Rb2I(OH): Ein Hydroxidiodid im System RbOH/RbI

Rb₂I(OH): A Hydroxide Iodide in the System RbOH/RbI The pseudobinary system RbOH/RbI was investigated by X-ray methods. The crystal structure of Rb₂I(OH) was solved by single crystal data: Rb₂I(OH): Pnma, Z = 4, a = 7.748(1) Å, b = 5.654(2) Å,c = 13.254(2) Å Z(F_o) with (F_o)² ? 3σ = (F_o)² = 449, Z (parameter) = 25, R/R_w = 0.021/0.023 Rb₂I(OH) crystallizes in a new type of structure, built up by a three dimensional network of [Rb₂(OH)⁺] containing the iodide ions.     

Darstellung und Kristallstruktur von Calciumimid,CaNH

Synthesis and Crystal Structure of Calcium Imide, CaNH Single-crystals of calcium imide were obtained for the first time by the reaction of a mixture of calcium amide with sodium amide at 850°C in an autoclave for salt melts. After cooling the autoclave to room temperature the crystals are embedded in solid Na which was extracted by liquid ammonia. The structure of calcium imide was determined from single-crystal diffractometer data: space group Fm3 m, Z = 4, a = 5.143(1) Å, R/R_w = 0.032/0.028 mit N(F ${}_{\text{º}}^{\text{2}}$ ? 3σ(F ${}_{\text{º}}^{\text{2}}$ )) = 26, N(Var.) = 5. Ca and N atoms are arranged in the motif of the NaCl structure type. The hydrogen atoms of the imide groups are disordered within the Ca octahedra, and they occupy a six fold split position.     

Verbindungen in den Systemen Kalium(Rubidium)/Gold/Antimon: K3Au3Sb2, Rb3Au3Sb2 und K1,74Rb0,26RbAu3Sb2

Compounds in the Systems Potassium(Rubidium)/Gold/Antimony: K₃Au₃Sb₂, Rb₃Au₃Sb₂, and K_1,74Rb_0,26RbAu₃Sb₂ Brittle, silver coloured single crystals of K₃Au₃Sb₂, Rb₃Au₃Sb₂ and K_1,74Rb_0,26RbAu₃Sb₂ were obtainded by reaction of the alkali metal azides (KN₃, RbN₃) with gold and antimon powder at 550°C. The structures of the isotypic compounds (R3 m, Z = 3) were determined by X-ray single-crystal diffractometer data: K₃Au₃Sb₂, a = 6,198(2) Å, c = 21,520(5) Å, R/R_w (w = 1) = 0,046/0,058, Z(F) ? 3σ(F) = 175, Z(Var.) = 14; Rb₃Au₃Sb₂, a = 6,443(3), c = 21,69(2), R/R_w (w = 1) = 0,059/0,082, Z(F) ? 3σ(F₀²) = 258, Z(Var.) = 14; K_1,74Rb_0,26RbAu₃Sb₂, a = 6,288(2) Å, c = 21,617(5) Å, R/R_w (w = 1) = 0,049/0,069, Z(F) ? 3σ(F) = 390, Z(Var) = 14. The compounds crystallize with the K₃Cu₃P₂-structure type. The Au? Sb partial structures consist of [AuSb_2/3] layers with linear Sb? Au? Sb dumb-bells and SbAu₃ pyramids. The layers are separated by two crystallographically independent alkali metal atoms along [001].     

Na7I2(OH)5: Ein Hydroxidiodid im System NaOH/NaI

Na₇I₂(OH)₅: A Hydroxide Iodide in the System NaOH/NaI The pseudobinary system NaOH/NaI is investigated by X-ray methods. The crystal structure of the compound Na₇I₂(OH)₅ was solved by single crystal data: Na₇I₂(OH)₅: P4/nmm, Z = 2, a = 7.748(2) Å, c = 10.260(3) Å, Z(F_o) = 443 with (F_o)² ≥ 3σ(F_o)², Z(parameter) = 28, R/R_w = 0.044/0.059 Na₇I₂(OH)₅ crystallizes in a new type of structure which contains puckered layers of ∞²[Na₇(OH)₅²⁺] connected via iodide ions.     

Zur Kenntnis von Na4Br(NH2)3: Ein Amidbromid im System NaNH2/NaBr

Na₄Br(NH₂)₃: An Amide Bromide in the System NaNH₂/NaBr The pseudobinary system NaNH₂/NaBr was investigated by X-ray methods. The crystal structure of Na₄Br(NH₂)₃ was solved by single crystal data: Pnnm, Z = 4, a = 6.579(2) Å, b = 12.755(4) Å, c = 8.776(2) Å Z(F_o) with (F_o)² ≥ 3σ = (F_o)² = 503, Z(parameter) = 39, R/R_w = 0.082/0.106. It is a new type of structure, built up by a three-dimensional network of [Na₄(NH₂)₃⁺] containing the bromide ions.     

