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Table of Content
24 August 1999, Volume 15 Issue 3
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Articles
Synthesis and Crystal Structure of di-p-Methyl pyridinium-p-methylpyridinidine Hexatungstate
LIN Xin-rong, CHEN Ming-qin, LIU Hui-zhang, XU Jin-yu, LI Pei, JIN Song-lin, XIE Gao-yang
1999, 15(3): 205-210.
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A novel isopolyanion salt [(CH
3
Py)
2
H]
2
W
6
O
19
was synthesized by the reaction of a white powdery tungstic acid (WPTA) with p-methylpyridine, and characterized by elemental analyses, infrared spectrometry and X-ray diffraction methods. In the crystal structure of the title compound there are a hexatungstate anion and two unique [(CH
3
Py)
2
H]
+
dimeric cations, and the most specific aspect of its structure is the first reported hydrogen bond existing between two of the p-methylpyridine molecules with a N_N distance of 0.267 3 nm. This hydrogen bond is analogous to that between the water molecules in H
5
O
2
+
, but is rather weaker.
Synthesis and Crystal Structure of Dicesium trans-Dicarbonatotetraaquomagnesium, Cs
2
[Mg(CO
3
)
2
(H
2
O)
4
]
ZHENG Yue-qing, ADAM Arnold
1999, 15(3): 211-217.
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The title compound, Cs
2
[Mg(CO
3
)
2
(H
2
O)
4
], was synthesized by the dropwise addition of an aqueous solution of Mg(NO
3
)
2
to a stirred aqueous Cs
2
CO
3
/CsHCO
3
solution. A colorless needle shaped crystal was formed by slow evaporation. The crystal structure was established on the basis of the single crystal X-ray diffraction data. Cs
2
[Mg(CO
3
)
2
(H
2
O)
4
] crystallized in the orthorhombic space group Pbca (No. 61) with a =0.658 4(1) nm, b =1.257 9(1) nm, c =1.301 3(1) nm, V =1.077 8 nm
3
, Z =4, D
x
=2.971 g·nm
-3
, μ =69.20 nm
-1
, F (000)=888, T =298 K, final R =0.029 and R
w
=0.024 for 1 037 observed reflections. The crystal consists of Cs
+
cations and the complex trans-[Mg(CO
3
)
2
(H
2
O)
4
]
2-
anions with each Mg atom coordinated by the six oxygens of two carbonate groups and four water molecules [ d (Mg_O)=0.203 6(4), 0.207 4(4), 0.213 4(4) nm]. The complex trans-[Mg(CO
3
)
2
(H
2
O)
4
]
2-
anions are arranged in a strongly compressed bcc pattern. A 3D network was formed through the intermolecular hydrogen bonds. The Cs
+
cations are located in cavities, each being surrounded by nine oxygens of five complex anions with d (Cs_O)=0.306 1-0.348 8 nm. The CO
3
2-
group reveals a lowering of D
3h
symmetry due to site and coordination effects, but not any observable deviation from co-planarity [ d (C_O)=0.127 2(6), 0.127 5(7), 0.130 5(6) nm and O_C_O=119.6(5)°, 120.1(5)°, 120.4(5)°].
Crystal Structure and Third order Nonlinear Optical Properties of cis-Configuration Biferrocene Trinuclear Complexes
WU Jie-ying, TIAN Yu-peng, XIE Fu-xin, NI Shi-sheng
1999, 15(3): 218-225.
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The syntheses and characterization of novel biferrocene trinuclear complexes of Schiff base ligand, S-methyl-N-(ferrocenyl-1-methyl methylidene)dithiocarbazate [hereafter abbreviated as HL (1)], are described. The X-ray diffraction studies have established the structures of PdL
2
(3) and CuL
2
(4). The geometry of Pd(Ⅱ) in (3) is close to a square plane and in the novel cis-configuration the two ferrocene moieties are in cis configuration, while that of Cu(Ⅱ) in (4) is close to a tetrahedral configuration. The electrochemical measurements suggested that the square planar configuration of Ni(Ⅱ) and Pd(Ⅱ) moieties can effectively transmit the redox effects of the ferrocene moieties, while the tetrahedral configuration of the Cu(Ⅱ) complex can not transmit the redox effects. The degenerate four wave mixing (DFWM) measurements showed that the complexes exhibit obviously nonlinear optical (NLO) response. The magnitude of their third order NLO susceptibility can be explained by their structure and electrochemical properties.
The Luminescence Properties of M'type of YTaO
4
∶Eu
LI Bo, GU Zhen-nan, DONG Yi, LIN Jian-hua, SU Mian-zeng
1999, 15(3): 226-231.
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A series of Eu
3+
doped of M'type of yttrium orthotantalate Y
1-x
Eu
x
TaO
4
( x =0—0.30) was sythesized. The influence of activator concentration on luminescence properties was studied in detail. The strong evidence from excitation spectra, emission spectra and diffusive reflection spectra of this system shows that there is energy transfer from TaO
4
3-
to Eu
3+
via the charge transfer and spectral overlap.
