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Cu2ZnSnS4crystal growth using an SnCl2based flux
The stoichiometry and phase homogeneity of the kesterite type compound Cu2ZnSnS4play a key role in its efficiency in solar cells. In this work, CuCl2, ZnCl2and SnCl2were applied as solvents in the Cu2ZnSnS4crystal growth for the first time. The multiphase ingot was obtained by direct fusion of the stoichiometric batch composed of constituent elements. Compared to that, the material recrystallized in SnCl2presented a single-phase Zn-rich kesterite with composition Cu1.94Zn1.06SnS4and unit cell parameters ofa= 5.4324(3) andc= 10.8383(2) ?. The crystal structure of Cu1.94Zn1.06SnS4was determined by single crystal X-ray diffraction analysis. The integral phase purity of the crystals grown with the use of the SnCl2solvent was verified by powder X-ray diffraction analysis and Raman measurements. In the Raman spectrum, the FWHM value of the 337 cm?1line was as low as 9.6 cm?1that indicates the minimal lattice disorder.
Kokh,Atuchin,Adichtchev,Gavrilova,Bakhadur,Klimov,Korolkov,Kuratieva,Mukherjee,Pervukhina,Surovtsev
p. 1025 - 1032
(2021/02/06)

DOUBLE GOLD(III)–ZINC(II) DI-ISO-BUTYLDITHIOCARBAMATO- CHLORIDO COMPLEXES OF THE COMPOSITION [Au(S2CNR2)2]2[Zn2Cl6] AND [Au(S2CNR2)2][Zn(S2CNR2)Cl2]: SYNTHESIS, STRUCTURAL ORGANIZATION, 13C CP-MAS NMR, AND THERMAL BEHAVIOR
Abstract: The interaction of zinc(II) di-iso-butyldithiocarbamate with [AuCl4]— anions in 2M HCl is studied. The result of chemisorption binding of gold(III) from a solution to the solid phase is the formation of double ionic complexes of the compositions [Au{S2CN(iso-C4H9)2}2]2[Zn2Cl6] (1) and [Au{S2CN(iso-C4H9)2}2][Zn{S2CN(iso-C4H9)2}Cl2] (2). The chemical identification of preparatively isolated crystalline compounds was performed by 13C CP-MAS NMR spectroscopy. According to single crystal X-ray diffraction data, structural units of complex 1 are a binuclear zinc anion and non-equivalent complex [Au{S2CN(iso-C4H9)2}2]+ cations: centrosymmetric A with the Au(1) atom and С – Au(3) and non-centrosymmetric В – Au(2). With the participation of secondary Cl?S bonds (3.2407?? and 3.2756??), В cations and anions form supramolecular ionic pairs. The structure of 2 in turn involves the centrosymmetric gold(III) cation whose counterion is a mixed-ligand dithiocarbamato-chlorido anion of zinc(II). Pairs of non-equivalent secondary Cl?S bonds (3.2337?? and 3.3151??) combine the ionic structural units of 2 into zigzag-like pseudo-polymeric chains along which the alternation of complex cations and anions is noted. Thermolysis of complexes in cationic and anionic parts is accompanied by the quantitative regeneration of bound gold along with the formation of ZnCl2 and ZnS.
Rodina,Loseva,Ivanov
p. 123 - 136
(2021/02/26)

The Tetrachloridoaurates(III) of Zinc(II) and Cadmium(II)
The first salt-like compounds of dications with [AuCl4]– anions are reported. The compounds Zn[AuCl4]2·(AuCl3)1.115 (1) and Cd[AuCl4]2 (2) are obtained from reactions of MCl2 (M = Zn, Cd) and elemental gold in liquid chlorine at ambient temperature under autogenous pressure and subsequent annealing at 230 °C. The structure of 1 represents an incommensurately modulated composite [superspace group C2/c(α0γ)0s] built of two subsystems. The first subsystem contains chains of zinc(II) tetrachloridoaurate(III), which feature a slightly distorted octahedral coordination of Zn and can be described by the Niggli formula 1∞{Zn[AuCl4]1/1[AuCl4]2/2}. The second subsystem consists of Au2Cl6 molecules, which are located in channels built up by the first subsystem. The structural parameters of the hosted Au2Cl6 molecules show only small deviations from neat AuCl3. The crystal structure of Cd[AuCl4]2 (2) consists of chains built of Cd2+ ions coordinated by bridging [AuCl4]– anions and alternating Cd-Au sequence. Cd has a distorted octahedral coordination environment.
Landvogt, Christian,Beck, Johannes
p. 391 - 396
(2018/04/09)

Synthesis, thermal study and some properties of Zn(II), Cd(II) and Pb(II) compounds with mono-, di- and trichloroacetates
New complexes with formulae: Zn(CClH2COO)2·2H2O, Zn(CCl2HCOO)2·2H2O, Zn(CCl3COO)2·2H2O, Cd(CCl2HCOO)2·H2O, Cd(CCl3/su
Czylkowska,Raducka,Mierczyński
p. 937 - 946
(2017/04/11)

Facile synthesis and an effective doping method for ZnO:In3+ nanorods with improved optical properties
The sol-gel spin-coating method is usually used for thin-film deposition rather than to grow one-dimensional nanostructures. In this study, a novel regrowth method for spin-coated ZnO:In3+ films is demonstrated, using vapor-confined face-to-face annealing (VC-FTFA) in which a mica sheet is inserted between the two films prior to FTFA. ZnO:In3+ nanorods are regrown when indium chloride is used as the solvent because ZnCl2 and InCl3 vapors are generated and confined between the films. The near-band-edge emission intensity of the ZnO:In3+ nanorods resulting from VC-FTFA at 700 °C is enhanced by a factor of 17 compared with that of ZnO:In3+ films annealed in open air at the same temperature. Our method offers a simple and low-cost route for the fabrication of ZnO nanorods.
Nam, Giwoong,Kim, Byunggu,Leem, Jae-Young
p. 1 - 7
(2015/09/01)

