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.
Temperaturabhängige elektrische Leitfähigkeit zeigt [{Ag(C5H4NS)}n]. Dieses anorganische Polymer mit Lamellenstruktur und graphitartiger Anordnung der Silber(I)-Ionen (siehe Bild) entstand bei der Behandlung von AgBF4 mit Pyridin-2-thiol in DMF bei 0°C. Wurde dieselbe Reaktion in Acetonitril durchgeführt, erhielt man dagegen das Polymer [{Ag5(C5H4NS)4(C5H5NS)BF4}n] mit einer Schichtstruktur.
We investigated three series of sulfonium bisphosphonates for their activity in inhibiting the growth of three human tumor cell lines. The first series consisted of 6 cyclic sulfonium bisphosphonates, the most active species having an (average) IC50 of 89 microM. The second consisted of 10 phenylalkyl and phenylalkoxy bisphosphonates, the most active species having an IC50 of 18 microM. The third series consisted of 17 n-alkyl sulfonium bisphosphonates, the most active species having an IC50 of approximately 240 nM. Three QSAR models showed that the experimental cell growth inhibition results could be well predicted. We also determined the structures of one sulfonium bisphosphonate bound to farnesyl diphosphate synthase, finding that it binds exclusively to the dimethylallyl diphosphate binding site. These results are of interest since they show that sulfonium bisphosphonates can have potent activity against a variety of tumor cell lines, the most active species having IC50 values much lower than conventional nitrogen-containing bisphosphonates.
This review presents the recent developments on FL-MOFs, including their structures and applications in gas adsorption, catalysis and proton conduction.
Heterojunction catalysts are attracting attention in the field of photocatalytic hydrogen generation for their effective light utilization and charge separation personalities. In this work, we report a simple and low-cost two-step solvothermal method for synthesizing Cu2O/TiO2 heterojunction catalysts with an octahedral morphology and a mean particle size of about 30 nm. It is found that the introduction of Cu2O astonishingly enhances the photocatalytic performance of TiO2. Under the condition of methanol acting as a sacrificial agent, the heterojunction with 0.19% Cu species shows an optimal hydrogen generation rate of 24.83 mmol g–1 h–1, which is nearly 3 orders of magnitude higher than that of the pristine TiO2 catalyst.
The trithio and tetrathio complexes of tungsten (PPh4)[Cp*WS3] (Cp* = η5-C5Me5) and (PPh4)2[WS4] undergo alkylation reactions with 2,6-bis(bromomethyl)pyridine to yield [(Cp*WS2)2{2,6-(SCH2)2(C5H3N)}]·CH3CN (1·CH3CN) (73.1% yield) and WS2{2,6-(SCH2)2(C5H3N)} (2) (76.0% yield), respectively. In the dinuclear complex 1, two Cp*WS3 units are linked by a 2,6-dimethylenepyridine bridge, and the pyridine nitrogen is not coordinated at tungsten. Complex 2 is the first example of bisalkylated tetrathiometalates, the mononuclear structure of which is stabilized by coordination of the pyridine nitrogen.
An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.
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