Preparation of β-Cyclodextrin Modified Fused Silica Capillary and Its Application in Capillary Electrophoresis Enantiomeric Separation
ZHANG Xin-xiang, HONG Feng, BAI Jing, CHANG Wen-bao, CI Yun-xiang
1999, 15(3): 232-237.
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A simple type of chiral selector immobilized capillaries was prepared and applied to the separation of some enantiomers by capillary electrophoresis(CE) without chiral selective reagents in a buffer solution. β-Cyclodextrin (CD) was bonded to the inner wall of fused silica capillary with the aid of 3-(2-cyclooxypropoxyl)-propyl-trimethoxy silane or 3-aminopropyltriethoxyl silane as bridge. The synthesis conditions such as reaction temperature, reaction ratios, solvents were optimized. The stability and reproducibility of the CD-modified capillaries were studied under different operation conditions. It is satisfactory to apply the capillary to the chiral separation of d,l-adrenaline and the atracurium besilate diastereoisomers under the optimized conditions.
Stereoselective Synthesis of the Pheromones of Ant Tetramorium Impurm and Leptogenys Diminuta
LI Yan, HUANG Jin-xia, ZHOU Zhong-qiang, CHEN Zu-xing, XU Zhang-huang
1999, 15(3): 238-242.
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(R,4S)-4-Methyl-3-hexanol and ( 3R,4S )-4-methyl-3-heptanol, which are the pheromones of ant Tetramorium impurm and Leptogenys diminuta, were stereoselectively synthesized by six-step sequence starting from N-bornane-10,2-sultam separately, the two asymmetric carbon atoms of the target products were created by employing asymmetric syn aldolization of N-acylbornane-10,2-sultam with propylaldehyde. The enantiomeric excess of the target products prepared by this route is over 92%.
Studies on α-Methacrylate Copper(Ⅱ) Complexes with Imidazole
WANG Yao-yu, SHI Qian, SHI Qi-zhen, GAO Yi-ci, ZHOU Zhong-yuan
1999, 15(3): 243-247.
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Two complexes of α-methacrylate copper(Ⅱ) with imidazole, Cu[CH
2
=C(CH
3
)COO]
2
· (imH)
2
(1) and Cu
2
[CH
2
C(CH
3
)COO]
4
(imH)
2
(2) were prepared and characterized. The single crystal X-ray diffraction study of complex 1 showed that the copper(Ⅱ) atom in the symmetric centre of the square planar environment was coordinated by two monodentate α methacrylate groups and two imidazole ligands that were in trans position with each other. Each molecular unit is linked with four neighbouring units by means of hydrogen bond interactions, forming a two-dimensional supermolecular compound( d
N
…O =0.278 1 nm). Complex 1 crystallizes in monoclinic, space group P2
1
/n with a =1.023 94(12) nm, b =0.842 94(8) nm, c =1.079 35(10) nm, β=117.231(7)°, Z =2. The forming mechanism of the complexes was discussed.
Synthesis of Enantiomeric Planar Square Ni
2+
-and Cu
2+
-Schiff Base Complexes
ZHAO Jian-zhang, WANG Shu-gang, WANG Xu, LIU Ju-zheng, QIAO Xiao-guang, LI Yao-xian, WANG Hua
1999, 15(3): 248-252.
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Enantiomeric four chelated planar square schiff base-Cu
2+
and Ni
2+
complexes were synthesized using ( 1R,trans )-and ( 1S,trans)-N,N'bis(2'-hydroxyphenyl methylene)-1,2-diaminocyclohexane. The chirality could not be shown by usual UV- Vis spectra. The intrinsic chiral difference of the enantiomeric complexes can be displayed by circular dichroism(CD) spectra. The Cotton effect of every polarlight-sensitive absorption of one enantiomer will be the opposite of that of the other enantiomer. It was found that no tetrahedron form exists for Ni
2+
complexes, which was determined with UV-Vis spectra and Electron Paramagnetic Resonance(EPR) measures.
Volumetric Properties of Sodium Chlorobenzoate in N,N-Dimethylformamide/water Mixtures at 298.15 K
LI Shu-qin, HU Xin-gen, YU Jia-miao, LIN Rui-sen, ZONG Han-xing
1999, 15(3): 253-257.
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Densities of sodium chlorobenzoate(o
-
, m
-
, p
-
) were measured in solutions up to 80 weight percent dimethylformamide(DMF) at 298.15 K with an oscillating tube densimeter. From these densities, apparent molar volumes of sodium chlorobenzoate in DMF-H
2
O mixtures were calculated, and partial molar volumes at infinite dilution were evaluated. Substituent and solvent effects on transfer volumes of each isomer from water to DMF-H
2
O mixed solvents were obtained. The results are explained in terms of solvent structure and solute-solvent interaction.
Preparation, Characterization of Solid Solution La
4
BaCu
5-x
Mn
x
O
13+λ
(x= 0—5) and Its Catalytic Activity in the Reduction of NO by CO
LIU Yu, YANG Xiang-guang, WU Yue
1999, 15(3): 258-266.
