be Rm. The structure of Na3H(SO4)2 remains invariant (P21/c) throughout the range of 100-500 K except for the usual contraction of the unit cell at 100 K and expansion at 500 K. The structural phase transitions with temperature for the compound K3H(SO4)2 are very different from those claimed in earlier literature. The hydrogen atom participating in the crucial hydrogen bond joining the two sulfate tetrahedra controls the structural phase transitions at low temperatures in all four compounds. The distortion of the SO4 tetrahedra and the coordination around the metal atom sites control the phase evolution in the Rb compound, while the Na and K analogues show no phase transitions at high temperature, and the NH4 system transforms to a higher symmetry space group resulting in a disorder of the sulfate moiety. 相似文献
98.
Dr. Sajesh P. Thomas Vijith Kumar Khidhir Alhameedi Prof. T. N. Guru Row 《Chemistry (Weinheim an der Bergstrasse, Germany)》2019,25(14):3591-3597
Classical examples of supramolecular recognition units or synthons are the ones formed by hydrogen bonds. Here, we report the ubiquity of a S⋅⋅⋅O chalcogen bonded synthon observed in a series of supramolecular complexes of the amyotrophic lateral sclerosis drug riluzole. Although the potential of higher chalcogens such as Se and Te to form robust and directional chalcogen bonded motifs is known, intermolecular sulfur chalcogen bonding is considered to be weak owing to the lower polarizability of S atoms. Here, the robustness and electronic nature of a S⋅⋅⋅O chalcogen bonding non-classical synthon, and the origin of its exceptional directionality have been explored. Bond orders of the drug–coformer chalcogen bonding are found to be as high as one third of a single bond, and they are largely ionic in nature. The contribution of the S⋅⋅⋅O chalcogen bonded motifs to the lattice energies of a series of crystals from the Cambridge Structural Database has been analyzed, showing they can be indeed significant, especially in molecules devoid of strong hydrogen bond donor groups. 相似文献
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100.
Vivekanandan K Swamy MG Prasad S Mukherjee R Burman AC 《Rapid communications in mass spectrometry : RCM》2006,20(11):1731-1735
A strategy is developed for the identification of isocephalomannine in the presence of alkali metal ion adducts and other cephalomannine isomers in a paclitaxel active pharmaceutical ingredient. Intact molecular ion analyses and a sub-structural study have been performed for the differentiation of isocephalomannine (2-debenzoylpaclitaxel-2-pentenoate) from cephalomannine and 7-epi-cephalomannine. A comparative study of the cephalomannine isomers was carried out using molecular ions (MS) and fragmentation patterns (MS/MS) for sub-structural analysis. An attempt has been made to identify isocephalomannine in Cremophor(R) EL formulations. 相似文献