• Macromolecular Research
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• 제14권4호
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• pp.408-415
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• 2006

Temperature-dependent, wide-angle, x-ray diffraction (WAXD) patterns and infrared (IR) spectra were measured for biodegradable poly(3-hydroxybutyrate) (PHB) and its copolymers, poly(3-hydroxybutyrate-co-3-hydroxyhexanoate) P(HB-co-HHx) (HHx=2.5, 3.4, 10.5, and 12 mol%), in order to explore their crystal and lamellar structure and their pattern of C-H...O=C hydrogen bonding. The WAXD patterns showed that the P(HB-co-HHx) copolymers have the same orthorhombic system as PHB. It was found from the temperature-dependent WAXD measurements of PHB and P(HB-co-HHx) that the a lattice parameter is more enlarged than the b lattice parameter during heating and that only the a lattice parameter shows reversibility during both heating and cooling processes. These observations suggest that an interaction occurs along the a axis in PHB and P(HB-co-HHx). This interaction seems to be due to an intermolecular C-H...O=C hydrogen bonding between the C=O group in one helical structure and the $CH_3$ group in the other helical structure. The x-ray crystallographic data of PHB showed that the distance between the O atom of the C=O group in one helical structure and the H atom of one of the three C-H bonds of the $CH_3$ group in the other helix structure is $2.63{\AA}$, which is significantly shorter than the sum of the van der Waals separation ($2.72{\AA}$). This result and the appearance of the $CH_3$ asymmetric stretching band at $3009 cm^{-1}$ suggest that there is a C-H...O=C hydrogen bond between the C=O group and the $CH_3$ group in PHB and P(HB-co-HHx). The temperature-dependent WAXD and IR measurements revealed that the crystallinity of P(HB-co-HHx) (HHx =10.5 and 12 mol%) decreases gradually from a fairly low temperature, while that of PHB and P(HB-co-HHx) (HHx = 2.5 and 3.5 mol%) remains almost unchanged until just below their melting temperatures. It was also shown from our studies that the weakening of the C-H...O = C interaction starts from just above room temperature and proceeds gradually increasing temperature. It seems that the C-H...O=C hydrogen bonding stabilizes the chain holding in the lamellar structure and affects the thermal behaviour of PHB and its copolymers.

• 한국결정학회지
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• 제17권1호
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• pp.6-9
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• 2006

Bis(N-Methylphenazinium)-Tetracyanopalladate(II) Hydrate $(C_{13}H_{11}N_2){_2}[Pd(CN)_4]{\cdot}H_2O$의 단위 착이온 및 결정의 구조들을 X-선 회절법으로 연구하였다. 이 결정은 사방정계이고 공간군은 $P2_1/b$(군번호=14)이다. 단위세포 a=9.783(4), b=10.788(4), c=13.666(4) ${\AA},\;{\beta}=104.59(5),\;V=1392.9{\AA}{^3},\;Z=2,\;Dc=1.476gcm^{-3},\;F(000)=632,\;{\mu}=7.05cm^{-1}$이다. 구조분석은 중금속법으로 풀었으며, 최소자승법으로 정밀화 하였고, 최종 신뢰도 값들은 1930 회절반점에 대하여 R=0.0257, Rw=0.0732, Rall=0.0283 및 S=1.07 이었다. 두 이온들은 근본적인 평면구조로써, 이들의 충진구조는 착음이온을 두개의 양이온들이 거의 평행하게 둘러싸고 있는 삼중체들을 형성하고 있다. 양이온과 음이온들의 이면각은 $10.16(4)^{\circ}$인 삼중체들이 b축을 따라서 배열되어 있다, 삼중체내 및 삼면체간의 면간 거리들은 3.419(3)와 $3.402(4){\AA}$이었다.

