bluuebunny/crossref_metadata_2025 huggingface dataset:
ChemInform Abstract: Axial [6,6′‐(2,4‐Pentadioxy)]‐1,1′‐biphenyl‐2,2′‐diamine (PD‐BIPHAM): Practical Synthesis and Applications in Asymmetric Hydrogenation.
Authors: Wang Chun‐Jiang , Xu Zhong‐Ping , Wang Xiang , Teng Huai‐Long
Published: September 2010

The application of the title compound as new ligand in the Rh(I)‐catalyzed asymmetric hydrogenation of α‐dehydroamino acid esters results in complete conversion and excellent enantioselectivities of ring substituted phenylalanine derivatives (II) and alanine ester (IV).
ChemInform Abstract: An Efficient Iron‐Catalyzed Carbon—Carbon Single‐Bond Cleavage via Retro‐Claisen Condensation: A Mild and Convenient Approach to Synthesize a Variety of Esters or Ketones.
Authors: Biswas Srijit , Maiti Sukhendu , Jana Umasish
Published: September 2010

An efficient, mild, and inexpensive iron(III) mediated C—C bond cleavage reaction for the synthesis of esters or ketones under solvent‐free conditions is reported.
ChemInform Abstract: Direct Method for Carbon—Carbon Bond Formation: The Functional Group Tolerant Cobalt‐Catalyzed Alkylation of Aryl Halides.
Authors: Amatore Muriel , Gosmini Corinne
Published: September 2010

Direct alkylation of electron‐poor aryl bromides and chlorides with alkyl bromides is smoothly achieved using a Co(II)—phosphane catalyst.
ChemInform Abstract: Effect of Phase Transfer Chemistry, Segmented Fluid Flow, and Sonication on the Synthesis of Cinnamic Esters.
Authors: Riccaboni Mauro , La Porta Elena , Martorana Andrea , Attanasio Roberta
Published: September 2010

Wittig reactions under phase‐transfer conditions are performed without the use of a phase‐transfer catalyst.
ChemInform Abstract: Sequential Reaction of Arynes via Insertion into the π‐Bond of Amides and Trapping Reaction with Dialkylzincs.
Authors: Yoshioka Eito , Kohtani Shigeru , Miyabe Hideto
Published: September 2010

The formal [2+2] cycloaddition adducts [cf.
ChemInform Abstract: Remarkably Mild and Efficient Cetrimonium Bromide Catalyzed Friedel—Crafts Amidoalkylation of Sesamols with N‐Boc Imines Generated in situ in Aqueous Medium.
Authors: Zhang Hui , Chen Ming‐Gui , Lian Chun‐Xia , Yuan Wei‐Cheng , Zhang Xiao‐Mei
Published: September 2010

The regioselective process is successfully applied to sesamol (I) and its derivatives (VI).
ChemInform Abstract: Cationic Pd(II)‐Catalyzed Fujiwara—Moritani Reactions at Room Temperature in Water.
Authors: Nishikata Takashi , Lipshutz Bruce H.
Published: September 2010

The ortho‐directed C—H activation reaction of a variety of anilides with acrylate esters affords electron‐rich cinnamates in good yields.
ChemInform Abstract: Stereoselective Chlorination of New Type Baylis—Hillman Adducts by Bis(trichloromethyl)carbonate with the Aid of Catalytic Amount of Triphenylphosphine Oxide.
Authors: Zhong Weihui , Hong Lingjuan , Zheng Yemin
Published: September 2010

The new method for the preparation of allyl chlorides is a convenient operational procedure yielding the products with high stereoselectivity.
ChemInform Abstract: Palladium‐Catalyzed Reductive Homocoupling of Aromatic Halides and Oxidation of Alcohols.
Authors: Zeng Minfeng , Du Yijun , Shao Linjun , Qi Chenze , Zhang Xian‐Man
Published: September 2010

Treatment of phenyl iodide and bromide as well as iodopyridine and bromopyridine with 3‐pentanol, CsF, and PdCl2(dppf) is found to result in the formation of biaryls.
ChemInform Abstract: Highly Recyclable Chemo‐/Biocatalyzed Cascade Reactions with Ionic Liquids: One‐Pot Synthesis of Chiral Biaryl Alcohols.
Authors: Gauchot Vincent , Kroutil Wolfgang , Schmitzer Andreea R.
Published: September 2010

The following is crucial for the success of the one‐pot preparation of the cascade sequence, leading to the biaryl alcohols: use of 1 equiv.
ChemInform Abstract: Chiral Phosphoric Acid Catalyzed Diastereo‐ and Enantioselective 1,4‐Conjugate Addition of β‐Ketoesters to Nitroolefins.
Authors: Zhang Hui , Cun Lin‐Feng , Zhang Xiao‐Mei , Yuan Wei‐Cheng
Published: September 2010

The corresponding adducts (III) are obtained in high yields and with moderate diastereoselectivities and enantioselectivities.
ChemInform Abstract: Tandem 1,5‐Hydride Shift/1,5‐S,N‐Cyclization with Ethylene Extrusion of 1,3‐Oxathiolane‐Substituted Ketenimines and Carbodiimines. An Experimental and Computational Study.
Authors: Alajarin Mateo , Bonillo Baltasar , Sanchez‐Andrada Pilar , Vidal Angel
Published: September 2010

Upon heating ketenimines of type (III) and carbodiimines derived from isocyanates (VIII) undergo unexpected transformation into benzisothiazolones via 1,5‐hydride shift, 1,5‐electrocyclization, and [3 + 2] cycloreversion.
ChemInform Abstract: Enantioselective Aza‐Diels—Alder Reaction of Brassard′s Diene with Aldimines Catalyzed by Chiral N,N′‐Dioxide—Yb(OTf)3 Complex.
Authors: Chen Zhenling , Lin Lili , Chen Donghui , Li Jiangting , Liu Xiaohua , Feng Xiaoming
Published: September 2010

The reaction is optimized with respect to the catalyst and used for the synthesis of α,β‐unsaturated δ‐lactams as precursors of highly functionalized piperidines.
ChemInform Abstract: Synthesis and Biological Activity of the Calcium Modulator (R) and (S)‐3‐Methyl 5‐Pentyl 2,6‐Dimethyl‐4‐(3‐nitrophenyl)‐1,4‐dihydropyridine‐3,5‐dicarboxylate.
Authors: Zhang Bang‐le , He Wei , Shi Xin , Huan Meng‐lei , Huang Qiu‐ju , Zhou Si‐yuan
Published: September 2010

Title compounds (VI) are synthesized in high optical purities via resolution of the racemic dihydropyridine (IV) using commercially available Cinchona alkaloids as resolving agents.
ChemInform Abstract: Rhodium‐Catalyzed Oxidative Coupling/Cyclization of 2‐Phenylindoles with Alkynes via C—H and N—H Bond Cleavages with Air as the Oxidant.
Authors: Morimoto Keisuke , Hirano Koji , Satoh Tetsuya , Miura Masahiro
Published: September 2010

