Bei der Reaktion von WO3 in einer Caesiumiodid‐Schmelze bei 700°C entsteht die hexagonale Wolframbronze Cs0.29WO3 in Form schwarzer, hexagonal‐prismatischer Kristalle. Ihre Struktur wurde durch Röntgenbeugung bestimmt (399 beobachtete unabhängige Reflexe, R = 5,8%). Kristalldaten: a = 741,2(3), c = 760,0(5) pm, Raumgruppe P6322, Z = 6. Es handelt sich um die bekannte Struktur der hexagonalen Wolframbronzen mit Wolframatomen, die aus den Oktaedermitten um 11,9 pm herausgerückt sind und mit drei verschiedenen WO‐Bindungslängen (198, 191, 187 pm). Die WO6‐Oktaeder sind leicht gegeneinander verkippt.
Polyselenide Complex o f Copper(I), Synthesis, IR Spectra, Crystal Structure (PPh4)4[Cu2S e14] has been prepared by the reaction o f a lithium polyselenide solution in D M F with CuCl at 120 °C in the presence o f PPh4Br. The compound forms black crystals, which were characterized by IR spectroscopy as well as by an X-ray structure determination. Space group P 2 ,, Z = 2, 2690 observed unique reflexions, R = 0.095. Lattice dim ensions at 19 °C: a = 2139.5(9), 6 = 1 6 1 1 .7 (3 ), c = 1365.1(3) pm, ß = 93.54(3)°. The com pound consists o f PPh4+ and [Cu2Se14]4" ions, in which the two copper atoms are bridged by an Se52-chain. One o f the Cu atom s is a member o f a CuSe4 ring, the other one o f a CuSe5 ring; the coordina tion at each Cu atom is trigonal-planar.
Beim Erhitzen von Vanadium(V)‐oxid mit Rubidiumiodid auf ca. 500°C wird Vanadium partiell reduziert, es entsteht Rb2V3O8. Dieses kristallisiert in der Fresnoit‐Struktur. Kristalldaten: a = 892,29(7), c = 554,49(9) pm bei 20°C, tetragonal, Raumgruppe P4bm, Z = 2. Röntgenstrukturbestimmung mit 620 beobachteten Reflexen, R = 2,7%. V2O7‐Einheiten und quadratische Pyramiden VO5 sind untereinander zu Schichten eckenverknüpft; die Schicht kann als Assoziat aus VO2+ ‐ und V2O74−‐Ionen aufgefaßt werden. Die Rb+‐Ionen zwischen den Schichten sind verzerrt pentagonal‐antiprismatisch koordiniert.
The title compounds have been prepared by reactions of sodium polyselenide solutions in DMF with FeCp(CO)2I, and CoCl2 · 6H2O , respectively, in the presence of (Ph3PNPPh3)Cl. They form black crystals, which were characterized by X-ray structure determinations.[Ph3PNPPh3]2[Fe2Se2(Se5)2] · 2 DMF: Space group P21/c, Z = 2, 2801 observed unique reflexions, R = 0.077. Lattice dimensions at 20 °C: a = 1091.6(7), b = 1247.3(5), c = 3070(2) pm, β = 90.77(4)°. In the dimeric anion the Fe atoms are linked via two bridging Se atoms, and each Fe atom is chelated by an Se5 group. In the crystals, there are alternating layers o f cations and anions. [Ph3PNPPh3]3[Co3(Se4)6] · 2 DMF : Space group P1̄, Z = 1, 3549 observed unique reflexions, R = 0.108. Lattice dimensions at 20 °C: a = 1496.2(5), b = 1504.8(5), c = 1904.1(6) pm, α = 100.31(2)°,β = 100.60(2)°, γ= 117.18(2)°. In the [Co3(Se4)6]3- ion two [Co(Se4)3]3- units, each with three chelating Se4 groups, are linked to a central Co3+ cation.
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