Darstellung und Kristallstruktur des K5Te3 / Preparation and Crystal Structure of K5Te3

1990 ◽  
Vol 45 (4) ◽  
pp. 417-422 ◽  
Author(s):  
I. Schewe ◽  
P. Böttcher

The structure of the first of the new alkali metal chalcogenides of the composition M5X3 has been solved (K5Te3: a = 13.742(2)Å, c = 6.364(2) Å, space group: I 4/m, Z = 4). It can be derived from the W5Si3 type of structure by substituting the · · · Si · · · Si · · · Si · · · chains by those of Te22--dumbbells · · · (Te–Te) · · · (Te–Te) · · · (Te–Te) · · · , both running along [001]. The Te22--dumbbells occur as a consequence of the necessity of charge compensation of the saltlike compound K5Te3, according to 2 K5Te3 ⇌ 10 K+ + Te22- + 4 Te2-. The remaining tellurium atoms not involved in the dumbbells build up strings of tetrahedra ∞1[ΚΤe4/2], with common edges along [001]. Therefore, the resulting K–K distances in these strings of tetrahedra are extremely short (3.18 A).

2010 ◽  
Vol 65 (10) ◽  
pp. 1177-1184 ◽  
Author(s):  
Sebastian A. Baer ◽  
Florian Kraus

Two new compounds containing cesium fluoride have been obtained as side-products from the reactions of Cs2CuF6 and Cs2KDyF6 with liquid ammonia. Cs2CuF6 reacts with the solvent forming a still unknown blue substance and the colorless ammoniate Cs3F3(NH3)4 which crystallizes in the cubic space group I 4̄3d (no. 220) with a = 10.273(1) Å and V = 1084.3(2) Å3 at 123 K with Z = 4. Its crystal structure is isopointal to Y3Au3Sb4 and shows an infinite three-dimensional network made up through N-H· · ·F hydrogen bonds. Ammonium cesium difluoride NH4CsF2 crystallizes in the orthorhombic space group Pnma (no. 62) with a = 7.1791(1), b = 4.1244(1), c = 13.6417(2) Å and V = 403.92(1) Å3 at 123 K with Z = 4. The crystal structure displays two-dimensional infinite layers of the composition 2 ∞[(NH4F2)−] with embedded Cs+ ions. Analogous to the structure of the compound Cs3F3(NH3)4, the structural motif is formed through strong N-H· · ·F hydrogen bonds, which seem to be the guiding force. To the best of our knowledge, the title compounds are the first reported ammoniates of alkali metal fluorides.


1996 ◽  
Vol 51 (9) ◽  
pp. 1301-1304 ◽  
Author(s):  
Matthias Asbrand ◽  
Brigitte Eisenmann

The compound K2[SnBi] was prepared by reaction of stoichiometric amounts of the elements in graphitized quartz ampoules. K2[SnBi] crystallizes in the orthorhombic system, space group Pbcm (No 57), Z = 4, with a = 680,4(3), b = 1339,(4) and c = 649,9(3) pm. The crystal structure of K2[SnBi] is characterized by folded infinite 1∞[SnBi] zigzag chains of alternating Sn and Bi atoms. The chains are bent at each Bi atom, the Sn atoms are located at the fold of the chain. Apart from the two covalent Sn-Bi bonds, each Sn atom has two additional collinear Sn-Sn contacts in direction of the fold of the chain which in terms of partial bonds can be assigned a bond order of one half. The repeating unit of the chain [Sn2Bi2]4− is strongly related to the isoelectronic butterfly [Si4]6− in Ba3Si4.


2021 ◽  
Vol 33 (6) ◽  
pp. 717-726
Author(s):  
Daniela Mauro ◽  
Cristian Biagioni ◽  
Federica Zaccarini