Dialkylacetylenes (X) react in an unexpected way: the required coupling product is only produced in a minor amount.
ChemInform Abstract: An Efficient Synthesis of 3,4‐Dihydropyrimidin‐2(1H)‐ones Catalyzed by Thiamine Hydrochloride in Water under Ultrasound Irradiation.
Authors: Mandhane Priyanka G. , Joshi Ratnadeep S. , Nagargoje Deepak R. , Gill Charansingh H.
Published: September 2010

The alternative procedure is of interest from an environmental and economic viewpoint.
ChemInform Abstract: Molecular Iodine Mediated One‐Step Synthesis of 3‐Substituted‐6‐(6‐substituted‐2‐oxochromen‐3‐yl)‐7H[1,2,4]triazolo [3,4‐b][1,3,4]thiadiazines.
Authors: Jakhar Anshu , Makrandi Jagdish K.
Published: September 2010

The iodine‐catalyzed condensation between 3‐acetyl‐coumarin and 4‐amino‐5‐mercapto‐1,2,4‐triazoles occurs in a single step and avoids the use of lachrymatory molecular bromine used in previously reported procedures.
ChemInform Abstract: Copper‐Catalyzed Diboration of Ketones: Facile Synthesis of Tertiary α‐Hydroxyboronate Esters.
Authors: McIntosh Melissa L. , Moore Cameron M. , Clark Timothy B.
Published: September 2010

The in‐situ generation of the (ICy)CuOtBu catalyst from (ICy)CuCl and NaOtBu provides convenient reaction conditions to achieve the high catalyst efficiency.
ChemInform Abstract: Vinylogous Aldol Products from Chiral Crotylsilanes Obtained by Enantioselective Rh(II) and Cu(I) Carbenoid Si—H Insertion.
Authors: Wu Jie , Chen Yu , Panek James S.
Published: September 2010

Chiral homoallylic ethers, bearing a α,β‐unsaturated ester or silyl ether moiety, are prepared with moderate to high syn‐selectivity via the crotylation reaction of chiral silanes, aldehydes and trimethylalkoxysilanes.
ChemInform Abstract: Chemoselective Protection of α‐Ketoacids by Direct Annulations with Oximes.
Authors: Flores Melissa A. , Bode Jeffrey W.
Published: September 2010

Cyclic nitrones, generated in the reaction of oximes with α‐ketoacids, serve as stable masked α‐ketoacids.
ChemInform Abstract: Enantioselective Synthesis of β‐Trifluoromethyl α‐Amino Acids.
Authors: Benhaim Cyril , Bouchard Luc , Pelletier Guillaume , Sellstedt John , Kristofova Livia , Daigneault Sylvain
Published: September 2010

The structure of the chiral catalysts is essential for the enantioselective hydrogenation of either (Z)‐alkyl or (Z)‐aryl trifluoroamidoenoates.
ChemInform Abstract: Recyclable Indium(III) Chloride Catalyzed Site‐Selective Double Substitution in One‐Pot for the Synthesis of Isatin N‐Ribonucleosides under Microwave Irradiation.
Authors: Siddiqui Ibadur R. , Singh Archana , Shamim Shayna , Srivastava Vishal , Singh Pravin K. , Yadav Sanjay , Singh Rana K. P.
Published: September 2010

The method affords the target compounds (III), which are of interest as antiviral nucleoside analogues, in a short time with good to excellent yield.
ChemInform Abstract: Magnetic Pyrochlore Oxides
Authors: Gardner Jason S. , Gingras Michel J. P. , Greedan John E.
Published: September 2010

Review: 356 refs.
ChemInform Abstract: Coordination Supramolecular Structures
Authors: Alekseev Yu. E. , Garnovskii A. D.
Published: September 2010

Review: 106 refs.
ChemInform Abstract: Catalytic Oxidation with Hydrogen Peroxide in Ionic Liquids
Authors: Gharnati Loubna , Doering Manfred , Arnold Ulrich
Published: September 2010

Review: 82 refs.
ChemInform Abstract: Cinchona Alkaloids in Chemistry
Authors: Song Choong Eui
Published: September 2010

Review: 44 refs.
ChemInform Abstract: Macrocycles and Cavitands Containing Phosphorus
Authors: Simulescu Vasile , Ilia Gheorghe
Published: September 2010

Review: 84 refs.
ChemInform Abstract: Synthesis and Biological Activity of Fluorinated Vitamin D
Authors: Fujishima Toshie , Fujii Sinya , Harayama Takashi
Published: September 2010

Review: 67 refs.
ChemInform Abstract: Recent Advances in Catalytic Enantioselective Fluorination of Active Methines
Authors: Kang Young Ku , Kim Dae Young
Published: September 2010

Review: 67 refs.
ChemInform Abstract: Novel Anodic Concepts for the Selective Phenol Coupling Reaction
Authors: Waldvogel Siegfried R.
Published: September 2010

Review: 66 refs.
ChemInform Abstract: Boryl Anion: Syntheses and Properties of Novel Borylmetals
Authors: Yamashita Makoto , Nozaki Kyoko
Published: September 2010

Review: ca. 100 refs.
ChemInform Abstract: Native Chemical Ligation with Nα‐Acyl Transfer Auxiliaries
Authors: Offer John
Published: September 2010

Review: 76 refs.
ChemInform Abstract: Solid State Metathesis Reactions as a Conceptual Tool in the Synthesis of New Materials
Authors: Meyer H.‐Juergen
Published: September 2010

Review: 93 refs.
ChemInform Abstract: Aiming for the Ideal Synthesis
Authors: Gaich Tanja , Baran Phil S.
Published: September 2010

Review: ca. 150 refs.
One‐Dimensional Modeling and Simulation of Bubble Column Reactors
Authors: Jung S. , Becker M. , Agar D. W. , Franke R.
Published: September 2010

Für eine praktische Auslegung von Blasensäulen im (halb)technischen Maßstab existieren in der Fachliteratur bisher nur wenige Reaktormodelle. Durch Implementierung eines eindimensionalen Modells in die gleichungsorientierte Simulationssoftware ASPEN Custom ModelerTM wird ein Kompromiss aus Modellgenauigkeit und Berechnungsaufwand erreicht. Die Vorgänge in einem Blasensäulenreaktor werden mit hinreichender Genauigkeit quantitativ beschrieben.
Sustainability of Solid Waste Recycling Processes – Case Study: Scrap Tire Recycling
Authors: Pehlken A. , Thoben K.‐D.
Published: September 2010