Radical-based epoxide opening by titanocenes
The binding of 2,2-diphenyloxirane to Cp2TiCl is studied on the electronic level by magnetic resonance spectroscopy and quantum chemical calculations. The complexation of 2,2-diphenyloxirane is accompanied by dissociation of the chloride ligand, and thus, the epoxide binds to the cationic titanocene(III) complex. The titanocene(III)-epoxide species persists only for short periods of time (A short-lived paramagnetic titanocene(IV)-epoxide radical species has not been directly observed. However, by a combination of isotope labeling and spin-trapping, evidence for the existence of such a species has been unequivocally demonstrated. The observation of a titanocene(III)-epoxide complex is unprecedented and provides direct evidence for inner-sphere electron transfer between epoxides and titanocenes, responsible for the high regioselectivity of ring-opening.
Cang?nül, Asli,Behlendorf, Maike,Gans?uer, Andreas,Van Gastel, Maurice
p. 11859 - 11866
(2013/11/19)

Immobilization of kojic acid in ZnAl-hydrotalcite like compounds
Kojic acid (KOJ) is a melanin synthesis inhibitor widely used as skin lightening agent in topical preparations. Unfortunately it is easily susceptible to photo-oxidation, phenomenon responsible for chemical and organoleptic modifications. The aim of this work was the intercalation of KOJ in hydrotalcite-like compounds (HTlc) in order to stabilize KOJ and to reduce its photolability. Hydrotalcite containing Zn and Al (ZnAl-HTlc) was used as host to obtain the final compound ZnAl-HTlc-KOJ. The intercalation was carried out, after many attempts, by ionic exchange mechanism by means of the strong base EtO- in anhydrous ethanol/dimethylsulfoxide (DMSO) mixture as solvent in order to generate KOJ- anions. The final product was characterized by the X-ray powder diffraction (XRPD), FT-IR spectroscopy, thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) and elemental analysis. The intercalated compound was formulated in a siliconic water free self-emulsifying ointment and the in vitro release profile was evaluated. All samples (intercalation compound and its formulation) were submitted also to spectrophotometric assays in order to evaluate the matrix protective effect towards ultraviolet rays.
Ambrogi, Valeria,Perioli, Luana,Nocchetti, Morena,Latterini, Loredana,Pagano, Cinzia,Massetti, Elena,Rossi, Carlo
p. 94 - 98
(2012/03/09)

Characteristic features of formation, synthesis, and properties of binuclear zinc(II) helicates with alkyl-substituted 3,3'-bis(dipyrrolylmethenes)
On the basis of spectrophotometric studies, it was demonstrated that complexation of hydrobromides of seven alkylated 3,3'-bis(dipyrrolylmethenes) (H2L · 2HBr) with zinc(II) acetate dihydrate in DMF (298.15 K) includes successive steps of formation of binuclear helicates of two types: [Zn2(AcO)2L] (heteroleptic single-helix complex) and [Zn2L2] (homoleptic double-helix complex). An increase in the degree of alkylation of the pyrrole rings of the ligands from 4 to 10 methyl groups induces an increase of overall complexation constants (logK°) from 7.60 to 13.73. The synthesis of helicates [Zn2L2] was described. The products were studied by elemental analysis and IR, 1H NMR, U/Vis, and fluorescence spectroscopy. The effect of the helicand structure and the solvent nature on the chromophore and fluorescence properties of [Zn2L2] was discussed. The kinetic stability of zinc(II) with decamethyl-substituted 3,3'-bis(dipyrrolylmethene) in HCl-DMF medium was estimated. Pleiades Publishing, Ltd., 2012.
Antina,Dudina,Guseva,Antina,Berezin,V'Yugin
p. 261 - 269
(2012/06/30)

Reaction of zinc oxide with ammonium chloride
The reaction of ammonium chloride with zinc oxide was studied kinetically and thermogravimet-rically. Reaction products were identified by IR spectroscopy and X-ray powder diffraction. Ammonium chlorozincates were found to form in the reaction and to deco
Borisov,D'Yachenko,Kraidenko
p. 499 - 501
(2012/07/03)

Influence of manganese on magnetic and electronic properties of ZnCr 2Se4
The Zn1-xMnxCr2Se4 crystals were prepared by chemical vapor transport in closed silica tubes using ZnSe and MnSe with CrCl3 as the transport agent. Four crystals with different Mn content (x = 0.12, 0.13, 0.18 and 0.24) were studied by X-ray photoelectron spectroscopy (XPS) and magnetic measurements in order to determine influence of manganese on their magnetic and electronic properties. The XPS revealed no change of chemical shifts of Cr core lines indicating a Cr3+ (3d 3) electronic configuration. Magnetization measurements revealed a systematic increase in saturation magnetic moments from 6.32 μB/mol for x = 0.12 to 7.63 μB/mol for x = 0.24, as well as effective paramagnetic Bohr magneton numbers from 4.87 μB/mol for x = 0.12 to 6.91 μB/mol for x = 0.24.
Jendrzejewska, Izabela,Zajdel, Pawe?,Heimann, Jan,Krok-Kowalski, Józef,Mydlarz, Tadeusz,Mrzigod, Janusz
p. 1881 - 1886
(2012/08/14)

Analysis of the conformational behavior and stability of the SAP and TSAP isomers of lanthanide(III) NB-DOTA-type chelates
Controlling the water exchange kinetics of macrocyclic Gd3+ chelates, a key parameter in the design of improved magnetic resonance imaging (MRI) contrast media, may be facilitated by selecting the coordination geometry of the chelate. The water exchange kinetics of the mono- capped twisted square antiprism (TSAP) being much closer to optimal than those of the mono capped square antiprism (SAP) render the TSAP isomer more desirable for high relaxivity applications. Two systems have been developed that allow for selection of the TSAP coordination geometry in 1,4,7,10-tetraazacyclododecane-1,4,7,10- tetraacetic acid (DOTA)-type Gd3+ chelates, both based upon the macrocycle nitrobenzyl cyclen. In this paper we report investigations into the stability and formation of these chelates. Particular focus is given to the production of two regioisomeric chelates during the chelation reaction. These regioisomers are distinguished by having the nitrobenzyl substituent either on a corner or on the side of the macrocyclic ring. The origin of these two regioisomers appears to stem from a conformation of the ligand in solution in which it is hypothesized that pendant arms lie both above and below the plane of the macrocycle. The conformational changes that then result during the formation of the intermediate H2GdL+ chelate give rise to differing positions of the nitrobenzyl substituent depending upon from which face of the macrocycle the Ln3+ approaches the ligand.
Tircso, Gyula,Webber, Benjamin C.,Kucera, Benjamin E.,Young, Victor G.,Woods, Mark
p. 7966 - 7979
(2011/10/09)

