Ag3BiO3 und Ag5BiO4, die ersten Silberoxobismutate(III)

Ag₃BiO₃ and Ag₅BiO₄,the first Silver Oxobismuthates(III) Applying high oxygen pressures (100 MPa) Ag₃BiO₃ and Ag₅BiO₄ were prepared for the first time by reacting the binary components Ag₂O and Bi₂O₃ at temperatures between 770 and 800 K. Single crystals of both compounds were grown hydrothermally from Ag₂O and Bi₂O₃ at 620 K and at oxygen pressures of 10 MPa. The crystal structure determination (Ag₃BiO₃: I4₁, a = 14.1924(1), c = 8.7997(1) Å, Z = 16, 1 729 diffractometer data, R_w = 0.057; Ag₅BiO₄: P2₁/n, a = 5.855(1), b = 8.984(1), c = 12.457(1) Å, β = 91.49(1)Å, Z = 4, 2716 diffractometer data, R_w = 0.036) shows that in Ag₅BiO₄ bismuth approximately has a square pyramidal coordination by five oxygen atoms. Two such pyramids share an edge thus forming ‘isolated’ Bi₂O₈^10? anions. In Ag₃BiO₃ the same groups are linked by the terminal oxygen atoms to form a three dimensional network. In both structures the cation arrangements form variants of the Laves-phases MgCu₂ with silver occupying the copper positions. The Mg positions are ordered occupied by bismuth and silver.     

Ag4Bi2O5 — ein neues Silberbismutat(III)

Ag₄Bi₂O₅ — A Novel Silverbismuthate(III) Yellow single crystals of Ag₄Bi₂O₅ have been obtained for the first time by solid state reaction of Ag₂O and Bi₂O₃ applying an oxygen pressure of 10 MPa at a temperature of 473 K. According to the results of a single crystal structure determination (Pnna, a = 1428.3(2), b = 569.2(1), c = 877.7(1) pm, Z = 4, 1544 diffractometer data, R₁ = 0.050, wR² = 0.094) the anionic partial structure of Ag₄Bi₂O₅ consists of chains of corner and edge sharing BiO₄-units. The silveratoms form a network of threedimensionally connected trigonal bipyramides with Ag? Ag-contacts between 285 and 323 pm.     

New Silver Tellurates – The Crystal Structures of a Third Modification of Ag2Te2O6 and of Ag4TeO5

Single crystals of a third modification of Ag₂Te₂O₆ (denoted as Ag₂Te₂O₆–III) and of Ag₄TeO₅ have been obtained as minor by‐products during hydrothermal phase formation experiments in the system Ag‐Hg‐Te‐O. The crystal structure of Ag₂Te₂O₆–III (P2₁/c, Z = 4, a = 6.4255(10), b = 6.9852(11), c = 13.204(2) Å, β = 90.090(3)°, 1885 independent reflections, R[F² > 2σ(F²)] = 0.0334, wR2(F² all) = 0.0817) comprises tellurium in oxidation states +IV and +VI and is topologically related to the structure of the Ag₂Te₂O₆–I modification, which consists of similar layers and interjacent layers of Ag⁺ cations. Ag₄TeO₅ (C2/c, Z = 8, a = 16.271(2), b = 6.0874(10), c = 11.4373(16) Å, β = 106.730(10)°, 2372 independent reflections, R[F² > 2σ(F²)] = 0.0288, wR2(F² all) = 0.0737) is made up of a layer‐like arrangement of isolated [Te^VI₂O₁₀] double octahedra and of Ag⁺ cations situated both in layers parallel and inside the layers of the anionic moieties.     

Zur Kenntnis von Ba4Ir3O10

About Ba₄Ir₃O₁₀ Single crystals of Ba₄Ir₃O₁₀ were prepared by a flux technique. X-ray investigations show monoclinic symmetry, space group C_2h⁵–P2₁/a; a = 5.788; b = 13.222; c = 7.242 Å; β = 112.98°; Z = 2. Ir₃O₁₂ tripel, built up by face-sharing of IrO₆ octahedra, are edge-connected into wave-like twodimensional planes. Ba₄Ir₃O₁₀ is related to Ba₄(Ti, Pt)₃O₁₀.     