Rohstoffsicherung gehört zu den Schwerpunktthemen der Europäischen Kommission. Durch sinnvoll eingesetztes Recycling können Ressourcen aus Abfallstoffen nicht nur langfristig genutzt werden sondern auch Primärrohstoffe substituieren und damit einen Betrag zum nachhaltigen Ressourcenmanagement leisten. Die Thematik wird am Beispiel des Altreifenrecyclings und der daraus entstehenden Materialströme behandelt.
Photoaddition of chloroform to ketones via a singlet exciplex: A photo‐CIDNP study
Authors: Zhang Mao‐Xi , Yang Li , Liu Zhong‐Li , Liu You‐Cheng
Published: September 2010

Photolysis of 4‐acetyl‐4‐ethoxyformylcyclohexanone, 4‐acetyl‐4‐phenylcyclohexanone and 1‐acetyl‐1‐phenylcyclohexane in deuteriochloroform using a high pressure Hg—Xe lamp showed unusual polarizations. The results are explained by the formation of a singlet exciplex of the ketone with deuteriochloroform and the photoaddition of deuteriochloroform to the ketone.
Studies on sulfinatodehalogenation XIX. The reaction of perfluoroalkyl iodides and perfluoroalkanesulfonyl bromides with conjugated dienes
Authors: Huang Wei‐Yuan , Zhang Han‐Zhong
Published: September 2010

Perfluoroalkyl iodides reacted with conjugated dienes in aqueous acetonitrile solution in the presence of sodium dithionite at room temperature to give dimerization products, whereas, perfluoroalkanesulfonyl bromides reacted with conjugated dienes to form 1,4‐adducts under actinic irradiation.
The synthesis of polyfluoroalkoxylbenzaldehydes
Authors: Huang Wei‐Yuan , Ma Wu‐Ping
Published: September 2010

Several polyfluoroalkoxyl benzaldehydes were synthesized from the nucleophilic reaction between polyfluoroalkanesulfonate and various sodium phenolates with cetyltrimethylammonium bromide or tetrabutylammonium bromide as PTC. The yields were in the range of 55%–70%. Using a modified procedure Cl(CF2)2SO2Cl was prepared from ClCF2CF2I with an improved yield of 91% and was used to synthesize the polyfluoroalkanesulfonate 2'.
The pentacyclic steroidal constituents of Tacca plantaginea: taccalonolide E and F
Authors: Shen Ji‐Hui , Chen Zhong‐Liang , Gao Yi‐Sheng
Published: September 2010

Two pentacyclic steroidal bitter principles, taccalonolide E and F, have been isolated from Tacca Plantaginea. Their structures were elucidated by spectroscopic methods.
Electronic structure and catalytic behavior of tungsten carbides
Authors: Qin Dai‐Yi , Fan Kang‐Nian , Gao Zi
Published: September 2010

The electronic structure of tungsten carbide was investigated by EHMO semiempirical method. The most stable structure of the carbide was predicted on the basis of binding energy calculations. The W‐C bonding is covalent in nature with some charge transfer from the W to the C atoms. The increase in the occupancy of the d shell of the W atoms and the position of the Fermi level may account for the platinum‐like catalytic behavior of tungsten carbide.
Time‐resolved studies of state‐to‐state vibrational energy transfer: I2(B3IIou+:v′ = 19) + He
Authors: Xiang Tian‐Xiang , Sun Sheng , Gong Shun‐Sheng , Wang Jia‐Min
Published: September 2010

This paper presents an experimental procedure to study state‐to‐state collisional dynamics by using tunable and pulsed laser techniques and time‐resolved and dispersed fluorescence methods. For the first time, the decay processes of electronically excited iodine, B3IIou+ (v′ = 19), to the adjacent vibrational states in collisions with He molecules have been directly observed in real time. The rate constants for the state‐to‐state vibrational energy transfer obtained are, k,vHe(19→18) = (2.76±0.05)x10−11cm3s−1 molecule−1 and kvHe(19→20) = (1.65±0.04) × 10−11 cm3s−1 molecule−1. These results are in satisfactory agreement with the detailed balance principle.
A new ent‐atis‐16‐ene type diterpenol from Euphorbia sieboldiana
Authors: Ding Yi‐Li , Jia Zhong‐Jian , Wang Qi‐Guang , Chen Ji‐Hong , Liu Yu‐Ting
Published: September 2010

From the acetone extract of the root of Euphorbia sieboldiana, a new ent‐atis‐16‐ene type diterpenol was isolated and its structure was demonstrated as ent‐atis‐16‐ene‐13 α‐hydroxy‐3,14‐dione (1) based on the chemical as well as NMR and MS spectroscopic evidences, and finally confirmed by X‐ray diffraction.
Studies on the chemical constituents of the South China Sea sponge Phacellia fusca
Authors: Zeng Long‐Mei , Fu Xiong , Su Jing‐Yu , De Guzman Florecita , Schmitz J. Francis , Hossain M. Bilayet , van Der Helm Dick
Published: September 2010

Three pyrrololactam alkaloids have been isolated from the marine sponge Phacellia fusca Schmidt collected from the South China Sea, and their structures were determined as 1–3, on the grounds of spectral data. This is the first report of these compounds from this sponge. The structure of 1 was confirmed by X‐ray analysis.
The spin delocalization substituent parameter σ 6. The spin‐delocalizing abilities of the thiomethyl, cyclopropyl and t‐butyl groups. Synthesis of three substituted trifluorostyrenes
Authors: Jiang Xi‐Kui , Ji Guo‐Zhen , Shi Yi‐Qun
Published: September 2010

Three substituted α, β, β‐trifluorostyrenes (TFS's), i. e., p‐thiomethyltrifluorostyrene (4), p‐cyclopropyltrifluorostyrene (5) and p‐t‐butyltrifluorostyrene (6), have been synthesized. The rate constants (k2) of the thermal cyclodimerization of these compounds have been measured in the temperature range 120–160°C. The polar parameters σmb of these TFS's calculated from 19F NMR chemical shifts are: for p‐thiomethyl, ‐0.18; p‐cyclopropyl, ‐0.31 and p‐t‐butyl, ‐0.22. The spin delocalization substituent parameters σ′T (140°) of p‐thiomethyl, cyclopropyl and t‐butyl groups are 0.59, 0.27 and 0.30 respectively. Thus all of these groups act as electron‐donating groups which can also effectively stabilize a spin.
A new method for the preparation of hydroperfluoroalkane from perfluoroalkyl chloride
Authors: Chen Qing‐Yun , Wu Jian‐Ping
Published: September 2010

Perfluoroalkyl chloride can be converted into hydroperfluoroalkane with zinc powder in the presence of nickel dichloride. A single electron transfer mechanism is proposed.
A simple and effective method for fluoroalkylation — the addition of fluoroalkyl iodide to olefins in the presence of hydrogen peroxide
Authors: Chen Qing‐Yun , Chen Ming‐Fang
Published: September 2010

