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Thiosaccharinate binding to palladium(II) and platinum(II): Synthesis and molecular structures of sulfur-bound complexes [M(kappa1-tsac) 2(kappa2-diphosphane)]

Palladium(II) and platinum(II) thiosaccharinate complexes [M(kappa1-tsac)2{kappa2-Ph 2P(CH2)nPPh2}] (M = Pd, Pt; n = 1-4) have been prepared, palladium complexes from reaction of [Pd(tsac) 2]¡¤H2O with diphosphanes and platinum complexes from addition of thiosaccharin to [PtCl2{kappa2-Ph 2P(CH2)nPPh2}] in the presence of triethylamine. All complexes have been fully characterized and the crystal structures of [Pd(kappa1-tsac)2(kappa2- dppp)] (n = 3) and [Pt(kappa1-tsac)2(kappa 2-dppm)] (n = 1) have been determined confirming that thiosaccharinate ligands are S-bound. The larger ring complexes (n = 3, 4) are fluxional in solution being attributed to the conformational flexibility of the diphosphane backbones The bis(diphosphane) complexes, [M(kappa1- tsac)2(kappa1-dppm)2] (M = Pd, Pt), have also been prepared upon treatment of [Pd(tsac)2]¡¤H2O with two equivalents of dppm or addition of thiosaccharin to [Pt(kappa2-dppm)2]Cl2 in the presence of triethylamine in which the diphosphanes bind in a monodentate fashion. Both are highly fluxional in solution, changes in the 31P{1H} NMR spectra as a function of temperature being interpreted as the exchange of bound and unbound phosphorus atoms.

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Pseudosaccharin amine derivatives: Synthesis and elastase inhibitory activity

Pseudosaccharin amines were synthesized from saccharin either by the reaction of pseudosaccharin chloride with amines, or via thiosaccharin which was treated with amines yielding thiosaccharinates, and their reaction with glacial acetic acid. This route gave lower yields than the first way. The synthesis of alkyl [(1,1-dioxo-benzo[d]isothiazol-3-yl)amino]alkanoates as possible Human Leukocyte Elastase (HLE) inhibitors was realized by the reaction between amino acid esters and pseudosaccharin chloride. Hydrolysis of the esters was possible under aqueous basic conditions. Selected compounds were screened for elastase inhibitory activity. Compounds 4k and 4m were found to be reversible inhibitors of HLE with Ki values of 45 muM and 60 muM.

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A comparative study of the coordination of saccharinate, thiosaccharinate and benzisothiozolinate ligands to cyclometalated [Pd(Me2NCH2C6H4-kappa2N,C)(mu-Cl)]2: Molecular structures of [Pd(Me2NCH2C6H4-kappa2N,C)(mu-X)]2 (X?=?sac, bit and tsac) and [Pd(Me2NCH2C6H4-kappa2N,C)Cl(ampyH-kappa1N)] (ampyH?=?2-amino-3-methylpyridine)

Reactions of [Pd(Me2NCH2C6H4-kappa2N,C)(mu-Cl)]2 with two equivalents of sodium saccharinate (Nasac), thiosaccharin (Htsac) or sodium benzisothiozolinate (Nabit) results in the stepwise substitution of the bridging halides to form sequentially [Pd2(Me2NCH2C6H4-kappa2N,C)2(mu-Cl)(mu-X)] (X = sac, tsac) and [Pd(Me2NCH2C6H4-kappa2N,C)(mu-X)]2 (X = sac, tsac, bit). The molecular structures of all three disubstituted complexes are reported. In each the two metalated ligands bind in a chelate manner adopting a relative anti conformation, while the new ligands bridge the two palladium atoms adopting a relative cis conformation. The local conformation about each palladium differs with small ligand changes. Thus in the sac and bit complexes all nitrogens lie trans to one another, in the tsac complex they are cis. Conformational changes also lead to large differences in the non-bonded Pd?Pd distance which range over 0.5 A. Treatment of [Pd(Me2NCH2C6H4-kappa2N,C)(mu-Cl)]2 with two equivalents of 2-amino-3-methylpyridine (ampyH) in the presence of NEt3 affords mononuclear [PdCl(Me2NCH2C6H4-kappa2N,C)(ampyH-kappa1N)] as a result of ?bridge-splitting?, the ampyH ligand binding through the pyridyl-nitrogen and lying approximately perpendicular to the PdCClN2 plane as shown by a crystallographic study.