Molecular complexes of cobalt(II) and Zinc(II) chlorides and bromides with 1-piperidinyl dimethylcarbamodithioate (L): Crystal structures of L and [ZnLBr2]
Complexes of MX2(M = Co, Zn; X = Cl, Br) with 1-piperidinyl dimethylcarbamodithioate (L) of composition [MLX2] have been synthesized. The compounds have been studied by elemental analysis; X-ray diffraction; thermogravimetry; conductometry; magnetochemistry; and IR, 1H NMR, and electronic absorption spectroscopy. The ligand molecule is coordinated to the metal atoms in a bidentate chelating mode through the thione sulfur atom and the sulfenamide nitrogen atom to form a five-membered chelate ring. The structures of L and [ZnLBr2] have been determined by X-ray crystallography.
Seifullina,Khitrich,Vologzhanina
p. 184 - 189
(2011/05/04)

Local investigation of hyperfine interactions in pure and Co-doped ZnO
In the present work bulk samples of pure as well as Co-doped ZnO with different concentrations were prepared by sol-gel method from highly pure metallic Zn (99.9999%) and Co (99.9999%). The samples were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), X-ray microanalysis (EDS) and perturbed gamma-gamma angular correlation (PAC) spectroscopy. Carrier-free 111In nuclei were introduced during preparation of the samples and used as probe nuclei at Zn sites for PAC measurements. PAC results show that both pure and Zn1 - x Cox O (x ≤ 0.15) samples have the same electric quadrupole frequency when Co-doped samples are annealed in air, argon or nitrogen atmosphere at 1173 K. SEM and EDS results showed that Co-doped samples are homogeneous without any secondary Co phases. These observations indicate that Co ions are substituted for Zn ions and have a similar electronic structure of Zn ions. A weak local magnetism was observed at temperatures below about 300 K for Co concentration of 10% when sample was annealed in Nitrogen.
Mercurio,Carbonari,Cordeiro,Saxena,D'Agostino
p. 1195 - 1197
(2010/07/04)

Crystal growth, structure and characterizations of a new semiorganic nonlinear optical material-β-Alanine zinc chloride
The title compound, β-alanine zinc chloride-a new semiorganic nonlinear optical crystal was grown by slow evaporation technique. Single crystals of β-alanine zinc chloride have been subjected to X-ray diffraction analysis to determine the crystal structure. The powder X-ray diffractogram of the crystal has also been recorded. The amount of carbon, nitrogen and hydrogen in the crystals was also estimated. Fourier Transform Infrared and Raman spectral measurements have been carried out on the grown crystals in order to identify the functional groups. The presence of hydrogen and carbon in the β-alanine zinc chloride was confirmed by using proton and carbon nuclear magnetic resonance spectral analyses. The percentage of zinc in the crystal was determined by atomic absorption spectroscopy. Optical behavior such as ultraviolet-vis-near infrared transmittance spectrum and second harmonic generation has been investigated. The mechanical strength and thermal behavior of the grown crystal have been analyzed.
Anbuchezhiyan,Ponnusamy,Muthamizhchelvan,Sivakumar
p. 897 - 904
(2010/10/01)

The role of metal ions and counterions in the switching behavior of a carboxylic acid functionalized spiropyran
The ability of a carboxylic acid functionalized spiropyran, SP, to act as a reversible and selective receptor for metal ions has been systematically examined. A series of spectroscopic measurements, combined with single-crystal X-ray diffraction have been employed in order to determine metal-ion sensitivity and selectivity, binding constants, solution compositions, binding kinetics as well as solid-state structure of a metal-complex of this ligand. This molecule acts as a chelating ligand and binds to metal ions using a triad of functionalities and will release the metal ion by application of visible light. Altering the complex from ZnCl2 and Zn(ClO4)2, leads to only a small change in the complex absorption maxima from 494 to 492 nm, but produced a drastic increase in the sensitivity for the zinc(ii) ion. Fluorescence spectroscopy was employed to establish that the detection limit for Zn(ii) is approximately 3 × 10-7 M for Zn(ClO 4)2. The counterion also influences binding constants and the equilibrium constants for Cu(ClO4)2 and CuCl 2 are K = 3.37 × 104 M-1 to K = 2.04 × 103 M-1, respectively. Additionally, in the presence of perchlorate, the spiropyran-Cu complex formation is fast enough to allow for real-time naked eye detection of this metal ion in less than three minutes; the formation of other metal complexes takes between 50 minutes to 2 hours. Finally, the single-crystal structure determination of the SP-zinc chloride complex shows that the Zn(ii) ion displays a distorted square-pyramidal arrangement, and neighbouring metal ions are bound together into a 1-D coordination polymer with a hydrophilic core, surrounded by hydrophobic 'cladding'.
Natali, Manuel,Aakeroey, Christer,Desper, John,Giordani, Silvia
p. 8269 - 8277
(2011/01/09)

Electrocarboxylation of CCI4 in MeCN during electrolysis with the sacrificial Zn anode
The regularities of galvanostatic electrocarboxylation of CCl4 in Alk4NBr/MeCN in an undivided cell with sacrificial Zn anode were studied. The major product of the electrolysis is zinc trichloroacetate, which is formed as a result o
Sigacheva,Neverov,Petrosyan
p. 297 - 302
(2010/07/09)

Synthesis, crystal structures, and thermal properties of new [ZnX 2(2,5-dimethylpyrazine)] (X = Cl, Br, I) coordination compounds
Eight new halidozinc(II) coordination compounds with 2,5-dimethylpyrazine as a ligand were prepared. The reaction of ZnX2 (X = Cl, Br, I) and 2,5-dimethylpyrazine in methanol results in the formation of catena-(μ2-2,5-dimethylpyrazin
Wriedt, Mario,Jess, Inke,Naether, Christian
p. 363 - 372
(2009/04/13)

The effect of ligand basicity on the thermal stability of heterodinuclear NiII-ZnII complexes
Four complexes of the nuclear structure NiII-ZnII were prepared with bis-N,N′-(salicylidene)-1,3-propanediamine (LH 2), bis-N,N′-(salicylidene)-2,2′-dimethyl-1,3- propanediamine (LDMH2) and the reduced derivativ
Zeybek, Bülent,Ate?, B. Meltem,Ercan, Filiz,Aksu, M. Levent,K?l??, Esma,Atakol, Orhan
p. 377 - 385
(2009/12/08)

