| 1. |
- Novikova, E. V., et al.
(författare)
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Principles of the Construction of Polymer Structures, Heteronuclear (13C, 15N) CP-MAS NMR, and Thermal Behavior of Heteroleptic Bismuth(III) Complexes of the General Composition [Bi(S2CNR2)2X] (X = NO3, Cl)
- 2019
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Ingår i: Russian journal of coordination chemistry. - : Springer. - 1070-3284 .- 1608-3318. ; 45:10, s. 695-705
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Tidskriftsartikel (refereegranskat)abstract
- The crystalline heteroleptic bismuth(III) complexes, [Bi{S2CN(iso-C4H9)2}2(NO3)] (I) and [Bi{S2CN(C3H7)2}2Cl] (II), are isolated in preparative yields. Both compounds form 1D polymer structures and are characterized by X-ray diffraction analysis (CIF files CCDC nos. 1877115 (I) and 1876364 (II)) and (13C, 15N) CP-MAS NMR spectroscopy. The coordination mode of each of the dialkyldithiocarbamate ligands is S,S′-anisobidentately terminal. The inorganic anions performing the μ2-bridging function participate in the binding of the adjacent metallic atoms to form zigzag polymer chains. A new mode of bismuth(III) binding involving all oxygen atoms (O,O'-anisobidentate coordination to each adjacent bismuth atom) is found for the bridging nitrate groups in compound I. The bismuth atoms in the studied compounds are characterized by the eightfold [BiS4O4] (I) or sixfold [BiS4Cl2] (II) environment. The thermal behavior of the synthesized complexes is characterized by the data of simultaneous thermal analysis, using parallel recording of thermogravimetry and differential scanning calorimetry curves. In both cases, Bi2S3 is the only final product of the thermal transformations of compounds I and II.
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| 2. |
- Loseva, O.V., et al.
(författare)
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Tetranuclear heteroleptic mercury(ii) complexes of the composition [Hg4(S2CNPr2)6(NO3)2] and [Hg4(S2CNPr2)4Cl4] : structural organization, principles of construction of supramolecular polymeric chains, and thermal behavior
- 2019
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Ingår i: Russian chemical bulletin. - : Springer. - 1066-5285 .- 1573-9171. ; 68:4, s. 782-792
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Tidskriftsartikel (refereegranskat)abstract
- New heteroleptic mercury(ii) complexes [Hg4(S2CNPr2)6(NO3)2] (1) and [Hg4(S2CNPr2)4Cl4] (2) were synthesized and characterized by single-crystal X-ray dif raction and 13C and 15N MAS NMR spectroscopy. In these complexes, the metal atoms are linked in pairs by bridging dipropyldithiocarbamate ligands (Pr2Dtc) to form tetranuclear cations and molecules. The further structural organization of compound 1 to the polymeric chains [Hg4(S2CNPr2)6(NO3)2]n occurs due to the linking of [Hg4(S2CNPr2)6]2+ cations by pairs of bridging nitrate groups. The formation of the supramolecular polymeric structure of 2 is determined by pairwise secondary Hg⋯Cl bonds between the cyclic [Hg4(S2CNPr2)4Cl4] molecules, in which the central eight-membered metallocycle [Hg4S4] adopts a distorted chair conformation. The thermal behavior of compounds 1 and 2 was studied by simultaneous thermal analysis.
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| 3. |
- Korneeva, E.V., et al.
(författare)
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Binding of gold(iii) with silver(i) dipropyldithiocarbamate : supramolecular self-assembly (role of secondary Au…S and Ag…S bonds) and thermal behavior of the ionic-polymer complex ([Au(S2CNPr2)2][AgCl2])n
- 2019
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Ingår i: Russian chemical bulletin. - : Springer. - 1066-5285 .- 1573-9171. ; 68:1, s. 40-47
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Tidskriftsartikel (refereegranskat)abstract
- The double ionic-polymer complex ([Au(S2CNPr2)2][AgCl2])n (1) was prepared as an individual fixation form of gold(III) from NaCl solutions with silver(I) dipropyldithiocarbamate and was characterized by single-crystal X-ray diffraction and 13C magic-angle spinning (MAS) NMR spectroscopy. The structure of 1 comprises two nonequivalent centrosymmetric complex cations [Au(S2CNPr2)2]+ (A and B) and the discrete linear anion [AgCl2]–. Gold(III) cations are linked by pairs of unsymmetrical secondary Au…S bonds to form linear supramolecular chains (…A…B…)n. Neighboring cations are additionally linked by [AgCl2]– anions via secondary Ag…S and Cl…S bonds, the anions being involved in the overall stabilization of the supramolecular structure. The cation–anion interactions lead to a distortion of the linear configuration of the [AgCl2]– anion. The character of thermolysis of 1 accompanied by quantitative regeneration of bound Au and Ag was established by simultaneous thermal analysis.
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| 4. |
- Korneeva, E.V., et al.