Synthesis and Crystal Structure of Bi（Hsal）3（1,10- phenanthroline） （Hsal = O2CC6H4-2-OH）

A new bismuth compound Bi（Hsal）3（1,10-phenanthroline） （Hsal = O2CC6H4-2-OH） has been synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in the triclinic system, space group P1, with a = 10.243（2）, b = 11.905（3）, c = 12.934（3） A, α= 76.780（6）, β= 68.683（6）,γ= 80.930（7）°, V = 1425.6（5） A^3, Dc = 1.865 g/cm^3, Mr = 800.51, F（000） = 780, μ= 6.247 mm^-1, Z = 2, R = 0.0456 and wR = 0.1131 for 5612 observed reflections （I 〉 2σ（I））. In this compound, three salicylate ligands coordinate to the Bi atom through the carboxylate groups to form a four-membered chelate ring, and phenanthroline ligand chelates the metal through two N atoms. The structure of the title compound manifests a possible coordination mode between bismuth subsalicylate and N atom containing amino acid in the biological system.     

Einkristallstrukturbestimmungen an KBiO2 und RbBiO2 und ein kristallchemischer Vergleich der Alkalimetallbismutate(III) vom Typ MBiO2 (M = Na,K, Rb,Cs)

Single Crystal Structure Determination on KBiO₂ and RbBiO₂ and a Crystal Chemical Comparison of MBiO₂ (M = Na, K, Rb, Cs) Single crystals of KBiO₂ (colourless) and RbBiO₂ (colourless) were obtained by solid state reaction of the respective binary metal oxides. Both crystal structures (KBiO₂: C2/c; a = 783.13(9), b = 790.92(1), c = 596.86(8) pm, β = 124.81(1)°; Z = 4; 445 diffractometer data; R₁ = 0.027; wR² = 0.069; RbBiO₂: C2/c; a = 806.20(5), b = 838.88(4), c = 598.14(4) pm, β = 123.68(1)°; Z = 4; 289 diffractometer data; R₁ = 0.040; wR² = 0.101) reveal infinite [BiO₂]-chains extending along the [0 0 1] direction. The compounds are isostructural with NaBiO₂ and CsBiO₂.     

Na0.74Ta3O6, ein niedervalentes Oxotantalat mit einer Ta–Ta‐Mehrfachbindung

Na_0.74Ta₃O₆, a Low‐Valent Oxotantalate with Multiple Ta–Ta Bonds The title compound was prepared in a sealed tantalum tube through the reaction of Ta₂O₅, tantalum and Na₂CO₃ in a NaCl flux at 1570 K within 5 d. The crystal structure of Na_0.74Ta₃O₆ (a = 713.5(1), b = 1027.4(2), c = 639.9(1) pm, Immm, Z = 4) was determined by single crystal X‐ray means. The structure is isomorphous with NaNb₃O₅F [1]. The characteristic structural units are triply bonded Ta1₂ dumb‐bells with eight square‐prismatically co‐ordinated O ligands. Four Ta2, each octahedrally surrounded by O atoms, are side‐on bonded weakly to the binuclear Ta₂O₈ complex, thus forming a Ta₆ propellane‐like cluster. The lattice parameters of three additional M_xTa₃O₆ phases, M = Li, Mn, and Yb, are reported.     

Bi2O3 Hierarchical Nanostructures: Controllable Synthesis,Growth Mechanism,and their Application in Photocatalysis

Flower power : Unique 3D flower‐like Bi₂O₃ hierarchical nanostructures were synthesized using a mild aqueous template‐free method (see figure). By introducing VO₃^? into the reaction system, which mediated the nucleation and growth of Bi₂O₃, the in situ self‐assembly of 3D hierarchitectures from 2D nanosheets has been realized.

