• 제목/요약/키워드: Single crystal X-ray analysis

검색결과 196건 처리시간 0.023초

One-Pot Synthesis, Crystal Structures and Thermal Properties of Two Three-Dimensional Cobalt(II) Complexes

  • Tao, Bo;Lei, Wen;Cheng, Feiran;Xia, Hua
    • Bulletin of the Korean Chemical Society
    • /
    • 제33권6호
    • /
    • pp.1929-1933
    • /
    • 2012
  • Two cobalt(II) compounds $[Co(2,2{^\prime}-bipy)(H_2O)_2(SO_4)]_n$ (1) and $[Co_2(2,2^{\prime}-bipy)_2(btec)(H_2O)_6]{\cdot}2H_2O$ (2) (2,2'-bipy = 2,2'-bipyridine, $H_4btec$ = 1,2,4,5-benzenetetracarboxylic acid), have been simultaneously synthesized by a one-pot slow solvent evaporation reaction. Their structures were determined by single-crystal X-ray diffraction and further characterized by X-ray powder diffraction (XRPD), IR, elemental and thermogravimetric analysis (TGA). The structural analysis reveals that compound 1 exhibits an infinite 1D chain structure with the octahedral Co(II) centers bridging by the tetrahedral ${\mu}_2-SO{_4}^{2-}$ ligands, while compound 2 possesses a dinuclear $Co_2(2,2^{\prime}-bipy)_2(btec)(H_2O)_6$ unit and the two adjacent octahedral Co(II) ions are linked by the bismonodentately coordinated btec ligand. Additionally, compound 2 exhibits blue fluorescent emission in the solid state at room temperature.

Experimental and ab initio Computational Studies on Dimethyl-(4-{4-{3-methyl-3-phenyl-cyclobutyl)-thiazol-2-yl]-hydrazonomethyl}-phenyl)-amine

  • Yuksektepe, Cigdem;Saracoglu, Hanife;Caliskan, Nezihe;Yilmaz, Ibrahim;Cukurovali, Alaaddin
    • Bulletin of the Korean Chemical Society
    • /
    • 제31권12호
    • /
    • pp.3553-3560
    • /
    • 2010
  • A new hydrazone derivative compound has been synthesized and characterized by IR, $^1H$-NMR, $^{13}C$-NMR and UV-vis. spectroscopy techniques, elemental analysis and single-crystal X-ray diffraction (XRD). The new compound crystallizes in monoclinic space group C2/c. In addition to the crystal structure from X-ray experiment, the molecular geometry, vibrational frequencies and frontier molecular orbitals analysis of the title compound in the ground state have been calculated by using the HF/6-31G(d, p), B3LYP/6-311G(d, p) and B3LYP/6-31G(d, p) methods. The computed vibrational frequencies are used to determine the types of molecular motions associated with each of the observed experimental bands. To determine conformational flexibility, molecular energy profile of (1) was obtained by semi-empirical (AM1) calculation with respect to a selected degree of torsional freedom, which was varied from $-180^{\circ}$ to $+180^{\circ}$ in steps of $10^{\circ}$. Molecular electrostatic potential of the compound was also performed by the theoretical method.

The Crystal Structure of Acemetacin Monohrdrate $(C_{21}H_{18}NO_6Cl-H_2O)$, A Non-Steroidal Antiinflammatory Agent

  • Kim, Yang-Bae;Kim, Jeong-Ae;Park, Yeong-Il
    • Archives of Pharmacal Research
    • /
    • 제16권2호
    • /
    • pp.134-139
    • /
    • 1993
  • The molecular structure of acemetacin, 1-(4-chlorobenzoyl)-5-methoxy-2-methyl-1H-indole-3-acetic acid carboxymethyl ester, was determined by single cystal X-ray diffraction analysis. The compound was recrystallized from a mixture of acetone and water in triclinic, space group P1, with a=7.796(1), b=10.245(2), c=13.542(3)$\AA,\;\alpha=97.35(1),\;\beta=96.34(1),\;\gamma=107.06(1)^\circ$, and Z=2. The calculated density is 1.422; the observed value is $1.42\;g/cm^3$. The structure was solved by the direct method and refined by full matrix least-squares procedure to the final R value of 0,037 for 2960 independent reflections. There are water molecules, which are thought to be co-crystallized during the evaporation procedure, with the ratio of one water per compound molecule in the crystal. The conformation of the compound is found to be very similar to that of indomethacin. The molecules are stabilized by three O-H.....O type intermolecular hydrogen bonds between the oxygen of water molecule and those of the compound.