(författare)
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Crystalline nickel(II) di-i-amyl dithiophosphate, [Ni{S2P(O-i-C5H11)2}2] : Preparation, structure, heteronuclear (13C, 31P) CP/MAS NMR spectra, and thermal behavior
- 2017
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Ingår i: Russian journal of coordination chemistry. - : Springer. - 1070-3284 .- 1608-3318. ; 43:4, s. 223-231
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Tidskriftsartikel (refereegranskat)abstract
- The crystalline nickel(II) di-i-amyl) dithiophosphate (Dtph), [Ni{S2P(O-i-C5H11)2}2] (I) was isolated on a preparative scale and characterized by 13C, 31P MAS NMR, and X-ray diffraction (CIF file CCDC no. 1469369). The χ2-statistic diagrams were constructed from full 31P CP/MAS NMR spectra for calculating the 31P chemical shift anisotropy: δaniso = δzz–δiso and the asymmetry parameter η = (δyy–δxx)/(δzz–δiso). The key structural unit of I is the centrosymmetric [Ni{S2P(O-i-C5H11)2}2] molecule in which the nickel atom coordinates two Dtph ligands in the isobidentate fashion. In molecule I, each carbon, oxygen, and sulfur atom is statistically disordered over two sites with equal occupancies. However, the disorder does not affect nickel and phosphorus. These results were interpreted as the presence in I of two [Ni{S2P(O-i-C5H11)2}2] molecules rotated through 21.0(1)° (the angle between the [NiS4] chromophore planes) relative to each other around the bisecting P–Ni–P axis passing through both four-membered [NiS2P] rings. The two molecules occupy crystal lattice sites with equal probabilities. The thermal behavior of I was studied by simultaneous thermal analysis under argon. The course of the thermal destruction of the complex was established, nickel pyrophosphate (Ni2P2O7) was identified as the final product of thermal transformations.
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| 5. |
- Loseva, Olga V., et al.
(författare)
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Two structural types of dithiocarbamato-chlorido complexes of mercury(II): Preparation, supramolecular self-assembly, solid-state 13C and 15N NMR characterisation and thermal behaviour of pseudo-polymeric compounds of [Hg2(S2CNBu2)2Cl2] and [Hg4(S2CNiBu2)6][Hg2Cl6]
- 2022
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Ingår i: Inorganica Chimica Acta. - : Elsevier. - 0020-1693 .- 1873-3255. ; 533
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Tidskriftsartikel (refereegranskat)abstract
- Two new crystalline dithiocarbamato-chlorido complexes of mercury(II), [Hg2{S2CN(C4H9)2}2Cl2] (1) and [Hg4{S2CN(iso-C4H9)2}6][Hg2Cl6] (2), have been prepared and chemically identified by solution (1H, 13C) NMR and solid-state (13C, 15N) CP-MAS NMR and FT-IR spectroscopy. The crystal, molecular and supramolecular structures of these compounds were established using single-crystal X-ray diffraction (XRD) analysis. The obtained complexes reveal two principally different types of structural organisation. In the structure of the former neutral complex, there are two isomeric doubly-bridged binuclear molecules [Hg2(S2CNBu2)2Cl2] (‘A’ and ‘B’), whereas the latter compound comprises two ionic structural moieties: the tetranuclear cation [Hg4(S2CNiBu2)6]2+ and the binuclear anion [Hg2Cl6]2−. In both ionic units, pairs of iBu2Dtc or chloride ligands, which perform a bridging structural function, combine with neighbouring mercury atoms. In turn, intermolecular/interionic secondary interactions Hg···S/Hg···Cl are involved in the formation of supramolecular structures of complexes 1/2, yielding pseudo-polymeric chains of (···‘A’···‘B’···)n/(···[Hg4(S2CNiBu2)6]···[Hg2Cl6]···)n, which exhibit alternation of isomeric molecules of 1/ionic moieties of 2 along their lengths. Despite the significant structural difference between the above complexes, we established, using simultaneous thermal analysis (STA), that both exhibit very similar thermal behaviour. Moreover, during the thermal transformations of both compounds 1 and 2, the same two substances are generated: HgCl2 and HgS.
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| 6. |
- Rodina, Tatyana A., et al.
(författare)
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Crystal structure, solid-state 13C and 15N NMR characterisation, chemisorption activity and thermal behaviour of new mercury(II) dipropyldithiocarbamate : Binuclear, pseudo-binuclear and heteronuclear complexes of [Hg2(PrDtc)4], [Hg(PrDtc)2]2 and [Au(PrDtc)2]2[Hg2Cl6]
- 2020
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Ingår i: Inorganica Chimica Acta. - : Elsevier. - 0020-1693 .- 1873-3255. ; 508
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Tidskriftsartikel (refereegranskat)abstract
- Two polymorphs of a new mercury(II) N,N-dipropyldithiocarbamate represented by centrosymmetric binuclear and pseudo-binuclear molecules, [Hg2(PrDtc)4] (1) and [Hg(PrDtc)2]2 (2), have been isolated, identified using heteronuclear (13C, 15N) CP-MAS NMR and structurally characterised by single-crystal X-ray diffraction analysis. There are two pairs of inequivalent PrDtc ligands playing either terminal chelating or tridentate bridging structural functions in the former compound; while the latter complex comprises two pairs of structurally inequivalent chelating PrDtc ligands. The reaction of freshly precipitated mercury(II) N,N-dipropyldithiocarbamate (HgPrDtc) with a [AuCl4]−/2 M HCl solution results in the formation of the ionic complex [Au(PrDtc)2]2[Hg2Cl6] (3). There are two inequivalent centrosymmetric cations, [Au(PrDtc)2]+ (‘A’ and ‘B’), and a binuclear centrosymmetric anion, [Hg2Cl6]2− in the structure of 3. In the cationic part of the complex, each of the gold(III) cations has two pairs of the relatively weak inequivalent secondary Au···S bonds with two neighbours, therefore forming linear supramolecular cationic chains (⋯‘A’⋯‘B’⋯‘A’⋯‘B’⋯)n. To study the thermal behaviour of the compounds, simultaneous thermal analysis was also performed. The formation of HgS and reduced elemental gold was established during the thermolysis of 1/2 and 3, respectively.
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