• Bulletin of the Korean Chemical Society
• /
• 제11권1호
• /
• pp.15-19
• /
• 1990

The crystal structure of $(C_{12}H_{24}O_6{\cdot}K)_2K[Co(OH)_6Mo_6O_{18}]{\cdot}12H_2O$ has been determined by X-ray diffraction. Crystal data as follows ; monoclinic, space group $C_2/m,\;a\;=\;22.512(4)\;{\AA},\;b\;=\;18.304(4)\;{\AA},\;c\;=\;7.641(1)\;{\AA},\;{\beta}\;=\;90.52(2)\;{\AA}$, and Z = 2. A final conventional R value of 0.044 was obtained by least-squares refinement of 4173 independent observed $[{\mid}Fo{\mid}{\geq}3{\sigma}({\mid}Fo{\mid})]$ reflections. The $[Co(OH)_6Mo_6O_}{18}]^{-3}$ polyanion shows the well-known Anderson-structure and has approximate 3m symmetry. A $[Co(OH)_6Mo_6O_{18}]^{-3}$ polyanion is located between two crown ether complexed cations forming a sandwich structure. One potassium ion interacts with the crown ether via electrostatic interactions. The other potassium ion only interacts with the water molecules and terminal oxygen atoms of the polyanion.

• Bulletin of the Korean Chemical Society
• /
• 제15권6호
• /
• pp.432-436
• /
• 1994

Monomeric rhodium and iridium-diaryltetrazene complexes $Cp^*$M(RNN=NNR)($Cp^*$=1,2,3,4,5-pentamethylcyclope ntadienyl; M=Rh, Ir; R=Ph, 4-tolyl) have been synthesized from [$Cp^*MCl_2]_2$(M=Rh, Ir) and 2 equiv. of $[Li(THF)_x]_2(RN_4$R) in benzene. We have determined the crystal structure of (${\eta}^5$-pentamethylcyclopentadienyl)diphenyltetrazene iridium by using graphite-monochromated Mo-$K_a$ radiation. The compound was crystallized in the monoclinic space group $P2_{1/c}$ with a=13.781(3), b=9.035(l), c=17.699(3) ${\AA}$, and ${\beta}=111.93(l)^{\circ}$. An X-ray crystal structure of complex 1 showed a short N(2)-N(3) distance ($1.265 {\AA}$) consistent with the valence tautomer A with Ir(III) rather than Ir(I). All complexes are highly colored and decompose on irradiation at 254 nm. Electrochemical studies show that complex 1 displays a quasi-reversible reduction.

• Bulletin of the Korean Chemical Society
• /
• 제19권4호
• /
• pp.457-462
• /
• 1998

A chiral pentadentate bis-amide ligand, 1,9-bis(S)-pyrrolidinyl-2,5,8-triazanonane-1,9-dio ne$(S,S-prodienH_2)$ has been synthesized from the reaction of bis(2-aminoethyl)amine(dien) and S-proline, and the structure of $[Co(S,S-prodien)H_2O]ClO_4$ has be en determined by single crystal X-ray diffraction. The geometrical structure of the Co(III) complex has been an αβ -form, where the dien moiety of ligand chelates to a facial in metal center, and the aqua ligand coordinates a cis site to the secondary nitrogen of dien. The Co-N(1), Co-N(3) distances of two amide moiety in S,S-prodien are shorter than the other Co-N(2), Co-N(4), and Co-N(5) distances because of the increased basicity of nitrogen in amide. The complex crystallizes in the monoclinic space group $P2_1$(#4), with a=7.838(1), b=12.675(1), c=9.710(1) Å, β=100.39(1) and z=2. Refinement gives the final R and $R_w$ values of 0.045 and 0.057, respectively for 2130 observed reflections. Based upon the CD and X-ray data, it is identified that the absolute configuration of the αβ -$[Co(S,S-prodien)H_2O]ClO_4$ has a Λ-form.

