• Journal of the Korean Chemical Society
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• v.53 no.5
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• pp.530-535
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• 2009

Dicyclohexyl telluride was obtained in a high yield by the reaction of cyclohexyl bromide with NaTeH(prepared in situ) in an aqueous ethanolic solution. A series of new organotelluronium salts of the general formula ${(cyclo-C_6H_11)}_2Te(R)X$ (where R = $CH_3$, X = I (1); R = $C_2H_5$, X = Br(2); R = $C_2H_5$, X = I (3); R = C_3H_5$, X = Br (4)) were prepared by the reaction of ${(cyclo-C_6H_11)}_2Te$ with the corresponding alkyl halide. Reaction of 1 with NaBPh4 gave compound 5 ( i.e. R = CH3, X = BPh4 ‒) in 78% yield. Reaction of ${(cyclo-C_6H_11)}_2Te$ with benzyl bromide and 4-bromophenacyl bromide gave unexpectedly dibenzylcyclohexyltelluronium bromide (6) and bis(4-bromophenacyl)cyclohexyltelluronium bromide (7), respectively. Reaction of 6 with NaBPh4 gave the corresponding tetraphenylborate derivative (8) in high yield. $^1H$ NMR studies revealed that in $CDCl_3$solution compound 1 eliminated alkyl halide. Conductivity, IR, $^1H\;and\;^{13}C$ NMR and thermal data for the new compounds are presented and discussed.

• Journal of the Korean Chemical Society
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• v.39 no.3
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• pp.198-203
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• 1995

The Mo(V) $di-\mu-oxo$ type $(Mo_2O_4(H_2O)_2L)$ complexes $(L:\;C_3H_7CH(SCH_2COOH)_2,\;C_6H_5CH(SCH_2COOH)_2,\;CH_3OC_6H_4CH(SCH_2COOH)_2,\;C_5H_{10}C(SCH_2COOH)_2,\;C_3H_7C(CH_3)(SCH_2COOH)_2,\;C_3H_7CH(SCH_2CH_2COOH)_2,\;C_6H_5CH(SCH_2CH_2COOH)_2)$ have been prepared by the reaction of $[Mo_2O_4(H_2O)_6]^{2+}$ with a series of dithiodicarboxy ligands. These complexes are completed by two terminal oxygens arranged trans to one another and each ligand forms a chelate type between two molybdenum. In $Mo_2O_4(H_2O)_2L$, two $H_2O$ coordinated at trans site of terminal oxygens. The prepared complexes have been characterized by elemental analysis, infrared spectra, electronic spectra, and nuclear magnetic resonance spectra. In the potential range -0.00 V to -1.00 V at a scan rate of 20 $mVs^{-1}$, a cathodic peak at -0.50∼-0.58 V (vs. SCE) and an anodic peak at -0.40∼-0.43 V (vs. SCE) have been observed in aquous solution. The ratio of the cathodic to anodic current ($I_{pc}/I_{pa}$) is almost 1, we infer that redox is reversible reaction.

• Journal of the Korean Chemical Society
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• v.27 no.6
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• pp.434-440
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• 1983

New procedures for the reduction of carboxylic acids, carboxylic acid salts, tertiary amides, and sulfoxides with sodium borohydride and triphenyl borate in tetrahydrofuran were developed. Thus carboxylic acids were reduced quantitatively in 6∼12 h at $25^{\circ}C$. Alphatic acid salts were quantitatively reduced to the corresponding alcohols in 6h at $25^{\circ}C$ whereas aromatic acid salts required 24h at $65^{\circ}C$. Tertiary amides were reduced to the corresponding amines in 88∼100% yields in 3∼6h at room temperature. Most sulfoxides examined were reduced to the corresponding sulfides in 98∼100% yields in 1∼6h at $25^{\circ}C$ and completely reduced at $65^{\circ}C$; however, diphenyl sulfoxide required 48h in a more vigorous condition.

• Journal of the Korean Chemical Society
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• v.30 no.5
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• pp.441-448
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• 1986

Dioxobis(sub.-salicylaldiminato) molybdenum (VI) complexes, $MoO_2\;(X-sal-N-R)_2,\;(X=H,\;5-CH_3,\;R=C_6H_5,\;p-F-C_6H_4,\;m-Cl-C_6H_4,p-I-C_6H_4\;and\;p-C_2H_5-C_6H_4)$, have been prepared by reactions of dioxobis(sub.-salicylaldehydato) molybdenum (VI), $MoO_2(X-sal)_2$ with primary amines, in which $MoO_2(X-sal)_2$ complexes were obtained by acidification of a mixture solution of ammonium paramolybdate in water and appropriate salicylaldehyde in methanol. All these complexes show two strong Mo=O stretching imodes in the 900-940$cm^{-1}$ and p.m.r. spectra exhibited only one signal for the azomethine group. These results confirmed that the complexes are six-coordinated octahedron with a $cis-MoO_2$ group and the geometrical configurations of the complexes possess a C2 axis of symmetry. From the mass analyses of the complexes, it found that the composition ratios of $MoO_2$ : ligand are 1 : 2. The charge transfer transition corresponding to N-Mo, and O-Mo occured at 29,000$cm^{-1}$ and 32,000$cm^{-1}$ respectively. Where, the complexes were found to be non-ionic materials by conductivity measurements in dimethylformamide.

