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  • 1.
    Gowda, Vasantha
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering. NMR Research Unit, University of Oulu.
    Sarma, Bipul
    Department of Chemical Sciences, Tezpur University.
    Laitinen, Risto S.
    Laboratory of Inorganic Chemistry, University of Oulu.
    Larsson, Anna-Carin
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Ivanov, Alexander V.
    Institute of Geology and Nature Management, Far Eastern Branch of the Russian Academy of Sciences .
    Iuga, Dinu
    Department of Physics, Warwick University.
    Lantto, Perttu
    NMR Research Unit, University of Oulu.
    Antzutkin, Oleg
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering. Department of Physics, Warwick University.
    Structural insights into the polymorphism of bismuth(III) di-n-butyldithiocarbamate by X-ray diffraction, solid-state (13C/15N) CP-MAS NMR and DFT calculations2017In: Polyhedron, ISSN 0277-5387, E-ISSN 1873-3719, Vol. 129, p. 123-132Article in journal (Refereed)
    Abstract [en]

    Two crystalline polymorphs of a binuclear tris(di-n-butyldithiocarbamato)bismuth(III) complex, I and II, with an empirical formula of [Bi{S2CN(n-C4H9)2}3] were synthesised and characterised by X-ray diffraction (XRD), solid-state NMR and density functional theory (DFT) calculations. At the supramolecular level, these mononuclear molecular units interact in pairs via secondary Bi⋯S bonds, yielding binuclear formations of [Bi2{S2CN(n-C4H9)2}6]. The polymorph I () contains two isomeric non-centrosymmetric binuclear molecules of [Bi2{S2CN(n-C4H9)2}6], which are related to each other as conformers, therefore having four structurally inequivalent bismuth atoms and twelve inequivalent dithiocarbamate ligands. In contrast, the structurally simpler polymorph II (P21/n) exists as a single molecular form of the corresponding centrosymmetric binuclear formation, comprising two structurally equivalent bismuth atoms and three structurally different dithiocarbamate groups. The polymorphs I and II were found to be interconvertible by altering the solvent system during the recrystallisation process. Sun et al. (2012) has reported a crystalline form of the title compound which resembles, but is not identical with, polymorph II. Experimental solid-state 13C and 15N cross-polarisation (CP) magic-angle-spinning (MAS) NMR spectra of both polymorphs I and II were in accord with the direct structural data on these complexes. Assignments of the resonance lines in the solid-state 13C and 15N NMR spectra were assisted by chemical shift calculations of the crystals using periodic DFT.

  • 2.
    Ivanov, Alexander V.
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Antzutkin, Oleg
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Isomorphism of bis(diethyldithiocarbamato)zinc(II) adduct with pyridine, [Zn(Py)(EDtc)2]: hysteresis in the reaction of the adduct formation2002In: Polyhedron, ISSN 0277-5387, E-ISSN 1873-3719, Vol. 21, no 27-28, p. 2727-3731Article in journal (Refereed)
    Abstract [en]

    The structure of the polycrystalline adduct bis(diethyldithiocarbamato)-pyridine zinc(II) depends on the pathway of physico-chemical conditions during the preparation procedure, as was revealed by solid state 15N CP/MAS spectroscopy in good correlation with known single crystal X-ray diffraction structures of this adduct. Two isomorphs of the adduct, namely α-[Zn(Py)(S2CNEt2)2] and β-[Zn(Py)(S2CNEt2)2], are the two molecules in the asymmetric unit of a single crystal (or polycrystalline) sample that can be obtained by recrystallization from toluene of the equimolar solution of the initial diethyldithiocarbamate zinc(II) complex and pyridine. The third isomorph, γ-[Zn(Py)(S2CNEt2)2], can be obtained by recrystallization from pure pyridine of the diethyldithiocarbamate zinc(II) complex, or by its equimolar absorption of pyridine, or by desorption of pyridine from the clathrated adduct, [Zn(Py)(S2CNEt2)2]·Py. Finally, the γ-[Zn(Py)(S2CNEt2)2] isomorph recrystallizes from the melt into α/β-isomorphs of the adduct.

