Chemistry of the Tetraselenomolybdate Anion: Syntheses, Spectroscopic Results, and Structural Characterizations of Polynuclear Mo−Cu−Se Compounds Containing Thiolate Ligands
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In the study on the reactivity of tetraselenomolybdate, a DMF solution of [Et4N]2[MoSe4] was found to react with 3 equiv of CuCl in the presence of NaS2CNR2 [R2 = Et2, C5H10, (PhCH2)2, Me2] to give a series of Mo−Cu−Se compounds, [Et4N]2[MoCu3Se4(R2NCS2)3] (R2 = Et2 (1a), C5H10 (1b), (PhCH2)2 (1c)) and [Et4N]2[MoCu4Se4(Me2NCS2)4] (2). Furthermore, the reaction of 2 or [Et4N]2[MoSe4(CuCN)2] with [Et4N]2[Cu(SPh)3] in DMF/MeCN afforded a polynuclear Mo−Cu−Se cluster compound, [Et4N]4[MoCu10Se4(PhS)12] (3). [Et4N]2[MoCu3Se4(Et2NCS2)3] (1a) crystallizes in the orthorhombic space group P212121 with cell dimensions a = 12.949(3) Å, b = 13.339(3) Å, c = 29.744(6) Å, V = 5137.6 Å3, and Z = 4. Full anisotropic refinements of the structure led to convergence with a value of R = 0.052 (Rw = 0.055) for 453 variables and 6854 reflections (F > 4.0σ(F)). The [MoCu3Se4(Et2NCS2)3]2- anion in 1a comprises three Et2NCS2Cu fragments linked by a slightly distorted tetrahedral MoSe4 moiety. Compound 2 crystallizes in the orthorhombic space group Pbca with cell constants a = 14.600(3) Å, b = 18.765(4) Å, c = 37.781(8) Å, V = 10351 Å3, and Z = 8. Anisotropic refinements with 5328 reflections (F > 4.0σ(F)) and 460 parameters for all non-hydrogen atoms yielded the values of R = 0.075 and Rw = 0.080. The [MoCu4Se4(Me2NCS2)4]2- anion structure of 2, which possesses a pseudo D2d symmetry of the MoSe4Cu4 core and a nearly planar MoCu4 array, consists of four Me2NCS2Cu fragments coordinated across four edges of the tetrahedral [MoSe4]2- moiety. The compound [Et4N]4[MoCu10Se4(PhS)12] (3) crystallizes in the tetragonal space group I4̄ with cell dimensions a = 18.344(3) Å, c = 18.368(4) Å, V = 6180.9 Å3, and Z = 2. A value of R = 0.079 (Rw = 0.084) for 218 parameters and 3314 observations (F > 4.0σ(F)) was obtained from anisotropic refinements of the non-hydrogen atoms. The [MoCu10Se4(PhS)12]4- anion structure of 3 can be described as six Cu atoms bonded across the six edges of a central MoSe4 tetrahedron, forming an octahedral MoSe4Cu6 array, to which the other four Cu atoms are added in a tetrahedral array bridged by 12 μ-SPh ligands. The 95Mo NMR spectra of the all compounds in DMF show a single resonance peak. Their chemical shifts are dependent on the deshielding effect from the number of the Cu atoms around Mo atom and the structures of the compounds. The 1H NMR, IR, and electronic spectroscopic data of these compounds are also consistent with their solid-state structures.Keywords:
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Abstract Ambiguity exists in the literature on the crystal structure of Ag 3 Sn: no agreement on neither the type of orthorhombic distortion nor the presence of ordering exists. Therefore, the exact crystal structure of Ag 3 Sn has been reinvestigated using high resolution X-ray powder dffraction. By applying Rietveld refinements, it could be shown that Ag 3 Sn is orthorhombic, with an ordered crystal structure of β-Cu 3 Ti-type (space group Pmmn ). The lattice parameters of a Sn-rich and an Ag-rich sample are a= 4.78233(1) Å, b= 5.99752(1) Å, c= 5.16393(1) Å and a= 4.78291(2) Å, b= 5.98854(2) Å, c= 5.15686(2) Å, respectively. The lattice parameters indicate κ-type orthorhombic distortion.
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Crystal and molecular structure of 1‐(p‐nitrophenyl)‐2‐acetylamino‐3‐brom‐propen‐2‐on‐1, C11H9BrN2O4
Abstract M r = 313.11, orthorhombic space group Pbca, a = 8.165(1), b = 9.491(2), c = 32.207(5) Å V = 2496(1) Å 3 , D X = 1.667 Mgm −3 , Z = 8, F(000) = 1248, λ(MoKα) = 0.71069 Å, μ = 32.7 mm −1 . The crystal structure was determined by direct methods and refined by least‐squares procedure to the discrepancy factor R = 0.065. Positions of hydrogen atoms were calculated. The structure determined by x‐ray analysis confirms the chemical results.
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Abstract The crystal and molecular structure of 1-(4-methoxyphenyl)-3-(phenyl)-2-propen-1-one derivative is determined by X-ray diffraction method. The compound, C16H14O2, crystallises in the orthorhombic space group Pbca with a=10.921(2) Å, b=30.583(1) Å, c=7.535(3) Å, V=2516.7(9) Å3, Z=4, D calc=1.242 Mg/m3, μ=0.327 mm−1, F 000=504, λ(MoKα)=0.71069 Å and the structure was refined to R=0.044.
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The compound C 36 H 26 N 4 O 4 , a derivative of Pigment Yellow 101, is one of the few organic pigments that show fluorescence in the solid state. Since single crystals could not be grown, the structure was determined from powder data. The X-ray powder pattern could be indexed with an orthorhombic unit cell. The space group remained ambiguous. The crystal structure was solved by lattice energy minimisation in different space groups using the program CRYSCA. Subsequently, the structure was refined by the Rietveld method using restraints. The compound crystallises in a herringbone pattern in Pbcn with a = 30.117(1) Å, b = 9.723(2) Å, c = 9.511(3) Å, Z = 4 with the molecule on an inversion centre. The insolubility and the solid-state fluorescence can be explained from the crystal structure.
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Two novel compounds [Zn(dien)2]Te2(1) and [Ni(dien)2]Se3(2)(dien=diethylenetriamine) have been synthesized under the mild solvothermal conditions and characterized structurally.The crystal 1 belongs to orthorhombic space group Cmca with the lattice parameters a=9.212(2),b=10.854(3),c=15.723(4),Z=4.The crystal 2 belongs to orthorhombic space group Pna21 with the lattice parameters a=18.047(4),b=9.8236(19),c=9.0079(19),Z=4.The crystal structure of 1 consists of discrete dumbbell Te22- anions and distorted-octahedron [Zn(dien)3]2+ cations.Compound 2 consists of discrete 'V' shape Se32- anions and distorted-octahedron [Ni(dien)3]2+ cations.
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