• Bulletin of the Korean Chemical Society
• /
• 제15권12호
• /
• pp.1108-1112
• /
• 1994

25-Acetoxy-26,27,28-trimethoxycalix[4]arene was synthesized by the treatment of calix[4]arene trimethyl ether with acetyl chloride in the presence of NaH. The solution conformation was inferred as a partial cone conformation based on the $^1H$-and $^{13}C$ NMR spectra. The crystal structure has been determined by X-ray diffraction method. The crystals are monoclinic, space group $P2_1$/n, a=8.186 (1), b=17.137 (2), c=19.878 (3) ${\AA}$, ${\beta}$=95.67 (1)$^{\circ}$, Z=4, V=2774.90 ${\AA}^3$, $D_c$= 1.22 g $cm^{-3}$, $D_m$=1.23 g $cm^{-3}$. The intensity data were collected on an Enraf-Noninus CAD-4 Diffractometer with a graphite monochromated $Cu-K{\alpha}$ radiation. The structure was solved by direct method and refined by full-matrix least-squares methods to a final R value of 0.054 for 3675 observed reflections. The molecule possesses a partial cone conformation with one flattened phenyl unit, in which one anisol ring, distal to the ester ring, is inverted. The acetoxyphenyl ring is flattened.

• Bulletin of the Korean Chemical Society
• /
• 제15권2호
• /
• pp.150-153
• /
• 1994

By treating mer, trans-Re(${\equiv}NC_6H_5)(PPh_3)_2Cl_3$, Ⅰ, with 5 atm of CO at room temperature for 52 h, fac-Re(${\equiv}NC_6H_5)(CO)(PPh_3)Cl_3$, Ⅱ, was obtained as dark green precipitates in 81% yield. The crystal structure of Ⅱ was determined through X-ray diffraction. Ⅱ crystallizes in the monoclinic system, space group $P2_1/n$ with cell parameters a=9.740 (2) ${\AA}$, b=16.210 (5) ${\AA}$, c=16.192 (6) ${\AA}$, ${\beta}$=97.50 $(2)^{\circ}$, and Z=4. Least-squares refinement of the structure led to a R$(R_w)$ factor of 0.030 (0.036) for 2878 unique reflections of I>3${\sigma}(I)$ and for 241 variables. In comparison to the starting material Ⅰ, the bond distance of Re-N became longer from 1.726 (6) to 1.736 (5) ${\AA}$ and the bond angle of Re-N-C(Ph) became smaller from 172.6 (6) to 167.0 $(2)^{\circ}$, indicating that the Re-N bond in Ⅱ is weakened and has a less triple-bond character than that in Ⅰ.

• 대한화학회지
• /
• 제67권1호
• /
• pp.33-41
• /
• 2023

Nanocrystallne WO₃ and MoO₃ with several different sizes and crystal structures were prepared by simple acid precipitation and subsequent heat treatment. The photochromic (PC) properties of these samples were comparatively investigated in powder state by monitoring diffuse reflectance spectral changes after bandgap irradiation. The PC effect of hexagonal WO₃ and monoclinic WO₃ strongly depended upon crystallite size rather than crystal structure. The smaller the crystallite size, the better the PC effect. However, orthorhombic WO·H₂O and MoO₃ having hexagonal and orthorhombic structures did not follow this trend. One consistent result for all WO₃ and MoO₃ samples is that the heat treatment in air, which changes crystallinity, whether it changes the crystal structure or only the crystallite size, reduces the PC effect. Since the thermal treatment reduces the surface oxygen defect sites, we believe that the PC effect of WO₃ and MoO₃ depends critically on the surface oxygen defect sites that serve as deep trap sites for photogenerated electrons and oxygen radical holes. We also found that the proton insertion claimed by double charge injection model is not critical for the PC effect.