Abstract. Gersdorffite, ideally NiAsS, and associated minerals from Contrada Zillì (Peloritani Mountains, Sicily, Italy) have been characterized through electron microprobe analysis and X-ray diffraction. Primary minerals, hosted in quartz veins, are represented by gersdorffite, tetrahedrite-(Fe), and chalcopyrite with minor pyrite and galena. Rare aikinite inclusions were observed in tetrahedrite-(Fe) and chalcopyrite. Gersdorffite occurs as euhedral to subhedral crystals, up to 1 mm in size, with (Sb,Bi)-enriched cores and (Fe,As)-enriched rims. Its chemical composition is (Ni0.79−0.95Fe0.18−0.04Co0.04−0.01)(As0.90−1.03Sb0.10−0.00Bi0.02−0.00)S0.98−0.92. It crystallizes in the space group P213, with unit-cell parameters a=5.6968(7) Å, V=184.88(7) Å3, and Z=4, and its crystal structure was refined down to R1= 0.035. Associated tetrahedrite-(Fe) has chemical formula (Cu5.79Ag0.07)Σ5.86(Cu3.96Fe1.59Zn0.45)Σ6.00(Sb3.95As0.17Bi0.03)Σ4.15S13.06, with unit-cell parameters a= 10.3815(10) Å, V=1118.9(3) Å3, and space group I-43m. Its crystal structure was refined to R1=0.027. Textural and crystallographic data suggest a polyphasic crystallization of gersdorffite under low-temperature conditions.


1994 ◽  
Vol 49 (3) ◽  
pp. 301-308 ◽  
Author(s):  
Rolf Meyer zu Köcker ◽  
Andreas Behrendt ◽  
Kurt Dehnicke ◽  
Dieter Fenske

Abstract The title compounds have been prepared as black-blue crystals with metallic lustre by the reaction of CuCl2 and CuCl, respectively, with Me3SiNPMe3 in CH2Cl2 suspensions. The complexes have been characterized by cyclic voltammetry and by crystal structure determinations.[Cu6Cl6(NPMe3)4]Cl[Me3SiNPMe3] · CH2Cl2: Space group P212121, Z = 4, structure solution with 4407 unique observed reflections, R = 0.057. Lattice dimensions at -70 °C: a -1159.3(8), b = 2027.1(14), c = 2063.3(12) pm. The compound consists of cluster ions [Cu6Cl6(NPMe3)4]+, in which the copper atoms form a regular octahedron. Four planes of the octahedra are capped by μ3-nitrogen atoms of the (NPMe3)- groups. Each of the Cu atoms is connected with a terminal chlorine atom . Another chloride ion serves for charge compensation; this ion occupies another Cu3 plane of the octahedron. Without bonding interaction one Me3SiNPMe3 molecule and one CH2Cl2 molecule are included in the lattice. [Cu6Cl6(NPMe3)4][Cu(Me3SiNPMe3)2]Cl2: Space group Pna21, Z = 4, structure solution with 5676 unique observed reflections, R = 0.071. Lattice dimensions at -70 °C: a = 3117.2(21), b = 1927.4(11), c = 1002.7(8) pm. The compound consists of cluster ions [Cu6Cl6(NPMe3)4]+, the complex ion [Cu(Me3SiNPMe3)2]+, and chloride ions. In the cation [Cu(Me3SiNPMe3)2]+ the copper atom is linearly coordinated by the nitrogen atoms of the phosphaneimine molecules.


1998 ◽  
Vol 51 (12) ◽  
pp. 1131 ◽  
Author(s):  
Donald C. Craig ◽  
Marcia L. Scudder ◽  
Wendy-Anne McHale ◽  
Harold A. Goodwin

The crystal structures of bis(2,2′:6′,2″-terpyridine)ruthenium(II) perchlorate hydrate, bis(2,2′:6′,2″- terpyridine)osmium(II) perchlorate hemihydrate and bis((1,10-phenanthrolin-2-yl)(pyridin-2-yl)- amine)iron(II) tetrafluoroborate dihydrate are described. In the terpyridine complexes the ruthenium-nitrogen distances and the corresponding osmium-nitrogen distances are not significantly different. In both complexes the ligand geometry and the metal ion environment show the distortions usual for bis(terpyridine) systems. Distortions are less marked in the bis((1,10-phenanthrolin-2-yl)(pyridin-2-yl)amine)iron(II) cation in which each tridentate unit forms one five-membered and one six-membered chelate ring. [Ru(trpy)2] [ClO4]2.(H2O)1.1: tetragonal, space group I 41/a, a, b 12·527(2), c 40·202(11) Å, Z 8. [Os(trpy)2] [ClO4]2.(H2O)0·5: monoclinic, space group P 21/n, a 8·842(3), b 8·861(1), c 39·22(2) Å, β93·89(2)°, Z 4. [Fe(phpyam)2] [BF4]2.(H2O)2: triclinic, space group P -1, a 12·43(1), b 12·45(1), c 13·35(1) Å, α 62·70(10), β 78·55(8), γ 72·46(9)°, Z 2.