• Bulletin of the Korean Chemical Society
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• v.7 no.6
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• pp.468-471
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• 1986

The isolated products from the reactions of $Rh(ClO_4)(CO)(PPh_3)_2$ (1) with CH_2$ = $CHCO_2C_2H_5$ (2) and trans-$CH_3CH$ = $CHCO_2C_2H_5$ (3) contain 80∼ 90% of $[Rh(CH_2 = CHCO_2C_2H_5)(CO)(PPh_3)_2]ClO_4$ (4) and [Rh(trans-$CH_3CH = CHCO_2C_2H_5(CO)(PPh_3)_2]ClO_4$ (5), respectively where 2 and 3 seem to be coordinated through the carbonyl oxygen. It has been found that complex 1 catalyzes the isomerization of $CH_2 = CH(CH_2)_8CO_2C_2H_5$ (6) to $CH_3(CH_2)_nCH = CH(CH_2)_{7-n}CO_2C_2H_5$ (n = 0∼7) under nitrogen at 25$^{\circ}C$. The isomerization of 6 is slower than that of $CH_2 = CH(CH_2)_9CH_3$ to $CH_3(CH_2)_nCH$ = $CH(CH_2)_{8-n}CH_3$ (n = 0∼8), which is understood in terms of the interactions between the carbonyl oxygen of 6 and the catalyst. It has been also observed that complex 1 catalyzes the hydrogenation of 2, 3, 6, trans-$C_6H_5CH = CHCO_2C_2H_5$ (7), $CH_3(CH_2)_7CH = CH(CH_2)_7CO_2C_2H_5$ (8) and $CH_2 = CH(CH_2)_9CH_3$ (9), and the isomerization (double bond migration) of 6 and 9 under hydrogen at 25$^{\circ}C$. The interactions between the carbonyl oxygen of the unsaturated esters and the catalyst affect the hydrogenation in such a way that the hydrogenation of the unsaturated esters becomes slower than that of simple olefins.

• Bulletin of the Korean Chemical Society
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• v.24 no.5
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• pp.605-609
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• 2003

The lower-order lithium organocyanocuprate compound, (THF)₃Li(NC)Cu($C_6$H₃-2,6-Mes₂) (1), and the bulky terphenyl Grignard reagent, Br(THF)₂Mg($C_6$H₃-2,6-Trip₂) (2), have been synthesized and structurally characterized both in the solid state by single crystal x-ray crystallography and in solution by multi-nuclear NMR and IR spectroscopy. The compound (1) was isolated as a monomeric contact ion-pair in which the C (organic ipso)-Cu-CN-Li atoms are coordinated linearly. The lithium has a tetrahedral geometry as a result of solvation by three THF molecules. The compound (1) is the first example of fully characterized monomeric lower order lithium organocyanocuprate. The bulky Grignard reagent (2) was also isolated as a monomer in which the magnesium, solvated by two THF molecules, has a distorted tetrahedral geometry. The crystals of (1) possess triclinic symmetry with the space group $P{\={1}}$, Z = 2, with a = 12.456(3) Å, b = 12.508(3) Å, c = 13.904(3) Å, α = 99.81°, β = 103.72(3)°, and γ = 119.44(3)°. The crystals (2) have a monoclinic symmetry of space group $P2_{1/C}$, Z = 4, with a = 13.071(3) Å, b = 14.967(3) Å, c = 22.070(4) Å, and β = 98.95(3)°.

