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61.
Kazuo Eda Yuichi Iriki Kenjiro Kawamura Takeshi Ikuki Masahiko Hayashi 《Journal of solid state chemistry》2007,180(12):3588-3593
We succeeded to prepare novel [Mo36O112(H2O)16]8− ({Mo36}) compounds by using 1,3-diamino-2-propanol (βOHC3-DA) and 1,3,5-tris(aminomethyl)benzene (MES-TA)+1,3-diaminopropane (C3-DA) as linkers, and determined their crystal structures. We have confirmed they have unique two-dimensional (2-D) molybdenum oxide frameworks, which are formed by condensation of {Mo36}s. Side-staggered arrays of {Mo36}s, connected in lying position by eight bridges per a {Mo36}, are formed in the compound with βOHC3-DA, while herringbone arrays of {Mo36}s, connected in standing position by four bridges per a {Mo36}, are built in the compound with MES-TA+C3-DA. The latter compound exhibited non-stoichiometric property, and its composition and cell parameters varied depending on the relative concentration of MES-TA in the mother solution. 相似文献
62.
Simultaneous quantification of brimonidine tartrate (BRI) and timolol maleate (TIM) in an eye drop formulation was performed by applying parallel factor analysis (PARAFAC) and trilinear (three way) partial least squares to the ultra performance liquid chromatography-photodiode array (UPLC-PDA) data array. In PARAFAC and 3 W-PLS1 applications, the co-elution of the related compounds in their chromatograms obtained in the presence of ornidazole as an internal standard (IS) was resolved, and then analyses were performed. On the other hand, a new conventional ultra performance liquid chromatography (UPLC) method was developed after long and tedious studies to get desirable elution of BRI and TIM in a chromatogram using different column and mobile phase system than that of chromatographic conditions of PARAFAC and 3 W-PLS1 applications. The performance and validity of all the proposed methods were confirmed by analyzing independent validation samples consisting of synthetic mixture, intraday and interday samples, and standard addition samples. Analysis results of BRI and TIM in eye drop samples by chemometric PARAFAC and 3 W-PLS1, and conventional UPLC were statistically compared to each other. It was concluded that PARAFAC and 3 W-PLS1 have shortest analysis time and lower cost than the developed conventional UPLC method for the analysis of the related compounds in commercial eye drop preparation with adequate selectivity and sensitivity. 相似文献
63.
Maeda S Goto T Takamoto M Eda K Himeno S Takahashi H Hori T 《Inorganic chemistry》2008,47(23):11197-11201
A yellow [(HPO(3))(2)(P(2)O(7))Mo(30)O(90)](8-) anion was prepared as a tetrapropylammonium (Pr(4)N(+)) salt from a 50 mM Mo(VI)-2 mM P(2)O(7)(4-)-4 mM HPO(3)(2-)-0.95 M HCl-60% (v/v) CH(3)CN system at ambient temperature. The (Pr(4)N)(8)[(HPO(3))(2)(P(2)O(7))Mo(30)O(90)] salt crystallized in the orthorhombic space group P(nma) (No. 62), with a = 30.827(2) A, b = 22.8060(15) A, c = 30.928(2) A, V = 21743(3) A(3), and Z = 4. The structure contained a (P(2)O(7))Mo(12)O(42) fragment derived from the removal of each corner-shared Mo(3)O(13) unit in a polar position from a [(P(2)O(7))Mo(18)O(54)](4-) structure, and each side of the (P(2)O(7))Mo(12)O(42) fragment was capped by a B-type (HPO(3))Mo(9)O(24) unit. The [(HPO(3))(2)(P(2)O(7))Mo(30)O(90)](8-) anion was characterized by voltammetry and IR, UV-vis, and (31)P NMR spectroscopy. Unlike the Keggin and Dawson anions and the parent [(P(2)O(7))Mo(18)O(54)](4-) anion, the [(HPO(3))(2)(P(2)O(7))Mo(30)O(90)](8-) anion exhibited two-electron redox waves in CH(3)CN with and without acid. 相似文献
64.
Air‐stable, orange‐red single crystals of [{ReN(PMe2Ph)3}{ReO3N}]2 are formed when mer‐[ReNCl2(PMe2Ph)3] reacts with strong bases in MeOH. The resulting centrosymmetric tetranuclear complex contains each two {ReN(PMe2Ph)3}2+ and {ReO3N}2? building blocks. They are connected by two oxygen and two nitrogen atoms giving an almost planar {Re4O2N2} ring. The Re–N–Re bridges are only slightly bent (175.2(2)°), while the Re–O–Re angles are 160.9(1)°. The coordination environment of the rhenium atom in the nitridotrioxorhenate(VII) anion is a slightly distorted tetrahedron with O–Re–O and O–Re–N angles between 108.7(1)° and 111.3(1)°. 相似文献
65.
Comprehensive Understanding of Structure‐Controlling Factors of a Zinc Tetraphenylporphyrin Thin Film Using pMAIRS and GIXD Techniques
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Miyako Hada Nobutaka Shioya Prof. Takafumi Shimoaka Prof. Kazuo Eda Prof. Masahiko Hada Prof. Takeshi Hasegawa 《Chemistry (Weinheim an der Bergstrasse, Germany)》2016,22(46):16539-16546
The performance of an organic electronic device is significantly influenced by the anisotropic molecular structure in the film, which has long been difficult to predict especially for a solution process. In the present study, a zinc tetraphenylporphyrin (ZnTPP) thin film prepared by a solution process was chosen to comprehensively explore the molecular‐arrangement mechanism as a function of representative film‐preparation parameters: solvent, film‐preparation technique, and thermal annealing. The anisotropic structure was first analyzed by using a combination of infrared p‐polarized multiple‐angle incidence resolution spectrometry (pMAIRS) and grazing incidence X‐ray diffraction (GIXD), which readily revealed the molecular orientation and crystal structure, respectively. As a result, the real dominant factor was found to be the evaporation time of the solvent that determines the initial two different molecular arrangements, types‐I and ‐II, while the thermal annealing was found to play an additional role of improving the molecular order. The correlation between the molecular orientation and the crystal structure was also revealed through the individual orientation analysis of the porphyrin and phenyl rings. 相似文献
66.