Addition of fluoroalkyl iodides to olefins in the presence of hydrogen peroxide (H2O2) in acetone, acetonitrile or ethanol gave the corresponding 1:1 adducts in good yields. Reaction of fluoroalkyl iodide with diallyl ether (DAE) yielded tetrahydrofuran derivatives. p‐Hydroquinone (p‐HQ) can partly suppress the reaction. A radical initiation mechanism is proposed.
13C NMR and structural study of solid state naphthol‐1 and naphthol‐2 arylazo‐derivatives
Authors: Fedorov L.A. , Rebrov A.I. , Hu Jian‐Zhi , Shen Lian‐Fang
Published: September 2010

Solid state 13C NMR spectra of a series of naphthol‐1 and naphthol‐2‐arylazo‐derivatives were studied and compared with respective results in solutions. Signals of carbon nuclei of naphthalene ring were assigned. Tautomeric forms of compounds were determined. It was shown that 4‐(p‐NO2C6H4)‐azonaphthol‐1 and 1‐(p‐NO2C6H4)‐azonaphthol‐2 in solid state existed exclusively in quinohydrazone form. The other two compounds—1‐(C6F5)‐azonaphthol‐2 and 2‐(p‐CH2C6H4)‐azonaphthol‐1 in solid state were not found in the form of individual tautomeric mixtures but in respective tautomeric equilibrium form. Thus, during transition from liquid to solid state, the tautomeric equilibrium was practically unchanged. In solid state it was found that rotation around aryl‐N bond was hindered in the time scale of NMR spectroscopy.
Synthesis and photochromism of 3‐indylfulgides
Authors: Li Yun‐Zheng , Wang Huan‐Zhong , Zhu He‐Sun , Wang Fan
Published: September 2010

Six fulgides of indole series are prepared. Three of them are photochromic. The others in which R1 is hydrogen atom do not show photochromism. Only Z‐E isomerizations occur on irradiation at 365 nm. The effects of molecular structural modifications on photochromic properties are also discussed.
Carbonium cyclization—studies on lignans containing the dibenzocyclooctadiene system, II
Authors: Tan Rui , Liang Xiao‐Tian
Published: September 2010

Studies of schisandrol B under Ritter reaction conditions showed similar results to that of schisandrin. However the carbonium cyclization product (4a) of schisandrol B undergoes oxidative ring opening when exposed to the air. Cyclization of schisantherin A (2) also occurs by treatment with thionyl chloride in pyridine. Here the presence of the extra benzoyloxy group somehow confers stability to the diosphenol system and 8 has to be stirred in solution under oxygen for extended periods to effect ring opening.
Studies of tris[(phenyldimethylsilyl)methylene]‐tin carboxylates
Authors: Xie Qing‐Lan , Li Jing , Yang Zhl‐Qiang , Zhang Dian‐Kun , Wang Ji‐Tao
Published: September 2010

Twenty‐six derivatives of tris[(phenyldimethylsilyl)methylene]tin carboxylates have been prepared. All compounds are new and characterized through elemental analysis IR spectra, and 1H, 13C, 110Sn NMR spectral studies. The spectral results showed that all compounds are four coordinated organotin compounds. The Δv (=υ−υ) of them are over 300 cm−1. The chemical shifts (δ) of 119Sn of ArCO2Sn(CH2SiMe2Ph)3 and ArOCH2CO2Sn(CH2SiMe2Ph)3 give good straight‐line correlation with para‐substituent constants. These compounds have good acaricide activity, but their action on the mite are slower than that of Torque.
Condensation of α‐ and β‐acetylnaphthalene with dimethy1 β,β‐dimethyl glutarate
Authors: El‐Bassiouny Fakhry Abdel‐Aziz
Published: September 2010

α‐ and β‐Acetylnaphthalenes condensed with dimethyl β,β‐dimethyl glutarate in the presence of sodium hydride to give the corresponding half‐esters, the E‐isomers 2a and 2b being predominant. The structure and configuration of the half‐esters were characterized by chemical and spectroscopic means.
Ab initio study of lithochlorosilylenoid H2SiLiCl
Authors: Feng Sheng‐Yu , Ju Guan‐Zhi , Deng Cong‐Hao
Published: September 2010

The structures of lithochlorosilylenoid H2SiLiCl have been studied by RHF/STO‐3G gradient method. Four equilibrium states and three isomerization transition states are located. The calculation shows that the structure with three‐membered ring is the most stable one and the stability of the equilibrium structures is in the order of three‐membered ring >p‐complex>σ‐complex>tetrahedron. The dipole moments, Mülliken populations, frontier molecular orbitals and peculiarities of various structures are also given and analyzed.
Copper(II)‐lanthanoid(III)‐copper(II) trinuclear complexes with N,N′‐bis(2‐aminopropyl)‐oxamido ligand
Authors: Liao Dai‐Zheng , Li Li‐Cun , Wang Geng‐Lin
Published: September 2010

Six novel μ‐oxamido trinuclear complexes, namely Cu2(oxap)2Ln(ClO4)3 (Ln: La, Pr, Nd, Gd, Yb, Ho), where oxap is N,N′‐bis(2‐aminopropyl)oxamido, have been synthesized. The complex Cu2(oxap)2Gd(ClO4)3 was characterized with variable temperature magnetic susceptibility (4—300 K). The exchange integrals J (Cu—Gd) and J′ (Cu–Cu) were found to be 0.83 cm−1 and −1.62 cm−1, indicating that very weakly ferromagnetic spin‐exchange interaction operates between Cu(II) and Gd (III) ions.
Synthetic and structural chemistry of hexacobalt cluster compounds II. Preparation and structure of Co6(μ‐S)8 (Ph2PCH2P(O)Ph2)6
Authors: Hong Mao‐Chun , Huang Zhi‐Ying , Lei Xin‐Jian , Kang Bei‐Sheng , Jiang Fei‐Long , Liu Han‐Qin
Published: September 2010

Co4(μ3‐S)8(Ph2PCH2sP(O)Ph2)6, MW = 3012.5, space group R3, has the hexagonal parameters, a = 26.764 (10), c = 16.979 (10) Å, V = 10532.8 Å3, Z = 3. Mo Ka radiation, λ = 0.71069 Å, Dc = 1.425 g/cm3, μ = 9.94 cm−3, F(000) = 4650, R = 0.073 and Rw = 0.077 for 1965 observed unique reflections with I > 3σ (I). The molecular structure consists of a distorted octahedral Co4—core. The Co—Co and Co—S distances fall in the range of 2.805—2.838 and 2.213—2.253 Å, respectively.
Computer‐assisted retention prediction system in reversed‐phase HPLC for O‐ethyl O‐aryl N‐isopropyl phosphoramidothioates
Authors: Wang Qin‐Sun , Gao Ru‐Yu , Yang Hua‐Zheng , Yan Bing‐Wen
Published: September 2010