• Bulletin of the Korean Chemical Society
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• v.26 no.8
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• pp.1185-1189
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• 2005

Two new copper vanadium borophosphate compounds, $(NH_4)(C_2H_{10}N_2)_{5.5}[Cu(C_2H_8N_2)_2]_3[V_2P_2BO_{12}]_6{\cdot}17H_2O,\;Cu-VBPO1\;and\;(NH_4)(C_2H_{10}N_2)_{3.5}[Cu(C_2H_8N_2)_2]_5[V_2P_2BO_{12}]_6{\cdot}18H_2O$, Cu-VBPO2 have been hydrothermally synthesized and characterized by single crystal X-ray diffraction, thermogravimetric analysis, IR spectroscopy, and elemental analysis. The structure of Cu-VBPO1 contains a layer anion, {$[Cu(C_2H_8N_2)_2]_3[V_2P_2BO_{12}]_6$}$^{12-}$, whereas Cu-VBPO2 has an open framework anion, {$[Cu(C_2H_8N_2)_2]_5[V_2P_2BO_{12}]_6$}$^{8-}$. Crystal Data: $(NH_4)(C_2H_{10}N_2)_{5.5}[Cu(C_2H_8N_2)_2]_3[V_2P_2BO_{12}]_6{\cdot}17H_2O$, monoclinic, space group I2/m (no. 12), $\alpha$ = 15.809(1) $\AA$, b = 31.107(2) $\AA$, c = 12.9343(8) $\AA$, $\beta$ = 104.325(1)$^{\circ}$, Z = 2; $(NH_4)(C_2H_{10}N_2)_{3.5}[Cu(C_2H_8N_2)_2]_5[V_2P_2BO_{12}]_6{\cdot}18H_2O$, tetragonal, space group $P4_2$/mnm (no.136), $\alpha$ = 26.832(1) $\AA$, c = 18.021(1) $\AA$, Z = 4.

• Advances in materials Research
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• v.6 no.3
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• pp.303-316
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• 2017

In this article, novel olefin polymerization catalyst with lower cost and simple synthetic process were developed, $ArOTiCl_3$ complexes [$(2-OMeC_6H_4O)TiCl_3(C1)$, $(2,4-Me_2C_6H_3O)TiCl_3(C2)$, $TiCl_3(1,4-OC_6H_4O)TiCl_3(C3)$, $TiCl_3(1,4-OC_6H_2O-Me_2-2,5)$ $TiCl_3(C4)$] and corresponding $(ArO)_2TiCl_2$ complexes [$TiCl_2(OC_6H_4-OMe-2)_2(C5)$ and $TiCl_2(OC_6H_3-Me_2-2,6)_2(C6)$] have been synthesized by the reaction of $TiCl_4$ with phenol, all these complexes were well characterized with $^1H$ NMR, $^{13}C$ NMR, MASS and EA. When combined with methylaluminoxane (MAO), the $ArOTiCl_3/MAO$ system shows high activity for ethylene copolymerization with 1-octene and copolymer was obtained with broaden molecular weight distribution (MWD). The $^{13}C$ NMR result of polymer indicates that the 1-octene incorporation in polymer reached up to 8.29 mol%. The effects of polymerization temperature, concentration of polymerization monomer and polymerization time on the catalytic activity have been investigated.

• Progress in Superconductivity
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• v.12 no.2
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• pp.104-109
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• 2011

We have investigated the anisotropy of the superconducting properties for $CaC_6$ and $SrC_6$ using upper critical fields ($H_{c2}$) and specific heat ($C_p$). From the upper critical fields of $CaC_6$ at different magnetic field orientations, H//c and H// ab, the anisotropy is found to be ~ 5 at low temperatures, much larger than that of $SrC_6$. These results are in contrast to the stronger anisotropy in the electronic structure for $SrC_6$ than for $CaC_6$ indicating a stronger anisotropy in the superconducting gap in $CaC_6$. The findings are confirmed by the temperature dependence of the superconducting specific heat below $T_c$ for $CaC_6$ and $SrC_6$, suggesting the important role of anisotropic electron-phonon coupling in superconducting intercalated graphites.

• Bulletin of the Korean Chemical Society
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• v.7 no.5
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• pp.338-341
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• 1986

Hydrocarbon solution of $Ir(PPh_3)_2(CO)OClO_3$ reacts with $Ph_2PC_6H_4$-o-CHO and 3-methyl-2-aminopyridinyl aldimine to yield ${\bar{Ir(Ph_2PC_6H_4-o-CO)}}\;(PPh_3)_2(CO)(H)ClO_4$(1) and ${\bar{Ir(NC_6H_6NC}}C_6H_5)(PPh_3)_2(CO)(H)ClO_4$(2), respectively. The compound $Ir(PPh_3)_2N_2Cl$ also reacts with $Ph_2PC_6H_4$-o-CHO and 3-methyl-2-aminopyridinyl aldimine to give ${\bar{Ir(Ph_2PC_6H_4-o-C}}O)(PPh_3)_2(H)Cl(3)$ and $Ir(NC_6H_5NCC_6H_5(PPh_3)_2(H)Cl(4)$, respectively. Compounds 1, 2, 3, and 4 were characterized by infrared, $^1H$ NMR, $^{31}p$ NMR, UV spectra, and conductivity measurements.