Über Oxoplumbate(IV). Die Kristallstruktur von TT-Li2PbO3 [1] .On Oxoplumbates(IV) The Crystal Structure of LT-Li2PbO3 [1]

1982 ◽  
Vol 37 (11) ◽  
pp. 1369-1374 ◽  
Author(s):  
Berthold Brazel ◽  
Rudolf Hoppe
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Structure Determination ◽  
Lattice Energy ◽  
Type Structure ◽  
Ionic Radii ◽  
Glass Ampoule ◽  
Space Group ◽  
Coordination Numbers ◽  
First Time

For the first time single crystals of LT-Li2PbO3 have been prepared by decomposition of K2Li6[Pb2O8] [Incompletely closed Ag cylinders, sealed in Supremax-glass ampoule, vacuum, 690 °C, 100 d]. The structure determination [533Io(hkl); four-circle-diffractometer PW 1100, ω - scan, Mo - Kα, R = 4,86%, Rw = 4,93% confirms space group C2/c with a = 544.52(7), b = 926.12(7), c = 547,56(8) pm, β = 111.216(13)°, Z = 4, drö = 6.94 g · cm-3, dpyk = 6.89 g · cm-3. The NaCl-type structure variant is characterized by alternating layers of Li(2)+ and Li(l)+/Pb4+ cations. All atoms have octahedral coordination. The Madelung Part of Lattice Energy, MAPLE, Effective Coordination Numbers, ECoN, these via Mean Fictive Ionic Radii, MEFIR, are calculated.

Über Oxoplumbate(IV) Die Kristallstruktur von HT-Li2PbO3 [1] The Crystal Structure of HT-Li2PbO3 [1] / On Oxoplumbates(IV) The Crystal Structure of HT-Li2PbO3 [1]

1983 ◽  
Vol 38 (6) ◽  
pp. 661-664 ◽  
Author(s):  
Berthold Brazel ◽  
Rudolf Hoppe
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Structure Determination ◽  
Type Structure ◽  
Ionic Radii ◽  
Space Group ◽  
Coordination Numbers

Abstract Single crystals of HT-Li2PbO3 have been prepared by heating of mixtures of Rb2PbO3 and Li2O [Ag-cylinders, 600 °C, 100 d]. The structure determination [1005 symmetry independent l0(hkl), R = 5.85%, Rw = 5.35%, confirms space group C2/c with a = 548.60(16), b = 949.51(22), c = 1027.35(27) pm, β = 100.11(3)°, drö = 6.78 g · cm-3 , dpyk = 6.80 g · cm-3 , Z - 8. The NaCl-type structure variant is characterized by alter-nating layers of Li+ and Pb4+ /Li+ cations, which are all octahedrally coordinated. Effective Coordination Numbers, ECoN are calculated via Mean Fictive Ionic Radii, MEFIR.

Preparation and Crystal Structure of CsNa2 [BO3] and RbNa2 [BO3]

1992 ◽  
Vol 45 (9) ◽  
pp. 1427 ◽  
Author(s):  
M Schlager ◽  
R Hoppe
Keyword(s):  
Crystal Structure ◽  
Characteristic Feature ◽  
Single Crystals ◽  
Structure Determination ◽  
Lattice Energy ◽  
Exchange Reactions ◽  
Orthorhombic Space Group ◽  
Ionic Radii ◽  
Coordination Numbers ◽  
New Compounds

Colourless single crystals of hitherto unknown CsNa2 [BO3] and RbNa2 [BO3] have been prepared by exchange reactions from intimate mixtures of Li3 [BO3], Na2O, CszO and Rb2O respectively. The new compounds are isostructural with KNa2 [BO3]. The structure determination from four-circle diffractometer data confirms the orthorhombic space group Pmmn with Z = 2. CsNa2 [BO3]: a = 626.33(4), b = 579.67(4), c = 560.09(5) pm (R = 2.0%, Rw = 1.8%). RbNa2 [BO3]: a = 613.3(2), b = 568.0(2), c = 554.9(2) pm (R = 6.0%, Rw = 4.0%). A characteristic feature of the structure is face-sharing of trigonal planar [BO3] groups with distorted anticuboctahedra of [MOI2]. The Madelung Part of the Lattice Energy (MAPLE), Effective Coordination Numbers ( ECoN ), Mean Fictive Ionic Radii (MEFIR) and Charge Distribution (CHARDI) are calculated and compared with results for KNa2 [BO3].

