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IR-LD(Solid-state linear-dichroic infrared) spectroscopic characterization of Aspirin form I

Difference IR-LD spectrum of form I (Fig. 1(1)) illustrated a signiﬁcant level of macro-orientation of solid guest molecule in nematic liquid crystal mesophase. The broad absorption peak between 3200 and 2300 cm-1 belongs to VOH stretching vibration of COOH group in the Aspirin molecule and indicated the strong intermolecular interactions, determined by single crystal X-ray diffraction [24,25]. According to[24,25], form I is characterized P21/C space group and consists of centrosymmetric carboxylic acid dimmer moieties (O---O: 2.635 A˚ , 177.7°) that are, in turn, joined via centrosymmetric methyl CH---O (C---O: 3.553 A˚ , 164.0°) contacts of acetyl groups, thus forming 1D chains [24,25]. Lest data assigned the observed higher frequency band in 1800–400 cm-1 region (Fig. 2(1)) at 1752 cm-1 to VC=O stretching mode of acetoxy group and the maximum at 1693 cm-1 to VC=O of carboxylic one as a result of different intermolecular hydrogen bondlengths. Both maxima are observed as doublets, which could be explained with crystal ﬁeld splitting effect. The other intensive peak at 1606 cm-1 corresponds to 8a skeletal in-plane vibration of aromatic ring [26]. The adequate experimentally IR-band assignment of the IR-bands in spectral region lower than 1400 cm-1 is possible through next IR-LD spectral analysis. Elimination of 1752 cm-1 and 1693 cm-1 peaks in different dichroic ratio (Fig. 3(1)) is a result of near to perpendicular orientation of both VC=O transition moments in the frame of Aspirin molecule, closing a dihedral angle of 83.6° (Scheme 2A) [24,25]. Elimination of 1606 cm-1 peak provoked the disappearance of peaks at 1307 cm-1and 917 cm-1 (Fig. 3(2)) belonging to same symmetry class (A1) and assigned as 3 and 1 modes of o-disubstituted benzene ring (Scheme 2B) [26]. Simultaneous disappearance of 836 cm-1 and 755 cm-1 (Fig. 4(1)) assigned their out-of-plane origin (B1 symmetry class) and belonged to 11-rCH and 4-rArbending vibrations (Scheme2B) [24]. Reduction of peaks at 668 cm-1and 599 cm-1 in same dichroic ratio (Fig. 4(2)) assigned their origin as 12(X) and 6a(X), both in-plane bending modes [26].

[ Last edited by 催化糞子 on 2011-3-24 at 19:24 ]

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催化糞子(金幣+108, 翻譯EPI+1): 感謝！！ 2011-03-25 10:21:39

阿司匹林形態(tài)I的 IR-LD (固態(tài)線(xiàn)二色紅外) 波譜表征
形態(tài)I的差示IR-LD光譜（圖 1（1））說(shuō)明了固態(tài)客體分子在向列液晶中間相中的宏觀(guān)取向顯著存在。3200-2300 cm-1 的寬吸收峰由阿司匹林分子中羧基的OH伸縮振動(dòng)（νOH）導(dǎo)致，它表明了阿司匹林分子間存在強(qiáng)的相互作用，這種相互作用已用單晶X射線(xiàn)衍射測(cè)定[24,25]。根據(jù)文獻(xiàn)[24,25]，形態(tài)I以P21/C空間群為特點(diǎn)，并由中心對(duì)稱(chēng)的羧酸二聚體(O---O: 2.635 A˚ , 177.7°)組成，這些二聚體依次通過(guò)中心對(duì)稱(chēng)的甲基-乙酰基CH---O (C---O: 3.553 A˚ , 164.0°)相互作用而形成一維的鏈狀結(jié)構(gòu)[24,25]。在1800–400 cm-1區(qū)，1752 cm-1處的高頻吸收峰被歸因于乙酰氧基的C=O伸縮振動(dòng)，而在1693 cm-1處的最高吸收峰則被認(rèn)為是羧基的C=O伸縮振動(dòng)峰，兩峰的位置不同是由分子間氫鍵鍵長(zhǎng)不同所致。此兩峰均是雙峰，這可用晶體場(chǎng)裂分效應(yīng)解釋。在1606 cm-1處的另一強(qiáng)峰對(duì)應(yīng)于苯環(huán)的8a面內(nèi)骨架振動(dòng)[26].波數(shù)在1400cm-1以下的IR吸收峰也許可以通過(guò)以下的IR-LD波譜分析合理地確定歸屬。不同雙色比條件下1752和1693cm-1處兩吸收峰的消失（圖3（1））是由于在阿司匹林骨架中兩種VC=O躍遷矩近似垂直的取向，其二面角接近83.6° (結(jié)構(gòu)式 2A) [24,25].1606cm-1處吸收峰的消失伴隨著屬于同一對(duì)稱(chēng)類(lèi)的1307cm-1和917cm-1處吸收峰的消失，這是由于鄰位二取代苯環(huán)的振動(dòng)模式3和1所致（結(jié)構(gòu)式 2B）[26]。836cm-1和755cm-1處兩峰的同時(shí)消失顯示它們同屬于面外振動(dòng)峰（B1 對(duì)稱(chēng)類(lèi)），分別由11-γCH和4-γAr彎曲振動(dòng)引起（結(jié)構(gòu)式 2B）[24]。在相同雙色比條件下，668 cm-1和 599 cm-1處兩峰的消失（圖4（2））則證實(shí)了它們對(duì)應(yīng)于12(X) 和 6a(X)的面內(nèi)彎曲振動(dòng)模式。

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