Die Kristallstruktur von K2S3 und K2Se3

The Crystal Structure of K₂S₃ and K₂Se₃ Well formed crystals of K₂S₃ and K₂Se₃ were obtained by reaction of the elements in liquid ammonia at 500 bar and 150°C. The substances are both orthorhombic, space group Cmc2₁. Cell constants are: The structure contains S₃^2?(Se₃^2?) polyanions, with S? S? S(Se? Se? Se) angles of 105.4(102.5)°. The S? S(Se? Se) distance is 2.083(2.383) Å.     

Synthese und Kristallstruktur von K2Mn3S4

Synthesis and Crystal Structure of K₂Mn₃S₄ Single crystals of K₂Mn₃S₄ have been prepared by a fusion reaction of potassium carbonate with manganese in a stream of hydrogen sulfide at 900 °C. K₂Mn₃S₄ crystallizes in a new monoclinic layered structure type (P2/c, a = 7.244(2) Å, b = 5.822(1) Å, c = 11.018(5) Å, β = 112.33(3)°, Z = 2) which can be described as a stacking variant of the orthorhombic Cs₂Mn₃S₄ structure type. Measurements of the magnetic susceptibilities show antiferro‐magnetic interactions.     

Die trikline Kristallstruktur von Ag2Bi2S3Cl2: Pseudosymmetrie und Zwillingsbildung

Ruby‐red crystals of Ag₂Bi₂S₃Cl₂ were synthesized from AgCl and Bi₂S₃ by cooling a melt from 770 K to room temperature. X‐ray diffraction on powders and single‐crystals revealed a triclinic crystal structure with special lattice constants (P &1macr; (No. 2), a = 1085.0(2), b = 717.2(1), c = 1137.6(1) pm, α = 89.80(1)?, β = 74.80(1)?, γ = 87.81(1)?). In the structure [Bi^IIIS₃Cl₄] polyhedra form 2[BiS_3/2Cl_4/4]^‐ double‐layers by sharing common faces and edges. The silver(I) cations between the layers are coordinated either octahedrally by sulfide ions or tetrahedrally by sulfide and chloride ions. The deviations from the monoclinic space group P 1 2₁/c 1 are small and induce twinning along [010]. Further pseudosymmetry is based on the stacking of layer packages with the symmetry of the layer group P (2/c) 2₁/c 2/b.     

Die Kristallstruktur von B(OC2H4)3N

Zusammenfassung B(OC₂H₄)₃N kristallisiert in der Raumgruppe P ca2₁ mit den Gitterkonstantena=11,46,b=6,62,c=9,79 Å undZ=4. Die Struktur konnte mit direkten Methoden und mit sukzessivenFouriersynthesen aufgeklärt werden [570 F(hkl), R=9,8%]. Bor befindet sich in tetraedrischer Umgebung von Sauerstoff (B–O 1,431, 1,432, 1,475 Å) und Stickstoff (B–N 1,693 Å). In der Struktur bestehen zwischen den Komplexen keine Wasserstoffbrücken.

---

The crystal structure ofB(OC ₂H₄)₃ N. Triethanolamine complexes, IV

B(OC₂H₄)₃N crystallizes in space group P ca2₁ with cell dimensionsa=11.46,b=6.62,c=9.79 Å andZ=4. The structure has been solved by direct methods and byFourier syntheses [570 F(hkl), R=9.8%]. Boron is tetrahedrally surrounded by oxygen (B–O 1.431, 1.432, 1.475 Å) and nitrogen atoms (B–N 1.693 Å). In the structure no hydrogen bonds exist between the complexes.

---

---

Mit 3 Abbildungen     

Die Kristallstruktur von Li2SnO3

Li₂SnO₃ crystallises monoclinic, C, with a = 5.295, b = 9.184, c = 10.032 Å and β = 100.13°; Z = 8. The positions of Sn were obtained from PATTERSON maps and the positions of O and Li by FOURIER difference method. Parameters were refined by least squares-method [1462 reflexes (h 01)–(h 71); R = 10.5%]. The average distances of Li? O are 2.07 Å, and 2.20 Å for Sn? O. The Li₂SnO₃ structure can be derived from the NaCl type: in a cubic closest packing of oxygen 2/3 of the octahedral holes are occupied by lithium and 1/3 by tin.     

Die Kristallstruktur von Ru2Si3

The crystal structure of Ru₂Si₃ has been refined by leastsquares using three-dimensional X-ray data from a twinned crystal (1355 reflections,R=5.8%). Ru₂Si₃ is isostructural with Ru₂Ge₃ and like this compound a member of the Mn₁₁Si₁₉ structure family. The lattice parameters of the orthorhombic unit cell (Pnca—D ₁₄ ^2h ) are:a=5.530 (1),b=11.060 (2) andc=8.952 (2) Å.

