Zur Synthese und Kristallstruktur von Bariumboroarsenat Ba(BAsO5) mit einem Beitrag über Bariumorthoarsenat Ba3(AsO4)2 / Synthesis and Crystal Structure of Barium Boroarsenate Ba(BAsO5) with a Contribution on Barium Orthoarsenate Ba3(AsO4)2

1996 ◽  
Vol 51 (5) ◽  
pp. 722-726 ◽  
Author(s):  
Cheong-Hwa Park ◽  
Karsten Bluhm

Single crystals of Ba(BAsO5) (I) and Ba3(AsO4)2 (II) were obtained by melting B2O3, arsenic pentoxide and BaO at 1100°C. Both compounds crystallize trigonally, space groups (I): C32 - P31 (Nr. 144), (II): D3d5 - R3̄m (Nr. 166), with the lattice parameters (I): a = 726.7(1), c = 710.6(1) pm, Z = 3 and (II): a = 576.7(1), c = 2116.3(2) pm, Z = 3. Ba(BAsO5) is isotypic to Pb(BAsO5) (Stillwellite structure) and Ba3(AsO4)2 to Ba3(PO4)2. The structure of Ba(BAsO5) is characterized by helical chains of rings of two borate tetrahedra and one arsenate tetrahedron. Barium is tenfold coordinated by oxygen. A rod-like sequence of coordination polyhedra, AsO4- Ba(2)O10-Ba(1)O12-Ba(2)O10-AsO4 is characteristic in the crystal structure of Ba3(AsO4)2.

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+.


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. 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.


IUCrData ◽  
2018 ◽  
Vol 3 (2) ◽  
Author(s):  
H. Lars Deubner ◽  
Florian Kraus

Single crystals of ThI4, thorium(IV) tetraiodide, were grown from thorium dioxide and aluminium triiodide. In comparison with the structure model reported previously for this compound [Zalkinet al.(1964).Inorg. Chem.3, 639–644], we have determined the lattice parameters and fractional coordinates to a much higher precision, also leading to a better reliability factor (R= 0.029versus0.09). The coordination number of the ThIVatom is eight. Its coordination polyhedron has the shape of an irregular square antiprism. The I atoms each bridge two ThIVatoms, resulting in the formation of infinite layers parallel to (-101) that can be described with the Niggli formula2∞[ThI6/2I2/2].


1990 ◽  
Vol 45 (10) ◽  
pp. 1393-1397 ◽  
Author(s):  
Gerlinde Frenzen ◽  
Werner Massa ◽  
Thilo Ernst ◽  
Kurt Dehnicke

[VCl2(15-crown-5)]+[VOCl4]- has been prepared by the reaction of VCl4 with 15-crown-5 in acetonitrile solution in the presence of water, forming black-brown single crystals. They were characterized by IR spectroscopy as well as by an X-ray structure determination. Space group Pnma, Z = 4, 1530 observed unique reflexions, R = 0.052. Lattice dimensions at -120°C: a = 1128.5(4), b = 1063.3(3), c = 1680(1) pm. The compound forms ions, in which the cation contains vanadium(+III), which is seven coordinate by the five oxygen atoms of the crown ether molecule and by two chlorine atoms in axial positions of a pentagonal bipyramide. The [VOCl4]- anion contains vanadium (+V) with approximately tetragonal symmetry


2012 ◽  
Vol 67 (6) ◽  
pp. 543-548 ◽  
Author(s):  
Hans-Christian Böttcher ◽  
Peter Mayer ◽  
Hubert Schmidbaur

The synthesis and the characterization of the complex salt [Au(tBu2PH)2][HCl2] (2) resulting from the reaction of hydrogen tetrachloridoaurate(III) hydrate with tBu2PH in dichloromethane at room temperature is reported. Single crystals of 2 have been analyzed by X-ray crystallography: monoclinic, P21=c, Z = 12, a = 12:0805(3), b = 12:3729(4), c = 46:7506(13) Å ; ß = 90:948(2)°; V = 6986:9(3) Å3; T = 173(2) K. The hydrogen bihalide anions [HCl2]- fill the interstices between the large complex cations [Au(tBu2PH)2]+ in the crystal.


2011 ◽  
Vol 66 (8) ◽  
pp. 868-870 ◽  
Author(s):  
Florian Kraus ◽  
Sebastian A. Baer

The synthesis and crystal structure of the first ammine complex of a cerium fluoride, tetraammine tetrafluorido cerium(IV) ammonia (1/1), [CeF4(NH3)4] ・NH3, are presented. The compound crystallizes in the form of colorless, block-shaped single crystals in the tetragonal space group P4/ncc with a = 9.03215(9), c = 10.96404(17) Å , V = 894.443(19) Å3, and Z = 4. The compound contains discrete [CeF4(NH3)4] molecules interconnected by N-H···F hydrogen bonds.


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.


Author(s):  
Elhassan Benhsina ◽  
Jamal Khmiyas ◽  
Said Ouaatta ◽  
Abderrazzak Assani ◽  
Mohamed Saadi ◽  
...  

Single crystals of sodium copper(II) indium bis[phosphate(V)], NaCuIn(PO4)2, were grown from the melt under atmospheric conditions. The title phosphate crystallizes in the space group P21/n and is isotypic with KCuFe(PO4)2. In the crystal, two [CuO5] trigonal bipyramids share an edge to form a dimer [Cu2O8] that is connected to two PO4 tetrahedra. The obtained [Cu2P2O12] units are interconnected through vertices to form sheets that are sandwiched between undulating layers resulting from the junction of PO4 tetrahedra and [InO6] octahedra. The two types of layers are alternately stacked along [101] and are joined into a three-dimensional framework through vertex- and edge-sharing, leaving channels parallel to the stacking direction. The channels host the sodium cations that are surrounded by four oxygen atoms in form of a distorted disphenoid.


2002 ◽  
Vol 57 (12) ◽  
pp. 1353-1358 ◽  
Author(s):  
Mar’yana Lukachuk ◽  
Rainer Pöttgen

The ternary indides Zr5Rh2In4 and Hf5Rh2In2 were synthesized by high-frequency melting of the elements in glassy carbon crucibles in a water-cooled sample chamber. Both compounds have been investigated by X-ray diffraction on powders and single crystals: Lu5Ni2In4 type, Pbam, a = 1739.8(2), b = 758.3(1), c = 337.42(5) pm, wR2 = 0.0420, 1015 F2 values for Zr5Rh2In4, and a = 1732.1(3), b = 757.5(2), c = 333.36(7) pm, wR2 = 0.0534, 739 F2 values for Hf5Rh2In4 with 36 variables per refinement. The structures contain three crystallographically different zirconium(hafnium) siteswith coordination numbers 12, 14, and 16. Striking structural motifs are distorted rhodium-centered trigonal prisms formed by the zirconium(hafnium) atoms and CuAu related distorted cubes of zirconium (hafnium) and indium atoms. The shortest interatomic distances occur for Zr-Rh and Hf-Rh followed by Rh-In. Chemical bonding in these intermetallics is briefly discussed.


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