scholarly journals Über Oxostannate(II), IV [1] Zur Kenntnis von Rb2SnO2 und K2SnO2 [2] / On Oxostannates(II), IV Rb2SnO2 and K2SnO2

1982 ◽  
Vol 37 (6) ◽  
pp. 688-694 ◽  
Author(s):  
Rolf M. Braun ◽  
Rudolf Hoppe
Keyword(s):  
Single Crystals ◽  
Lattice Energy ◽  
Yellow Powder ◽  
Light Yellow Powder ◽  
Ionic Radii ◽  
Space Group ◽  
Coordination Numbers ◽  
Binary Oxides ◽  
Light Yellow ◽  
Brown Powder

Abstract The new compound Rb2SnO2 was obtained as a light yellow powder by heating mixtures of the binary oxides (RbO0.48 + SnO, Rb: Sn = 2:1) under argon (sealed Ag cylinders, 600 °C, 3d). Subsequent annealing (550 °C, 8d and 500 °C, 17 d) led to light yellow transparent single crystals. Rb2SnO2 is extremely sensitive to moisture and decomposes into black products. It crystallizes orthorhombicly in the space group P212121-D42, with a = 5.761, b = 7.493, c= 11.167 Å, Z = 4, drö = 4.43 and dpyk = 4.46 gcm-3 , R= 11.8 and Rw = 12.0%. Effective Coordination Numbers, ECoN, these via Mean Fictive Ionic Radii, MEFIR, and the Madelung Part of Lattice Energy, MAPLE, have been calculated. Isotypic K2SnO2 was obtained similarly as a brown powder, a = 5.579, b = 7.246, c = 16.744 Å.

Two lithium tricyanomethanide compounds: syntheses and single-crystal structure determination of LiK[C(CN)3]2 and Li[C(CN)3]·½ (H3C)2CO

2015 ◽  
Vol 70 (3) ◽  
pp. 191-196 ◽  
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Structure Determination ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Cell Parameters ◽  
New Compounds

AbstractThe new compounds LiK[C(CN)3]2 and Li[C(CN)3]·½ (H3C)2CO were synthesized and their crystal structures were determined. Li[C(CN)3]·½ (H3C)2CO crystallizes in the orthorhombic space group Ima2 (no. 46) with the cell parameters a=794.97(14), b=1165.1(2) and c=1485.4(3) pm, while LiK[C(CN)3]2 adopts the monoclinic space group P21/c (no. 14) with the cell parameters a=1265.7(2), b=1068.0(2) and c=778.36(12) pm and the angle β=95.775(7)°. Single crystals of K[C(CN)3] were also acquired, and the crystal structure was refined more precisely than before corroborating earlier results.

On the dimorphism of Pr6Mo10O39

2017 ◽  
Vol 72 (11) ◽  
pp. 765-774
Author(s):  
Daniel Rudolph ◽  
Sonja Laufer ◽  
Ingo Hartenbach
Keyword(s):  
Crystal Structure ◽  
Thermal Decomposition ◽  
Single Crystals ◽  
Main Product ◽  
Molar Ratio ◽  
Coordination Environment ◽  
Space Group ◽  
Coordination Numbers ◽  
Dense Modification

