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Summary The synthesis and coordination behaviour of 1-allylbenzotriazole (ABT), containing both -donating heterocyclic ring nitrogen(s) and a -bonding olefinic group, has been studied by complexation with CoII, NiII, CuII, CuI and AgI salts. The solid complexes M(ABT)2X2 (M=Co, Ni or Cu and X=a counterion) and M(ABT)X (M=Cu or Ag and X=Br, I, or NO3) have been characterised by1H-n.m.r. (representative CuI species) and other physical data. Different modes coordination for the title ligand have been proposed based upon i.r. data which indicate the participation of a -donating ring nitrogen only in complexes with bivalent metal salts, and the involvement of both the ring nitrogen and the allylic olefinic component in bonding to a monovalent metal ion.1H-n.m.r. data are qualitatively commensurate with participation of the allyl group in monovalent metal complexes. 相似文献
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Summary Cobalt(II), nickel(II) and copper(II) complexes of 3, 5-dimethyl-1-(4, 6-dimethyl-2-pyrimidyl)pyrazole (DPymPz) have been synthesized and characterized. Magnetic and electronic spectral features show that both [M(DPymPz)2X2]·nH2O [M=cobalt(II) or nickel(II), X=Cl, Br, I, SCN, NO3, ClO4 or BF4 andn=0 or 2] and [Cu(DPymPz)X2(H2O)2] (X=Cl, Br or SCN) are essentially octahedral species. The i.r. spectra indicate that DPymPz is a neutral bidentate ligand being the pyrazolyl and one pyrimidyl ring nitrogen. The X is bonded to the central metal ion in a majority of the complexes.Part 5: N. Saha and D. Mukherjee,Polyhedron,5, 1317 (1986). 相似文献
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4-(N,N-diethylamino)benzaldehyde thiosemicarbazone(DEABT) is proposed as a sensitive and selective analytical reagent for the spectrophotometric determination of palladium(II). The reagent reacts with palladium (II) in a potassium hydrogen phthalate-hydrochloric acid buffer of pH 3.0, to form a yellow complex. Beer's law is obeyed in the concentration range up to 3.60 microgmL(-1). The optimum concentration range for minimum photometric error as determined by Ringbom plot method is 0.36 - 3.24 microg mL(-1). The yellow Pd(II)-DEABT complex shows a maximum absorbance at 408 nm, with molar absorptivity of 3.33 x 10(4) dm3 mol(-1) cm(-1) and Sandell's sensitivity of the complex from Beer's data, for D = 0.001, is 0.0032 microg cm(-2). The composition of the Pd(II)-DEABT complex is found to be 1:2 (M:L). The interference of various cations and anions in the method were studied. The proposed method was successfully used for the determination of Pd(II) in alloys, catalysts, complexes and model mixtures with a fair degree of accuracy. 相似文献
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Bera Pulakesh Saha Nityananda Kumar Sanjay Banerjee D. Bhattacharya R. 《Transition Metal Chemistry》1999,24(4):425-430
New iron(III) complexes of 5-methyl-3-formylpyrazole thiosemicarbazone (HMPzTS) and 5-methyl-3-formylpyrazole-4-phenylthiosemicarbazone (HMPzPTS), namely [Fe(MPzTS)2]X and [Fe(MPzPTS)2]X respectively, where X=Cl, NO3, SCN and ClO4, have been synthesised and physico-chemically characterised by magnetic measurements (polycrystalline state), electronic, i.r., e.s.r. and Mössbauer spectra. All are cationic complexes containing two monoprotonic tridentate ligands with NNS donor sites and an anionic counterpart; they behave as 1:1 electrolytes in MeOH/DMF. Coordination to central iron(III) via the pyrazolyl nitrogen (2N), the azomethine nitrogen and the thiolato sulphur atom is confirmed in the complexes from i.r. data. E.s.r. data (RT & LNT) reveal the presence of a spin-paired iron(III) cation with d2
xyd2
yzd1
xy configuration. The 57Fe Mössbauer spectral data (RT) are commensurate with the presence of two iron(III) spin states, the percentage of each being dependent upon the counterion of the species. 相似文献
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A selective complexometric method for the determination of mercury(II) in the presence of associated metal ions is reported,
based on the selective masking ability of 2-mercaptopropionylglycine (MPGH2) towards mercury. Mercury, along with other associated metal ions, is first complexed with excess of EDTA and the surplus
EDTA is back titrated at pH 5–6 (hexamine buffer) with standard zinc sulfate solution using xylenol orange as indicator. An
aqueous 1% solution of MPGH2 is then added to displace EDTA selectively from the Hg-EDTA complex and the released EDTA is titrated with the same standard
zinc sulfate solution. Reproducible and accurate results are obtained for 4–85 mg of mercury with a relative error of ≤ 0.26%
and coefficient of variation not exceeding 0.42%. The interferences of various cations and anions are studied. The method
is used for the analysis of mercury in its complexes and alloy samples.
Received August 30, 2000. Revision January 15, 2001. 相似文献
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Certain recent semi‐classical theories of spin‐half quantum plasmas are examined with regard to their internal consistency, physical applicability and relevance to fusion, astrophysical and condensed matter plasmas. It is shown that the derivations and some of the results obtained in these theories are internally inconsistent and contradict well‐established principles of quantum and statistical mechanics, especially in their treatment of fermions and spin. Claims of large semi‐classical effects of spin magnetic moments that could dominate the plasma dynamics are found to be invalid both for single‐particles and collectively. Larmor moments dominate at high temperature while spin moments cancel due to Pauli blocking at low temperatures. Explicit numerical estimates from a variety of plasmas are provided to demonstrate that spin effects are indeed much smaller than many neglected classical effects. The analysis presented suggests that the aforementioned ‘Spin Quantum Hydrodynamic’ theories are not relevant to conventional laboratory or astrophysical plasmas. (© 2015 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim) 相似文献
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Empirical model potentials are found to be very useful for generating most competitive minima of large water clusters, whereas correlated (e.g. second order-Møller–Plesset perturbation (MP2) theory or higher) calculations are necessary for predicting their accurate energetics and vibrational features. The present study reports the structures and energetics of (H2O)32 clusters at MP2 level using aug-cc-pvDZ basis set, starting with low-lying structures generated from model potentials. Such high-end and accurate calculations are made feasible by the cost-effective fragment-based molecular tailoring approach (MTA) in conjunction with the grafting procedure. The latter is found to yield electronic energies with a sub-millihartree accuracy with reference to their full calculation counterparts. The vibrational spectra of nine low-lying (H2O)32 isomers are obtained from the corresponding MTA-based Hessian matrix. All these low-lying isomers show almost similar spectral features, which are in fair agreement with the experiment. The experimental spectrum of (H2O)32 is thus better understood from the vibrational features of this set of very closely spaced isomers. The present case study of (H2O)32 clearly demonstrates the efficacy in obtaining accurate structures, energetics and spectra at correlated level of theory by combining model potential-based structures with fragmentation methods. 相似文献