Synthese und Kristallstruktur der ersten zinkhaltigen Pyroborate Ni1,5Zn0,5(B2O5) und Co1,5Zn0,5(B2O5) / Synthesis and Crystal Structure of the First Zinc Containing Pyroborates Ni1,5Zn0,5(B2O5) and Co1,5Zn0,5(B2O5)

1995 ◽  
Vol 50 (10) ◽  
pp. 1445-1449 ◽  
Author(s):  
Silke Busche ◽  
Karsten Bluhm

The first zinc containing pyroborates Ni1,5Zn0,5(B2O5) (A ) and Co1,5Zn0,5(B2O5) (B) were prepared by using a B2O3 flux technique. Single crystals were investigated by X-ray diffraction and showed triclinic symmetry, space group Ci1-P1̅. The structures are isotypic to Co2(B2O5) with the lattice parameters (A ) a = 331.28(6), b = 613.87(11), c = 922.2(2), α = 104.067(11) °, β = 90.672(13) °, γ = 92.413(12) ° and (B) a = 315.89(2), b = 612.84(6), c = 927.72(6), α = 104.103(7) °, β = 91.020(6) °, γ = 92.540(7) °, Z = 2. All metal point positions show an octahedral oxygen coordination and a partly statistical distribution of Zn2+ and Ni2+ or Co2+, respectively. Isolated nearly planar B2O5 units connect ribbons consisting of edge sharing metal octahedra.

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.


1996 ◽  
Vol 51 (10) ◽  
pp. 1433-1438 ◽  
Author(s):  
Anne Utzolino ◽  
Karsten Bluhm

The compounds MnII2MnIII(BO3)O2 (I) and MnIISrMnIII(BO3)O2 (II) were prepared by using a B2O3 flux technique. Single crystals were investigated by X-ray diffraction. I showed orthorhombic symmetry, space group D92h - Pbam (No. 55), a = 926.0; b = 1241.5; c = 304.96pm ; Z = 4 and II monoclinic symmetry, space group C12h - P2/m (No. 10), a = 1107.5; b = 311.04; c = 542.93 pm, β = 95,10(2)°; Z = 2. MnII2MnIII(BO3)O2 i is isotypic with the mineral Ludwigite while MnnIISrMnmIII(BO3)O2 is isostructural with the mineral Hulsite. In the structure of MnII2Mnlll(BO3)O2 (I) all metal point positions showed octahedral oxygen coordination, one point position is occupied by Mn3+ . The structure of Mnll2Sr2Mnlll2(BO3)2O4 (II) contains five octahedrally coordinated metal sites, three of them statistically occupied by Mn2+ or Mn 3+ and Sr2+. The incorperation of Sr2+ seems to be responsible for the Hulsite structure. Both structures contain isolated, trigonal planar BO3 units and oxygen atoms that are not coordinated to boron.


1996 ◽  
Vol 51 (7) ◽  
pp. 912-916 ◽  
Author(s):  
Anne Utzolino ◽  
Karsten Bluhm

The compounds MnCo(B2O5) (I) and MnMg(B2O5) (II) were prepared by using B2O3 flux techniques in an argon atmosphere. X-ray investigations on single crystals showed triclinic symmetry, space group Ci1 - P1̄, I: a = 320.94(10), b = 619.20(11), c = 939.0(2) pm, a = 104.38(2)°, β = 90.76(2)°, γ = 92.046(14)° and II: a = 318.97(7), b = 619.8(2), c = 936.7(2) pm, α = 104.47(2)°, β = 90.60(2)°, γ = 91.98(2)° Z = 2. Their structures are isotypic with Co2(B2O5). All metal ions are octahedrally coordinated by six oxygen atoms. The structures contain diborate anions B2O54-. Each boron atom is threefold coordinated by oxygen.


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 (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.


