Methanolothermale Synthese und Kristallstruktur von Tetraselenidoarsenaten( V) und -antimonaten(V) des Rubidiums und Cäsiums / Methanolothermal Synthesis and Crystal Structure of Tetraselenidoarsenates(V) and -antimonates(V) of Rubidium and Cesium

1996 ◽  
Vol 51 (1) ◽  
pp. 32-36 ◽  
Author(s):  
Michael Wachhold ◽  
William S. Sheldrick

Abstract Tetraselenidoarsenates(V) and -antimonates(V), Rubidium, Cesium, Methanolothermal Synthesis, Crystal Structure Methanolothermal reaction of M2CO3 (M = Rb, Cs) with E2Se3 (E = As, Sb) and Se at temperatures in the range 180 -200°C leads to the formation of tetraselenidoarsenates(V) and -antimonates(V) M3ESe4 in moderate to quantitative yields. All four compounds crystallize in the (NH4)3AsS4 structure type (space group Pnma) and contain isolated slightly distorted tetrahedral ESe3-4 anions with crystallographic CS symmetry. Both of the independent cations are coordinated in an irregular manner by seven Se atoms.

1996 ◽  
Vol 51 (3) ◽  
pp. 319-324 ◽  
Author(s):  
Silke Busche ◽  
Karsten Bluhm

Abstract Single crystals of the new compound Ba2KZn3(B3O6)(B6O13) were obtained by using a B2O3 flux technique; they crystallize in an as yet unknown structure type. X-ray investigations led to the space group Ci1-P1̄ (Nr.2) with lattice parameters a = 705.2(2), b = 712.5(2), c = 1880.3(6), a = 93.43(3)°, β = 90.72(2)°, γ = 119.57(2)°, Z = 2. The structure contains (B3O6)3--rings and a new discrete (B6O13)8- anion, which is composed of two BO4 and two B2O5 units. Zn2+ is tetrahedrally coordinated by oxygen and two out of three tenfold coordinated Ba-sites are statistically occupied by Ba2+ and K+.


Inorganics ◽  
2018 ◽  
Vol 6 (4) ◽  
pp. 109 ◽  
Author(s):  
Dickson O. Ojwang ◽  
Svilen Bobev

Reported are the synthesis and crystal structure of Ba7Li11Bi10, a new ternary compound crystallizing in its own type with the monoclinic space group C2/m (a = 18.407(3) Å, b = 5.0258(9) Å, and c = 18.353(3) Å; β = 104.43(1)°; Pearson symbol mS56), and those of the structurally related quaternary phases Ba4(Li1−xGax)7Sb6, Ba4(Li1−xInx)7Sb6, Ba4(Li1−xInx)7Bi6, and Eu4(Li1−xInx)7Bi6 (crystallizing in the Eu4Li7Bi6 structure type with the same monoclinic space group C2/m (a = 18.4045(13)–17.642(4) Å, b = 5.012(4)–4.8297(10) Å, and c = 13.2792(10)–12.850(3) Å, β = 126.80(1)–125.85(1)°; Pearson symbol mS34). All studied compounds are identified among the products of the high-temperature reactions of the corresponding elements. Both types of crystal structures are based on corner- and edge-linked Li-centered Sb4 (or Bi4) tetrahedra, Sb6 (or Bi6) octahedra, and Sb2 or Bi2 dumbbells. Given the similarities between the two structures, it might be proposed that they represent the simplest members of a potentially large homologous series described with the general formulae (BaLi3Sb2)n(Ba3Li4Sb4)m or (BaLi3Bi2)n(Ba3Li4Bi4)m, where the more complicated “7-11-10” phase is the member with n = 2 and m = 1, while the “4-7-6” one is the intergrowth of the two components in an equal ratio. The computed electronic band structures of Ba7Li11Bi10 and idealized Ba4Li7Bi6 (a model for Ba4(Li1−xInx)7Bi6) are also discussed.