  • PDF

Crystal Growth, Spectral, Magnetic, Antibacterial and Antifungal Studies of Co(II) and Ni(II) Complexes of 4-Nitrobenzoic Acid

  • Roy, Sunalya M.;Sudarsanakumar, M.R.;Dhanya, V.S.;Suma, S.;Kurup, M.R. Prathapachandra
    • 대한화학회지
    • /
    • 제58권3호
    • /
    • pp.258-266
    • /
    • 2014
  • Single crystals of cobalt(II) and nickel(II) complexes of 4-nitrobenzoic acid have been successfully grown by gel diffusion technique. The grown crystals were characterized by elemental analysis, FT-IR and UV-Visible spectroscopy. The structure of the grown crystals was elucidated using single crystal X-ray diffraction studies. The title compounds $[Co(Pnba)_2(H_2O)_4]{\cdot}2H_2O$ 1 and $[Ni(Pnba)_2(H_2O)_4]{\cdot}2H_2O$ 2 where PnbaH=4-nitrobenzoic acid, crystallize in centrosymmetric triclinic space group P-1. Magnetic susceptibility measurements reveal that the compounds are paramagnetic in nature. The mechanical strength of the grown crystals was determined by Vicker's microhardness studies. The ligand (4-nitrobenzoic acid) and the complexes have been screened for their biological activity against various bacteria and fungi. The activity data show that the biological activity of the complexes is higher than that of the ligand.

Crystal Growth of InP by VGF Method using Auqrtz Ampoule Characterization

  • Park, E.S.;C.H. Jung;J.J. Myung;J.Y. Hong;Kim, M.K.
    • 한국결정성장학회:학술대회논문집
    • /
    • 한국결정성장학회 1999년도 PROCEEDINGS OF 99 INTERNATIONAL CONFERENCE OF THE KACG AND 6TH KOREA·JAPAN EMG SYMPOSIUM (ELECTRONIC MATERIALS GROWTH SYMPOSIUM), HANYANG UNIVERSITY, SEOUL, 06월 09일 JUNE 1999
    • /
    • pp.419-431
    • /
    • 1999
  • InP, III-V binary compound semiconductor, single crystal was grown by VGF (vertical gradient freeze) method using quartz ampoule and its electrical optical properties were investigated. Phosphorous powders were put in the bottom of quartz ampoule and Indium metal changed in conical quartz crucible hat was attached at the upper side position inside the quartz ampoule. It was vacuous under the pressure of 10-5 Torr and sealed up. In metal in the quartz crucible was melted at 1070$^{\circ}C$ and phophorous sublimated at 450$^{\circ}C$, there after it was diffused in In melt and so InP composition was formed. By cooling the InP composition melt (2$^{\circ}C$∼5$^{\circ}C$/hr of cooling rate) in range of 1070$^{\circ}C$∼900$^{\circ}C$, InP crystal was grown. the grown InP single crystals were investigated by X-ray analysis and polarized optical microscopy. Electrical properties of them were measured by Van der Pauw method. At the cooling rate of 2$^{\circ}C$/hr, its direction was (111), quality of the ingot ws better upper side of the ingot than lower. It was found that the InP crystals were n-type semiconductor and the carrier concentration, electron mobility and relative resistivity were 1015∼1016/㎤, 2x103∼3x104$\textrm{cm}^2$/Vsec and 2x10-1∼2x10-3Ωcm in the range of 150K∼300K, respectively.

