The preparation, structures and thermal properties of [MEn3][Cd(S2CNEt2)3]2 [M = zinc(II), cadmium(II)] complexes

Glinskaya, L. A.; Zemskova, S. M.; Клевцова, Р. Ф.; Ларионов, С. В.; Gromilov, S. A.

doi:10.1016/s0277-5387(00)83600-1

Cited by 15 publications

(12 citation statements)

References 8 publications

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“…The average of all Cd−N bonds is ∼2.6 Å for 1a and 1b . This distance is similar to those observed in other eight-coordinate cadmium−amine complexes , and is significantly longer than the <2.4 Å Cd−N distances for six-coordinate Cd−N complexes. − ,− …”

Section: Discussionsupporting

confidence: 83%

“…Similar conformations were observed in [Cu 2 L](OAc) 3 ( lel ) and [CuL](NO 3 ) 3 ( ob ), and in the crystal structure of [PbL](ClO 4 ) 2 ·H 2 O, the ligand appears to adopt the ob conformation − Typically, the lel form is favored over the ob form due to less severe hydrogen−carbon van der Waals interactions . Molecular mechanics calculations of L strain energy for the two conformations predict that the lel form of the free ligand is 2.3 kcal/mol lower in energy than the ob form ( lel = 29.1 and ob = 31.4 kcal/mol).…”

Section: Discussionsupporting

confidence: 57%

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Solution and Solid State Characterization of a Cadmium Octaazacryptand Complex

et al. 1996

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The constant for cadmium binding by octaazacryptand L ) N(CH 2 CH 2 NHCH 2 CH 2 NHCH 2 CH 2 ) 3 N was determined by potentiometry; log ML )18.3(1). Calculation of pM values (pM ) -log [M]) show that L has the highest reported binding affinity for cadmium relative to other [2.2.2] polyoxa-polyaza cryptates. Two cadmium cryptate complexes, [CdL](BF 4 ) 2 (1a) and [CdL](OAc) 2 ‚2H 2 O (1b), were synthesized by metalation of the free cryptand. The molecular structures of compounds 1a and 1b were determined by X-ray diffraction. Crystallographic data for 1a: trigonal, P3 h1c, Z ) 2, a ) 9.581(2) Å, c ) 17.003(4) Å, V ) 1351.2(5) Å 3 . Crystallographic data for 1b: monoclinic, C2/c, Z ) 4, a ) 10.500(2) Å, b ) 14.782(3) Å, c ) 19.395(4) Å, ) 99.30(2)°, V ) 2971(1) Å 3 . The cadmium ions in both complexes are eight-coordinate and display similar coordination geometries but different ligand conformations, designated as parallel and oblique. The cadmium coordination sphere is best described as a bicapped octahedron. Through 2D NMR experiments we have found that the Cd is in a symmetric environment and the conformation of the ligand in solution is consistent with the parallel conformation observed in one of the solid state structures. The 113 Cd NMR shift of this eight-coordinate amine complex is 75 ppm relative to 0.1 M aqueous Cd(ClO 4 ) 2 , which correlates with shifts observed for other [2.2.2] cadmium polyoxapolyaza cryptates.

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Section: Discussionsupporting

confidence: 83%

Section: Discussionsupporting

confidence: 57%

Solution and Solid State Characterization of a Cadmium Octaazacryptand Complex

et al. 1996

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“…The weight loss stops at 340 °C and corresponds to the formation of NbS 2 . The thermolysis of other metal dithiocarbamates, such as M(Et 2 dtc) 2 (M = Zn, Cd), also results in metal sulfides …”

Section: Resultsmentioning

confidence: 99%

Dinuclear Vanadium Sulfide Clusters: Synthesis, Redox Behavior, and Magnetic Properties

et al. 2018

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The complex [V 2 S 4 (nBu 2 dtc) 4 ] (1) (dtc = dithiocarbamate) was prepared by a self-assembly reaction from [VO(nBu 2 dtc) 3 ] and H 2 S. 1 H, 13 C, and 51 V NMR spectra indicate the presence in solution of two isomers (centrosymmetric and non-centrosymmetric) with different relative orientations of the dithiocarbamate chelate rings. Thermogravimetric studies of 1 show that the thermolysis products are VS 2 (in He) or VS (in H 2 ). The cyclic voltammogram (CV) in dichloromethane reveals a chemically reversible one-electron oxidation at +0.61 V followed by an irreversible oxidation at +1.51 V (vs. Ag/AgCl). The redox processes can be attributed to V-centered oxidation. This interpretation is supported by DFT calculations, indicating the predominantly V-V bonding character of the HOMO in both cases. The removal of one electron from the HOMO causes [a] Nikolaev

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“…) for I, whose structural characterization can be found elsewhere. [10] To confirm this explanation, we performed a NMR spectroscopic study of CD 3 OD solutions of I, for several reaction times, in the presence of ethylenediamine. In order to obtain accurate NMR spectra, this spectroscopic study was carried out in reaction solutions without TiO 2 (or SiO 2 ) particles.…”

Section: Resultsmentioning

confidence: 95%

“…In the presence of inorganic substrates, such as TiO 2 or SiO 2 particles, the metal-sulfide phase grows at the particles' surfaces. [9] As will be discussed later, this probably involves an intermediate metal complex [10] which then decomposes into metal sulfide. In the current work, this method was investigated to grow Ag 2 S nanophases at the surface of synthetic TiO 2 (anatase) submicrometric particles.…”

Section: Resultsmentioning

confidence: 99%

From Single‐Molecule Precursors to Coupled Ag₂S/TiO₂ Nanocomposites

et al. 2008

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A single-source approach using mild temperatures was applied to prepare morphological well-defined and coupled TiO 2 /metal-sulfide nanocomposites. Metal N-alkyldithiocarbamates were used as the precursors to the metal-sulfide nanophases and, in particular, Ag 2 S nanostructures were investigated in more detail. These were observed as nanoislands at the surface of TiO 2 (anatase) particles, which were used as substrates. To explain the formation of these nanocomposite particulates, a tentative mechanism has been pro-

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The preparation, structures and thermal properties of [MEn3][Cd(S2CNEt2)3]2 [M = zinc(II), cadmium(II)] complexes

Cited by 15 publications

References 8 publications

Solution and Solid State Characterization of a Cadmium Octaazacryptand Complex

Solution and Solid State Characterization of a Cadmium Octaazacryptand Complex

Dinuclear Vanadium Sulfide Clusters: Synthesis, Redox Behavior, and Magnetic Properties

From Single‐Molecule Precursors to Coupled Ag₂S/TiO₂ Nanocomposites

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The preparation, structures and thermal properties of [MEn3][Cd(S2CNEt2)3]2 [M = zinc(II), cadmium(II)] complexes

Cited by 15 publications

References 8 publications

Solution and Solid State Characterization of a Cadmium Octaazacryptand Complex

Solution and Solid State Characterization of a Cadmium Octaazacryptand Complex

Dinuclear Vanadium Sulfide Clusters: Synthesis, Redox Behavior, and Magnetic Properties

From Single‐Molecule Precursors to Coupled Ag2S/TiO2 Nanocomposites

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Product

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From Single‐Molecule Precursors to Coupled Ag₂S/TiO₂ Nanocomposites