• Title/Summary/Keyword: X-ray diffractometry

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First Example of Monometallic Palladium(II) Compound with Trans-Chelating Tridentate Ligand: Synthesis, Crystal Structure, and Characterizations

  • Tae Hwan Noh
    • Mass Spectrometry Letters
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    • v.14 no.3
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    • pp.110-115
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    • 2023
  • The reaction of (COD)PdCl2 with new C3-symmetric tridentate L (COD = 1,5-cyclooctadien; L = 1,3,5-tris(picolinoyloxyethyl)cyanurate) in a mixture of acetone and dichloromethane produces single crystals consisting of unprecedented monometallacyclic [PdCl2(L)]. This cyclic compound arises from trans-chelation of two of three donating pyridyl groups of L, while the third pyridyl group remains uncoordinated. Electrospray ionization mass spectrometry (ESI-MS) data on L exhibited the major peak corresponding to [C27H24N6O9 + H+]+. Fast atom bombardment mass spectrometry (FABMS) data on [PdCl2(L)], however, showed the mass peak corresponding to the L instead of the present palladium(II) compound species, due to the insolubility and dissociation in solution. The physicochemical properties of the present palladium(II) compound were fully characterized by means of infrared (IR) and nuclear magnetic resonance (NMR) spectroscopy, thermal analysis, single-crystal X-ray diffraction (SC-XRD) measurement.

Application Study of Chemoinfometrical Near-Infrared Spectroscopic Method to Evaluate for Polymorphic Content of Pharmaceutical Powders (일본의 근적외선분광법에 대한 제약회사 응용 및 현황)

  • Otsuka, Makoto
    • Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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    • 2002.11a
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    • pp.97-117
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    • 2002
  • A chemoinfometrical method for quantitative determination of crystal content of indomethacin (IMC) polymorphs based on fourie-transformed near-infrared (FT-NIR) spectroscopy was established. A direct comparison of the data with the ones collected from using the conventional powder X-ray diffraction method was performed. Pure $\alpha$ and ${\gamma}$ forms of IMC were prepared using published methods. Powder X-ray diffraction profiles and NIR spectra were recorded for six kinds of standard materials with various content of ${\gamma}$ form IMC. The principal component regression (PCR) analyses were performed based on normalized NIR spectra sets of standard samples of known content of IMC ${\gamma}$ form. A calibration equation was determined to minimize the root mean square error of the prediction. The predicted ${\gamma}$ form content values were reproducible and had a relatively small standard deviation. The values of ${\gamma}$ form content predicted by two methods were in close agreement. The results were indicated that NIR spectroscopy provides for an accurate quantitative analysis of crystallinity in polymorphs compared with the results obtained by conventional powder X-ray diffractometry.

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Application of Inverse Pole Figure to Rietveld Refinement: III. Rietveld Refinement of $SnO_2$ Thin Film using X-ray Diffraction Data

  • Kim, Yong-Il;Jung, Maeng-Joon;Kim, Kwang-Ho
    • The Korean Journal of Ceramics
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    • v.6 no.4
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    • pp.354-358
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    • 2000
  • The SnO$_2$film was deposited on a corning glass 1737 substrate by plasma enhanced chemical vapor deposition using a gas mixture of SnCl$_4$, $O_2$, and Ar. The film thickness was measured using $\alpha$-step and was about 9400$\AA$. The conventional X-ray diffractometry and pole figure attachment were used to refine the crystal structure of SnO$_2$ thin film. Six pole figures, (200), (211), (310), (301), (321), and (411), were measured with CoK$_\alpha$ radiation in reflection geometry. The X-ray diffraction data were measured at room temperature using CuK$_\alpha$ radiation with graphite monochromator. The agreement between calculated and observed patterns for the normal direction of SnO$_2$ thin film was not satisfactory due to the severely preferred orientation effect. The Rietveld refinement of heavily textured SnO$_2$ thin film was successfully achieved by adopting the pole density distribution of each reflection obtained from the inverse pole figure as a correction factor for the preferred orientation effect. The R-weighted pattern, R$_wp$, was 15.30%.

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Preparation and Identification of Crystal Modification of Piroxicam

  • Suh, Jung-Jin;Kim, Bong-Hee;Ko, Jung-Gil
    • Journal of Pharmaceutical Investigation
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    • v.15 no.1
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    • pp.8-14
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    • 1985
  • Data obtained from X-ray diffractometry, thermal analysis, IR spectroscopy and microscopic observation were used for the identification and characterization of four crystalline modifications of piroxicam. form a was crystallized from sodium hydroxide-hydrochloric acid and from c was obtained by crystallization from toluene. Form b and d was crystallized from methanol under the different temperature conditions. Relative rates of dissolution and solubility of four crystal forms of piroxicam in distilled water were measured.

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Study on Inclusion Complex of Fenbufen with ${\beta}-Cyclodextrin$

  • Kim, Young-Il;Park, Young-Ju
    • Journal of Pharmaceutical Investigation
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    • v.14 no.3
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    • pp.136-143
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    • 1984
  • Inclusion complex formation of fenbufen with ${\beta}-cyclodextrin$ in water and in solid state was comfirmed by solubility method, ultra violet absorption, circular dichroism and infra-red spectroscopies, differential thermal analysis, and X-ray diffractometry. A solid complex of fenbufen with ${\beta}-cyclodextrin$ in 1 : 1 molar ratio was prepared by the freeze-drying method, its dissolution characteristics in water and its analgesic and antiinflammatory effect in mouse or rat were examined. The apparent release of fenbufen from the inclusion complex was significantly improved, hut no significant difference in its analgesic and antiinflammatory effect was found.

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Crystal Forms of Ziprasidone (지프라시돈의 결정형)

  • Youn, Mi-Hee;Bang, Hyo-Chun;Sohn, Young-Taek
    • Journal of Pharmaceutical Investigation
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    • v.39 no.2
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    • pp.117-120
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    • 2009
  • Two crystal forms of ziprasidone have been isolated by recrystallization from different organic solvents and characterized by differential scanning calorimetry, powder X-ray diffractometry and thermogravimetric analysis. It was confirmed that Form 2 has the same crystal structure as Form 1.

Polymorphism of Doxazosin Mesylate

  • Sohn Young-Taek;Lee Yoon-Hee
    • Archives of Pharmacal Research
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    • v.28 no.6
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    • pp.730-735
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    • 2005
  • Nine polymorphic modifications of doxazosin mesylate have been obtained by recrystallization in organic solvents under variable conditions. Different polymorphs of doxazosin mesylate were characterized by powder X-ray crystallography diffractometry (PXRD), differential scanning calorimetry (DSC), and thermogravimetric analysis (TG). Transformation of Form 1 and Form 2 was not occurred in three relative humidities ($0\%$, $51\%$, and $99\%$) at 20$\pm$0.5 for 30 days.

Synthesis and characterization of Reactive Banana-Shaped Mesogens

  • Choi, Min-Ho;Choi, E-Joon;Kim, Young-Chul;Park, Sang-Hyon
    • 한국정보디스플레이학회:학술대회논문집
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    • 2006.08a
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    • pp.854-857
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    • 2006
  • The synthesis of ester type, banana-shaped, photo - crosslinkable mesogens is described. The reactive mesogens, derivatives of 1,3-phenylene bis{4-[4'- (alken-1-yloxy)-biphenyl-4-carboxylate]benzoate}s, were synthesized varying the length of alkyl end groups. The obtained monomers and polymers were characterized by FT/IR, NMR spectroscopy, DSC, polarized optical microscopy, and X-ray diffractometry.

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