• 한국가시화정보학회지
• /
• 제22권1호
• /
• pp.18-27
• /
• 2024

A series of shock wave pulses with Mach number 2.2 of 100, 200, and 300 shocks were applied to lead sulfide (PbS) nanomaterials at intervals of 5 sec per shock pulse. To investigate the crystallographic, electronic, and magnetic phase stabilities, powder X-ray diffractometry (XRD), diffused reflectance spectroscopy (DRS), and vibrating-sample magnetometry (VSM) were employed. The material exhibited a rock salt structure (NaCl-type structure); XRD results indicated that material is monoclinic with space group C121 (5). Further, XRD results showed shifts due to lattice contraction and expansion when material was subjected to shock wave pulses, indicating stable material structure. Based on the data obtained, we believe that the PbS material is a good choice for high-pressure, high-temperature, and aerospace applications due to its superior shock resistance characteristics.

• 한국진공학회지
• /
• 제7권4호
• /
• pp.361-367
• /
• 1998

유기 박막 트렌지스터의 활성층으로 사용하기 위하여 공액성 소중합체인 $\alpha$ -sexithiophene($\alpha$-6T)이라는 시료를 가지고 유기 분자선 증착법(OMBD)을 이용하여 박막 을 제작하였으며 $\alpha$-6T박막의 성막 조건에 따른 박막의 분자 배향, 결정구조 그리고 표면 특성을 알아보기 위해 angle-resolved UV/visible absorption spectroscopy, X-ray diffractometry(XRD) 그리고 atomic force microscopy(AFM)를 이용하였으며 그 분석 결과 성막 조건에 관계없이 모두 monoclinic한 결정구조를 갖으나, 초고진공, 낮은 성막 속도, 기 판의 온도가 높은 조건일 경우 $\alpha$-6T 분자들이 기판에 수직적으로 배열한다는 것을 확일할 수 있었다.

• 대한화학회지
• /
• 제35권4호
• /
• pp.324-328
• /
• 1991

$Li_2SO_4$를 기질로 한 Li$_2SO_4-CaSO_4$4 계를 합성하여 상온에서 700$^{\circ}C$까지의 온도구간에서 구조와 전도성을 연구하였다. CaSO$_4$의 몰비가 5${\%}$ 이상일 경우 Li$_2SO_4-CaSO_4$는 고용체를 형성하지 않음을 규명하였다. 치환되는 Ca$^{2+}$ 이온에 의해 단사정계에서 면심입방으로의 전이온도는 다소 낮아졌다. 단사정계의 전도도는 Ca$^{2+}$ 치환에 의해 생성되는 Li 공위에 의해 증가되나 면심입방구조의 전도도는 Ca$^{2+}$ 치환에 별 영향을 받지 않았다.

• 한국재료학회지
• /
• 제21권7호
• /
• pp.391-395
• /
• 2011

The structure and dielectric properties of poled <001>-oriented 0.7Pb($Mg_{1/3}Nb_{2/3})O_3-0.3PbTiO_3$ (PMN-0.3PT) crystals have been investigated for orientations both parallel and perpendicular to the [001] poling direction. An electric field induced monoclinic phase was observed for the initial poled sample. The phase remained stable after the field was removed. A quite different temperature dependence of dielectric constant has been observed between heating and cooling due to an irreversible phase transformation. The results of mesh scans and temperature dependence of the dielectric constant demonstrate that the initial monoclinic phase changes to a single domain tetragonal phase at 370K and to a paraelectric cubic phase at 405K upon heating. However, upon subsequent cooling from the unpoled state, the cubic phase changes to a poly domain tetragonal phase and to a rhombohedral phase. In the ferroelectric tetragonal phase with a single domain state, the dielectric constant measured perpendicular to the poling direction was dramatically higher than that of the parallel direction. A large dielectric constant implies easier polarization rotation away from the polar axis. This enhancement is believed to be related to dielectric softening close to the morphotropic phase boundary and at the phase transition temperature.