Syntheses, characterization and thermal properties of [M(Spy)2(SpyH)2] (M=Cd and Hg; Spy−=pyridine-4-thiolate; SpyH=pyridinium-4-thiolate)) and [M(SpyH)4](ClO4)2 (M=Zn, Cd and Hg)

“…A large number of one-, two-and three-dimensional coordination polymers containing pyridine-2-thiol have been synthesized (Hong et al, 1999;Kato et al, 2002;Wen et al, 2004). However, only a small number of analogues containing pyridine-4-thiol have been reported (Nunokawa et al, 2001;Anjali et al, 2003). We are interested in investigating the thio-pyridine±copper halide system because of its potentially interesting reaction chemistry (Cheng et al, 2004).…”

Section: Commentmentioning

confidence: 99%

4,4′-Thiodipyridinium tetrachlorocopper(II)

et al. 2004

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The title compound, (C(10)H(10)N(2)S)[CuCl(4)], was obtained by the reaction of cupric chloride with pyridine-4-thiol in a mixture of acetonitrile and tetrahydrofuran, suggesting that the desulfurization and coupling reactions of pyridine-4-thiol occurred in the presence of the Cu(2+) ion. X-ray diffraction analysis reveals the presence of one 4,4'-thiodipyridinium cation, H(2)bps(2+), and one [CuCl(4)](2-) anion. The cations interact with the anions via N-H...Cl hydrogen-bonding interactions to form a closed 'chair' conformation.

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“…Although the structure of Cd(py4S) 2 remains unknown -as noted above, attempts to crystallize this compound by the method used for Cd(tzt) 2 yielded Cd(py4SH) 2 (py4S) 2 -the chemical shift approaches the region where resonances from CdS 4 kernels are found (see, e.g., Table 5 and refs. 26 and 27), although it is smaller than those found (12) for [Cd(py4S) 4-n (py4SH) n ] (2-n)+ (n = 0, 2, 4) in a DMF-MeOH solvent mixture (616-617 ppm at 213 K).…”

Section: Cadmium-113 Nmr Spectra Of 1 7 and Related Compoundsmentioning

confidence: 58%

“…The yellow crystals that were produced were found, by complete X-ray analysis, to be Cd(py4S) 2 (py4SH) 2 (6), which had been characterized independently (12).…”

Section: Attempted Crystallization Ofmentioning

confidence: 99%

A synthetic, structural, and¹¹³Cd NMR study of cadmium complexes of 1,3-thiazolidine-2-thionate, including the structures of Cd(C₃H₄NS₂)₂, (Cd(C₃H₄NS₂)₂(C₅H₅N)₃·C₅H₅N, and (Ph₄P)₂[I₂Cd(µ-C₃H₄NS₂)₂CdI₂]

Craig¹,

Dance²,

Dean³

et al. 2005

Can. J. Chem.

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The crystallization of cadmium bis(1,3-thiazolidine-2-thionate), Cd(C 3 H 4 NS 2 ) 2 (1), is reported. Freshly prepared 1 reacts with Ph 4 P + X -in a 1:2 ratio to give (Ph 4 P) 2 [Cd 2 (C 3 H 4 NS 2 ) 2 X 4 ] (X = I (4) or Br (5)). Crystallization of 1 from pyridine produces a solvate 7, which loses pyridine readily. X-ray analyses show that 1 has a polymeric sheet structure in which the C 3 H 4 NS 2 -ligands act as bidentate bridges through N and the exocyclic S and the Cd has a CdN 2 S 2 kernel; 5 is isomorphous with 4, which contains a dimeric anion again with bridging through the N and exocyclic S of the heterocyclic ligands; and 7 is Cd(C 3 H 4 NS 2 ) 2 (C 5 H 5 N) 3 ·C 5 H 5 N, containing trigonal bipyramidal Cd(C 3 H 4 NS 2 ) 2 (C 5 H 5 N) 3 molecules, in which the C 3 H 4 NS 2 -ligands, both of which are monodentate and in equatorial positions, occur as a unique combination of S-and N-bound. Cadmium-113 NMR data for 1 in pyridine solution and solid-state CP-MAS 113 Cd data for 1, 7, bis(pyridinium-4-thiolate)cadmium, and tetrakis(pyridinium-2-thiolate)cadmium nitrate are reported and discussed. The compound 1 has chemical and NMR spectroscopic properties that make it a useful standard for solid-state CP-MAS 113 Cd NMR spectroscopy.Résumé : On a effectué la cristallisation du bis(1,3-thiazolidine-2-thionate) de cadmium, Cd(C 3 H 4 NS 2 ) 2 (1). Le composé 1 fraîchement préparé réagit avec le Ph 4 P + X -dans un rapport 1 : 2 pour conduire à la formation de (Ph 4 P) 2 [Cd 2 (C 3 H 4 NS 2 ) 2 X 4 ] (X = I (4) et Br (5)). La cristallisation du composé 1 dans la pyridine conduit à la formation du produit solvaté 7 qui perd facilement de la pyridine. Les données de la diffraction des rayons X montrent que le composé 1 existe dans une structure en feuillets polymériques dans laquelle les ligands C 3 H 4 NS 2 -agissent comme ponts bidentates entre l'azote et le soufre exocyclique et que le cadmium se trouve dans un noyau CdN 2 S 2 ; que le composé 5 est isomorphe de 4 qui contient un anion dimère qui se lie lui aussi par des ponts à l'azote et au soufre exocyclique des ligands hétérocycliques; que 7, Cd(C 3 H 4 NS 2 ) 2 (C 5 H 5 N) 3 ·C 5 H 5 N, comporte des molécules bipyramidales trigonales Cd(C 3 H 4 NS 2 ) 2 (C 5 H 5 N) 3 dans lesquelles les ligands C 3 H 4 NS 2 -, qui sont tous les deux monodentates et dans des positions équatoriales, se retrouvent comme une combinaison unique avec des liaisons au soufre et à l'azote. On a obtenu et on discute des données de RMN du 113 Cd pour le composé 1, en solution dans la pyridine, et des données de « CP-MAS » à l'état solide du 113 Cd pour les composés 1 et 7, le bis(pyridinium-4-thiolate)cadmium et le nitrate de tétrakis(pyridinium-2-thiolate)cadmium. Le composé 1 a des propriétés chimiques et spectroscopiques qui pourraient le rendre utile comme standard pour la spectroscopie RMN 113 Cd « CP-MAS » à l'état solide.Mots clés : cadmium, 1,3-thiazolidine-2-thionate, diffraction des rayons X, RMN du 113 Cd à l'état solide, composé standard pour la RMN du 113 Cd.[Traduit ...