AbstractAttempts to synthesize Pr4Mo7O27 using Pr, Pr6O11 and MoO3 in a molar ratio of 8:6:77 led to a main product of scheelite-type Pr0.667[MoO4] and few single crystals of the triclinic A-type Pr6Mo10O39. The latter crystallizes in space group P1̅ (a=945.25(1), b=1058.49(2), c=1815.16(3) pm; α=104.149(1), β=95.220(1), γ=102.617(1)°, Z=2). Its crystal structure comprises six crystallographically independent Pr3+ cations, eight tetrahedral [MoO4]2− units, and one [Mo2O7]2− entity. The cations display coordination numbers of seven (1×) and eight (5×), while the [MoO4]2− tetrahedra are surrounded by five Pr3+ cations each. The [Mo2O7]2− anions exhibit a coordination environment of seven Pr3+ cations. The attempt to synthesize PrF[MoO4] using PrOF (from in situ thermal decomposition of PrF[CO3]) as reagent did not lead to the desired product but to monoclinic B-type Pr6Mo10O39. This slightly less dense modification compared to its triclinic analogue crystallizes in space group C2/c (a=1247.93(3), b=1989.68(6), c=1392.52 (4) pm, β=100.505(2)°, Z=4) with three crystallographically independent Pr3+ cations, four [MoO4]2− tetrahedra, and again one [Mo2O7]2− unit in the crystal structure. Thus, both Pr6Mo10O39 modifications are better described with the structured formula Pr6[MoO4]8[Mo2O7]. The coordination numbers around the Pr3+ cations are seven (1×) and eight (2×) while all four [MoO4]2− anions are again surrounded by five Pr3+ cations each. Six of the latter represent the coordination environment around the [Mo2O7]2− entities. Besides the thorough comparison of the crystal structures single crystal Raman spectra were recorded for both Pr6Mo10O39 phases.

scholarly journals The crystal structure of alstonite, BaCa(CO3)2: an extraordinary example of ‘hidden’ complex twinning in large single crystals

2020 ◽  
Vol 84 (5) ◽  
pp. 699-704
Author(s):  
Luca Bindi ◽  
Andrew C. Roberts ◽  
Cristian Biagioni
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Structure Determination ◽  
Unit Cell ◽  
Crystal Structure Determination ◽  
Unit Cell Parameters ◽  
Space Group ◽  
Cell Parameters ◽  
Structure Determinations

AbstractAlstonite, BaCa(CO3)2, is a mineral described almost two centuries ago. It is widespread in Nature and forms magnificent cm-sized crystals. Notwithstanding, its crystal structure was still unknown. Here, we report the crystal-structure determination of the mineral and discuss it in relationship to other polymorphs of BaCa(CO3)2. Alstonite is trigonal, space group P31m, with unit-cell parameters a = 17.4360(6), c = 6.1295(2) Å, V = 1613.80(9) Å3 and Z = 12. The crystal structure was solved and refined to R1 = 0.0727 on the basis of 4515 reflections with Fo > 4σ(Fo) and 195 refined parameters. Alstonite is formed by the alternation, along c, of Ba-dominant and Ca-dominant layers, separated by CO3 groups parallel to {0001}. The main take-home message is to show that not all structure determinations of minerals/compounds can be solved routinely. Some crystals, even large ones displaying excellent diffraction quality, can be twinned in complex ways, thus making their study a crystallographic challenge.

Synthesis, single-crystal structure determination and Raman spectrum of Cu[C(CN)3]2·2 NH3

2015 ◽  
Vol 70 (3) ◽  
pp. 177-181
Author(s):  
Olaf Reckeweg ◽  
Armin Schulz ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Raman Spectroscopy ◽  
Raman Spectrum ◽  
Single Crystals ◽  
Structure Determination ◽  
Aqueous Ammonia ◽  
Ambient Conditions ◽  
Light Blue ◽  
Cell Parameters ◽  
First Time

AbstractTransparent, light blue crystals of Cu[C(CN)3]2·2 NH3 were obtained by dissolving Cu[C(CN)3]2 in aqueous ammonia and subsequent evaporation of the solvent under ambient conditions. Cu[C(CN)3]2·2 NH3 crystallizes in the space group C2/c (no. 15, Z = 4) with the cell parameters a = 1291.9(3), b = 753.18(15) and c = 1200.8(2) pm, and β = 92.68(3)°. The nature of the tricyanomethanide anion and the ammonia molecules were verified by Raman spectroscopy. Single crystals of Ag[C(CN)3] and Cu[C(CN)3]2 were synthesized, the known structures were confirmed and their Raman spectra were recorded for the first time for comparison.