Salts of Fatty Acids and Methods of Making and Using thereof
Disclosed are methods of making salts of fatty acids (e.g., marine oils) and to salts prepared by the disclosed methods. Methods of using the disclosed salts are also disclosed.
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(2009/07/25)

PROCESS FOR PRODUCING DICYANONORBORNANE AND ZEROVALENT-NICKEL COMPLEX CATALYST
The present invention is to provide a process for producing dicyanonorbornane characterized by causing hydrogen cyanide to undergo addition reaction with cyanonorbornene (bicyclo[2.2.1]-5-heptene-2-carbonitrile) in the presence of a zerovalent nickel complex catalyst which is produced by using a phosphite represented by P (x) (y) (z) (wherein P is a phosphorus atom, and x, y and z are each OR, where R represents an aryl group having not more than 18 carbon atoms) as a ligand to reduce a nickel halide with at least one metal selected among zinc, cadmium, beryllium, aluminum, iron and cobalt, wherein the phosphite is one which has a phosphate content of 1.0 weight % or lower based on the whole phosphite.
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Page/Page column 5-6

(2009/04/23)

Structural and spectral characterization of the compounds nGly·ZnCl2·mH2O (n = 1,2,3; m = 0,2)
The coordination behaviour of Zn2+ ions in chloride-glycine aqueous solutions and the formation of different complexes were discussed to predict the crystallization of compounds. The crystal structures of three compounds, Gly·ZnCl2,
Tepavitcharova,Havlí?ek,Němec,Vojtí?ek,Rabadjieva,Plocek
p. 55 - 63
(2009/05/09)

Facile dichloromethane activation and phosphine methylation. Isolation of unprecedented zwitterionic organozinc and organocobalt intermediates
Both C-Cl bonds of CH2Cl2 are readily activated by CoCl2 and metallic Zn allowing quantitative methylation of phosphines; unprecedented zwitterionic Co(ii) and Zn(ii) intermediates have been characterized which display α-m
Pattacini, Roberto,Jie, Suyun,Braunstein, Pierre
p. 890 - 892
(2009/07/10)

Boraguanidinates: Synthesis, X-ray structures, and reactions of {Li 2[iPr2NB(NDipp)2]}2 with p-block and group 12 element halides
The new Dipp-substituted boranes (Dipp = 2,6-diisopropylphenyl) iPr2NB(NHDipp)2 (5), BrB(NHDipp)2 (7b), and B(NHDipp)3 (8) have been prepared in high yields and characterized in solution by multinuclear NMR spectroscopy (1H, 11B and 13C) and in the solid state by X-ray crystallography. Reaction of 5 with 2 equiv of nBuLi in n-hexane produces {Li2[iPr2NB(NDipp)2]} 2 (6) the first example of a stable dilithiated boraguanidinate. The unsolvated complex 6 has a dimeric structure in the solid state. A survey of the reactions of 6 with p-block and Group 12 element halides revealed various types of reactivity including (a) disproportionation (InCl), (b) reduction to the metal (PbCl2, CdCl2, TeBr4, TeI4, and TlCl), and (c) simple metathesis (GeCl2, MgCl2, and ZnCl2). The metathetical products were characterized by multinuclear NMR spectra but, in contrast to the dilithiated complex 6, they readily decompose in non-coordinating solvents to form the diprotonated compound 5.
Corrente, Andrea M.,Chivers, Tristram
p. 10073 - 10080
(2009/05/15)

Effect of SO2 on chlorination of zinc ferrite ZnFe 2O4 and a mixture of ZnO and Fe2O3
Results of thermodynamic calculations and kinetic studies of the reaction of zinc ferrite ZnFe2O4 and of a mixture of oxides, ZnO and Fe2O3, with chlorine and SO2 are presented.
Derlyukova,Vinokurova
p. 370 - 374
(2008/09/20)

The mechanochemical reduction of AgCl with metals : RRRRevisiting an experiment of M. Faraday
Faraday induced the mechanochemical reduction of AgCl with Zn, Sn, Fe and Cu in 1820, using trituration in a mortar. This experiment is revisited, employing a mortar-and-pestle and a ball mill as mechanochemical reactors. The reaction kinetics depends both on the thermochemical properties and the hardness of the reactants. When using Zn as the reducing agent, Faraday likely observed a mechanically induced self-sustaining process (MSR), or at least he came very close to doing so.
Takacs
p. 81 - 84
(2008/10/09)

A PROCESS FOR PREPARATION OF ADAPALENE
The present invention discloses a process for preparation of highly pure Adapalene, chemically designated as 6-[3-(l-adamantyl)-4-methoxy phenyl]-2-naphthoic acid (I) comprising: a) reacting 1-adamantanol with 4-bromophenol (II) in presence of sulphonic acid with or without the use of organic solvent to give 2-(l-adamantyl)-4- bromophenol (III); b) alkylating compound of formula(III) with dimethylsulphate in presence of base in organic solvent to obtain 2-(l-adamantyl)-4-bromoanisole (IV); c) C-C coupling the compound of formula (IV) with methyl-6-bromo-2- naphthoate using magnesium, purified zinc chloride and NiCl2-DPPE in THF at a temperature of 40-60°C tO obtain methyl ester of 6-[3-(l- adamantyl)-4-methoxy phenyl] -2-naphthoic acid (V); d) purifying crude methyl ester of 6-[3-(l-adamantyl)-4-methoxy phenyl]-2- naphthoic acid (V) using a mixture of organic solvent to obtain pure compound (V); e) hydrolyzing the compound (V) with a solution of alkali in organic solvent to obtain metal salt of 6-[3-(l-adamantyl)-4-methoxy phenyl] -2-naphthoic acid (VI); f) acidifying metal salt of adapalene (VI) using organic or inorganic acid to obtain crude adapalene (I) and g) recrystallizing the crude adapalene (I) using a mixture of organic solvents to obtain pure adapalene (I).
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Page/Page column 18

(2010/11/29)

Covalent palladium-zinc bonds and their reactivity
Photolysis of (FPNP)Pd-Et in the presence of Et2Zn leads to the formation of (FPNP)Pd-Zn-Pd(PNPF), the first example of a compound with a covalent Pd-Zn bond. The Royal Society of Chemistry.
Fafard, Claudia M.,Chen, Chun-Hsing,Foxman, Bruce M.,Ozerov, Oleg V.
p. 4465 - 4467
(2008/09/16)