---

---

Mit 1 Abbildung     

Zur Kristallstruktur von Ba2ZnO3

On the Crystal Structure of Ba₂ZnO₃ Single crystals of Ba₂ZnO₃ were prepared by solid state reaction. It crystallizes monoclinic: space group C ? C12/c1; a = 5.833; b = 11.376; c = 12.585 Å; β = 93.63°; Z = 8. The crystal structure is characterised by [ZnO₃] chains along [100]. They are connected by Ba²⁺ in seven fold oxygen coordination.     

Zur Kristallstruktur von Tb2Se3

Crystal Structure of Tb₂Se₃ Single crystals of Tb₂Se₃ could be prepared by chemical transport reaction with AlCl₃. By starting from TbSe_1.9 and terbium metal black needles of Tb₂Se₃ in the U₂S₃ type structure with the space group Pnma and a = 1113,0(1) pm, b = 402,4(1) pm and c = 1095,1(3) pm were obtained.     

Die Kristallstruktur von Ru2Ge3

The crystal structure of Ru₂Ge₃ has been determined and refined by Fourier synthesis using pseudo-tetragonal X-ray data resulting from twinned crystals. The true symmetry is orthorhombic with space group Pnca-D _2h ¹⁴ and the lattice parameters are:a=5.718,b=11.436 andc-9.240 Å. Ru₂Ge₃ is a member of the Mn₁₁Si₁₉ structure family which is characterized by the occurrence of different compositions in the rangeTB _2?x (x≤0.75,T=transition metal andB=group III or IV metal). The compounds Ru₂Si₃, Os₂Si₃, Os₂Ge₃, and Ir₂(Ga_0.6Ge_0.4)₃ are isostructural.     

Die Kristallstruktur von Ti3GeC2

Ohne Zusammenfassung     

Die Kristallstruktur von Li2GeO3

Zusammenfassung Die Kristallstruktur von Li₂GeO₃ wird mit Hilfe dreidimensionalerFourier-Synthesen und nach der Methode der kleinsten Quadrate bestimmt. Li₂GeO₃ ist isotyp mit Li₂SiO₃ und enthält [GeO₃]^2–-Ketten (Zweiereinfachkette). Die Gitterparameter der rhombischen Elementarzelle (C _2v ¹² –Cmc2₁) betragen:a=9,63₀,b=5,46₅ undc=4,85₀ Å. Als mittlere interatomare Abstände wurden erhalten: Ge–O=1,74 und Li–O=2,01 Å.

---

The crystal structure of Li₂GeO₃ has been determined by means of 3-dimensional Fourier syntheses and least-squares method. Li₂GeO₃ is isostructural with Li₂SiO₃, containing [GeO₃]^2–-chains (Zweiereinfachkette). The lattice parameters of the orthorhombic cell (C _2v ¹² –Cmc2₁) are:a=9,63₀;b=5,46₅ andc=4,85₀ Å. The average interatomic distances are found to be: Ge–O=1,74 and Li–O=2,01 Å.

---

---

Mit 3 Abbildungen     

Die Kristallstruktur von Li2TeO3

Crystal Structure of Li₂TeO₃ Crystals of Li₂TeO₃ were prepared from melts. Li₂TeO₃ crystallizes in the monoclinic system, space group C2/c. The lattice parameters are a = 5.06₉, b = 9.56₆, c = 13.72₇ Å, β = 95.4°. The formular unit is 8. The crystal structure has been determined by Patterson and threedimensional differential Fourier synthesis refined by least squares using isotropic temperature corrections. The final R-value of 772 observed reflections is 0.101. Li₂TeO₃ forms a layer lattice consisting of trigonal TeO₃ pyramids and deformed LiO₄ tetrahedrons. The TeO₃ pyramids are only connected with the corners of LiO₄ groups, which are linked one with another by common corners and edges.     

Kristallstruktur von AuCd3

No structural transformation was found in AuCd₃, but instead a new phase AuCd_√5 with a transformation temperature of about 270 °C. AuCd₃ crystallizes in a hexagonal structure similar to the Cu₃P.r-type. The structure may be described as a vacancy and displacement variant of the CsCl structure of beta brass. One vacancy of the cell is fixed by the displacements of the surrounding atoms. The other vacancies are fairly free and appear to be responsible for the maximum in damping capacity at 400 °C. The outer core electrons may be assumed in a correlation which is also found in many representatives of the NiAs-type, while the valence electrons must be in a hexagonal primitive correlation which is highly commensurable to the core electron correlation.     