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Reactions of [Ru3(CO)12] with thiosaccharin: Synthesis and structure of di-, tri-, tetra- and penta-ruthenium complexes containing a thiosaccharinate ligand(s)

Reactions of [Ru3(CO)12] with thiosaccharin (tsacH) at different temperatures have been investigated. At 40 C, the diruthenium complex [Ru2(CO)6(mu-N,S-tsac)2] (1) is produced and whose ruthenium atoms are bridged by two tsac ligands that are oriented in a head-to-tail fashion. When this reaction is carried out at 66 C, the tri-, tetra- and penta-ruthenium complexes [H2Ru3(CO)7(mu-N,S-tsac)(mu-C,N?C6H4CNSO2)(mu3-S)] (2), [Ru4(CO)12(mu-N,S-tsac)2(mu4-S)] (3) and [H2Ru5(CO)13(mu-N,S-tsac)(mu-C,N?C6H4CNSO2)(mu3-S)(mu4-S)] (4), respectively, are also isolated in addition to 1. The triruthenium complex 2 exhibits an arachno SRu3 polyhedron containing edge-bridging tsac and C6H4CNSO2 ligands. The tetraruthenium complex 3 consists of two [Ru2(CO)6(mu-N,S-tsac)] fragments linked via a mu4-S ligand, while the pentaruthenium complex 4 is composed of individual Ru3 and Ru2 units linked via a mu4-S ligand. At 81 C, the same reaction furnishes the pentaruthenium complex [HRu5(CO)15(mu-N,S-tsac)(mu5-S)] (5) containing tsac and mu5-S bridging ligands. The molecular structures of the new complexes have been determined by single-crystal X-ray diffraction analyses, and the bonding in each product has been examined by DFT.

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Zn thiosacharinates: From ionic to polymeric structures. Synthesis, characterization and cell proliferation inhibition studies

A series of Zn thiosacharinates complexes with nitrogen donor co-ligands were synthesized: [Zn(tsac)2(o-phen)], [Zn(tsac)2(TMDP)]n, [(4,4?-bipy)H2][Zn(tsac)4] [Zn(tsac)2(2,2?-bipy)], [Zn(tsac)2(2,2?-bquin)], (tsac, thiosaccharinate anion: 1,1-dioxo-1,2-benzisothiazole-3-thiolato, C7H4NO2S2?, o-phen: 1,10?-phenantroline, TMDP: trimethylenedipyridine, 2,2?-bipy: 2,2?-bipyridine, 4,4?-bipy: 4,4?-bipyridine, 2,2?-bquin: 2,2?-biquinoline). They were fully characterized by means of FTIR, 13C and 1H NMR, elemental analysis and conductivity measurements. Three of them, [Zn(tsac)2(o-phen)], [(4,4?-bipy)H2][Zn(tsac)4], [Zn(tsac)2(TMDP)]n were also characterized by X-ray single crystal diffractometry and their crystal structures are described herein. DFT geometry optimization for the [Zn(tsac)2(o-phen)] complex was performed and its vibrational spectra was predicted. Moreover, we studied the effects of the five complexes on cell proliferation, thus providing preliminary evidence for their therapeutic potential as anti-cancer drugs.

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Poly[(mu3-1,1-dioxo-1,2-benzo-iso-thiazole-3-thiol-ato- kappa3 N:S 3:S 3)silver(I)]

The centrosymmetric title compound, [Ag(C7H4NO2S2)] n , consists of dinuclear units in which two thio-saccharinate anions each bridge two Ag atoms via an endocyclic N atom and an exocyclic S atom across a crystallographic centre of inversion midway between the Ag atoms. The dimeric units are connected via Ag – Sexo inter-actions to create two-dimensional networks. The thio-saccharinate anions bridge in a 3-S:S:N manner. The Ag…Ag distance can be considered a strong argentophilic inter-action. International Union of Crystallography 2007.

Sometimes chemists are able to propose two or more mechanisms that are consistent with the available data. Application In Synthesis of Benzo[d]isothiazole-3(2H)-thione 1,1-dioxide, If a proposed mechanism predicts the wrong experimental rate law, however, the mechanism must be incorrect.Welcome to check out more blogs about 27148-03-4, in my other articles.