  • 3.
    Ivanov, Alexander V.
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Mitrofanova, Valentina I.
    Russian Adademy of Sciences.
    Kritikos, Mikael
    Stockholm University.
    Antzutkin, Oleg
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Rotation isomers of bis(diethyldithiocarbamato)zinc(II) adduct with pyridine, Zn(EDtc)(2)center dot Py: ESR, C-13 and N-15 CP/MAS NMR and single-crystal X-ray diffraction studies1999In: Polyhedron, ISSN 0277-5387, E-ISSN 1873-3719, Vol. 18, no 15, p. 2069-2078Article in journal (Refereed)
    Abstract [en]

    The adduct of bis(diethyldithiocarbamato)zinc(II) with pyridine, Zn(EDtc)2·Py, was prepared and studied by means of ESR (63Cu2+ and 65Cu2+ were used as spin labels), solid-state natural abundance 13C and 15N CP/MAS NMR spectroscopy and single-crystal X-ray diffraction data analysis. Two rotation isomers of the adduct were unambiguously determined by these three independent methods. It was found that these two isomers have different orientations of the pyridine ring about the N(Py)-Zn axis. The acute angles of the plane of the pyridine molecules relative to the most weak Zn-S bond are equal to 45.6 and 52.7° in the different isomers. Adduct molecules adopt a geometry which is intermediate between the square pyramidal (C4v) and the trigonal bipyramidal (D3h). All ESR and NMR resonances of Zn(EDtc)2·Py were assigned

  • 4.
    Ivanov, Alexander V.
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Rody, Tatyana
    Amur State University, Blagoveshchensk, Russian Federation.
    Antzutkin, Oleg
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Structural organisation of [Ni(II)--Me(II)--Dtc] (Me = Zn, Cd, Hg) Dithiocarbamate complexes: ESR, 13C and 15N CP/MAS NMR studies1998In: Polyhedron, ISSN 0277-5387, E-ISSN 1873-3719, Vol. 17, no 18, p. 3101-3109Article in journal (Refereed)
    Abstract [en]

    Magnetically diluted systems of dithiocarbamate complexes of the type 63,65Cu/[Ni(II)--Me(II)--Dtc] (Me = Zn, Cd, Hg; Dtc = MDtc (dimethyl-) or EDtc (diethyldithiocarbamate)), which model the structural heterogeneity on the local, molecular and supramolecular levels, have been prepared and studied by means of ESR and solid state 13C and 15N CP/MAS NMR spectroscopy.

  • 5.
    Ivanov, Maxim A.
    et al.
    Institute of Geology and Nature Management, Far Eastern Branch of the Russian Academy of Sciences.
    Larsson, Anna-Carin
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Ivanov, Alexander V.
    Institute of Geology and Nature Management, Far Eastern Branch of the Russian Academy of Sciences .
    Gerasimenko, Andrey V.
    Institute of Chemistry, Far Eastern Branch of the Russian Academy of Sciences.
    Merkulov, Eugene B.
    Institute of Chemistry, Far Eastern Branch of the Russian Academy of Sciences.
    An example of S,S′-bidentate coordination mode of the dithiophosphate group in the heteroleptic tetraphenylantimony(V) complex, [Sb(C6H5)4{S2P(O-cyclo-C6H11)2}]: multinuclear (13C, 31P) CP MAS NMR, single-crystal X-ray diffraction studies and thermal behaviour2017In: Polyhedron, ISSN 0277-5387, E-ISSN 1873-3719Article in journal (Refereed)
    Abstract [en]

    Crystalline O,O′-di-cyclo-hexyl dithiophosphate (Dtph) tetraphenylantimony(V) complex, [Sb(C6H5)4{S2P(O-cyclo-C6H11)2}] (1) was prepared and studied by means of heteronuclear (31C, 31P) CP MAS NMR spectroscopy, single-crystal X-ray diffraction and thermal analysis. To characterise quantitatively the phosphorous site in complex 1, 31P chemical shift anisotropy parameters (δaniso and η) were successfully defined from spinning sideband manifolds in experimental MAS NMR spectra. The positive sign of the calculated δaniso unambiguously reveals the terminal S,S′-chelating structural function of di-cyclo-hexyl Dtph groups; whereas, the minimal δ22 value among all presently known tetraphenylantimony(V) dialkyl Dtphs points out to extremely low value of the S–P–S angle. Distorted octahedral molecular structure comprising Dtph ligand with S,S′-bidentate chelating coordination mode has been established for the prepared complex. Therefore, in comparison with tetraphenylantimony(V) Dtph complexes containing S-unidentately coordinated Dtph groups, terminally chelating di-cyclo-hexyl Dtph ligand of crystalline complex 1 expectedly exhibits the smallest S–P–S angle of 113.49°. The thermal behaviour of this compound was studied by means of thermal analysis technique as a combination of TG and DSC. The thermal decomposition involves the organic and inorganic parts of 1, yielding almost equal quantities of Sb2S3 and SbPO4, which were identified using powder XRD.