Syntheses and structures of magnesium and zinc boraamidinates: EPR and DFT investigations of Li, Mg, Zn, B, and in complexes of the [PhB(N?Bu) 2]?- anion radical
The first magnesium and zinc boraamidinate (bam) complexes have been synthesized via metathetical reactions between dilithio bams and Grignard reagents or MCI2 (M = Mg, Zn). The following new classes of bam complexes have been structurally characterized: heterobimetallic spirocycles {(L)μ-Li[PhB(μ-NtBu)2]}2M (6a,b, M = Mg, L = Et2O, THF; 6c, M = Zn, L = Et2O); bis(organomagnesium) complexes {[PhB(μ3-NtBu)2](Mg tBu)2(μ3-CI)Li(OEt2) 3} (8) and {[PhB(μ3-NtBu) 2](MgR)2(THF)2} (9a, R = iPr; 9b, R = Ph); mononuclear complex {[PhB(μ-NDipp)2]Mg-(OEt 2)2} (10). Oxidation of 6a or 6c with iodine produces persistent pink (16a, M = Mg) or purple (16b, M = Zn) neutral radicals {L x-μ-Li[PhB(μ-NtBu)2]2M} ? (L = solvent molecule), which are shown by EPR spectra supported by DFT calculations to be Cs-symmetric species with spin density localized on one of the bam ligands. In contrast, characterization of the intensely colored neutral radicals {[PhB(μ-NtBu) 2]2M)? (5c, M = In, dark green; 5d, M = B, dark purple) reveals that the spin density is equally delocalized over all four nitrogen atoms in these D2d-symmetric spirocyclic systems. Oxidation of the dimeric dilithio complex {Li2[PhB(μ4-N tBu)2]}2 with iodine produces the monomeric neutral radical {[PhB(μ-NtBu)2]Li(OEt2) x}? (17), characterized by EPR spectra and DFT calculations. These findings establish that the bam anionic radical [PhB(N tBu)2]?- can be stabilized by coordination to a variety of early main-group metal centers to give neutral radicals whose relative stabilities are compared and discussed.
Chivers, Tristram,Eisler, Dana J.,Fedorchuk, Chantall,Schatte, Gabriele,Tuononen, Heikki M.,Boere, Rene T.
p. 2119 - 2131
(2008/10/09)

Catalytic electroreduction of oxygen on products of pyrolysis of heterobimetallic complexes of zinc
Electrocatalysts for reduction of oxygen were synthesized from AG-3 activated carbon promoted with pyrolized heterobimetallic complexes [CoLCl 2] [ZnDMFACl3] and [ML][ZnCl4] (M = Cu 2+, Ni2+; L = 4,6,
Pirskii,Kublanovskii,Shevchenko,Kokozei
p. 1964 - 1968
(2008/02/08)

Synthesis, characterization and calorimetric study of zinc group halide adducts with aniline
The adducts ZnCl2·2an, ZnBr2·1.5an, CdCl2·2an, CdBr2·2an, CdI2·2an, HgCl2·2an and HgBr2·2an (where an = aniline) were synthesized and characterized by elemental analysis, infrare
da Silva Jr., Umberto G.,de Oliveira, ótom A.,de Farias, Robson F.
p. 2 - 4
(2008/10/09)

METHOD FOR THE PRODUCTION OF ADIPODINITRILE BY HYDROCYANATION OF 1,3-BUTADIENE
Disclosed is a method for the production of adipodinitrile by hydrocyanation of 1,3-butadiene on a catalyst, wherein in a first step 1,3-Butadiene is hydrocyanated to form 3-Pentene nitrile on at least one nickel(0) catalyst and, in a second step, 3-Pentene nitrile is hydrocyanated to form adipodinitrile on at least one nickel(0)-catalyst by adding at least one Lewis acid. At least one of the at least one nickel(0) catalysts used in the respective steps of the inventive method is converted in the other step.
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Page/Page column 33

(2008/06/13)

On the chemical vapor transport of ternary transition metal- and earth
The chemical vapor transport of transition metal tungstates MWO4 (M=Mn, Co, Ni, Cu, Zn, Cd) was investigated in dependence on mean transport temperature (923 K to 1223 K) and amount of transport agent Cl2. All tungstates migrate in a temperature gradient ΕT = 100 K from the region of higher temperature to the lower temperature with migration rates of 0.5 to 8 mg/h depending on experimental conditions. The transport behaviour was determined by continuous measurement of mass change during the transport experiments. The results were compared to thermo chemical calculations and the influence of moisture content discussed in detail. MgWO4 migrates under the influence of Cl2 in a temperature gradient 1273 K to 1173 K (migration rate 0.7 mg/h), CaWO4 and SrWO4 in a temperature gradient 1423 K to 1323 K (migration rate 0.1 mg/h).
Steiner, Udo
p. 1706 - 1714
(2008/10/09)

Oxidation of zinc with dicarbonylcyclopentadienyliron chloride in polar solvents
The kinetic and activation parameters of zinc oxidation with dicarbonylcyclopentadienyliron chloride in dimethylformamide were found. The apparent equilibrium constants, enthalpy, and entropy of the adsorption of the reagents on the metal surface were determined. A reaction scheme was suggested. 2005 Pleiades Publishing, Inc.
Usanov,Maslennikov,Spirina
p. 332 - 334
(2007/10/03)