A computer‐assisted retention prediction system (RPS) of fifteen O‐ethyl O‐aryl N‐isopropyl phosphoramidothioates (1) in reversed‐phase HPLC was investigated. The system is based on the use of four physicochemical parameters (hydrophobicity II, electric effect σ, field effect F and steric effect Es) which is closely related to the retention mechanism in reversed‐phase HPLC. The system was evaluated by comparing the measured retention data with the predicted ones. The predicted values were consistent with the measured values within a relative error of 11.5%.
Crystal and molecular structure of main adduct of benzaldoxime dehydrodimer and styrene
Authors: Hu Hong‐Wen , Wei Xu‐Dong , Li Cun , Sun Hong‐Zhe , Yao Yi‐Ming , Zhou Zhong‐Yuan , Yu Kai‐Bei
Published: September 2010

Three 1:1 adducts have been obtained by heating benzaldoxime dehydrodimer with styrene. The main product possesses the structure of bis‐nitrone type. A radical addition mechanism is proposed.
Synthesis of substituted pyrazolo [1,5 — a] pyrimidines
Authors: Deeb A. , El‐Mobayed M. , Essawy A. , El‐Hamid Abd A. , Abd El‐Hamid M. Atef
Published: September 2010

Condensation of 3‐amino‐4‐cyanopyrazole (1) with ethylacetoacetate, ethyl cyanoacetate, diethyl malonate and acetylacetone afforded pyrazolo[1,5‐a]pyrimidine derivatives (2—8a). Other compounds (8b—h) of this ring system were obtained by treatment of 1 with arylidenemalononitrile and ethylarylidenecyanoacetate. And the reaction of compound (1) with activated acetylenes yeilded pyrazolo[1,5‐a]pyrimidine derivatives (11a—b).
A potentiometric determination of the dissociation constants of glycine in {14.926 mass% urea + water} mixed solvent at 278.15 to 318.15 K
Authors: Yuan Chang‐Bo , Yang Jia‐Zhen
Published: September 2010

First and second thermodynamic dissociation constants of glycine at five temperatures from 278.15K to 318.15K in {14.926 mass% urea + water} mixed solvent have been determined from precise emf measurements of hydrogen‐silver chloride electrodes in two cells, (A) and (B), without liquid junction, by the new method of polynomial approximation proposed on the basis of Pitzer's electrolytic solution theory in our previous papers, as compared with traditional extrapolation on the basis of the extended Debye‐Hückel equation. The results obtained from both methods are in agreement within experimental error. The thermodynamic quantities ΔG°, ΔH°, ΔS° and ΔCp° were derived from the dependence of pK° values on temperature, and pK1 = 367.60 (K / T) − 0.3973 + 3.108 × 10−2 (T / K), whereas pK2, = 2028.77 (K / T) + 2.8791 – 2.110 × 10−3 (T / K). The results have been discussed in terms of the solute‐solvent interaction and have been compared with those results in water and in other mixed solvents.
Heterobimetallic complexes CpNiCo(CO)2(PPh3)(PhC2C6H4‐R ‐p): their synthesis, electrochemistry and ESR
Authors: Sun Shou‐Heng , Meng Qing‐Jin , Zhu Hui‐Zhen , Yao Yi‐Ming , You Xiao‐Zeng
Published: September 2010

Three new heterobimetallic acetylene complexes CpNiCo (CO)3 (PPh3) (PhC2C4H4‐R‐p) [R = H (2), Br (3), COCH2 (4)] have been synthesized in suitable yield (31–47%) via the reaction of (PhC2C3H4‐R‐p)CO2(CO)5 PPh2 with nickelcene in n‐octane. The complex CpNiCo(CO)3 (Ph2C3) (1) has also been obtained in 12% by the reaction of (Ph2C2) Co2 (CO)4 with nickelcene. The complexes have been characterized by elemental analysis, IR and 1H NMR. Electrochemical study of redox couples of these complexes was presented by using cyclic voltammetry on Pt electrodes in acetone. At room temperature, all complexes underwent electrochemically reversible or guasi‐reversible oneelectron oxidation or reduction to the stable radicals. The radical anions of the complexes could be easily detected by ESR method in situ electrolysis in the THF solution. The isotropic parameters, CO=2.20mT,  = 2.052 for the radical anion of complex 1, CO= 2.20 mT, P = 1.42 mT, =2.057 for the radical anion of complex 2, might indicate that NiCoC2 framework is a delocalized unit and the ligand obitals in the complex have more contribution to the LUMO of the complex.
1,6‐Asymmetric induction: A higher enantioselective synthesis of γ‐butyrolactone
Authors: Ding Yu , Li Ja‐Yao , Wang Lai‐Xi
Published: September 2010

A novel 1,6‐asymmetric induction has been observed in the iodolactonization of γ, delta;‐unsaturated amides. The optically active γ‐butyrolactone was synthesized by employing iodolactonization reaction as a key step.
Hydrogenation of CO over carbides of tungsten
Authors: Qin Dai‐Yi , Gao Zi , Qiu Yue‐Ming , Dong Shu‐Zhong
Published: September 2010

CO hydrogenation on tungsten carbides has been investigated. The methanation activities of tungsten carbides are comparable to that of supported Group VIII metal catalysts. Temperature‐programmed thermal desorption spectra of CO on tungsten carbide show that CO is adsorbed non‐dissociatively, and the surface‐CO bond appears to be rather weak.
NMR double resonance study of azide binding to cytochrome c
Authors: Tang Wen‐Xia , Concar D. , Moore G. R. , Williams R. J. P.
Published: September 2010

Equilibrium constants for the binding of azide to ferri‐cytochrome c at temperature range‐of 305–325 K were determined at pH =7 by using 1H double resonance method. Thermodynamic values (ΔH° =‐34.5 kJ/mol, ΔS°=‐100 J/mol) were obtained from van't Hoff's relation and were compared with those for azide binding to other ferric hemeproteins. The reason of lower affinity of cytochrome c for azide was discussed.
Triplet rearrangement of 1‐biphenylyl‐2,2‐dimethylcyclopropane
Authors: Wu Guo‐Sheng , Hu Jun , Li Jiang‐Pin , Xu Jian‐Hua
Published: September 2010