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A series of layered mixed oxides La
4
BaCu
5-x
Mn
x
O
13+λ
( x =0—5) was prepared, characterized and used as catalysts for NO+CO reaction. It was found that all the samples were single phase having a structure with five-layered-perovskite. La
4
BaCu
2
Mn
3
O
13+λ
showed the highest activity in the title reaction, this could be attributed to the synergetic effect between Cu and Mn. The results of TPR, TPD and excess oxygen investigations confirmed that the Cu ion would be the active center. The displacement of the Cu ion by Mn caused the Cu ion to be more easily reducible and more content of excess oxygen, and it was beneficial to the activity of the catalyst. The reaction mechanism was also proposed.
Synthesis, Structure and Dielectric Property of Ba
1- x
Sr
x
Zr
y
Ti
1- y
O
3
DING Shi-wen, ZHAI Yong-qing, ZHANG Xue-jian, WANG Hong-ge, LIU Hai-yan
1999, 15(3): 267-270.
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A sieres of Ba
1- x
Sr
x
Zr
Y
Ti
1- Y
O
3
(0≤ x ≤0.4, 0< y <0.3) solid solutions was synthesized by soft chemical method below 100 ℃. The XRD and cell parameters component figures of the series of the solid solutions powder demonstrate that the compounds are mutually miscible in the solid solutions. Furthermore, the observation through a TEM showed that the product has a shape of uniform, substantially spherical particles with an average particle size of 60 nm in diameter. The result of prepared ceramics shows that after being adulterated with Sr
2+
and Zr
4+
in pure BaTiO
3
phase, the dielectric constant was increased eight times at room temperature, while the dielectric loss was decreased three times.
Ordered Charge Distribution in Superconductor Tl-Ba-Ca-Cu-O
LI Ping, XIAO Shen-xiu, WANG Rong-shun
1999, 15(3): 271-280.
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The layered charges were calculated by means of constructing the complete structure of Tl-Ba-Ca-Cu-O superconductor. The weak link between Cu-O and Ba-O, or between Cu-O and Tl-O or Ba-O or Tl-O layers is explained with the aid of the charge of limited layer unit calculated from the values of ions obtained, in addition to the possibility of forming charges fluctuation, which depends on the π coordination covalent bond on Cu-O plane and O-Tl-O structure. The possible chemical tight bonding orbitals are in accordance with those of other superconductors obtained by quantum theoretical method, which occur at Cu
3d
(x
2
-y
2
)
and O
2p
x,y
. The valence band composed of Cu 3
3d
and O
2p
orbital energy levels is obviously an energy band of conduction. The ordered charge on layers is the main reason that raises T
C
of superconductors. The difference of electronic structure of ab plane and c axis leads to the anisotropy properties.
Syntheses of Substituted Indan-1-ones and Indenes
YASIN Tariq, FAN Zhi-qiang, FENG Lin-xian
1999, 15(3): 281-285.
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The syntheses of three novel substituted indanones namely 2,7-dimethylindan-1-one, 2-methyl-4,7-diethylindan-1-one and 2,4-dimethyl-7-methoxyindan-1-one are described. These indanones were prepared by different routes involving intramolecular ring closure of aryl-substituted compounds by Friedel-Crafts reaction. The t-butyl was used as the positional protective group in the selective preparation of 2,7-dimethylindan-1-one. The corresponding indenes were prepared by reduction and dehydration reactions from these indanones.
Studies on Chemical Composition of Iron-molybdenum Cofactor from Nitrogenase by Fluorescence Analysis
ZHANG Feng-zhang, XU Liang-shu, HUANG He-qing, LONG Min-nan, QIU Xue-hui, CHEN Zhong
1999, 15(3): 286-293.
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The iron molybdenum cofactor(FeMoco) of nitrogenase MoFe-protein from Azotobacter vinelandii OP was extracted by N-methylformamide(NMF). The effects of FeMoco(in NMF) on electronic spectrum and fluorescence intensity of fluorescein dimercury acetate(FDMA)(in 1 mol/L NaOH) were investigated by fluorophotometric titrations and compared with those of (NH
4
)
2
MoS
4
and complexes of (NH
4
)
2
MoS
4
with Na
2
S or Na
2
S
2
or (NH
4
)
2
S
x
on the relative properties of FDMA. It was found that the electronic spectrum of FDMA displayed hypsochromic shift(17 nm) in the presence of FeMoco just like that in the presence of other inorganic sulfides and that the titration curve for the quench of FDMA with FeMoco is very similar to that for the quench of FDMA with complex of (NH
4
)
2
MoS
4
with Na
2
S
2
(mole ratio is 1∶3). The results showed that FeMoco(N) probably contained S—S bonds and its structure was found to be changed compared with Kim-Rees structural model. This change should profit the formation of the polymer.
Synthesis of Analogs of Anacardoside from Semecarpus Anacardium
WANG Yu-lan, CAI Meng-shen
1999, 15(3): 294-299.
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Editor-in-Chief:
Jihong YU
ISSN 1005-9040
CN 22-1183/O6
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