  • PDF

EFG법에 의한 ${\gamma}-6Bi_2O_3 {\cdot}SiO_2$(BSO)단결정의 육성 (Growth of ${\gamma}-6Bi_2O_3 {\cdot}SiO_2$( Single Crystals by EFG Method)

  • 김호건;유건종
    • 한국결정성장학회지
    • /
    • 제1권1호
    • /
    • pp.26-38
    • /
    • 1991
  • 광기능소자로 응용성이 넓은 전기광학결정 $r-6Bi_2O_3{\cdot}SiO_2$(이하 BSO로 약칭)을 EFG(Edge-defined Film-fed Growth)법에 의하여 판상단결정으로 육성하는 기초적 조건을 조사하고 육성된 판단결정의 characterization 및 평가와 물성측정을 하였다. 본 연구에서 얻어진 최적성장조건은 온도구배가 $24^{\circ}C/cm$, 인상속도는 2.0mm/h이었다. 결정성장 최적조건에서 육성된 BSO결정은 제 2상의 석출이 없고 grain boundary가 존재하지 않으며 X선 분석으로도 단결정임이 확인되었다. 육성된 판상단결정의 판면은 (100)면이었고 결정성장 방위는 <100>이었다. 육성된 판상단결정은 편광현미경하에서는 pore, void, inclusion, striation 등의 성장결함이 없는 양질의 단결정이었으나 미세결함인 전위(dislocation)의 존재가 확인되었고 전위밀도는 $5.1{\times}10^5/\textrm{cm}^2$이었다.

  • PDF

Hydrothermal Synthesis, Crystal Structure of Four Novel Complexes Based on Thiabendazole Ligand

  • Wei, Shui-Qiang;Lin, Cui-Wu;Yin, Xian-Hong;Huang, Yue-Jiao;Luo, Pei-Qi
    • Bulletin of the Korean Chemical Society
    • /
    • 제33권9호
    • /
    • pp.2917-2924
    • /
    • 2012
  • Four novel metal-organic complexes $[Cd_2(IP)_2(TBZ)_2(H_2O)_2]{\cdot}(H_2O)$ (1), $[Zn_4(IP)_4(TBZ)_4]{\cdot}2(H_2O)$ (2), $[Zn_2(BTC)(TBZ)_2(CO_2H)]$ (3), [Co(PDC)(TBZ)] (4) (where IP = isophthalate; TBZ = thiabendazole; BTC = 1,3,5-benzenetricarboxylate; PDC = pyridine-3,4-dicarboxylate) have been prepared and characterized by IR spectrum, elemental analysis, thermogravimetric analysis, and single-crystal X-ray diffraction. X-ray structure analysis reveals that 1, 2, and 3 are one-dimensional chain polymers, while 4 is a two-dimensional network polymer. The TBZ acts as a typical chelating ligand coordinated to the metal center in all complexes. The 1D chain architecture of 1 is constructed from isophthalates and cadmium atoms. A simultaneous presence of chelating, monodentate and bidentate coordination modes of IP ligands is observed in complex 2. In complex 3, the 16-membered rings are alternately arranged forming an infinite 1D double-chain structure. The 2D skeleton of 4 is formed by cobalt ions as nodes and PDC dianions as spacers, through coordination bonds. The hydrogen bonds and ${\pi}-{\pi}$ stacking play important roles in affecting the final structure where complexes 1 and 3 have 2D supramolecular networks, while complexes 2 and 4 have 3D supramolecular architectures.

니켈절삭시 CBN, 소결 및 단결정 다이아몬드 공구의 마멸과 예측에 관한 연구 (A Study on the Tool Wear and Prediction of CBN, Poly Crystal and Single Crystal Diamond Tools in Cutting of Nickel)