  • 6.
    Rodina, Tatyana A.
    et al.
    Institute of Geology and Nature Management, Far East Branch, Russian Academy of Sciences, Blagoveshchensk.
    Ivanov, Alexander V.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Gerasimenko, Andrey V.
    Institute of Chemistry, Far Eastern Branch of the Russian Academy of Sciences.
    Loseva, Olga V.
    Institute of Geology and Nature Management, Far East Branch, Russian Academy of Sciences, Blagoveshchensk.
    Antzutkin, Oleg
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Sergienko, Valentin I.
    Institute of Chemistry, Far Eastern Branch of the Russian Academy of Sciences.
    Fixation modes of gold(III) from solutions using cadmium(II) dithiocarbamates: Preparation, supramolecular structure and thermal behaviour of polynuclear and heteropolynuclear gold(III) complexes: bis(N,N-dialkyldithiocarbamato-S,S’)gold(III) polychlorometallates, [Au(S2CNR2)2]nX (n =1: X = [AuCl4]–; n = 2: X = [CdCl4]2–, [Cd2Cl6]2–)2012In: Polyhedron, ISSN 0277-5387, E-ISSN 1873-3719, Vol. 40, no 1, p. 53-64Article in journal (Refereed)
    Abstract [en]

    Four novel heteropolynuclear and polynuclear complexes of the general formulae [Au(S2CNR2)2]2X (X = [CdCl4]2-, R = CH3 (1); X = [Cd2Cl6]2-, R = C3H7 (2)) and [Au(S2CNR2)2][AuCl4] (R = iso-C3H7 (3); R = iso-C4H9 (4)) were prepared using heterogeneous reactions between appropriate freshly precipitated binuclear cadmium(II) dialkyl dithiocarbamates and AuCl3 in 2 M hydrochloric acid. The isolated complexes were studied by 13C CP/MAS NMR spectroscopy, single-crystal X-ray diffraction and simultaneous thermal analysis (STA) under an argon atmosphere. In all molecular structures (1–4), one of the gold atoms coordinates two dialkyl dithiocarbamate ligands in the S,S’-bidentate mode, forming a square-planar coordination polygon [AuS4], while the other gold atom (in 3 and 4) has four neighbouring chlorine atoms [AuCl4]. At the supramolecular level, compounds 1 and 2 comprise binuclear cations, [Au2{S2CN(CH3)2}4]2+ and polynuclear chains, ([Au{S2CN(C3H7)2}2]+)n in a combination with [CdCl4]2- and [Cd2Cl6]2- anions, respectively. Unexpected structural distinctions at the supramolecular level were discovered for the chemically related compounds 3 and 4. In these ionic complexes, there are either cationic trinuclear formations, {[Au{S2CN(iso-C3H7)2}2]2[AuCl4]}+, or polynuclear chains, ([Au{S2CN(iso-C4H9)2}2]+)n, both combined with [AuCl4]– anions, in the structural basis of compounds 3 and 4, respectively.

  • 7.
    Rodina, Tatyana A.
    et al.
    Institute of Geology and Nature Management, Far East Branch, Russian Academy of Sciences, Blagoveshchensk.
    Ivanov, Alexander V.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Gerasimenko, Andrey V.
    Institute of Chemistry, Far Eastern Branch of the Russian Academy of Sciences, 690022, Vladivostok.
    Lutsenko, Irina A.
    Institute of Geology and Nature Management, Far East Branch, Russian Academy of Sciences, Blagoveshchensk.
    Ivanov, Maxim A.
    Institute of Geology and Nature Management, Far East Branch, Russian Academy of Sciences, Blagoveshchensk.
    Hanna, John V.
    Department of Physics, Warwick University, Coventry.
    Antzutkin, Oleg
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Sergienko, Valentin I.
    Institute of Chemistry, Far Eastern Branch of the Russian Academy of Sciences, 690022, Vladivostok.
    Crystalline O,O’-di-sec-butyl and O,O’-diethyl dithiophosphate platinum(II) complexes: Synthesis, 13C and 31P CP/MAS NMR, single crystal X-ray diffraction studies and thermal behaviour2011In: Polyhedron, ISSN 0277-5387, E-ISSN 1873-3719, Vol. 30, no 13, p. 2210-2217Article in journal (Refereed)
    Abstract [en]