Direct and sensitized photolyses of 1‐biphenylyl‐2,2‐dimethylcyclopropane gave 2‐methyl‐4‐biphenylyl‐1‐butene as sole product. Comparison of the product formation quantum yields at zero conversion in direct and sensitized photolyses (1.7 × 10−3 vs. 1.8 × 10−3) indicated that the rearrangement took place from the triplet excited state in both cases. A stepwise mechanism involving disrotatory ring opening of the cyclopropane and subsequent 1,3‐H suprafacial shift is proposed and is consistent with the reaction multiplicity result, the orbital and state correlation diagram analyses as well as the prediction based on the Large K and Small K Concept.
Calculations of heat of solvation by a simple electrostatic approach to molecular interactions
Authors: Cachau R. E. , Villar H. O. , Castro E. A.
Published: September 2010

An extremely simple formula to estimate the heat of formation of complexes between an ion and a polar molecule or between highly polar systems is presented. The formula is entirely electrostatic and the expression used is verified by means of perturbation theory. This formula is tested for several ion‐molecule and molecule‐molecule pairs. It is also applied to estimate the heat of hydration of simple salts.
Optimization of two‐factor (pH and ion concentration) simultaneous selection in HPLC using a statistical method
Authors: Wang Qin‐Sun , Gao Ru‐Yu , Yan Bing‐Wen
Published: September 2010

A computer‐assisted method is presented for simultaneous optimization of pH and ion concentration selection for the optimal separation in reversed‐phase HPLC. The method is based on a polynomial estimation from nine preliminary experiments according to two‐factor rectangular design. This is followed by a two‐dimension computer scanning technique. Resolution is used as the selection criterion. Good agreement was obtained between predicted data and experimental results.
A study on the mechanism of reaction between BNAH and chloranil: Evidence for electron transfer
Authors: Gao Zhong‐Li , Zhang Min‐Bao , Liu You‐Cheng
Published: September 2010

The reaction between chloranil and N−benzyldihydronicotinamide (BNAH) in borate buffer/DMF was investigated. The reaction mixture gave a strong esr signal, which is consistent with that of chloranil anion radical, and tetrachlorohydrophenol (QH2) and N−benzylnicotinamide (BNA+) were obtained as the sole products. When the reaction was run in benzene solution, a green coloured charge‐transfer complex between the reactants could be isolated, which decomposed in polar solvents to give BNA+ and QH2. Based on kinetic studies by esr spectroscopy by the stopped‐flow technique, a two‐step electron‐transfer mechanism for the reaction is proposed in contrast to the hydride‐transfer mechanism reported in the literature.
Two new diterpenoids from the marine soft coral Clavularia viridis
Authors: Su Jing‐Yu , Zhong Yong‐Li , Zeng Long‐Mei
Published: September 2010

Two new dolabellane diterpenoids named clavudiol B(2) and clavirolide F(5), have been isolated from the soft coral Clavularia viridis, collected from Xisha Islands in the South China Sea. Their structures have been determined as 2 and 5 by spectral analysis and chemical reactions.
Studies on organophosphorus compounds 52. Structure‐reactivity studies of organophosphorus compounds by MNDO calculations
Authors: Li Shu‐Sen , Yuan Cheng‐Ye
Published: September 2010

MNDO and MM2 (85) methods were used to study the conformation and the structure‐reactivity relationship of neutral and acidic phosphorus esters. The calculation results indicate that for the most stable conformation, the charge density of phosphoryl oxygen (qo) is determined not only by the electronegativity of the substituents, but also by the conformation of the alkoxyl groups on the phosphorus atom. Meanwhile, the conformation of the alkoxyl group provides, as a rule, more important influence on the charge density of the phosphoryl oxygen. However, the energy of the highest occupied molecular orbital (EHOMO) is basically dependent on the eletronegativity of the substituents, while the donating ability or the withdrawing ability of the neutral phosphorus compounds is mainly governed by the EHOMO but not the qO. This is also true for other kinds of the neutral oxygen‐containing compounds.
Flow microcalorimetry of adsorption of anionic alkyl surfactants at the solid/liquid interface
Authors: Tan Xin‐Yi , Yan Hai‐Ke , Hu Ri‐Heng , Loren Hepler G.
Published: September 2010

Flow microcalorimetry was used to study the adsoption of anionic alkyl surfactants from aqueous solutions onto silica. It is found that for alkyl sulfate systems the strength of adsorption interaction increases with increases of the alkyl chain length and decreases as temperature rises. The adsorption depends only on monomer concentration of the solution even above the critical micelle concentration (cmc). The assumption is made that the adsorption involves only a transfer of monomers from bulk to surface phase. A different adsorption mechanism is operative for the alkyl carboxylate.
Studies on conjugated fluoro‐polymers II. Characterization and electrical conductivity of polyperfluorobutyne‐2
Authors: Yang Shi‐Yong , Hong Jie , Huang Yao‐Zeng , Zhang Jing‐Yun
Published: September 2010

Polyperfluorobutyne‐2 (PPFB), a conjugated polymer, was characterized with IR, UV‐VIS, fluorescence spectra etc. The electrical conductivities of the polymer doped with various dopants were investigated. The effect of the molecular structure of PPFB on the electrical properties was discussed.
Stereochemistry of the coupling step in photo‐SRN 1 reaction
Authors: Wu Bi‐Qi , Zeng Fan‐Wen , Zhao Yong , Wu Guo‐Sheng
Published: September 2010

The photo‐SRN 1 reaction of (+)‐camphor and aryl halides was investigated in order to estimate the stereochemistry of the coupling step of aryl radicals with a nucleophile. The ratio of endo to exo products determined by 1H NMR and CD spectra was found to be 99:1. MNDO calculations of the orbital parameters showed a favorable one‐sided overlap of the enolate ion with the SOMO of aryl radical. In addition, fragmentation of (ArX)− was found to be related to the energy of SOMO of (ArX)−.
Syntheses of (C8H8)Ln(C9H7) · (THF)2(Ln = Pr,Nd) and crystal structure of (C8H8)Pr(C9H7) · (THF)2
Authors: Wen Ke , Jin Zhong‐Sheng , Wei Ge‐Cheng , Chen Wen‐Qi
Published: September 2010

This paper reports two lanthanide complexes of formula (C9,H7)Ln(C8H8) · (THF)2 where Ln is Pr or Nd, C9H7 is indenyl, and C8H8 is cyclooctatetraene (COT). The complexes were prepared by the reaction of LnCl2 with K(C9H7) and K2(C2H2) in THF. (C9H7)Pr(C8H8) · (THF)2 crystallizes in THF at −15°C in the monoclinic space group P212 with unit cell dimensions a = 8.446 (0), b = 10.083(2), c = 13.407 (3)Å, β = 105.48 (1)°, V = 1100.43 (35)Å2, Dc = 1.52 g / cm3 and Z = 2. The final R value is 0.033, Rw value is 0.030, respectively. In (C9H7)Pr(C8H8) · (THF)2 a five‐membered ring centroid of C, the C8H8 ring centroid and the two oxygen atoms from the two THF molecules form a distorted tetrahedral geometry around the metal.
Some reactions of fluorosulfonyldifluoroacetic acid with N‐heterocyclic compounds
Authors: Chen Qing‐Yun , Yang Guo‐Ying , Wu Sheng‐Wen
Published: September 2010