     

铋配合物[Bi(S2CNC5H10)2(NO3)]·[1，10-Phen]·0.5H2O的合成及晶体结构

The bismuth complex with dithiopiperdylcarbamate [Bi(S₂CNC₅H₁₀)₂(NO₃)]·[1，10-Phen]·0.5H₂O was synthesized. The crystal and molecular structure were determined by X-ray single crystal diffraction. The crystal belongs to monoiclinic with space group C2/c, a=3.140(2) nm, b=1.176 4(9) nm, c=2.021 6(15) nm, β=103.081(12)°, V=5.713(7) nm³, Z=8, F(000)=3064, D_c=1.815 g·cm^-3, μ=6.502mm^-1. The final R₁=0.0332, wR₂=0.040 3. In the complex, the bismuth atom is eight-coordinated in a capped distorted pentagonal bipyramidal geometry. CCDC: 222655.     

NaAg3S2, ein Thioargentat mit dem Clusteranion [Ag6S4]2−

NaAg₃S₂, a Thioargentate Containing the Anionic Cluster [Ag₆S₄]^2? . Dark-red octahedrally shaped crystals of NaAg₃S₂ could be obtained by the reaction of NaAg(CN)₂ and NaCN in a stream of hydrogen sulfide at 630 K. NaAg₃S₂ crystallizes cubic, a=12.358(1) Å, space group Fd3 m, Z=16. The structure was determined from four-circle diffractometer data. NaAg₃S₂ contains the anionic cluster [Ag₆S₄]^2?. The structure can be traced back to the spinel structure typ. An extended Hückel calculation for the cluster anion, which is considered to be isolated, shows weak bonding silver-silver interactions. NaAg₃S₂ is diamagnetic at room temperature.     

Synthesis and Crystal Structure of the Heteropolymate Compound Na_3H_2[Ce_3(H_2O)_(18)Bi_2W_(22)O_(76)]·23H_2O

1 INTRODUCTION As a rich remarkable class of inorganic cluster systems, polyoxometalates continue to be the focus of significant attention in the 21th century because of their various and alluring topologies as well as their unusual physicochemical prope…     

Crystallographic report: Bi(S2CNC5H10)2(NO3)(1,10‐phenanthroline)

The structure of Bi(S₂CNC₅H₁₀)₂(NO₃)(1,10‐Phen) features an eight‐coordinated distorted square antiprismatic geometry around bismuth, defined by an N₂O₂S₄ donor set, with Bi? S distances ranging from 2.641(2) to 2.824(2) Å. Copyright © 2004 John Wiley & Sons, Ltd.     

[Rb2(H2O)2][Re3(μ-Cl)3Br7(H2O)2]2 · H2O,ein gemischtes Halogenid-Hydrat mit anionischen Dimeren {[Re3(μ-Cl)3Br7(H2O)2]2 · H2O}2−

[Rb₂(H₂O)₂][Re₃(μ-Cl)₃Br₇(H₂O)₂]₂ · H₂O, a Mixed Halide-Hydrate with the Anionic Dimer {[Re₃(μ-Cl)₃Br₇(H₂O)₂]₂ · H₂O}^2? [Rb₂(H₂O)₂][Re₃(μ-Cl)₃Br₇(H₂O)₂]₂ · H₂O crystallizes as dark redbrown single crystals from an hydrobromic-acid solution of ReCl₃ and RbBr at 0°C. An important feature of the crystal structure (monoclinic, C2/c; a = 1494.61(8); b = 835.71(4); c = 3079.96(19) pm; β = 97.801(4)°; V_m = 573.9(4) cm³mol^?1; R = 0.060; R_w = 0.038) is the connection of two anions [Re₃(μ-Cl)₃Br₇(H₂O)₂]^? via a water molecule to dimers, {[Re₃(μ-Cl)₃Br₇(H₂O)₂]₂ · H₂O}^2?. These dimeric units are contained in slabs that are stacked in the [001] direction and held together by Rb⁺ cations and crystal water.