1994 ◽  
Vol 49 (8) ◽  
pp. 1145-1149 ◽  
Author(s):  
Holger Szillat ◽  
Hanskarl Müller-Buschbaum

Single crystals of Cu0.25Ho1.25W2O8 were prepared by recrystallization from melts and investigated by X-ray diffractometer technique. Cu0.25Ho1.25W2O8 crystallizes with mono­clinic symmetry, space group C2/c, a = 19.123, b = 5.613, c = 11.479 Å, β = 111.44°. Z = 8. It represents a new structure type characterized by W4O18 groups and Cu+/Ho3+ at one point position in statistical distribution. Cu+/Ho3+ show an octahedral coordination. Another point position is occupied by Ho3+ with C. N. = 7.


1995 ◽  
Vol 50 (2) ◽  
pp. 252-256 ◽  
Author(s):  
H. Szillat ◽  
Hk. Müller-Buschbaum

Single crystals of AgKCu3Mo4O16 have been prepared by crystallization from melts and investigated by X-ray diffractometer techniques. This compound crystallizes with monoclinic symmetry, space group C2h5 - P21/c, a = 5.056(1), b = 14.546(4), c = 19.858(9) Å, β = 86.64(5)°, Z = 4. The crystal structure of AgKCu3Mo4O16 is closely related to K2Cu3Mo4O16 showing ribbons of edge-sharing CuO6 and AgO7 polyhedra. The ribbons are linked by tetrahedrally coordinated molybdenum and K2O10 groups. Another kind of MoO4 tetrahedra occupies the cavities inside the ribbons. The crystal structure and the coordination of silver, copper, potassium and molybdenum by oxygen are discussed with respect to K2Cu3Mo4O16.


1995 ◽  
Vol 50 (4) ◽  
pp. 585-588 ◽  
Author(s):  
S. Frenzen ◽  
Hk. Müller-Buschbaum

Single crystals of Ba9Ru3.2Mn5.8O27 have been prepared by flux techniques. X-ray four circle diffractometer measurements led to trigonal (rhombohedral) symmetry, space group D53d - R3̄̄̄m , a = 5.7043(5), c = 21.255(4) Å , Z = 1. This phase is isotypic to BaRuO3. The crystal structure and the occupation of the M3O12 triple octahedra by ruthenium and manganese are discussed with respect to other oxides containing M3O12 groups in an ordered and disordered way.


1995 ◽  
Vol 50 (8) ◽  
pp. 1146-1150 ◽  
Author(s):  
Anne Utzolino ◽  
Karsten Bluhm

Single crystals of the compounds MnFe(BO3)O (I) and MnAl0.5Y0.5(BO3)O (II), were obtained by a B2O3 flux technique. I crystallizes with orthorhombic symmetry, space group D162h -Pnma (Nr.62), a = 939.92; b = 319.41; c = 939.11 pm; Z = 4 and II with monoclinic symmetry, space group C52h-P21/n (Nr. 14). a = 325.6; b = 955.1; c = 929.2 pm; β = 90.70° ; Z = 4. I is isotypic to the mineral Warwickite, while II is a distorded variant of this structure. All metal ions are octahedrally coordinated. Both structures contain isolated, trigonal planar BO3 units and oxygen atoms that are not coordinated to boron.


1995 ◽  
Vol 50 (6) ◽  
pp. 879-883 ◽  
Author(s):  
H. Szillat ◽  
Hk. Müller-Buschbaum

Single crystals of Ag0.5Cu3V0,5Mo2,5O12 have been prepared by crystallization from melts and investigated by X -ray methods. They crystallize with triclinic symmetry, space group Ci1 -P 1̄ , a = 6.797(6), b = 8.575(6), c = 9.897(7) Å, α = 103.47(6), β = 103.69(6), γ = 101.48(6)° and Z = 4. The crystal structure is characterized by chains of edge-sharing CuO6 octahedra and CuO5 pyramids. Special features of this com pound are the square planar surrounding of Ag+ by O2− and a statistical distribution of molybdenum and vanadium at one point position.


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