ZnCl2 supported on NaY zeolite by solid-state interaction under microwave irradiation and used as heterogeneous catalysts for high regioselective Diels-Alder reaction of myrcene and acrolein
A novel catalyst preparation method is developed by solid-state interaction between ZnCl2 and NaY zeolite under microwave irradiation. The solid-state interaction is investigated by powder X-ray diffraction, FT-IR spectroscopy, and by testing the catalytic properties in the Diels-Alder reaction of myrcene and acrolein. XRD patterns indicate that ZnCl2 can disperse completely on the surface of NaY zeolite at the ZnCl2 loading less than 2.75mmolg-1. FT-IR spectra of pyridine adsorption on catalyst show that Lewis acid sites are the predominant acid sites. The catalyst of ZnCl2/NaY prepared by the treatment of microwave irradiation is proved to be an effective heterogeneous catalyst for high regioselective Diels-Alder reaction of myrcene and acrolein. The catalytic activity and the regioselectivity of p/m strongly depend on the ZnCl 2 loading. With an increase of the ZnCl2 loading up to 0.92mmolg-1, the activity and selectivity increase a little. In this case, the active site is deduced from the zinc ion species formed by solid-state ion exchange. The Lewis acid sites are too weak to catalyze efficiently the Diels-Alder reaction. Keeping an increase of ZnCl2 loading from 0.92mmolg-1 to 1.84mmolg-1, the activity and the regioselctivity of p/m increased markedly due to the formation of new zinc ion species of -O-Zn-Cl as Lewis acid sites on NaY zeolite. The catalysts leached with a mixture solvent of acrolein and dichloromethane show little loss of catalytic activity and selectivity. Thanks to the possibility of simple and safe handling of the ZnCl2/NaY and to its easy separation from organic products, it becomes an alternative Lewis acid catalyst for the Diels-Alder reaction to homogeneous Lewis acids.
Liu, Jianfu,Yin, Donghong,Yin, Dulin,Fu, Zaihui,Li, Qianhe,Lu, Gongxuan
p. 171 - 177
(2008/10/08)

Complexation of 2-hydroxynicotinic and 3-hydroxypicolinic acids with zinc(II). Solution state study and crystal structure of trans-diaqua-bis-(3- hydroxypicolinato)zinc(II)
The interactions between zinc(II) and the two ligands 2-hydroxynicotinic acid (HNic) and 3-hydroxypicolinic acid (HPic) have been investigated by means of potentiometric titrations in aqueous 0.6 m (Na)Cl at 25 °C. In both cases, only mononuclear complexes are formed. The qualitative and quantitative results obtained have been confirmed in part by UV-Vis spectrophotometry and 1H NMR spectroscopy. The complex trans-diaqua-bis-(3- hydroxypicolinato)zinc(II) was obtained as a crystal and examined by X-ray crystallography. The thermodynamic results allow drawing some conclusions regarding the extent of Zn(II) interference in a hypothetical chelation therapy treatment of aluminium or iron overload with these two ligands.
Di Marco, Valerio B.,Tapparo, Andrea,Dolmella, Alessandro,Bombi, G. Giorgio
p. 135 - 142
(2008/10/09)

Synthesis, spectral and thermal properties of macrocyclic zinc(II) complexes
The new zinc ternary complexes [Zn(cyclen)NO3]ClO4 (I), [Zn2(cyclen)2( -nic)](ClO4)3 (II), [Zn2(cyclen)2( -pic)](ClO4)3 (III) (cyclen=1,4,7,10-te
Vargova,Gyoeryova,Zelenak
p. 97 - 105
(2008/10/09)

Preparation, crystal structure and thermochemistry of Zn(AMP) 2Cl2
The complex of zinc chloride and 2-amino-4,6-dimethyloxyl pyrimidine (AMP) was prepared, and the composition of the complex was determined by chemical and elemental analyses. Complex was characterized by IR, XPS, 1H NMR and TG-DTG techniques. In addition X-ray structural analysis was performed. Crystals of [Zn(AMP)2Cl2] revealed the following parameters: Mr=446.59; orthorhombic Pbca; a=13.0208 (10); b=13.8531 (11); c=20.0652 (15)?; V=3619.3 (5)?3; Z=8; D calc=1.639Mgm-3; Mo Kα λ=0.71073?; μ=1.683mm-1; T=293K; R=0.0431 for 2510 observed reflections. The constant-volume combustion energies of the ligand and the complex, Δ cE, were determined by a precise rotating-bomb calorimeter at 298.15K. They were -3340.01±1.54 and -6552.76±3.55kJmol -1, respectively. Their standard enthalpy of combustion, Δ cHmθ, and standard enthalpy of formation, ΔfHmθ, were calculated, which were -3339.39±1.54, -6546.56±3.35 and -307.91±1.74, -995.10±3.93kJmol-1.
Fan, Xue-Zhong,Xie, Gang,Chen, San-Ping,Gao, Sheng-Li,Shi, Qi-Zhen
p. 87 - 91
(2008/10/09)

Synthesis, structure and third-order nonlinear optical properties of 1,3,5-triazine-based Zn(II) three-dimensional supramolecule
A novel zinc(II) 1,3,5-triazine-based complex [Zn(TIPT)Cl 2]·2CH3OH (1) (TIPT=2,4,6-tri(2-ispropylidene-1-ly) hydrazono-1,3,5-triazine) was prepared and structurally characterized by means of X-ray single crystal diffraction. The zinc(II) atom is coordinated at a distorted triangle bispyramid by three nitrogen atoms from TIPT and two Cl - anions. This compound exhibits a three-dimensional solid-state structure constituted by N-H?O, O-H?Cl, N-H?Cl and C-H?Cl hydrogen bonds. The third-order nonlinear optical properties were determined by Z-scan techniques. The results indicate the compound exhibit strong self-focusing effect, and the hyperpolarizability γ value is 8.26×10-30esu. Its thermal properties were also determined in air.
Yaoting, Fan,Gang, Li,Zifeng, Li,Hongwei, Hou,Hairong, Mao
p. 217 - 224
(2007/10/03)

Preparation of a High Surface Area Nickel Electrode by Alloying and Dealloying in a ZnCl2-NaCl Melt
An electrochemical method of preparing a high surface area nickel electrode by NiZn alloy formation and subsequent dealloying in ZnCl 2-NaCl (60-40 mol %) at 450°C was studied. A nickel electrode was kept at 0.22 V vs. Zn in ZnCl2-NaCl(sat) where γ-NiZn alloy was formed, and then at 0.5 V where partial dealloying occurred to yield α-NiZn alloy. Scanning electron microscope observation showed that the microporous structure was formed on the surface. The roughness factor of a sample was determined to be 240 from the double layer capacitance obtained in the ac impedance measurement. Thickness, porosity, and pore size of the surface layer were estimated.
Katagiri,Nakata
p. C585-C590
(2008/10/08)