1996 ◽  
Vol 51 (3) ◽  
pp. 309-312 ◽  
Author(s):  
Silke Busche ◽  
Karsten Bluhm

Abstract Single crystals of the new compound Ba2Zn(B3O6)2 were obtained by using a B2O3 flux technique. They crystallize in an as yet unknown structure type. X-ray investigations led to space group Ci1-P1̄ (Nr.2) with lattice parameters a = 715.5(2), b = 720.5(2), c = 1178.9(4), a = 78.96(2)°, β = 85.45(2)°, γ = 60.12(1)°, Z = 2. The structure is characterized by iso­lated (B3O6)3--rings and contains two ninefold coordinated Ba-sites. Zn2+ is tetrahedrally coordinated by oxygen. The relation to the crystal structures of high-temperature BaB2O4 and Ba2Ca(B3O6)2 is discussed.


1979 ◽  
Vol 34 (9) ◽  
pp. 1213-1217 ◽  
Author(s):  
R. Schmelczer ◽  
D. Schwarzenbach ◽  
F. Hulliger

Abstract Eu11Sb10 crystallizes in the tetragonal Ho11Ge10 structure type, space group I4/mmm, with a = 12.325(2), c = 18.024(4) Å; Z = 4. Large thermal parameters of certain atoms and unusual interatomic distances might suggest that the true structure is slightly distorted, but attempts to desymmetrize the structure were unsuccessful. Analogous anomalies occur in most of the other representatives of the Ho11Ge10 type. Eu11Sb10 appears to be metallic. It contains divalent Eu and is antiferromagnetic below TN ≈ 5 K. Other new representatives of the Ho11Ge10 structure type are Sr11Sb10, Sr11Bi10 and Ba11Sb10.


2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Julia Rienmüller ◽  
Jascha Bandemehr ◽  
Florian Kraus

Abstract We report on the syntheses and single-crystal structure determinations of the compounds A 2SiF6 (A = Tl, Rb, Cs). In comparison to the previous powder-based structure models we achieved more precise atom positions and distances. The compounds crystallize in the K2PtCl6 structure type, space group Fm 3 ‾ $‾{3}$ m (No. 225, cF36) with a = 8.4749(10) Å, V = 608.7(2) Å3, Z = 4 at T = 100 K for Tl2SiF6, a = 8.3918(10) Å, V = 591.0(2) Å3, Z = 4 at T = 100 K for Rb2SiF6, and a = 8.8638(11) Å, V = 696.4(3) Å3, Z = 4 at T = 200 K for Cs2SiF6. For the compound Tl3[SiF6]F we present a previously unknown tetragonal modification and correct the crystal structure of its trigonal modification to hexagonal. The tetragonal one crystallizes in the (NH4)3[SiF6]F structure type, space group P4/mbm (No. 127, tP22) with a = 8.0313(8), c = 5.8932(6) Å, V = 380.13(7) Å3, Z = 2, T = 298 K, and the crystal structure of the hexagonal modification is best described in space group P63 mc (No. 186, hP22) with a = 7.8248(4), c = 6.8768(4) Å, V = 364.64(4) Å3, Z = 2, T = 100 K.


1995 ◽  
Vol 50 (5) ◽  
pp. 717-720 ◽  
Author(s):  
H. Szillat ◽  
Hk. Müller-Buschbaum

Abstract Single crystals of the hitherto unknown compound CuSbMo2O8 were prepared by recrystallization from melts in closed copper tubes and investigated by X-ray diffractometer technique. CuSbMo2O8 crystallizes in a new structure type with monoclinic symmetry, space group C62h - I12/a1, a = 5.554(2), b = 4.916(1), c = 21.519(4) Å, β = 93.42(3)°, Z = 4. The crystal structure shows SbIII in a one-sided coordination by four oxygen. Molybdenum shows the rare octahedral coordination by oxygen. MoO6 and CuO6 octahedra form triple layers stacked and connected by Sb ions along [001].


