12 research outputs found
A dimethylsulfide osmium(III,IV) complex synthesized via the microwave-assisted interaction of K2[OsCl6] with DMSO
Crystal Structure of Na<sub>2</sub>[OsCl<sub>6</sub>]
Salt Na2[OsCl6] is obtained by the interaction of H2[OsCl6]·H2O with NaCl in boiling concentrated hydrochloric acid. According to the single crystal X-ray diffraction data, the substance crystallizes in the cubic system, space group Fm3̄m, a = 9.7461(11) Å, V= 925.8(3) Å3, Z = 4, R1= 0.029, wR2 = 0.070. The compound is characterized by UV-vis and IR spectroscopy
Crystal Structure of Na2[OsCl6]
Salt Na2[OsCl6] is obtained by the interaction of H2[OsCl6]·H2O with NaCl in boiling concentrated hydrochloric acid. According to the single crystal X-ray diffraction data, the substance crystallizes in the cubic system, space group Fm3̄m, a = 9.7461(11) Å, V= 925.8(3) Å3, Z = 4, R1= 0.029, wR2 = 0.070. The compound is characterized by UV-vis and IR spectroscopy. © 2019, Pleiades Publishing, Ltd
Osmium(IV) Halide Complexes with Dimethyl Sulfoxide[H(dmso)<sub>2</sub>][OsX<sub>5</sub>(dmso-κO)], X=Cl, Br: Synthesis, Structure, and Properties
Osmium(IV) Halide Complexes with Dimethyl Sulfoxide[H(dmso)2][OsX5(dmso-κO)], X=Cl, Br: Synthesis, Structure, and Properties
Two osmium complexes of common formula [H(dmso)2][OsIVХ5(dmso-κO)] 1 (Х=Cl) and 2 (Х=Br) are synthesized via the reaction of H2OsX6 (Х=Cl, Br) with DMSO. The complex 1 crystallized in the orthorhombic space group Pca21. For 2, two orthorhombic polymorphs are found, namely, 2 a in space group Cmcm and 2 b in space group Pbca. Within the [H(dmso)2]+ cations of 1 and 2 a, the cis-configuration of the DMSO moieties has been observed for the first time. The complexes are characterized by a set of spectroscopic (NMR, IR, UV-Vis, EXAFS/XANES) and diffraction (single crystal and powder) techniques. Both complexes 1 and 2 retain their molecular structures in DMSO and acetone solutions, as evidenced by Os L3-edge EXAFS/XANES. 1H NMR spectra of 1 and 2 in DMSO solutions reveal signals of coordinated DMSO. In acetone solutions, signals of the [H(dmso)2]+ cations are observed in addition to those of coordinated neutral DMSO. © 2020 Wiley-VCH Verlag GmbH & Co. KGaA, Weinhei
The synthesis, characterization, and structure of (ThioH)2[OsX6] (X = Cl, Br)
Novel osmium complexes (ThioH)2[OsCl6] (1) and (ThioH)2[OsBr6] (2) have been synthesized via the interaction of H2[OsX6] (X = Cl, Br) with thiourea (Thio) in concentrated HX and characterized by chemical analysis, potentiometry, IR- and UV–Vis spectroscopy, X-ray powder and single-crystal diffraction. UV–Vis spectroscopy of 1 and 2 in solutions supports the preservation of [OsX6]2− ions that however demonstrate considerable solvatochromism. The longer-wavelength bands experience a hypsochromic shift with respect to the crystalline state. Intense bands of Os-halogen vibrations in ATR IR spectra are red-shifted with respect to those for K2[OsX6]. The complexes are isostructural and crystallized in the triclinic space group P1¯, Z = 1. Unit cell parameters are for 1: a = 7.1800(14) Å, b = 7.2700(15) Å, c = 7.7800(16) Å, α = 78.89(3)°, β = 87.83(3)°, γ = 65.11(3)°; for 2: a = 7.3169(15) Å, b = 7.5504(15) Å, c = 8.2065(16) Å, α = 80.00(3)°, β = 88.55(3)°, γ = 63.37(3)°. The cations (NH2)2CSH+ and anions [OsX6]2− are assembled into two-tier layers by N–H…X and S–H…X hydrogen-bonds and S…X non-valent contacts. © 2017 Elsevier Lt
The synthesis, characterization, and structure of (ThioH)2[OsX6] (X = Cl, Br)
Novel osmium complexes (ThioH)2[OsCl6] (1) and (ThioH)2[OsBr6] (2) have been synthesized via the interaction of H2[OsX6] (X = Cl, Br) with thiourea (Thio) in concentrated HX and characterized by chemical analysis, potentiometry, IR- and UV–Vis spectroscopy, X-ray powder and single-crystal diffraction. UV–Vis spectroscopy of 1 and 2 in solutions supports the preservation of [OsX6]2− ions that however demonstrate considerable solvatochromism. The longer-wavelength bands experience a hypsochromic shift with respect to the crystalline state. Intense bands of Os-halogen vibrations in ATR IR spectra are red-shifted with respect to those for K2[OsX6]. The complexes are isostructural and crystallized in the triclinic space group P1¯, Z = 1. Unit cell parameters are for 1: a = 7.1800(14) Å, b = 7.2700(15) Å, c = 7.7800(16) Å, α = 78.89(3)°, β = 87.83(3)°, γ = 65.11(3)°; for 2: a = 7.3169(15) Å, b = 7.5504(15) Å, c = 8.2065(16) Å, α = 80.00(3)°, β = 88.55(3)°, γ = 63.37(3)°. The cations (NH2)2CSH+ and anions [OsX6]2− are assembled into two-tier layers by N–H…X and S–H…X hydrogen-bonds and S…X non-valent contacts. © 2017 Elsevier Lt
Monoprotonated Dimethyl Sulfoxide, [HOSMe2]+: Synthesis, Crystal Structure, Spectroscopic and Theoretical Studies of [HOSMe2]2[OsCl6] ⋅ 2H2O
Complex [H(dmso)]2[OsIVCl6] ⋅ 2H2O (1) was synthesized by refluxing of [H(dmso)2]2[OsCl6] in concentrated HCl and characterized by the IR and UV/Vis spectroscopy and X-ray powder and single-crystal diffraction studies. In this complex, rare highly electrophilic [Me2S=O⋅⋅⋅H]+ cation is stabilized by multiple chalcogen bonds including bifurcated S⋅⋅⋅(Cl)3 and S⋅⋅⋅Cl non-covalent interactions. DFT calculations and topological analysis of the electron density distribution within the formalism of Bader's theory (QTAIM method) support the presence of intermolecular non-covalent interactions S⋅⋅⋅Cl and O⋅⋅⋅Cl in the solid state. © 2021 Wiley-VCH Gmb