Synthesis and structural studies of binuclear platinum(II) complexes with a novel phosphorus-nitrogen-phosphorus ligand
The new pyridinediphosphinite ligand PONOP (1) was synthesized in one step from 2,6-pyridinedimethanol and diphenylchlorophosphane. Reaction of 1 with PtCl2(PhCN)2 led to the neutral homobimetallic complex [Pt2Cl4(PONOP)2] (2), where the benzonitriles have been substituted by the phosphorus atoms of 1. The X-ray structure of 2 revealed a metallamacrocycle where the pyridines remained free. Addition of 2 equiv of [Cu(MeCN)4](BF4) to 2 led to CuCl and to the binuclear dicationic complex [Pt2Cl2(PONOP)2](BF4)2 (3), where chloro ligands have been substituted by pyridine groups. Conversely, reaction of 3 with chloride anions gave back complex 2. Solid-state (X-ray) and solution (NMR) studies indicated that after the transformation of 2 into 3, the platinum centers were brought much closer and the pyridinediphosphinite ligand was stiffened. The methylene NMR protons of 3 were strongly deshielded, and the corresponding proton-phosphorus coupling constants followed a Karplus-type relationship.
Barloy, Laurent,Malaise, Gregory,Ramdeehul, Shailesh,Newton, Claire,Osborn, John A.,Kyritsakas, Nathalie
p. 2902 - 2907
(2008/10/08)

Empirical correlations involving calorimetric, thermogravimetric and infrared data for zinc halides adducts
The use of the non-isothermal Coats-Redfern method to obtain the activation energy values for the processes ZnX2·2hmpa(c) → ZnX2(c)+2hmpa(g) (X = Cl, Br, I and hmpa = hexamethylphosphoramide), by using thermogravimetric data, gave the values 44; 94 and 215 kJ mol-1 for the given sequence of halides. These values correlated to the standard molar enthalpy of formation in the condensed phase for the same sequence of adducts: - 1596, - 1532 and - 1408 kJ mol-1, respectively, providing the equation: ΔfH°m = 1.086 × Ea - 1639.738, which shows a linear correlation between the thermodynamic and kinetic parameters for such solid adducts. The IR spectroscopy data for a series of adducts of zinc halides with amides enabled the acquisition of an equation to estimate the mean metal-ligand bond enthalpy 〈D〉(M-L) values: the spectroscopic data were adjusted to the expression 〈D〉(M-L) = α + β + Δν, where αand β are related to Lewis acidity and basicity coordination features, respectively, and Δν is the difference between C=O or P=O stretching vibrations of the coordinated and uncoordinated ligands. This equation was applied for 15 adducts, showing a deviation less than 10% from the thermochemical values.
De Farias, Robson F.,Airoldi, Claudio,Scatena Jr., Hélio
p. 1677 - 1681
(2008/10/08)

Head-on versus side-on [5-5]bitrovacenes featuring benzene and naphthalene units as spacers: How π-stacking affects exchange coupling and redox splitting
The biradicals 1,8-di([5]trovacenyl)naphthalene (6), 1,5-di([5]trovacenyl)naphthalene (7), and 1,3-di([5]trovacenyl)benzene (8) and the monoradical 1-[5]trovacenylnaphthalene (9) have been prepared and studied by means of single-crystal X-ray diffraction
Elschenbroich, Christoph,Wolf, Matthias,Schiemann, Olav,Harms, Klaus,Burghaus, Olaf,Pebler, Jürgen
p. 5810 - 5819
(2008/10/08)

Organosilicon compound, a process for its preparation and its use
Organosilicon compounds of general formula (I) R1R2R3Si—R4—S—Zn—S—R4—SiR1R2R3??(I) wherein R1, R2, R independently, represent H, a halogen, alkyl or alkoxy and R4represents an alkylidene group, their preparation and their use in rubber mixtures.
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(2008/06/13)

Thermal and spectral studies of binary complexes of cyanodithioformate with transition metal ions
Binary complexes of the type [M(S2CCN)2] (M = Mn2+, Fe2+, Co2+, Ni2+, Cu2+ and Zn2+) have been synthesised from alcoholic solutions. They have been characterised using elemental analyses, IR, UV-VIS spectroscopy, magnetic susceptibility measurement and solution conductance data. In thermogravimetry (TG) studies, all these complexes exhibit a prominent weight loss step between 100 and 330 °C under a N2 atmosphere. Besides, a second weight loss step has also been observed beyond 800° C for the Mn2+, Fe2+ and Co2+ complexes, between 400 and 600 °C for Zn2+ complex and beyond 380 °C for Cu2+ complex. Broad differential thermal analysis (DTA) endotherms are observed corresponding to these weight loss steps. The first weight loss in the TG scan of the complexes follows a deceleratiory α-time curve with D3 mechanism for all complexes. The activation energy (Ea) for the thermal decomposition varies between 43 and 115 kJ/mol and removal of CS2 and/or CS have been suggested. Various decomposition parameters have been calculated.
Prasad, Rajendra,Kumar, Azad
p. 59 - 67
(2008/10/08)

Oxidative alkoxylation of zinc phosphide in alcoholic solutions of copper(II) chloride
Oxidative alkoxylation of Zn3P2 with the formation of valuable phosphoric and phosphorous acid esters occurred at a high rate and with a high selectivity in alcoholic solutions of CuCl2 under the action of oxygen at 30-60°C. Depending on the nature of the alcohol, two products were formed, namely, trialkyl phosphates (RO)3PO and dialkyl phosphites (RO)2HPO. Water favored the formation of dialkyl phosphates (RO)2(HO)PO. The kinetics and mechanism of the new catalytic reaction were studied, and the optimal conditions for conducting this reaction were found. The reaction proceeded in a topochemical mode by a separate redox mechanism.
Dorfman,Ibraimova,Polimbetova
p. 50 - 55
(2007/10/03)