Darstellung und Kristallstruktur von ZrP2S6 und ThP2S6

Preparation and Crystal Structure of ZrP₂S₆ and ThP₂S₆ The compounds ZrP₂S₆ ( I ) and ThP₂S₆ ( II ) are synthesized from the elements at 750–800°C. They are isotypic (P4₂/m, Z = 2; I : a = 668.2, c = 948.9 pm; II : a = 688.0, c = 990.3 pm) and to be described as M⁴⁺(P₂S₆)^4?. The thiohypodiphosphate anion has ideal staggered conformation. The cation is coordinated by a (slightly deformed) 42 m dodecahedron of S atoms. The geometrical details correspond to the most favourable ligand distribution.     

Nitridsulfidchloride der Lanthanide: III. Synthese und Kristallstruktur von Pr5N3S2Cl2

Nitride Sulfide Chlorides of the Lanthanides. III. Synthesis and Crystal Structure of Pr₅N₃S₂Cl₂ By reacting praseodymium with sulfur, sodium azide and praseodymium trichloride in sealed, evacuated silica tubes (850°C, 7 d), the nitride sulfide chloride Pr₅N₃S₂Cl₂ is obtained in case of a 4:2:1:1 molar ratio of the reactants (Pr:S:NaN₃:PrCl₃). A slight excess of trichloride or the addition of NaCl as a flux supports the yield of brownish red, rod-shaped transparent crystals which prove to be stable against hydrolysis. The crystal structure (monoclinic, C2/m (no. 12), a = 1540.2(1), b = 400.92(3), c = 1656.3(1) pm, β = 101.24(1)°, Z = 4, R = 0.039, R_w = 0.028) was determined by means of X-ray single crystal data. Thus five crystallographically different cations (Pr³⁺) are present which with three distinct kinds of nitride anions (N^3?) build up two types of translationally commensurate chains from interconnected [NPr₄] tetrahedra. With an additional edge per “chain-link” in chain I, two single chains [NPr_3/3^ePr_1/1^t]³⁺ (?[NPr₂]³⁺) of cis-edge connected [NPr₄] tetrahedra (known from the Sm₄N₂S₃-type structure) are condensed into the double chain [(N1){(Pr1)_(2+2)/(2+2)^e,e(Pr2)_(2+1)/(2+1)^e,v}(N2)(Pr3)_1/1^t]³⁺ (?[N₂Pr₃]³⁺). Chain II consists of two single chains [NPr_2/2^vPr_2/1^t] ⁶⁺ (?[NPr₃]⁶⁺) of vertex-connected [NPr₄] tetrahedra (known from the Sm₃NS₃-type structure), which are condensed to the double chain [(N3)(Pr4)_2/2^e(Pr5)_2/2^v]³⁺ (?[NPr₂]³⁺) via an additional edge per “chain-link” too. Both types of chains are bundled along [010] like a closest packing of rods. Four crystallographically different but by X-ray diffraction indistinguishable anions S^2? and Cl^? hold both cationic double chains together and also adjust the charge balance in a molar ratio of 1 : 1.     

Die Kristallstruktur von ThGa2 und RuIn3

Zusammenfassung Im System: Th-Ga wird die Phase ThGa₂ mit -ThSi₂-Typ aufgefunden, im System: Ru-In werden die Phasen RuIn₃ mit CoGa₃-Struktur sowie eine Ru-reiche Phase mit hexagonal dichter Packung machgewiesen.Herrn Professor Dr.Erich Hayek zum 60. Geburtstag.     

Kristallstruktur von Pd16S7

Part of the phase diagram for the system Pd-S has been amended and part of the Pd-Cu-S diagram determined. The phase Pd₁₆S₇ has a cubic body-centred structure with 46 atoms in the cubic cell, and is related to the γ-brass structure. The phases Pd₄S, Pd₃S.h, Pd₁₆S₇, PdS and PdS₂ may be interpreted as energetically favourable in terms of the two-electron correlation model. Thus this model is also compatible with experimental results for brass-like structures with electron-rich B components.     

Darstellung und Kristallstruktur von Rb2Sb4S7

Preparation and Crystal Structure of Rb₂Sb₄S₇ The first thioantimonite of rubidium has been synthesized and its crystal structure determined. The substance crystallizes triclinic with spacegroup P1 . The lattice constants are a = 968.0(5) pm, b = 1193.4(5) pm, c = 723.1(5) pm, α = 87.68(5)°, β = 101.39(5)° and γ = 102.66(5)°. There are two formula units in the unit cell.     

Darstellung und Kristallstruktur von Cs2Sb4S7

Preparation and Crystal Structure of Cs₂Sb₄S₇ The first thioantimonite of Cesium has been synthesized and its crystal structure determined. The substance crystallizes monoclinic with spacegroup P2₁/_c. The lattice constants are a = 1111.2(5) pm, b = 1227.1(5) pm, c = 1163.7(5) pm and ß = 97.60(5)°. There are four formula units in the unit cell. Sb–S chains are formed by trigonal SbS₃ pyramids and ψ-trigonal SbS₄ bipyramids.