    Crystalline bis(O,O’-di-sec-butyldithiophosphato)platinum(II) was prepared and studied by means of 31P, 13C CP/MAS NMR spectroscopy and single-crystal X-ray diffraction. The unit cell of the platinum(II) compound is comprised of one centrosymmetric mononuclear molecule [Pt{S2P(O-sec-C4H9)2}2], in which the dithiophosphate groups display structural equivalence in both 31P NMR and XRD data. A pair of the dithiophosphate ligands exhibit the same S,S’-bidentate chelating structural function and form two planar four-membered chelate rings, [PtS2P], in this molecule. The planar configuration of the [PtS4] chromophore in structure 1 is governed by the dsp2-hybrid state of platinum(II). The structural states of the dithiophosphate groups in two different samples of complex 1 (one crystallised from ethanol and the other one precipitated from an aqueous solution) are all characterised by almost rhombic 31P chemical shift tensors. The observed essential dispersion of the 31P NMR chemical shift is caused by a coexistence of six optical isomers of molecule 1. The thermal behaviour of this compound was studied by means of simultaneous thermal analysis (a combination of TG and DSC) under an argon atmosphere. The thermal behaviour shows that the mass of 1 is lost in three steps, involving successive thermal decompositions of the organic and inorganic parts of this compound with platinum(II) dithio-meta-phosphate and reduced metallic platinum as the intermediate and the final products, respectively.

  • 8. Rusanova, Daniela
    et al.
    Pike, Kevin J.
    Lucas Heights Research Laboratories.
    Persson, Ingmar
    Swedish University of Agricultural Sciences.
    Dupree, Ray
    University of Warwick.
    Lindberg, Mats
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Hanna, John V.
    Lucas Heights Research Laboratories.
    Antzutkin, Oleg
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Forsling, Willis
    Solid-state static 65Cu and 31P CP/MAS NMR, and liquid-state EXAFS studies on copper(I) O,O′-dialkyldithiophosphate cluster compounds: formation of the copper(I) O,O′-di-iso-amyldithiophosphate cluster compound on the surface of synthetic chalcocite2006In: Polyhedron, ISSN 0277-5387, E-ISSN 1873-3719, Vol. 25, no 18, p. 3569-3580Article in journal (Refereed)
    Abstract [en]

    Polycrystalline octa-nuclear copper(I) O,O′-di-i-propyl- and O,O′-di-i-amyldithiophosphate cluster compounds, {Cu8[S2P(OR)2]6(μ8-S)} where R = iPr and iAm, were synthesized and characterized by 31P CP/MAS NMR at 8.46 T and static 65Cu NMR at multiple magnetic field strengths (7.05, 9.4 and 14.1 T). The symmetries of the electronic environments around the P sites were estimated from the 31P chemical shift anisotropy (CSA) parameters, δaniso and η. Analyses of the 65Cu chemical shift and quadrupolar splitting parameters for these compounds are presented with the data being compared to those for the analogous octa-nuclear cluster compounds with R = nBu and iBu. The 65Cu transverse relaxation for the copper sites in {Cu8[S2P(OiPr)2]6(μ8-S)} and {Cu8[S2P(OiAm)2]6(μ8-S)} was found to be very different, with a relaxation time, T2, of 590 μs (Gaussian) and 90 μs (exponential), respectively. The structures of {Cu4[S2P(OiPr)2]4} and {Cu8[S2P(OiPr)2]6(μ8-S)} cluster compounds in the liquid- and the solid-state were studied by Cu K-edge EXAFS. The disulfide, [S2P(OiAm)2]2, was obtained and characterized by 31P{1H} NMR. The interactions of the disulfide and of the potassium O,O′-di-i-amyldithiophosphate salt with the surfaces of synthetic chalcocite (Cu2S) were probed using solid-state 31P NMR spectroscopy and only the presence of copper(I) dithiophosphate species with the {Cu8[S2P(OiAm)2]6(μ8-S)} structure was observed.

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