Tetraammin-Lithium-Kationen zur Stabilisierung phenylsubstituierter Zintl-Anionen: Die Verbindung [Li(NH3)4]2[Sn2Ph4]

Tetraammine Lithium Cations Stabilizing Phenylsubstituted Zintl-Anions: The Compound [Li(NH₃)₄]₂[Sn₂Ph₄] Ruby-red, brittle single crystals of [Li(NH₃)₄]₂[Sn₂Ph₄] were synthesized by the reaction of diphenyltin dichloride and metallic lithium in liquid ammonia at ?35°C. The structure was determined from X-ray singlecrystal diffractometer data: Space group, P1 , Z = 1, a = 9.462(2) Å, b = 9.727(2) Å, c = 11.232(2) Å, α = 66.22(3)°, β = 85.78(3)°, γ = 61.83(3)°, R₁ (F ? 4σF) = 5.13%, wR₂ (F₀² ? 4σF) = 10.5%, N(F ? 4σF) = 779, N(Var.) = 163. The compound contains to Sb₂Ph₄ isosteric centres [Sn₂Ph₄]^2? as anions which are connected to rods by lithium cations in distorted tetrahedral coordination by ammonia. These rods are arranged parallel to one another in the b,c-plane, but stacked along [100].     

NaAuIn2, ein ternäres Aurid mit ethananalogen In2Au6-Baueinheiten und [In2/2]-Ketten

NaAuIn₂, a Ternary Auride with Ethane Analogous In₂Au₆ Building Units and [In_2/2] Chains Silver coloured, brittle single crystals of NaAuIn₂ were synthesized by the reaction of NaN₃, gold-sponge and indium at 500°C. The structure was determined from X-ray single-crystal diffractometry data: space group Cmcm, Z = 4, a = 4.482(1) Å, b = 10.366(2) Å, c = 7.869(2) Å, R/R_w(w = 1) = 0.017/0.020, Z(F) ≥ 3σ(F) = 547 and N(var.) = 16. NaAuIn₂ crystallizes in the MgCuAl₂-structure type. Gold and indium form a framework structure. [AuIn_6/3] layers with trigonal prismatically coordinated gold are connected via In—In contacts along [010] which consist of ethane analogous In₂Au₆-building units. The In-partial structure consists of saw tooth like [In_2/2] chains along [001]. The sodium atoms occupy channel-like cavities within the Au—In framework structure.     

Na5Br(OH)4: Darstellung und Kristallstruktur einer Verbindung im System NaOH/NaBr

Na₅Br(OH)₄: Synthesis and Structure of a Compound in the System NaOH/NaBr The pseudobinary system NaOH/NaBr is investigated by X-ray methods. The structure of the compound Na₅Br(OH)₄ was solved by single crystal data: Na₅Br(OH)₄: Pnma, Z = 8, a = 11.846(2) Å, b = 18.782(4) Å, c = 6.431(1) Å, Z(F_o) = 1 202 with (F_o)² ≥ 3σ(F_o)², Z(parameter) = 100, R/R_w = 0.030/0.035 The compound crystallizes in a new type of structure. Pairs of octahedra around O by 5 Na and 1 H to [Na₅(OH)]₂ are orientated in such a way to one another that two ions OH^? form a parallelogram hinting to unusual bent hydrogen bridge bonding.     

Unusually Stable Triazine‐based Organic Superstructures

Solid‐state reactions have been rapidly gaining popularity in organic chemistry owing to their simplicity, efficiency, and selectivity compared to liquid‐phase reactions. Herein, we describe the formation of superstructures through the solid‐state reaction of an organic single‐crystal. The superstructure of 5,5′,5′′‐(1,3,5‐triazine‐2,4,6‐triyl)triisophthalonitrile (TIPN) can be formed by cyclotrimerization of 1,3,5‐tricyanobenzene (TCB) single crystals. The TIPN superstructure was confirmed by single crystal X‐ray diffraction and visualized by transmission electron microscopy. The superstructure has hexagonally packed 1‐dimensional (1D) channels along the crystal axis. Furthermore, the superstructure arises from interdigitated nitrile interactions in the crystal lattice, and thus has electron‐beam tolerance and very high thermal stability.     

NaAuGe,ein weiteres ternäres Aurid mit ethan-analogen Ge2Au6-Baueinheiten

NaAuGe, a Further Ternary Auride with Ethane Analogous Ge₂Au₆ Building Units Black, brittle single crystals of NaAuGe were obtained by the reaction of NaN₃, gold sponge and germanium at 800°C. The structure was determined from X-ray single-crystal diffractometry data: space group Imm2, Z = 4, a = 4.422(1) Å, b = 7.238(2) Å, c = 7.531(2) Å, R1/wR2 = 0.0195/0.0482, N(F) ≥ 2σ(F) = 811 and N(var.) = 21. NaAuGe crystallizes in a new ternary variant of the KHg₂ (CeCu₂)structure type. Gold and germanium form puckered [AuGe_3/3] layers with trigonal planar coordinated gold. The [AuGe_3/3] nets are connected to a framework structure via Ge—Ge contacts along [010] which consist of ethane analogous Ge₂Au₆ building units. The sodium atoms are placed in channels of the Au—Ge framework structure which run along [100] and [010].