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Table of Content
24 April 2000, Volume 16 Issue 2
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Articles
Synthesis and Structure of a Novel Tetranuclear Erbium(Ⅲ) Complex with
L
-Proline(HPro)[Er
4
(HPro)
4
(Pro)
2
·(μ
3
-OH)
4
(H
2
O)
7
](ClO
4
)
6
·6H
2
O
ZHANG Da-shun, BU Wei-ming, YANG Wei-chun, LI Jun-ran, JIN Tian-zhu, YE Ling, FAN Yu-guo
2000, 16(2): 97-101.
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The title complex was synthesized in an aqueous solution and its crystal structure was determined by X-ray diffraction. The crystal is rhombohedral, space group R3 with a=1.9470(3) nm, b=1.9470(3) nm, c=1.7683(3) nm, α=90°, β=90°, γ=120°, V=5.805(2) nm
3
, Z=3 , the final Rvalue is 0.0512. The complex contains a novel tetranuclear cation with four Er
3+
ions connected by four μ
3
-OH ions and six bridging carboxyl groups. Each erbium ion is coordinated by three μ
3
-OH, three carboxylic oxygen atoms from three Lproline, and two or one oxygen atoms from water molecules.
Synthesis and Structure of a Novel Tetranuclear Erbium( Ⅲ) Complex with α-Alanine[Er
4
(HAla)
6
·(μ
3
-OH)
4
(H
2
O)
8
](ClO
4
)
8
·3H
2
O
ZHANG Da-shun, BU Wei-ming, YANG Wei-chun, LI Jun-ran, JIN Tian-zhu, YE Ling, FAN Yu-guo
2000, 16(2): 102-107.
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The title complex was synthesized in an aqueous solution and its crystal structure was determined by X-ray diffraction. The crystal crystallizes in a triclinic system, space group P1 with a= 1.3063(2) nm , b=1.3194(4) nm, c=1.9502(4) nm, α=90.597(14)°, β= 93.998(11)° , γ=94.093(13)°, V=3.3441(12) nm
3
, Z=2, the final Rindices are R 1= 0.0654 , wR 2=0.1262 respectively. The complex contains a novel tetranuclear cluster cation with four Er
3+
ions connected by four μ
3
-OH ions and six bridging carboxyl groups. Each erbium ion is coordinated by three μ
3
-OH, three carboxylic oxygen atoms from three α-alanine and two oxygen atoms from water molecules, forming a square-antiprismatic coordination polyhedron.
Potentiometric Determination of Chloride and Cyanide Ions in Nanoliter Samples with Capillary Indicating Electrodes
HU Xiaoya, CHEN Hong-yuan
2000, 16(2): 108-115.
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The samples of 25 nL of chloride and cyanide were determined with a kind of glass capillary indicating electrodes by potentiometry. Silver was deposited by the silver-mirror reaction on the inner surface of the glass capillary with a volume of 25 nL. The AgCl film and the AgI film were formed by the treatment of the capillary with a FeCl
3
solution and further with a KIsolution. The samples were collected automatically into the capillary by the capillary ascension. The procedure in the measurement was merely to place a reference electrode and a capillary indicating electrode vertically on a strip filter paper containing a 0.1 mol/L NaNO
3
solution. The various i.d. of the capillary electrodes were used to determine samples ranging from 25 nLto dozens of microliters. The ranges of the linear response to chloride and cyanide were 3.2×10
-4
—2.2×10
-1
mol/Land 1.0×10
-5
—1.0×10
-1
mol/Lwith an average slope of 55.2 and 52—62 mV/decade , respectively. The samples with various concentrations of chloride and cyanide were determined, and the relative standard deviations were less than 7%.
Review
Synthesis, Structure and Properties of Two Photochromic Compounds Containing A Pyrazolone-ring
TANG Xin-cun, JIA Dian-zeng, ZHANG Xiao-gang, XIA Xi, ZHOU Zhong-yuan
2000, 16(2): 116-121.
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Two photochromic compounds with the pyrazolonering as the photochromic functional structure, 2-(1'-phenyl-3'-methyl-4'-benzoformylpyrazolone-5')-thiosemicarbazone(PMBP-TSC) and 2-(1'-phenyl-3'-methyl-4'-benzoformylpyrazolone-5')-S-methylthiosemicarbazone(PMBP-MTSC), were synthesized and characterized by elemental analysis, MS, IRspectra, NMRspectra. The crystal structure of the photocolored product of PMBP-TSC was determined by single crystal XRDanalysis. The results show that the photochromic phenomenon is due to the photoisomerization from enol form to keto form. Their photochromic properties were studied by powder-UV reflectance spectra under the irradiation of 200—380 nm light. The firstorder rate constants of the photocoloring reaction were found to be 7.80×10
-3
s
-1
for compound 1A and 1.03×10
-3
s
-1
for compound 2A.