1994 ◽  
Vol 49 (1) ◽  
pp. 1-4 ◽  
Author(s):  
Rolf Minkwitz ◽  
Detlef Konikowski ◽  
Hans Preut

Abstract The crystal structure of SbCl4F is reported. SbCl4F crystallizes in the tetragonal space group I 4̄ with a = 1278.4(6), c = 774.1(5) pm, V = 1265(1) • 106 pm3 and Z = 8. Four SbCl4F units are linked via symmetric Sb-F-contacts forming an eight-membered heterocycles.


1992 ◽  
Vol 47 (2) ◽  
pp. 201-204 ◽  
Author(s):  
Kurt O. Klepp

Fibrous red crystals of the new compound K2TiS3 were obtained by reacting K2S, Ti and S at 1070 K. K2TiS3 is monoclinic, space group C 2/c with a = 11.667(6) Å, b = 8.325(4) Å, c = 6.494(4) Å, β = 9 i.81(4)°, Z = 4. The crystal structure was refined to a conventional residual of 0.070. The atomic arrangement is characterized by pseudo-one-dimensional -∞-[TiS3]2− chains formed by distorted TiS5 square pyramids sharing opposite edges of their basal planes. The structure - though closely related to that of Cs2TiS3 - is of a new type.


2009 ◽  
Vol 64 (11-12) ◽  
pp. 1325-1328 ◽  
Author(s):  
Hanne Nuss ◽  
Martin Jansen

The two new ozonide compounds K([12]crown-4)2O3 ・ 1.5 NH3 (1) and Rb([12]crown-4)2O3 ・ 1.5 NH3 (2) were synthesized from the binary alkali metal ozonides and [12]crown-4 in liquid ammonia. The air- and temperature-sensitive red, needle-shaped compounds crystallize isostructurally in the non-centrosymmetric space group Fdd2 (no. 43) with 16 formula units per unit cell. The lattice parameters are a = 26.917(8), b = 43.25(1), c = 7.823(2) Å, V = 9108(5) Å3; and a = 26.730(6), b = 44.70(1), c = 7.739(2) Å, V = 9245(4) Å3 for 1 and 2, respectively. The structure comprises rod-like [([M([12]crown-4)2(NH3)]O3)2(NH3)] supramolecular units, forming a fishbone pattern parallel to (001). The ozonide anions are separated from the metal cations and interact only weakly with two ammonia molecules via N-H・ ・ ・O hydrogen bonds


1989 ◽  
Vol 44 (10) ◽  
pp. 1228-1232 ◽  
Author(s):  
B. Eisenmann ◽  
M. Somer

The new compounds Na4HgP2, K4ZnP2 and K4HgP2 are isotypic and crystallize in the rhombohedral system, space group R3m, Z = 3, with the lattice constants: Na4HgP2: a = 500.8(2) pm, c = 2544.7(8) pm, c/a = 5.081; K4ZnP2: a = 566.4(2) pm, c = 2610.1(8) pm, c/a = 4.608; K4HgP2: a = 567.1(2) pm, c = 2697.7(8) pm, c/a = 4.757. The crystal structure of the compound K4CdP2, formerly described in the monoclinic system (space group C2/m), has been revised (R3m, a = 568.1(2) pm, c = 2698.4(8) pm, c/a = 4.750). Linear units [P—T—P]4- with T = Zn, Cd, Hg, which are isoelectronic to the molecule HgCl2, represent the characteristic structure elements. The far infrared spectra are recorded and assigned on the basis of the [P—T—P]4- anions.


1994 ◽  
Vol 49 (8) ◽  
pp. 1123-1126
Author(s):  
Kerstin Müllera ◽  
Klaus-Jürgen Range ◽  
Anton M. Heyns

Single crystals of the title compound have been obtained by neutralization of formic acid with solid rubidium carbonate and subsequent solvent evaporation at room temperature. The very hygroscopic crystals are orthorhombic, space group Pbca (Nr. 61), with a = 7.614(1), b = 17.926(2), c = 7.862(1) Å and Z = 8. The structure, which has been refined to R = 0.072 and Rw = 0.067 for 1008 unique reflections, is isotypic with that of the analogous potassium compound. It comprises layers of edge-sharing distorted RbO8 square antiprisms, sandwiched between two adjacent formate layers. The sandwiches are hold together by O···H···O inter­actions, which are, however, rather weak.


Sign in / Sign up

Export Citation Format

Share Document