Zinctellurido Clusters with Tellurido- or Tellurido- and Organyltellurolato Ligands. The Crystal Structures of {[Zn10Te(TePh)12(P(n)Pr3)4]2[Zn14Te13(tmeda)6][Fe(CO)4SiMe3]2}, [Zn16Te13(TePh)6(tmeda)5], [Zn(TePh)2(tmeda)], [Zn14Te13Cl2(tmeda)6].cntdot.[ZnCl2(tmeda)], [Zn14Te13(TeMes)(tmed
In the presence of P(n)Pr3 [(ZnCl)2Fe(CO)4(-)(tmeda)2] reacts with PhTeSiMe3 to form the crystalline {[Zn10Te4(TePh)12(P(n)Pr3)4]2[Zn14Te13(tmeda)6][Fe(CO)4SiMe3]2} (1). The use of PPh(n)Pr2 instead of P(n)Pr3 in DME, leads to the formation of the cluster [Zn16Te13(TePh)6(tmeda)5] (2). Reactions of ZnCl2 with PhTeSiMe3 and different amounts of TMEDA result in crystallisation of [Zn(TePh)2(tmeda)] (3) and [Zn14Te13Cl2(tmeda)6].cntdot.[ZnCl2(tmeda)] (4). Using MesTeSiMe3 instead of PhTeSiMe3 leads to [Zn14Te13(TeMes)(tmeda)6][Zn(TeMes)3] (5). The consequence of replacing TMEDA by DPPM is another new type of structure realized in the complex [Zn12Te9(TeMes)6(dppm)4] (6). The structures of 1-6 were obtained by X-ray single crystal structure analysis. 1: space group R3- (No.148), Z=3, a=b=2106,4(3) pm, c=7381,8(2) pm, 2: space group C2/c (No.15), Z=4, a=3327,8(7) pm, b=1784,8(4) pm, c=2321,7(5) pm, β=118,32(3)°, 3: space group P21/n (No.14), Z=4, a=1099,3(2) pm, b=1324,5(3) pm, c=1576,9(3) pm, β=109.69(3)°; 4: space group P1- (No.2), Z=2, a=1484,1(3) pm, b=2094,0(4) pm, c=2508,5(5) pm, α=91,15(3)°, β=97,29(3)°, γ=105,69(3)°; 5: space group P21/c (No.14), Z=4, a=1368,4(3) pm, b=4279,3(9) pm, c=2469,6(5) pm, β=102,73(3)°; 6: space group P21/n (No.14), Z=4, a=2001,1(4) pm, b=4141,8(8) pm, 2857,4(6) pm, β=101,77(3)°.
Pfistner, Heike
(2008/10/08)

A low temperature chlorination-volatilization process for the treatment of chalcopyrite concentrates
Chlorination of two chalcopyrite concentrates with Cl2 + N2 was investigated under isothermal conditions in the temperature range of 20-750°C using boat experiments. The effects of gas flow rate, chlorine content of the gas mixture and residence time on the reaction rate were also investigated. Scanning electron microscopy (SEM), X-ray diffraction (XRD), and chemical analysis are used for the physico-chemical characterization of the reaction products. The chlorination of chalcopyrite concentrates started at room temperature generating chlorides of Cu, Pb, Zn, Fe, and S. The reaction of chlorine with sulfides is almost complete at about 300°C and the overall reaction is exothermic. At this temperature, the valuable metal chlorides were concentrated in the chlorination residues, while those of iron and sulfur were volatilized. A flow sheet is proposed for the selective chlorination of chalcopyrite concentrates at low temperatures. Such flow sheet could be considered as an attractive route for the sulfide concentrates' treatment without SOx emissions. It could be also regarded as energy saving with respect to the classical pyrometallurgical routes.
Kanaria,Gaballaha,Allain
p. 75 - 93
(2008/10/08)

Synthesis and crystal structure of Ba6ZnIn2Cl20
Colourless single crystals of Ba6ZnIn2Cl20 are obtained from a 6:3:2 molar mixture of BaCl2, ZnCl2 and InCl3 at 420 °C in a Pyrex ampoule. It crystallizes with the monoclinic space group P21/c (Z = 4) with a = 1957.8(2), b= 1014.69(8), c = 1778.7(2) pm, β= 110.94(1)°, in a new structure. Zn2+ is surrounded tetrahedrally and In3+ octahedrally by chloride ions. Half of the [InCl6] octahedra are isolated from each other, the other half shares common edges to form [In2Cl10] double octahedra. Ba2+ has coordination numbers of eight and nine. There are chloride ions that do not belong to Zn2+ or In3+ so that the formula may be written as Ba12Cl10[ZnCl4]2[InCl 6]2[In2Cl10].
Masselmann, Soenke,Meyer, Gerd
p. 269 - 273
(2008/10/08)

Unexpected Competition between Vanadium and Zinc in the Synthesis of Sterically Bulky Metallocenes
Attempts to form (Cp3i)2V and (Cp4i)2V (Cpni = C5(iPr)nH5-n) from the reaction of zinc-reduced VCl3 and K[Cpni] in THF at room temperature produces the corresponding zincocenes (Cp3i)2Zn and (Cp4i)2Zn instead. In refluxing THF, the same reactions generate the expected (Cpni)2V vanadocenes. The latter are also formed from the reaction of aluminum-reduced VCl3 with K[Cpni] at room temperature. Reaction of 3 equiv of K[Cp3i] or K[C5Ph4H] with VCl3 in THF produces (Cp3i)2V and (C5Ph4H)2V, respectively, whereas the equivalent reaction with K[Cp4i] generates (Cp4i)2VCl. These experiments suggest that zincocenes are intermediates whenever vanadocenes are synthesized from zinc-reduced VCl3 but that zinc complexes will be isolated only when certain cyclopentadienyl rings and temperature conditions are used. A single-crystal X-ray diffraction study of (Cp3i)2V found the metal to reside on a crystallographically imposed inversion center, with an average V-C(ring) distance of 2.274-(9) A?; the isopropyl groups orient themselves to minimize unfavorable steric interactions between the rings.
Overby, Jason S.,Jayaratne, Kumudini C.,Schoell, Nathan J.,Hanusa, Timothy P.
p. 1663 - 1667
(2008/10/08)

Preparation of α-tocopherol or α-tocopheryl acetate by reacting trimethylhydroquinone and phytol or isophytol, with recycling of the zinc halide condensation catalyst
A process for preparing α-tocopherol or α-tocopheryl acetate by reacting 2,3,5-trimethylhydroquinone with isophytol or phytol in the presence of a zinc halide condensation catalyst and a proton donor in a solvent with or without subsequent esterification with acetic anhydride, which comprises A. carrying out the reaction in a nonpolar solvent which is only slightly water-miscible, if at all and B. introducing the required zinc halide into the reaction in the form of a mixture of from 1 to 4 mol of water per mol of zinc halide. The possibility of introducing the zinc halide required in the process according to the invention in the form of a mixture of zinc halide and water which can be readily handled and metered at from 50 to 200° C. without impairing the yield and purity of the tocopherol opens the way to an advantageous recycling of the zinc halide after the reaction by separating off or extracting and recycling the zinc halide in the form of a from 60 to 90% strength by weight solution or pumpable magma.
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(2008/06/13)