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A new supramolecular assembly obtained by reaction between thiosaccharin and pyridine

The crystal structure of pyridinium thiosaccharinate thiosaccharin, [HNC5H5]+ [(tsac)(Htsac)]- (Htsac = C7H5NO2S2, the thiosaccharin molecule), was determined by single-crystal X-ray diffraction. Both, the thiosaccharinate anion, the corresponding neutral molecule and the pyridinium cation are nearly planar and arranged in the solid state in an almost parallel fashion, hence giving rise to a layered supramolecular structure. The anion shows small but significant modifications in the bonding of the thioamide group as compared with the neutral molecule. The crystal is further stabilized by an extensive H-bonding network. The FTIR spectrum of the compound is briefly commented.

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In heterogeneous catalysis, the catalyst is in a different phase from the reactants. Safety of Benzo[d]isothiazole-3(2H)-thione 1,1-dioxide, At least one of the reactants interacts with the solid surface in a physical process called adsorption in such a way. 27148-03-4, name is Benzo[d]isothiazole-3(2H)-thione 1,1-dioxide. In an article£¬Which mentioned a new discovery about 27148-03-4

Aurophilic interaction in gold(I) thiosaccharinates: Synthesis, characterization, crystal structures and DFT theoretical study

The reaction of gold with thiosaccharin ligand and additional phosphorous coligands is studied. Four new Au(I) complexes with thiosaccharinate as coordinating counteranion: [Au(tsac)(PPh3)], [Au2(tsac) 2(dppm)]¡¤EtOH, Au2(tsac)2(dppe) ¡¤EtOH, and Au(tsac)(Htsac)2¡¤0.25 EtOH (tsac: thiosaccharinate, C6H4C(S)NSO2-, dppm: bis(diphenylphosphino)methane, dppe: bis(diphenylphosphino)ethane) were synthesized and characterized by means of spectroscopic techniques (IR, UV-Vis, and 1H, 13C and 13P NMR). The crystal structure of two of them, [Au(tsac)(PPh3)] and [Au2(tsac) 2(dppm)]¡¤EtOH, were solved applying single crystal X-ray diffraction and studied using the density functional theory (DFT) formalism. In the latter, the aurophilic interaction between the two gold centers was analyzed and theoretically confirmed.

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Bismuth(III) saccharinate and thiosaccharinate complexes and the effect of ligand substitution on their activity against helicobacter pylori

Five bismuth(III) saccharinate and thiosaccharinate complexes, [Ph 2Bi(sac)]?1, [Bi(sac)3]n2, [Ph2Bi(tsac)]?4, [PhBi(tsac)2] n5, [Bi(tsac)3]n6 (sacH = saccharin, tsacH = thiosaccharin), have been synthesized and fully characterized. The tendency for ligand redistribution in [Ph2Bi(sac)]? has been investigated in solution by NMR spectroscopy. The structures of [Ph 2Bi(sac)]?1 and [Ph2Bi(tsac)] ?4 have been confirmed by X-ray crystallography. In Ph 2Bi(sac) the sac ligand is bound to a four-coordinate bismuth center via its imino nitrogen atom with an accompanying long-range Bi-O interaction. However, in the structure of [Ph2Bi(tsac)]? the ligand is sigma-bound through the exocyclic sulfur atom, giving a thiolate complex, confirming the more thiophilic nature of bismuth(III). Both complexes consist of polymeric chain structures with formally four-coordinated bismuth atoms. The complexes were assessed for their activity against H. pylori. The activity is both ligand dependent and sensitive to the degree of ligand substitution. The saccharinate complexes, 1 and 2, show activity comparable with standard tris-carboxylato bismuth(III) compounds, 6.25 mug/mL, while the activity of the thiolato complexes, 4-6, increases dramatically on increasing the number of thiolate groups from one to three (range 50-6.25 mug/mL). Saccharin, thiosaccharin, and BiPh3 were found to be inactive.

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Structure of potassium thiosaccharinate monohydrate

K[C7H4NO2S2].H2O, Mr = 255¡¤36, orthorhombic, Pbca, a = 8¡¤873 (1), b = 27¡¤108 (6), c = 8¡¤708 (1) A, V = 2094¡¤5 A3, Z = 8, Dx – 1¡¤62 Mg m-3, lambda(Mo Kalpha) = 0¡¤71069 A, mu = 0¡¤81 mm -1, F(000)= 1032, room temperature, final R = 0¡¤032 for 1801 observed unique reflections. The structure is built up of K + cations, thiosaccharinate anions and water molecules. The K + ion is six coordinated to two water O atoms, three O atoms from the SO2 groups and one N atom from the thiosaccharinate ion. The K – O distances range from 2¡¤722 (3) to 3¡¤158 (3)A, while the K – N distance is 2¡¤825 (2) A. The coordination polyhedron is irregular.

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