Synthesis of Mesoporous Lithium Titanate Thin Films and Monoliths as an Anode Material for High‐Rate Lithium‐Ion Batteries
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Dr. Fadime Mert Balcı Ömer Ulaş Kudu Prof. Eda Yılmaz Prof. Ömer Dag 《Chemistry (Weinheim an der Bergstrasse, Germany)》2016,22(52):18873-18880
Mesoporous Li4Ti5O12 (LTO) thin film is an important anode material for lithium‐ion batteries (LIBs). Mesoporous films could be prepared by self‐assembly processes. A molten‐salt‐assisted self‐assembly (MASA) process is used to prepare mesoporous thin films of LTOs. Clear solutions of CTAB, P123, LiNO3, HNO3, and Ti(OC4H9)4 in ethanol form gel‐like meso‐ordered films upon either spin or spray coating. In the assembly process, the CTAB/P123 molar ratio of 14 is required to accommodate enough salt species in the mesophase, in which the LiI/P123 ratio can be varied between molar ratios of 28 and 72. Calcination of the meso‐ordered films produces transparent mesoporous spinel LTO films that are abbreviated as Cxx‐yyy‐zzz or CAxx‐yyy‐zzz (C=calcined, CA=calcined–annealed, xx=LiI/P123 molar ratio, and yyy=calcination and zzz=annealing temperatures in Celsius) herein. All samples were characterized by using XRD, TEM, N2‐sorption, and Raman techniques and it was found that, at all compositions, the LTO spinel phase formed with or without an anatase phase as an impurity. Electrochemical characterization of the films shows excellent performance at different current rates. The CA40‐350‐450 sample performs best among all samples tested, yielding an average discharge capacity of (176±1) mA h g?1 at C/2 and (139±4) mA h g?1 at 50 C and keeping 92 % of its initial discharge capacity upon 50 cycles at C/2. 相似文献
67.
We prove the existence of a 2-dimensional nonaspherical simply connected cell-like Peano continuum (the space itself was constructed in one of our earlier papers). We also indicate some relations between this space and the well-known Griffiths' space from the 1950s. 相似文献
68.
Yusaku Eda 《Tetrahedron letters》2008,49(16):2519-2522
2,5-Bis(chloromethyl)pyrazine reacted with sodium alkoxide to give unexpected 2-dialkoxymethyl-5-methylpyrazine along with normal substitution product, 2,5-bis(alkoxymethyl)pyrazine. The reaction of 2,3,5,6-tetrakis(chloromethyl)pyrazine with sodium alkoxide afforded similar results to yield 2,6-bis(dialkoxymethyl)-3,5-dimethylpyrazine along with other alkoxymethylpyrazines. The ratio of products depended on the solvent and alkoxide used. A general discussion of the mechanism of such a pyrazine acetal synthesis in the basic conditions is given. 相似文献
69.
Two new coordination polymers, [Ag2(barb)(pipet)]n (1) and {Na3[Ag2(barb)2](pippr)·2H2O}n (2) (where H2barb, pipet and Hpippr are 5,5-diethylbarbituric acid, N-piperidineethanol and 1,3-bis(4-piperidyl)propane, respectively) have been synthesized and characterized by elemental analysis, IR, thermal analysis and X-ray single-crystal diffraction techniques. Silver(I) ions in complexes 1 and 2 are bridged by barb dianions, leading to one-dimensional coordination polymers. In 1, the barb ligand acts as a tetradentate bridging ligand, while in 2 as a bidendate bridging ligand. The pipet ligand behaves as a bidentate chelating donor, whereas the pippr anion is not involved in coordination and remains as a counter-ion. The one-dimensional chains of 1 and 2 are further extended into supramolecular networks. Spectral and thermal analysis data for 1 and 2 are in agreement with the crystal structures. 相似文献
70.
A new application of continuous wavelet transform (CWT) to overlapping peaks in a chromatogram was developed for the quantitative analysis of amiloride hydrochloride (AML) and hydrochlorothiazide (HCT) in tablets. Chromatographic analysis was done by using an ACQUITY ultra-performance LC (UPLC) BEH C18 column (50 x 2.1 mm id, 1.7 pm particle size) and a mobile phase consisting of methanol-0.1 M acetic acid (21 + 79, v/v) at a constant flow rate of 0.3 mL/min with diode array detection at 274 nm. The overlapping chromatographic peaks of the calibration set consisting of AML and HCT mixtures were recorded rapidly by using an ACQUITY UPLC H-Class system. The overlapping UPLC data vectors of AML and HCT drugs and their samples were processed by CWT signal processing methods. The calibration graphs for AML and HCT were computed from the relationship between concentration and areas of chromatographic CWT peaks. The applicability and validity of the improved UPLC-CWT approaches were confirmed by recovery studies and the standard addition technique. The proposed UPLC-CWT methods were applied to the determination of AML and HCT in tablets. The experimental results indicated that the suggested UPLC-CWT signal processing provides accurate and precise results for industrial QC and quantitative evaluation of AML-HCT tablets. 相似文献