Category: 27148-03-4

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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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Palladium(II) benzisothiazolinate (bit) complexes with amino-, acetylamino-, heterocyclic and phosphine co-ligands. Crystal structure of [Pd(bit)2(kappa2-dppe)]¡¤2EtOH

Abstract A series of square-planar palladium(II) benzisothiazolinate (bit) of the general type [Pd(bit)2L2] have been prepared and characterized by analytical and spectroscopic methods. Two synthetic routes have been employed, namely reactions of [Pd(bit)2]¡¤H2O with two equivalents of ligands (L = amine, amide, phosphine) or nucleophile displacement of chloride by benzisothiazolinate starting from trans-[PdCl2L2]. Both routes afford the new complexes in good yields as easily isolated, air and moisture stable, colored solids. The precursor, [Pd(bit)2]¡¤H2O, is itself prepared in high yields upon reaction of Na[bit] with Na2[PdCl4] in methanol and the analogous platinum complex, [Pt(bit)2]¡¤H2O, is similarly prepared from K2[PtCl4]. It is not clear if these species are mono- or dimeric, and formulation as [M2(mu-bit)4(H2O)2] with the four benzisothiazolinate spanning the metal-metal vector and possibly binding through coordination of nitrogen and oxygen is suggested. Diphosphine adducts, cis-[Pd(bit)2{kappa2-Ph2P(CH2)nPPh2}] (n = 1-4) can be prepared both upon addition of the diphosphine to [Pd(bit)2]¡¤H2O and from reactions of cis-[PdCl2{kappa2-Ph2P(CH2)nPPh2}] with two equivalents of Na[bit]. A crystal structure of cis-[Pd(bit)2(kappa2-dppe)] reveals that the benzisothiazolinate ligands are bonded in a monodentate fashion through nitrogen and this binding mode is proposed for all [Pd(bit)2L2] and [Pd(bit)2L] complexes. With dppb (n = 4) a second product is seen by NMR spectroscopy being proposed to be the part-substituted complex cis-[PdCl(bit)(kappa2-dppb)], while with dppm (n = 1) two further products are seen spectroscopically, proposed as trans-[Pd(bit)2(kappa1-dppm)2] and (more tenuously) [Pd2(bit)4(dppm)2]. The former is also prepared in good yields from reaction of [Pd(kappa2-dppm)2]Cl2 with Na[bit]. These studies show that palladium benzisothiazolinate are easily accessed and show good air and moisture stability.

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Structural and spectroscopic characterization of bis(thiosaccharinato)bis(benzimidazole)cadmium(II)

The crystal structure of [Cd(tsac)2(bzim)2]¡¤CH3OH (tsac, anion of thiosaccharine; bzim, benzimidazole) has been determined by single crystal X-ray diffractometry. It crystallizes in the triclinic space group P over(1, -) with Z = 2. The Cd(II) cation is in a distorted tetrahedral environment coordinated to two thiosaccharinate anions [Cd-S bond lengths of 2.5117(6) and 2.5598(6) A?] and two benzimidazole molecules [Cd-N lengths of 2.235(2) and 2.256(2) A?]. The FTIR spectrum of the complex is also recorded and briefly discussed. Some comparisons with related complexes are made.

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Synthesis of 1,2,3-Benzothiadiazine-1,1 -dioxide Derivatives and their Pharmacological Properties

Formation of 4-(Sub)-amino-1,2,3-benzothiadiazine-1,1-dioxide was established by earlier reported base catalysed ring expansion reaction. Products thus obtained, were stable in aqueous alkaline and acidic medium and on alkylation/acylation furnished 4-amino derivative (4, 5) exclusively, instead of 2-N-derivative (3). Preliminary pharmacological screening was done and the results were positive.

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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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One of the major reasons for studying chemical kinetics is to use measurements of the macroscopic properties of a system, Computed Properties of C7H5NO2S2, such as the rate of change in the concentration of reactants or products with time.In a article, mentioned the application of 27148-03-4, Name is Benzo[d]isothiazole-3(2H)-thione 1,1-dioxide, molecular formula is C7H5NO2S2

Mono and polynuclear silver(I) complexes with thiosaccharine and triphenylphosphine or 2,2?-bipyridine. Synthesis, spectroscopic and structural characterization

Reaction of Ag6(tsac)6 (tsac- = thiosaccharinate anion) with PPh3 and 2,2?-bipyridine (bipy) ligands give rise to three new silver-thiosaccharinate complexes, [Ag(tsac)(PPh3)3], [Ag4(tsac)4(PPh3)3], and [Ag2(tsac)2(bipy)2]. Their crystal structures established by single-crystal X-ray diffraction and IR spectroscopic characterizations are reported here. In each complex a singular coordination mode for the thiosaccharinate ligands is observed. The most important features of the different coordination modes of the thionates are discussed.

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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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Reference of 27148-03-4, A catalyst don’t appear in the overall stoichiometry of the reaction it catalyzes, but it must appear in at least one of the elementary reactions in the mechanism for the catalyzed reaction. 27148-03-4, Name is Benzo[d]isothiazole-3(2H)-thione 1,1-dioxide, molecular formula is C7H5NO2S2. In a Article£¬once mentioned of 27148-03-4

Activation of thiosaccharin at a polynuclear osmium cluster

The reaction of thiosaccharin (tsacH) with the triosmium cluster [Os3(CO)10(NCMe)2] furnishes the decacarbonyl isomers [HOs3(CO)10(mu-S-tsac)] (1) and [HOs3(CO)10(mu-N,S-1,3-tsac)] (2) in a 3:1 ratio at room temperature. These isomers differ by the coordination mode displayed by tsac ligand. The tsac moiety functions as an edge-bridging ligand via the sulfur atom in 1 while in 2 the bridging of adjacent osmium centers is achieved through the sulfur and nitrogen groups. The ancillary hydride in both products shares the Os?Os edge that is bridged by the heterocyclic ligand. Heating 1 at 80 C affords 2 and demonstrates that the former cluster is the product of kinetic control. The conversion of 1 ? 2 has been investigated by DFT and the isomerization pathway elucidated. The DFT calculations confirm cluster 2 as the thermodynamically preferred isomer in this pair of products. Thermolysis of 2 in refluxing toluene affords the hexanuclear cluster [H2Os6(CO)17(mu-C,N-1,2-C6H4CNSO2)2(mu3-S)(mu4-S)] (3) via carbon-sulfur bond scission and subsequent capture of the extruded sulfur by the cluster core. The molecular structures for the three new clusters have been determined by single-crystal X-ray diffraction analyses.

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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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Accelerators for increasing the rate of formation of free radicals and reactive oxygen species

The formation of free radicals is enhanced with photodynamic agents, sonodynamic agents, and systems and therapies utilizing ultrasound by subjecting the agent to light waves or sound waves in the presence of a metal, a reductant, or a chelate, or mixtures thereof.

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