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Syntheses, characterization and thermal properties of [M(Spy)2(SpyH)2] (M=Cd and Hg; Spy−=pyridine-4-thiolate; SpyH=pyridinium-4-thiolate)) and [M(SpyH)4](ClO4)2 (M=Zn, Cd and Hg)

Cited by 15 publications

References 30 publications

Crystal structure of catena-[(5-sulfosalicylato-) k2O,O')-bis(μ2-4- thiolatopyridinium-)k2S:S)cadmium(II)] hydrate, Cd(C7H4O6S)(C5H5NS)2 · 2.5H2O

Crystal structure of catena-[(5-sulfosalicylato-) k2O,O')-bis(μ2-4- thiolatopyridinium-)k2S:S)cadmium(II)] hydrate, Cd(C7H4O6S)(C5H5NS)2 · 2.5H2O

4,4′-Thiodipyridinium tetrachlorocopper(II)

A synthetic, structural, and¹¹³Cd NMR study of cadmium complexes of 1,3-thiazolidine-2-thionate, including the structures of Cd(C₃H₄NS₂)₂, (Cd(C₃H₄NS₂)₂(C₅H₅N)₃·C₅H₅N, and (Ph₄P)₂[I₂Cd(µ-C₃H₄NS₂)₂CdI₂]

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Syntheses, characterization and thermal properties of [M(Spy)2(SpyH)2] (M=Cd and Hg; Spy−=pyridine-4-thiolate; SpyH=pyridinium-4-thiolate)) and [M(SpyH)4](ClO4)2 (M=Zn, Cd and Hg)

Cited by 15 publications

References 30 publications

Crystal structure of catena-[(5-sulfosalicylato-) k2O,O')-bis(μ2-4- thiolatopyridinium-)k2S:S)cadmium(II)] hydrate, Cd(C7H4O6S)(C5H5NS)2 · 2.5H2O

Crystal structure of catena-[(5-sulfosalicylato-) k2O,O')-bis(μ2-4- thiolatopyridinium-)k2S:S)cadmium(II)] hydrate, Cd(C7H4O6S)(C5H5NS)2 · 2.5H2O

4,4′-Thiodipyridinium tetrachlorocopper(II)

A synthetic, structural, and113Cd NMR study of cadmium complexes of 1,3-thiazolidine-2-thionate, including the structures of Cd(C3H4NS2)2, (Cd(C3H4NS2)2(C5H5N)3·C5H5N, and (Ph4P)2[I2Cd(µ-C3H4NS2)2CdI2]

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A synthetic, structural, and¹¹³Cd NMR study of cadmium complexes of 1,3-thiazolidine-2-thionate, including the structures of Cd(C₃H₄NS₂)₂, (Cd(C₃H₄NS₂)₂(C₅H₅N)₃·C₅H₅N, and (Ph₄P)₂[I₂Cd(µ-C₃H₄NS₂)₂CdI₂]