Articles
Design of Ligands for Affinity Purification of G-CSF Based on Peptide Ligands Derived from a Peptide Library
FANG Rui, ZHANG Chang-dong, WANG Li-pin, ZHOU Hui, LI Wei
2000, 16(2): 122-125.
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Combinatorial peptide libraries have become powerful tools to screen functional ligands by the principle of affinity selection. We screened in a phage peptide library to investigate potential peptide affinity ligands for the purification of human granulocyte colony-stimulation factor(hG-CSF). Peptide ligands will be promising to replace monoclonal antibodies as they have advantages of high stability, efficiency, selectivity and low price.
Studies on β
2
-Glycoprotein Ⅰ Recognizing Molecules from a Phage Peptide Library
WANG Li-ping, LI Ting-you, SUN Hui, ZHOU Hui, LI Wei
2000, 16(2): 126-130.
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Glycoprotein I(β
2
-GPI) has been identified as a cofactor in the recognition of phospholipid Ag cardiolipin (CL) by anticardiolipin Ab(aCL) purified from patients' serum with autoimmune disease. However, there is a considerable controversy as to the anti-β
2
-GPI antibodies occurred in aCL. In order to select β
2
-GPI recognizing molecules, β
2
-GPIwas used as a probe to screen affinity phage clones panned from a phage peptide library. After four cycles of selection, the phage recovery increased from 2.4×10
-5
% to 1.1×10
-3
%, indicating that a specific enrichment had been achieved. In order to characterize these phage clones, we investigated their specific binding to β
2
-GPI and their inhibition of β
2
-GPIbinding to antiβ
2
-GPIantibodies. Almost 40 percent of clones reflected considerable binding abilities and inhibitory activities towards antiβ
2
-GPIantibodies. Agroup of related peptides were identified by DNAsequencing, in which there were seven related peptide sequences, with four of them representing more than once. These peptide sequences display similarities at several positions. Sequence motif (—F—S—L—) was evident in most of the peptides. It suggests that these peptides may specifically block the anti-β
2
-GPI antibodies binding to β
2
-GPI. Our result supports the idea that β
2
-GPI acts as a Ag for these anti-β
2
-GPI antibodies occurred in the aCL.
Synthesis of Symmetrical Biaryls via Rhodium Catalyzed Dimerization of Arylmercurials and Mechanism of the Dimerization
WANG Yu-lan, WU Yang-jie
2000, 16(2): 131-135.
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Aseries of symmetrical biaryls was synthesized from arylmercuric chlorides and biarylmercurials in the presence of [ClRh(CO)
2
]
2
in hexamethylphosphoramide(HMPA). The mechanism of the [ClRh(CO)
2
]
2
catalyzed dimerization of biarylmercurials was studied, and shown to be mainly intermolecular reaction.
Ab Initio
Studies on MCH
2
(OH) and CH
3
OM(M=H, -, Li, Na)
WANG Yi-gui, SUN Chang-jun, BIAN Wen-sheng, DENG Cong-hao
2000, 16(2): 136-140.
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MCH
2
(OH) and CH
3
OM(M=-, Li, Na) were calculated by means of ab initio method at the MP
2
/6-31+G
*
level. The results show that the metals have the ability to localize charge on Oin CH
3
OM(M= Li, Na). MCH
2
(OH)(M=Li, Na) has four possible structures, among which carbonoxygenbridged structure 1 is the most stable and observable kinetically. For MCH
2
(OH)(M=Li, Na), the existence of the metal increases the rigidity of the carbon configuration. This may be the reason why MCH
2
(OR)(M=Li, Na) is widely used in stereoselective syntheses.
Kinetic Studies of Solvent and Pressure Effects on the Thermal Isomerization of Palladium Dithizonate
Yoshimi Sueishi, Kazumi Matsumoto
2000, 16(2): 141-145.
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Synthesis, Electrochemistry, and Photophysics of a Novel Binuclear Polypyridyl Ru(Ⅱ)Complex with and 1,8-Adipoylamido- bis(1,10-phenanthroline-5-yl) Ligand
WANG Peng, WANG Jun, JING Xiao-yan, WANG Xiang-ping, ZHU Guo-yi
2000, 16(2): 146-151.
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The present paper covers the syntheses of 1,8-adipoylamidobis(1,10-phenanthroline-5-yl)(bphaa) and its binuclear complex {[(bpy)
2
Ru]
2
(bphaa)}(PF
6
)
4
, where bpy is 2,2′-bipyridine. The two novel compounds were confirmed by means of elemental analysis, IR, LDMSand
1
H NMR , and
1
H NMRspectra were completely assigned in virtue of
1
H-
1
H COSY. The electrochemical behavior of the binuclear Ru(Ⅱ) complex was obtained using cyclic and square-wave voltammetry. Its photophysical property was investigated by electronic absorption, fluorescence excitation and emission spectra.