• 한국결정학회지
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• 제2권2호
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• pp.7-12
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• 1991

C13H18N2O3(Mr=250.29)는 단사정계의 P211a의 공간군을 갖고 있으며 a=8.765(4), b=17.679 (3), c=9.238(4)A, p=105.6(3)A, z=4, V= 1378.53A3, A(Mo Ka)=0.71069A, 1:0. 81cm-1, F(000)=536, T=298 이며 1.0 σ(I)보다 큰 강도를 가진 1783개의 회절반점에 대하여 최종 R값은 0.080이다. 직접법에 의하여 구조를 풀었으며 C-H 결합길이와 메칠기는 길이를 고정시켜 이 상적인 기하학적 구조에 맞추어 계단식 대각최소자 승법에 의하여 정밀화하였다 두 에토오키시기중의 하나는 다른 기에 비해 100°나 더 기울어져있다. 결정격자내에 한개의 N-H‥‥0(2.798A) 수소결합이 있어 두 분자를 연결하면서 b-축에 따라 쌓여져 있다.

• 대한화학회지
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• 제21권5호
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• pp.307-319
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• 1977

Thiourea derivative인 $N-({\alpha}-dimethyl\;{\beta}-hydroxy)ethyl\;N'-cyclohexyl\;thiourea,\;C_{ll}H_{22}N_2OS)$의 결정 및 분자구조를 X-선 회절법으로 해명하였다. 이 화합물의 결정은 공간군 $P_{bca}$에 속하는 orthorhombic 형으로 a = 10.33(3), b = 11.82(3), c = 22.57(4)${\AA}$ 이고 Z = 8이다. Weissenberg 사진촬영으로 얻은 회절반점의 총수는 1414개이며 중원자법을 이용하여 구조해명을 한 후 최소자승법으로 정밀화하였으며 최종 R값은 0.13이다. Cyclohexane ring은 normal chair conformation을, thiourea 부분은 평면을 이루고 있다. 일차 알코올의 hydroxyl group은 N(2)원자와 분자내 수소결합을 이뤄서 전체분자를 안정화시키고 있다. 분자들은 결정내에서 수소결합과 van der Waals힘으로 서로 결합되어 있다. 분자내 수소결합 N(2)-H${\cdot}{\cdot}{\cdot}$O는 강한 수소결합으로 N${\cdot}{\cdot}{\cdot}$O 길이는 2.71${\AA}$이고, 분자간 수소결합 O${\cdot}{\cdot}{\cdot}$H${\cdot}{\cdot}{\cdot}$S의 O${\cdot}{\cdot}{\cdot}$S 길이는 3.02${\AA}$으로 b축에 나란하다.

• 대한전기학회:학술대회논문집
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• 대한전기학회 1999년도 하계학술대회 논문집 G
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• pp.3304-3306
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• 1999

In this study, we used the sputtering method with single target to obtain the thick and uniform PZT($PbZrTiO_3$) films for micromached IR sensor application. Then, we investigated the etching characteristics and conditions which is necessary process to fabricate the IR sensor. We tested the C-axis orientation and P-E loop of the deposited PZT films with the XRD and RT66A, respectively. Also we investigated the surface of the films by the AFM and SEM analysis.

• 한국초전도ㆍ저온공학회논문지
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• 제13권1호
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• pp.6-11
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• 2011

The $BaHfO_3$ (BHO) buffer layer on the IBAD MgO template was turned to be effective for a successful fabrication of $GdBa_2Cu_3O_{7-{\delta}}$ (GdBCO) films with high critical current density ($J_c$). Both the BHO buffer layers and GdBCO films were prepared by pulsed laser deposition (PLD). The effects of the PLD conditions, including substrate temperature ($T_s$), oxygen partial pressure ($PO_2$), and deposition time on the in-plane texture, surface roughness, and microstructures of the BHO buffer layers on the IBAD MgO template were systematically studied for processing optimization. The c-axis oriented growth of BHO layers was insensitive to the deposition temperature and the film thickness, while the in-plane texture and surface roughness of those were improved with increasing $T_s$ from 700 to $800^{\circ}C$. On the optimally processed BHO buffer layer, the highest $J_c$ value (77 K, self-field) of 3.68 $MA/cm^2$ could be obtained from GdBCO film deposited at $780^{\circ}C$, representing that BHO is a strong candidate for the buffer layer on the IBAD MgO template.