  • 성기석;김정두
    • 대한기계학회논문집
    • /
    • 제17권1호
    • /
    • pp.120-130
    • /
    • 1993
  • 본 연구에서는 니켈의 가공시 나타나는 공구의 마멸에 대한 정량화 및 절삭변 수와의 연관성에 대한 연구는 그 자체가 마멸에 대한 데이터 베이스 측면에서 중요하 고, 이러한 접근방법으로는 연구가 거의 이루어지지 않았다는 측면에서도 큰 의미를 갖는다. 본 연구는 특히 경도가 큰 공구인 CBN, 소결 다이아몬드(poly crystal dia- mond 이하 PCD), 단결정 다이아몬드(single crystal diamond 이하 SCD)공구를 사용하 여 니켈의 절삭에서 나타나는 공구의 마멸에 대한 분석을 선행한 후 수집한 정보로부 터 절삭속도, 이송, 절삭깊이 및 공구의 nose반경이 공구의 마멸 및 표면의 성상(su- rface quality)에 미치는 영향에 대하여 고찰하였고 절삭조건의 변화에 따라 마멸에 대한 예상 곡선을 구하였다.

Pd 삽입 니켈모노실리사이드의 물성과 미세구조 변화 (Property and Microstructure Evaluation of Pd-inserted Nickel Monosilicides)

  • 윤기정;송오성
    • 대한금속재료학회지
    • /
    • 제46권2호
    • /
    • pp.69-79
    • /
    • 2008
  • A composition consisting of 10 nm-Ni/1 nm-Pd/(30 nm or 70 nm-poly)Si was thermally annealed using rapid thermal for 40 seconds at $300{\sim}1100^{\circ}C$ to improve the thermal stability of conventional nickel monosilicide. The annealed bilayer structure developed into $Ni(Pd)Si_x$, and the resulting changes in sheet resistance, microstructure, phase, chemical composition, and surface roughness were investigated. The silicide, which formed on single crystal silicon, could defer the transformation of $NiSi_2$, and was stable at temperatures up to $1100^{\circ}C$. It remained unchanged on polysilicon substrate compared with the sheet resistance of conventional nickel silicide. The silicides annealed at $700^{\circ}C$, formed on single crystal silicon and 30 nm polysilicon substrates exhibited 30 nm-thick uniform silicide layers. However, silicide annealed at $1,000^{\circ}C$ showed preferred and agglomerated phase. The high resistance was due to the agglomerated and mixed microstructures. Through X-ray diffraction analysis, the silicide formed on single crystal silicon and 30 nm polysilicon substrate, showed NiSi phase on the entire temperature range and mixed phases of NiSi and $NiSi_2$ on 70 nm polysilicon substrate. Through scanning probe microscope (SPM) analysis, we confirmed that the surface roughness increased abruptly until 36 nm on 30 nm polysilicon substrate while not changed on single crystal and 70 nm polysilicon substrates. The Pd-inserted nickel monosilicide could maintain low resistance in a wide temperature range and is considered suitable for nano-thick silicide processing.

Skull melting법에 의해 성장된 rutile 단결정 분석 (Analysis of rutile single crystals grown by skull melting method)

  • 석정원;최종건
    • 한국결정성장학회지
    • /
    • 제16권5호
    • /
    • pp.181-188
    • /
    • 2006
  • 스컬용융법에 의해 성장시킨 rutile단결정을 성장 축과 수평 또는 수직으로 절단한 후 ${\phi}5.5mmx1.0mm$ 크기의 웨이퍼로 양면연마 하였다. 연마한 흑색 웨이퍼들은 $1200^{\circ}C$에서 $3{\sim}15$시간, $1300^{\circ}C$에서 $10{\sim}50$시간 annealing을 행함에 의해 옅은 황색으로 변화되었다. Annealing 후 구조적 및 광학적 특성은 비중, SEM-EBSP, XRD, FT-IR, laser Raman, PL 그리고 XPS 등으로 분석하였고, 이들 결과들은 공기중의 무게 증가, 수중의 무게 및 비중의 감소,침상의 2차상, 산소이온 확산 및 $Ti^{3+}$ 이온이 감소되는 것으로 분석되었다. 이는 스컬용융법에 의해 성장된 rutile 단결정에 $O_v,\;Ti^{3+},\;O_v-Ti^{3+}$ interstitial 그리고 $F^+-H^+$와 같은 결함의 존재를 의미한다.