Synthesis and Structure Control of A New Kind of Inelastomer Impact Modifier with Core-shell Structure and Impact Modification to PVC/CPE
TANG Jun, LI Wen-jiang, PAN Rong, YANG Bai
2000, 16(2): 152-155.
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A new kind of inelastomer impact modifier with a core-shell structure was synthesized by employing a multi-step composite emulsion polymerization technique, the size and morphology structure of the coreshell particles could be controlled by the multistep composite emulsion polymerization technique. The study of the impact strength and the elongation at break of the PVC/CPE blend with different contents of core-shell particles(C-S) indicated that the mechanical properties of PVC/CPE/C-Scomposite were the best when the concentration of the particle was 25%(mass fraction) which showed the different regularities and characteristics of elastomer toughening plastic.
Molecular Weight and Aggregation of
Erwinia
Gum in Aqueous Solutions
ZHANG Lina, XU Xiao-juan, ZHU Rong-Ping, Iijima Hideki
2000, 16(2): 156-162.
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Erwinia(E) gum is composed of glucose, fucose, galactose and glucuronic acid. The weight-average molecular weights M
w
, number-average molecular weights M
n
and intrinsic viscosities[η] of the four fractions and the unfractionated Egum in aqueous solutions at desired temperatures were studied by light scattering, membrane osmometry, size exclusion chromatography(SEC) and viscometry. The experimental results prove that Egum formed aggregates in the aqueous solution at 25 ℃ and the aggregates were broken gradually with increasing temperature. The dissociation of the aggregates of Egum in the aqueous solution started at 36 ℃, and was completed at around 90 ℃. The [η] values of Egum and its fractions are much higher than those of the conventional polymers with the similar molecular weights, and decrease with increasing NaCl concentration.
Phase Behavior of the Ternary Solution Involving Rodlike and Random Coil Polymers
LIN Jia-ping, WU He-rong, LI Shi-jing
2000, 16(2): 163-168.
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The present paper covers the phase behavior of poly(p-benzamide)(PBA)/Nylon 6/H
2
SO
4
and poly(p-phenylene terephthalamide) (PPTA)/Nylon 6/H
2
SO
4
systems. The transition temperatures detected by the Depolarized Light Intensity measurements were used to construct the phase diagram in which the influence of temperature was shown. The enhanced depolarized light intensity observed in the ternary system suggests that the coil polymer chains may tend to be extended and contribute to the overall anisotropy of the liquid crystal phase.
Stiffening of Semirigid Polymer Chains Before the Isotropic-Aniostropic Transition
LIN Jia-ping, ZHOU Da-fei
2000, 16(2): 169-175.
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The phase behavior of a semirigid polymer manifested by the polypeptide such as poly(β-phenethyl L-aspartate)(PPLA) in a mixed solvent system containing a denaturant acid was studied. The obtained results suggest that there is a marked enhancement of the propensity for the semirigid polymer chain to adopt a rigid conformation upon increasing polymer concentration before the critical value for the incipience of a liquid crystal phase, which has been firmly confirmed both theoretically and experimentally. In consideration of the first order estimation of polymerpolymer interaction, a theoretical approach was attempted within the framework of a helixcoil transition model proposed by Rajan and Woo. According to the analysis, the semirigid chains could become rather rigid before reaching liquid crystal phase. Such a kind of chain stiffening effect was verified by
1
H NMR and
13
C NMR measurements. The experimental results show that the PPLA molecules convert gradually from the random coil to the rigid rod conformation as polymer concentration turns higher in the isotropic phase.
Letters
Crystal Structure And Magnetic Property of the Complex of Hydrogen-bonded Two-dimensional Layer Copper(Ⅱ)Acrylate with Trimethyl Phosphate
WANG Yao-yu, SHI Qian, YANG Bing-qin, GAO Yi-ci, SHI Qi-zhen
2000, 16(2): 176-178.
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)
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A New Zirconocene Complex and Its Catalytic Properties for Olefin Polymerization
ZHANG Fan, MU Ying, BU Wei-ming, ZHAO Li-gang, CHEN Cong-xi, ZHAI Hui-min, YANG Guang-di
2000, 16(2): 179-181.
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Research Notes
Novel Syntheses of Aryl and Benzyl Selenides Promted by Metallic Zinc in Aqueous Media
WU Jian-yi, LU Gen-liang, MA Zhi-xian, CHEN Jian
2000, 16(2): 182-184.
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WO
3
/ZrO
2
Strong Acid as a Catalyst for the Decomposition of Chlorofluorocarbon (CFC-12)
HUA Wei-ming, ZHANG Feng, MA Zhen, TANG Yi, GAO Zi
2000, 16(2): 185-187.
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)
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Direct Vapor Phase Carbonylation of Methanol over NiCl
2
/C Catalyst
PENG Feng
2000, 16(2): 188-190.
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)
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Editor-in-Chief:
Jihong YU
ISSN 1005-9040
CN 22-1183/O6
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