• Archives of Pharmacal Research
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• 제14권1호
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• pp.1-6
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• 1991

The crystal structure of licarin-B, a component of Myristicae Semen was determined by single crystal X-ray diffraction analysis. Crystal of the compound, which was recrystallized from the mixture of hexane and ether, is monoclinic with a=12.740(1), b=7.219(1), c=9.284(1) ${\AA}$, ${\beta}=94.75(1)^{\circ}$, $D_x=1.26$, $D_m=1.27\;g/cm^3$, space group P21, and Z=2. The structure was solved by direct method and refined by least-squares procedure to the final R value of 0.040 for 1532 independent reflections ${F{\ge}3{\sigma}(F)}$. The compound is a dimeric phenylpropanoid, and belongs to the neolignan analogues. The molecules are arranged along with the screw axis. The intermolecular contacts appear to be the normal van der Waals' forces.

• Archives of Pharmacal Research
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• 제13권2호
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• pp.166-173
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• 1990

The structure of the anti-inflammatory agent, naproxen sodium was determined by single crystal X-ray diffraction analysis. Crystal of the compound, which was recrystallized from methanol solution, is nomoclinic, space group $P2_1$ with a = 21. 177(6), b = 5.785(2), c = 5.443(2) $\AA, \beta$ = 91.41(3)$\{\circ}$ and Z = 2. The calculated density is 1.346; the observed value is nements based on 1093 reflections ($F\geq3\sigma$(F)) gave the final R value of 0.043. There are of one water per one compound molecule in the crystal. The carboxyl group of the molecule is nearly perpendicular to the naphthalene ring. The molecules are arranged along with the screw axis, and stabilized by five 0...Na type interactions. The molecule retains nearly same dimensions and similar conformation compared to its parent compound, naproxen, except for the torsion angles around C(5)-C(11) bond.

• 분석과학
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• 제21권6호
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• pp.562-568
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• 2008

A novel two-dimensional cadmium(II)-nickel(II) bimetallic host clathrate, $[Cd{NH_2CH_2CH_2OH}_2Ni(CN)_4]{\cdot}3C_6H_5NH_2{\cdot}H_2O$, 1, has been synthesized and structurally characterized by X-ray single crystallographic method. The clathrate 1 crystallizes in the monoclinic system, space group $P2_1/c$ with a = 14.370(3), b = 7.728(1), c = 28.172(4) ${\AA}$, ${\beta}=97.58(1)^{\circ}$, V = 3101.1(9) ${\AA}^3$, Z = 4. The host framework of the clathrate 1 is built of the cyanide bridges between octahedral Cd(II) atom and square planar Ni(II) atom. The octahedral Cd atoms ligated by two 2-aminoethanol molecules and four cyanide ligands bridged with square planar Ni atoms. The Ni atoms bridges to four Cd atoms via cyanides is made up of puckered quadrangles of composition $\{CdNi(CN)_2\}_2$, all edges are shared. This cyanide bridges form an infinite two-dimensional host networks stacking along b axis. 2-Aminoethanol ligands bond to Cd atom through N atom as a monodentate ligand in the axial position and four cyanides take an equatorial plane with all in trans-configurations. The aniline guest molecules and water molecules are located in between the host layer sheets, respectively.

• 한국결정학회지
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• 제3권1호
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• pp.37-43
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• 1992

비선형광학 단결정인 KTiOP04는 Nd:YAG 레 이저의 제2고조파 발생장치로 가장 널리 이용되 는 물질이다. 본 연구에서는 낮은 점도를 갖는 3K2W04. P2O5 응제를 이용하여 TSSG법에 의한 KTiOP04 단결 정 육성 실 험 을 하였다. KTiOP04 육 성에 적합하도록 온도구배가 작은 전기로와 정밀 한 회전인상장치를 제작하였으며,용액 내 수직온도 구배는 용액표면과 용액 밑부분의 온도차가 1℃로 매우 작았다. 성장 과정의 관찰과 조절이 용이하도록 종자정을 용액 표면에 위치시켰다. 용액의 조성은 66.7mol%의 KTiOP04를 포함하도록 고정하였으며 이 용액의 포화온도는 1020℃ 였다. 냉각속도가 0 2℃/h, 결정의 회전속도가 50 rpm인 성장조건에서 a-, b-, c-축으로의 길이 가 각각 23 ×25 ×25mm3인 포유물이 없는 양질의 단결정을 얻을 수 있었다. 성장된 K,Tiop04 단결정은 크게 발달한 (201)면과 (011), (110), (100) 면들로 이루어져 있었으며 (101) 면이 관찰되기도 하였다.