Difluorocarbene generated from the decomposition of fluorosulfonyldifluoroacetic acid (2) reacted with various sodium salts of N‐heterocyclic compounds(1) giving the corresponding difluoromethylated products in acetonitrile at 10–40°C. Benzotriazole(1a), benzimidazole(1b) and imidazole (1c) were converted into 1‐(difluoromethyl)benzotriazole(3a), 1‐(difluoromethyl)benzimidazole(3b) and 1‐(difluoromethyl)imidazole(3c) respectively. Indole(1d) reacted with 2 to give N‐(fluorosulfonyldifluoroacetate)indole(2d) rather than the expected difluoromethylated derivatives.
A microbially based approach for the asymmetric synthesis of both enantiomers of R‐ and S‐fluoxetine
Authors: Gu Jian‐Xin , Li Zu‐Yi , Lin Guo‐Qiang
Published: September 2010

Both enantiomers of fluoxetine were synthesized in five steps from ethyl benzoylacetate (1) using microbial‐chemical approach with overall yields of 59% and 62% respectively. (S)‐Enantiomer can be obtained in >99% e.e. by resting cell of baker's yeast and the R form was produced in 81% e.e. by immobilized Geotrichum sp. G 38.
Studies on the synthesis of some new biflavanoids VII. Synthesis and structures of 2,2″‐biflavanones
Authors: Li Yu‐Lin , Zhang Fang‐Jie , Wang Qi‐Guang
Published: September 2010

A new approach to the synthesis of 2,2″‐biflavanones by the reductive dimerization of flavones is reported. The products, the racemate and meso biflavanones, have been separated and their structures have been determined on the basis of their spectral data. The configuration of 3b has been determined by X‐ray crystallography as well.
Investigation on the potential barrier to internal rotation in molecules—Ab initio calculation and energy partition of the internal rotation barrier in complex molecule H3N–BH3
Authors: Zhang Qi‐Yuan , Yan Ji‐Min
Published: September 2010

Based on the ab initio/6–31G* calculation, the potential barrier to internal rotation in molecule H3N‐BH3 has been studied by means of PD/LSF atomic charge model and Buckingham(exp‐6–1) energy partition method. The results indicate that the order of the contributions of the components to the total energy barrier ΔE is |ΔVed|(electrostatic)>|ΔV| (charge transfer)> |ΔVex| (exchange repulsion) > |ΔVdi| (dispersion). For ΔVes there are maxima at θ = 30° and 90°, and a saddle at θ = 60°. There are good linear relationships for the total barrier ΔE, ΔVex and ΔV| with cos3θ respectively, and the same for the dipole moment from PD/LSF model (μPD) and that from ab initio calculation (μQM) vs. cos3θ respectively.
Characterization and phase transition study for vesicles of fluorocarbon amphiphiles with 1,3‐disubstituted glycerol structure
Authors: Liang Kang‐Ning , Hui Yong‐Zheng
Published: September 2010

This paper presents the preparations and characterization of vesicles of four new fluorocarbon amphiphiles with 1,3‐disubstituted glycerol structure in common and different headgroups (OH, 1; CO2H, 2; quaternary ammonium salt, 3; and pyridinium salt, 4). These vesicles have higher transition temperature due to the stronger hydrophobic interaction between fluorocarbon chains. Addition of fluorocarbon additives with carboxylic acid or quaternary ammonium salt head group respectively shows different influences on phase behavior of vesicles of 2. These results are discussed based on the interaction within headgroup, hydrophobicity and specific mutahydrophobic interaction between fluoro‐ and hydrocarbon chains.
Synthesis and reactions of some 6‐aryl and 2,6‐diaryl‐4‐(4′‐antipyrinyl)‐2,3,4,5‐tetrahydropyridazin‐3‐ones and screening for their antibacterial activities
Authors: Sayed G. H. , Shiba S. A. , Radwan A. , Mohamed S. M. , Khalil M.
Published: September 2010

Some new pyridazinone derivatives(3) were synthesized through addition of antipyrin to β‐aroylacrylic acids (1) followed by cyclization of the adducts. Reactions of 3 with ethyl bromoacetate, benzenesulfonyl chloride, benzoyl chloride and POCl3 give N‐substituted products and monochlorosubstituted pyridazines (4), respectively. The reactions of the latter with thiourea give unexpected dithio‐derivatives (5), which react with phenylhydrazine to give pyrazolopyridazino pyridazine derivatives (6). Reactions of 2 with NH2OH in ethanol and pyridine afford oxime and oxazinone derivatives 7 and 8, respectively. The antibacterial activities of several compounds were screened.
Studies on electrical properties of system La2‐x(Sr1‐yCay)xNiO4
Authors: Meng Jian , Ren Yu‐Fang , Pa Ya‐Nan
Published: September 2010

A new series of solid solutions of composition La2 1.4) were prepared. All the members of the system are of the tetragonal K2NiF4 type structure. The tetragonality ratio c/a shows a progressive decrease with increasing y except for the group of x = 1.4. The room temperature resistivity exhibits a gradual increase with y, which is interpreted by assuming that the single eg electron of Ni3+ is present in localized dZ2 orbital but the te electron gradually becomes itinerant because it is delocalized into dx2y2 orbital leads to a strong Ni3−O2− covalent interaction with increasing the Sr content. Variation of resistance with temperature shows semiconducting properties except for the composition of x=1.4, y<0.3 which shows a semiconductor‐to‐metal transition.
Multinuclear NMR study of lanthanide(III) complexes of 1,2‐PDTA in aqueous solution
Authors: Song Rui‐Fang , Zhang Cun‐Zhi , Li Fei , Hua Shi‐Ying
Published: September 2010

The complexation of lanthanide(III) cations with 1,2‐propanediaminetetraacetate (1,2‐PDTA) in aqueous solution has been investigated by 10Na, 35Cl, 2H and 11O NMR shift measurements. It has been shown that the contact shifts are dominant for 17O, 16Cl and 2H (only for the heavier lanthanide series) and the pseudocontact shifts are dominant for 25Na. It is suggested that the 1,2‐PDTA ligand is bound pentadentately via the two nitrogens and the three carboxylates for the lighter lanthanide complexes, hexdentately via the two nitrogens and the four carboxylates for the heavier ones. The numbers of the water coordinated were determined. The small amount of chloride anion in inner coordination sphere was observed.
Determination of thorium with DBF‐arsenaz by flow‐injection analysis
Authors: Yang Yi , Cai Ru‐Xiu , Zeng Yun‐E
Published: September 2010

