Synthese und Kristallstruktur von Lanthanoidzinkboraten LnZn(B5O10) mit Ln = Ce, Nd, Tb / Synthesis and Crystal Structure of Rare Earth Zinc Borates LnZn(B5O10) with Ln = Ce, Nd, Tb

1996 ◽  
Vol 51 (5) ◽  
pp. 671-676 ◽  
Author(s):  
Silke Busche ◽  
Karsten Bluhm

Single crystals of the new compounds LnZn(B5O10) (Ln = (A) Ce3+, (B) Nd3+, (C) T b3+) were obtained by using a B2O3 flux technique. X-ray investigations led to space group C2h5-P21/n (Nr. 14) with lattice parameters: (A) a = 874.5(1), b = 761.4(1), c = 950.0(1), β = 92.80(1)°, (B) a = 868.6(2), b = 760.9(2), c = 946.0(2), β = 92.99(2)°, (C) a = 858.2(2), b = 760.5(2), c = 939.3(2), β = 93.56(2)°, Z = 4. The structure is isotypic with CoSm(B5O10) and is characterized by two-dimensional infinite 2∞ (B5O 10)5- ions. Ln is tenfold coordinated by oxygen, and Zn2+ occupies distorted ZnO6 polyhedra.

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+.


1995 ◽  
Vol 50 (10) ◽  
pp. 1450-1454 ◽  
Author(s):  
Silke Busche ◽  
Karsten Bluhm

Single crystals of the new compounds Zn5Mn(BO3)2O4 (A ) and ZnFe(BO3)O (B) were prepared by using a B2O3 flux technique. Zn5Mn(BO3)2O4 is isostructural with Ni5Ti(BO3)2O4 and ZnFe(BO3)O is isotypic with the mineral warwickite. X-ray investigations on single crystals led to (A ) space group D92h -Pbam, a = 926.41(10), b = 1236.67(8), c = 304.55(3) pm, Z = 2, and (B) space group D162h-Pnma, a = 924.62(4), b = 314.1(10), c = 935.3(2) pm, Z = 4. The structure of Zn5Mn(BO3)2O4 (A ) contains four octahedrally coordinated metal sites, one of these statistically occupied by Zn2+ and Mn4+. In the structure of ZnFe(BO3)O the ions Zn2+ and Fe3+ occupy statistically both distorted octahedral sites. Both structures contain isolated BO3 units and oxygen that is not coordinated to boron.


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.


1996 ◽  
Vol 51 (5) ◽  
pp. 677-680 ◽  
Author(s):  
Karsten Bluhm ◽  
André Wiesch

Single crystals of NiHo2(B2O5)2 were prepared by a B2O3 flux-technique in high temperature reactions at 1450 °C and investigated by X-ray diffraction. They crystallize in the space group C2h5-P21/c (Nr. 14) with a = 451.0(4); b = 724.8(3); c = 938.8(6) pm; β = 91,39( 1)°; Z = 2. The compound is isotypic to CuTb2 (B2O5)2 as well as to the gadolinite structure (FeY2(BeSiO5)2) and contains a two dimensional infinite anion with the formula 2∞ (B2O5)4-. The borate layers consist of four- and eight-membered rings of edge-sharing BO4 tetrahedra. The layers are connected via copper-centered elongated oxygen-octahedra and slightly distorted tetragonal HoO8 antiprisms.


1995 ◽  
Vol 50 (4) ◽  
pp. 577-580 ◽  
Author(s):  
H. Szillat ◽  
Hk. Müller-Buschbaum

Single crystals of (Cu0.22Mg0.78)BaNd2Mo4O16 have been prepared by crystallization from melts and investigated by X-ray methods. The compound crystallizes monoclinically, space group C62h - C12/c1, Z = 4, a = 5.351(1), b = 12.891(2), c = 19.391(4) Å,β = 90.899(14)° and is isotypic to CuKHo2Mo4O16. The crystal structure is dominated by BaO10 and NdO8 polyhedra forming a three-dimensional polyhedra network, which is filled by axially distorted (Cu,Mg)O6 octahedra and MoO4 tetrahedra.