Die Kristallstruktur von [Na4(OSiPh3)4(H2O)3] / The Crystal Structure of [Na4(OSiPh3)4(H2O)3]

1996 ◽  
Vol 51 (11) ◽  
pp. 1583-1586 ◽  
Author(s):  
A. Mommertza ◽  
K. Dehnickea ◽  
J. Magull
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Single Crystals ◽  
Coordination Number ◽  
Structure Determination ◽  
Title Compound ◽  
Saturated Solution ◽  
Crystal Structure Determination ◽  
Humid Atmosphere ◽  
Space Group

Colourless single crystals of the title compound are obtained from a saturated solution of NaOSiPh3 in toluene in a humid atmosphere. We have characterized [Na4(OSiPh3)H2O)3] by IR spectroscopy and by a crystal structure determination. Space group R3, Z = 6 , R = 0.056. Lattice dimensions at -70°C: a = b = 1540.3 pm, c = 2639.6 pm. The compound has the structure of a Na4O4 heterocubane which is only slighty distorted and in which one of the sodium atoms is not hydrated and shows coordination number three.

Zur Kenntnis des Systems CsF/CuF2: Über Cs7Cu6F19 [1] / On the Knowledge of the System CsF/CuF2: On Cs7CuhF19 [1]

1988 ◽  
Vol 43 (12) ◽  
pp. 1556-1566 ◽  
Author(s):  
Dieter Kissel ◽  
Rudolf Hoppe
Keyword(s):  
Single Crystals ◽  
Lattice Energy ◽  
Double Layers ◽  
Remarkable Difference ◽  
Ionic Radii ◽  
Monoclinic System ◽  
Coordination Numbers ◽  
Moisture Sensitive

Abstract In the system CsF/CuF2 Cs7Cu6F19 was obtained as transparent pale blue single crystals [closed Au-tube; carefully dried Ar; 4 weaks 720 °C. 12 weaks 760 °C] and its structure was determined. The crystals are moisture sensitive. The new fluorocuprate(II) crystallizes in the monoclinic system (P21/c) with a = 1173.1(1) pm; b = 626.56(6) pm; c = 1568.5(2) pm; β = 99.18° and Z = 2. In the structure there are units of three face shared octahedra [Cu3F12] as in Cs4Cu3F10. These triples of octahedra are connected to "double-layers" a remarkable difference as compared to Cs4Cu3F10. The distances d(Cu-F) are ranging from 185.3 to 240.5 pm. The Madelung Part of Lattice Energy, MAPLE, has been calculated and discussed and related to Effective Coordination Numbers, ECON, via Mean Fictive Ionic Radii. MEFIR

Die Kristallstruktur von [YbCl2(THF)5]+[WOCl4(THF)]- / Crystal Structure of [YbCl2(THF)5]+[WOCl4(THF)]-

1999 ◽  
Vol 54 (12) ◽  
pp. 1609-1610 ◽  
Author(s):  
M. Karl ◽  
G. Seybert ◽  
W. Massa ◽  
K. Dehnicke
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Structure Determination ◽  
Crystal Structure Determination ◽  
Chlorine Atoms ◽  
Space Group ◽  
X Ray ◽  
Ytterbium Atom ◽  
Moisture Sensitive ◽  
Tungsten Hexachloride

Blue moisture sensitive single crystals of [YbCl2(THF)5]+[WOCl4(THF)]- were obtained as a by-product from the reaction of the ytterbium trisamide Yb[N(SiMe3)2]3 with tungsten hexachloride in THF solution. The crystals were suitable for an X-ray crystal structure determination. Space group P2/c, Z = 2, lattice dimensions at -80 °C: a = 1192.5(1), b = 1117.1(1), c = 1349.9(1) pm, ß = 104.115(7)°, R = 0.0424. The structure consists of cations [YbCl2(THF)5]+ in which the ytterbium atom is coordinated in a pentagonalbipyramidal way by the chlorine atoms in the axial positions and by the oxygen atoms of the THF molecules in equatorial positions. Counterions are the well-known [WOCl4(THF)]- ions.

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