A sensitive, selective, rapid, simple, and convenient method for the determination of thorium was developed. The method was based on the color reaction of thorium with DBF‐arsenazo in a strong acidic medium (4 mol/L HCl). The flow‐injection technique was used with an automated flow‐injection analyzer. Beer's law was obeyed in the range of 0–1.4 μg/mL. The relative standard deviations were less than 1%.
Phosphonium and arsonium ylides. XVII. A facile synthesis of methyl 2,6‐bisperfluoroalkylbenzoates via acyclic precursors
Authors: Ding Wei‐Yu , Cao Wei‐Guo , Xu Zhen‐Rong , Shi Zhi‐Jian , Yao Yuan
Published: September 2010

The title compounds 6a—6f were prepared with high yield via intramolecular Wittig reaction of methyl 3‐perfluoroalkyl‐6‐peifluoroacyl‐2‐triphenylphosphoranylidenchex‐3,5‐dienoates (5a—5i) which were obtained from the reaction of 3‐perfluoroacylprop‐2‐enylidenetriphenylphosphoranes (3a—3c) with methyl perfluoroalkynoates (4a—4c).
Quenching of zinc phthalocyanine excited states by viologen surfactant assemblies—The influence of microenvironment
Authors: Liu Ji‐Xiang , Zhou Qing‐Fu , Xu Hui‐Jun
Published: September 2010

A series of functional surfactants of N‐alkyl‐N′‐butyl viologens has been synthesized. The quenching of excited singlet and triplet states of zinc phthalocyanine was studied in DMSO and in mixed micelles containing the functional surfactant as one and cationic cetyl trimethylammonium bromide (CTAB), anionic sodium dodecylsulfate (SDS) and neutral TX‐100 surfactant as the other component. Fluorescence quenching and laser photolysis studies indicate that the functional surfactants are solubilized at different sites in micelles, the process depends on chain length and exerts great influence on the quenching of zinc phthalocyanine excited states.
Structural comparison to the molybdenum site of nitrogenase. Synthesis and crystal structure of binuclear oxomolybdenum(V) complex with both o‐mercaptophenolate and alkoxide ligands
Authors: Hu Yong‐Han , Kang Bei‐Sheng , Chen Xue‐Tai , Huang Liang‐Ren , Weng Ling‐Hong , Xu Yong‐Jin
Published: September 2010

Complex (n‐Bu4N)[Mo2O2(OMe)(mp)3] [1, mp = (o‐OC6H4S)2−] was synthesized by the reaction of MoOCl3(THF)2 and Na2mp in EtOH and crystallized in monoclinic space group P21/n with crystal data: a = 13.910(3), b = 23.554(3), c=12.558(2) Å, β = 105.20(2)˙. Z = 4, Do = 1.455g/ cm3, final R = 0.077 for 5325 reflections [I>3s̀(I)]. The two [Mo(O)mp]+ moieties are bridged by one 1,2‐bidentate ligand mp2− with exceedingly small bite angle (69.0˙) and bite distance · (2.70Å) and by a methoxy group. The structure can be interpreted as two distorted octahedra around the Mo atoms sharing a face. Attempts have been made to provide structural informations for the syntheses of modelling compounds of FeMoco by comparing the Mo—O and Mo—S bond distances of o‐mercaptophenolate ligated compounds to those of the molybdenum site of nitrogenase.
Studies on polyhaloalkanes. II. A facile method for mono‐fluorination of α, ω‐dihaloperfluoroalkanes
Authors: Huang Bing‐Nan , Prescher Dietrich
Published: September 2010

A facile monofluorination of α, ω‐dihaloperfluoroalkanes was achieved by the reaction of them with antimony trifluoride and chlorine in anhydrous antimony pentachloride when monofluorinated products were removed immediately after their formation from the reaction mixture by fractionation. The reaction conditions were also investigated.
Molecular structure of imidazolate bridged binuclear zinc complex and its single crystal ESR spectra doped with bridged Cu—Zn complex
Authors: Mao Zong‐Wan , Chen Dong , Han Shi‐Ying , Sui Yun‐Xia , Tang Wen‐Xia , Yu Kai‐Bei
Published: September 2010

The X‐ray crystal structure of [(dtma)ZnImZn(dtma)]C1O4·2.5H2O (Hdtma=4‐Diethyl‐enetriamineacetic acid) was determined. The crystal is of orthorhombic, space group Pbcn with a=14.104(5), b=14.897(5), c=25.384(9)Å, and Z=8. The least‐square refinement of the structure leads to conventional R factor of 0.066. The magnetic properties of [(dtma)CuImZn(dtma)]CIO4·2.5H2O were investigated. From the single crystal ESR spectra of Zn—Im—Zn dimer doped with Cu—Im—Zn complex, the anisotropic g and A tensors and electronic spin‐density of the Cu—Zn complex are obtained and the bonding nature of Cu is discussed.
Synthesis, structure and electrochemistry of dithiocarbamato phenthiolate oxo‐molybdenum(IV) complexes [MoO(SΦ)2(S2CNEt2)]‐
Authors: Zhuang Bo‐Tao , Pan Bing‐Hua , Huang Liang‐Ren , Lan An‐Jian
Published: September 2010

The reaction of Mo(0) complex [Mo(CO)4(S2CNEt2)]‐ with phenthiolate [Et4N]SΦ in acetonitrile in the presence of small amount of air affords a new oxo‐molybdenum complex [MoO(SΦ)2(S2CNEt2)], which crystallizes in two forms of crystals. [Et4N][MoO(SΦ)2Φ(S2CNEt2)] (1a) and [Et4N][MoO(SΦ)2(S2CNEt2)]Φ(CH3)2CHOH (1b). The structures of 1a and 1b were determined from three‐dimensional X‐ray data. 1a crystallizes in the monoclinic, space group Ce with a=12.321(4), b=15.245(4), c=16.087(9)Å; β= 98.44(4)Φ, V=2989Å3, Z=4, Dc = 1.35g/cm3 and R=0.031 for 2434 reflections [I>36(I)]. 1b crystallizes in the monoclinic space group F21/n with a=9.861(1), b=20.357(3), c=17.122(5)Å; β= 92.27 (2)*, V=3434.3Å3, Z=4; De = 1.29g/cm3 and R= 0.051 for 2852 independent reflections [I>3σ(I)]. The structures of 1a and 1b reveal that the anion [MoO(SΦ)2(S2CNEt2)]‐ contains a single oxo ligand coordinating to a molybdenum(IV) and the geometry around Mo(IV) atom is a distorted square pyramid. Interestingly, the solvate molecule isopropanol of 1b is linked to oxo group by a hydrogen‐bond of 1.928Å, leading to the increase of MoO bond distance (1.718Å). Mo—S distances are 2.44 and 2.39Å. The electrochemical behavior of 1 was discussed also.