2011 ◽  
Vol 66 (1) ◽  
pp. 21-26
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo

Single crystals of Sr2H3I andBa5H2I3.9(2)O2 were obtained by reacting Sr or Ba, respectively, with dried and sublimed NH4I in a 4 : 1 molar ratio in silica-jacketed Nb ampoules for 13 h at 1200 K. The crystal structures of the new compounds have been determined by means of single-crystal X-ray diffraction. Sr2H3I crystallizes in a stuffed anti-CdI2 structure isotypic to Ba2H3Cl in the space group P3m1 (no. 164) with the lattice parameters a = 426.0(1) and c = 774.9(2) pm, while Ba5H2I3.9(2)O2 crystallizes in a new structure type in the space group Cmcm (no. 63) with the lattice parameters a = 1721.0(2), b = 1452.5(2) and c = 639.03(9) pm. The structural results for Sr2H3I are corroborated by EUTAX calculations. For the disordered compound Ba5H2I3.9(2)O2, EUTAX calculations on an approximated, ordered structural model were used to find possible insights into the disorder


1994 ◽  
Vol 49 (3) ◽  
pp. 355-359 ◽  
Author(s):  
F.-D. Martin ◽  
H. Müller-Buschbaum

Abstract Single crystals of KBaCuV2O7Cl have been prepared by a flux technique and investigated by X-ray analysis. The compound crystallizes with tetragonal symmetry, space group C24v-P4 bm, a = 8.8581, c = 5.4711 Å, Z = 2. The crystal structure shows Cu2+ within a one sided strongly distorted CuO4Cl2 octahedron. The copper ion is shifted towards the nearer Cl- neighbour to form a CuO4Cl square pyramid. Two VO4 tetrahedra are connected to give stretched V2O7 double tetrahedra, and linked in planes via the oxygen corners of the CuO4Cl pyramids. The crystal structure and the structure of the complex BaO8Cl2 polyhedron are discussed.


2011 ◽  
Vol 66 (11) ◽  
pp. 1087-1091 ◽  
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo

Colorless and transparent single crystals of Ba2H3I were obtained by reacting Ba with dried and sublimed NH4I in a 4 : 1 molar ratio in silica-jacketed Nb ampoules at 1100 K for 13 h. The crystal structure of the title compound was determined and refined by means of single-crystal X-ray diffraction. Ba2H3I crystallizes in a stuffed anti-CdI2 structure isotypic to Sr2H3I in the space group P3̄m1 (no. 164) with the lattice parameters a = 451.86(12) and c = 811.84(23) pm. The structural results for Ba2H3I are consistent with bond lengths and coordination geometries of related binary and ternary hydrides


1997 ◽  
Vol 52 (1) ◽  
pp. 102-106 ◽  
Author(s):  
K. Bluhm ◽  
C. H. Park

Single crystals of the compound α -Zn3(BO3)(PO4) were obtained at 1050 °C by using B2O3, P2O5 and ZnCO3 as starting materials and subsequent cooling to 600°C with 20°C/h. X-ray investigations on single crystals yield a new crystal structure in the monoclinic space group Cm - (Nr. 8) with a = 972.5(2); b = 1272.0(3); c = 487.4(3) pm; β = 119.80 (4)°; Z = 4. The structure contains isolated trigonally planar BO3 and tetrahedral PO4 units which are not joined together. Zinc occupies three crystallographically different point positions and is trigonal-bipyramidally, tetragonal-pyramidally or distorted tetrahedrally coordinated by oxygen


1995 ◽  
Vol 50 (2) ◽  
pp. 261-264 ◽  
Author(s):  
H. Szillat ◽  
Hk. Müller-Buschbaum

Single crystals of Cu3MgSb1.4O6 have been prepared by crystallization from melts and investigated by X-ray diffractometer techniques. Cu3MgSb1.4O6 crystallizes trigonally, space group C3v6 - R3/c, a = 5.348(1), c = 34.482(8) A, Z = 6, with a Delafossite related new structure, characterized by layers containing SbO6 and MgO6 octahedra. These layers are connected by O-Cu-O dumb-bells. The crystal structure is discussed with respect to the Delafossite type.


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