1994 ◽  
Vol 49 (10) ◽  
pp. 1329-1333 ◽  
Author(s):  
F.-D. Martin ◽  
Hk. Müller-Buschbaum

Abstract Single crystals of NaMg1.64Cu0.36V3O10 have been prepared by heating mixtures of Na2CO3, MgCO3, CuO and V2O5 above the melting point. The yellow crystals show triclinic symmetry, space group Ci1-P1̅, a = 6.726(8), b = 6.743(7), c = 9.625(2) Å, α = 100.705(9), β = 104.57(1), γ = 101.700(9)°, Z = 2. NaMg1.64Cu0.36V3O10 represents a new structure type showing V3O10 groups, a statistical distribution of Mg2+ and Cu2+ on two point positions, and Na+ in an irregular coordination.


1992 ◽  
Vol 47 (12) ◽  
pp. 1746-1748 ◽  
Author(s):  
Christian Hardt ◽  
Petra Vogt ◽  
Horst Sabrowsky

Colorless K4O(CN)2 has been prepared. The compound crystallizes in the tetragonal anti-K2NiF4 structure type (space group I4/mmm) with a = 515.5(1) and c = 1606.7(3) pm, Z = 2. The structure was determined by single crystal X-ray diffraction, R = 3.35%.


1994 ◽  
Vol 49 (3) ◽  
pp. 350-354 ◽  
Author(s):  
Holger Szillat ◽  
Hanskarl Müller-Buschbaum

Abstract Single crystals of KCuHo2Mo4O16 have been prepared by recrystallisation from melts and investigated by X-ray diffractometer techniques. The compound crystallizes with monoclinic symmetry, space group C 2/c, a = 521.6(1), b = 1251.3(2), c = 1953.1(2) pm, β = 92.903(18)°, Z = 4. KCuHo2Mo4O16 represents a new structure type characterized by HoO8 and alternate CuO6/KO10 polyhedra chains. The connection of these polyhedra chains to each other and by MoO4 tetrahedra is described and the crystal structure discussed with respect to related compounds of the CuLnMo2O8 and KLnMo2O8 types.


2010 ◽  
Vol 65 (12) ◽  
pp. 1416-1426 ◽  
Author(s):  
Johannes Bender ◽  
Andreas Wohlfarth ◽  
Constantin Hoch

Several new alkali metal oxometallates with anions built up from tetrahedral [MO4] units were obtained in reactions aimed at the formation of alkali metal suboxometallates or by thermally decomposing the latter. Rubidium orthoaluminate tetrahydroxide Rb9(AlO4)(OH)4 crystallizes with a new structure type (space group P21/c, a = 13.116(1), b = 6.9266(5), c = 18.934(2) A , β = 92.05(1)°, V = 1719.0(3) Å3, Z = 4, R1 = 0.0352) and contains orthoaluminate anions [AlO4]5− and isolated hydroxide anions. Rubidium orthogallate Rb5GaO4 crystallizes with the Na5GaO4 structure type (space group Pbca, a = 6.9318(5), b = 21.309(2), c = 11.740(1) Å, V = 1734.2(3) Å3, Z = 8, R1 = 0.0423) with isolated orthogallate anions [GaO4]5−. Cesium chromate oxide Cs10(CrO4)2O adopts the Cs10(GeO4)2O structure type (space group P21/c, a = 12.903(1), b = 11.4523(8), c = 19.074(3) Å , β = 127.903(8)°,V = 2223.9(4) Å3, Z = 4, R1 = 0.0326) with orthochromate(IV) anions [CrO4]4− and isolated oxide anions. In all orthometallates the anions [MO4]n− deviate only slightly from ideal tetrahedral symmetry. Cesium diindate Cs8In2O7 crystallizes with the Cs8Fe2O7 structure type (space group P21/c, a = 7.4307(6), b = 18.6181(14), c = 7.2639(6) Å , β = 119.225(8)°, V = 877.0(1) Å3, Z = 2, R1 = 0.0349). A single-crystal structure investigation at r. t. has shown linear diindate units, but the temperature dependence of the libration angles from TLS studies for the bridging oxygen atom suggests a slightly bent and dynamically disordered diindate anion.


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