Synthesis and Crystal Structure of Tetraphenylarsonium Pentachlorocarbonylosmate(IV), (Ph4As)[OsCl5(CO)]

1997 ◽  
Vol 52 (8) ◽  
pp. 978-980 ◽  
Author(s):  
M Höhling ◽  
W Preetz
Keyword(s):  
Crystal Structure ◽  
Complex Anion ◽  
Structure Type ◽  
Close Packing ◽  
Cation Sublattice ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Positional Disorder ◽  
Intermolecular Contacts

The structure of tetraphenylarsonium pentachlorocarbonylosmate(IV), (Ph4As)[OsCl5(CO)], the first example of a halogenocarbonyl complex with osmium in the oxidation state +IV, has been determined at 208 K by single crystal X-ray diffraction: tetragonal, space group P4/n with a = 12.821 , c = 8.084 Å, Z = 2. There are short intermolecular contacts between neighbouring anions along the tetragonal axis c and unusually large displacement ellipsoids of the carbonyl group and the four equatorial Cl ligands arising from a positional disorder of the complex anion. By analogy with a variety of reported structures of the (Ph4As)[RuNCl4] structure type this is attributed to the close packing of the cation sublattice. Compared to other monocarbonylosmates the Os-C bond of 1.94(2) Å is extraordinaryly long while the bond between Os and the trans coordinated Cl ligand of 2.286(3) Å is rather short.

Synthesis and crystal structure of (Ag,Pd)22Se6

2013 ◽  
Vol 28 (1) ◽  
pp. 13-17 ◽  
Author(s):  
F. Laufek ◽  
A. Vymazalová ◽  
D.A. Chareev ◽  
A.V. Kristavchuk ◽  
J. Drahokoupil ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Diffraction Data ◽  
Glass Tube ◽  
Structure Type ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Cell Parameters ◽  
Silica Glass Tube

The (Ag,Pd)22Se6 phase was synthesized from individual elements by silica glass tube technique and structurally characterized from powder X-ray diffraction data. The (Ag,Pd)22Se6 phase crystallizes in Fm$\overline3$m symmetry, unit-cell parameters: a = 12.3169(2) Å, V = 1862.55(5) Å3, Z = 4, and Dc = 10.01 g/cm3. The crystal structure of the (Ag,Pd)22Se6 phase represents a stuffed 3a.3a.3a superstructure of the Pd structure (fcc), where only 4 from 108 available octahedral holes are occupied. Its crystal structure is related to the Cr23C6 structure type.

Formamidinhim-Hexachloroferrat(III) Synthese und Kristallstruktur / Formamidinium-Hexachloroferrate(III) Synthesis and Crystal Structure

1985 ◽  
Vol 40 (3) ◽  
pp. 443-446 ◽  
Author(s):  
Udo Demant ◽  
Elke Conradi ◽  
Ulrich Müller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Diffraction Data ◽  
The Other ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Positional Disorder ◽  
Lattice Constants ◽  
Bond Lengths

[HC(NH2)2]3FeCl6 was obtained together with other products from the reaction of S4N4 with HCl in H2CCl2 in the presence of FeCl3. Its crystal structure was determined from X-ray diffraction data (473 independent observed reflexions, R = 0.047). Lattice constants: a = 961.6, c = 876.4 pm; tetragonal, space group P42/m, Z = 2. Of the two crystallographically independent formamidinium ions HC(NH2)2⊕, one exhibits positional disorder; the other one has C-N bond lengths of 128 pm. The FeCl63⊖ ions have symmetry C2h, but the deviation from Oh is small.

Synthesis and crystal structure of a novel hexaborate, Na2ZnB6O11

2010 ◽  
Vol 25 (1) ◽  
pp. 9-14 ◽  
Author(s):  
Y. Q. Chen ◽  
J. K. Liang ◽  
Y. X. Gu ◽  
J. Luo ◽  
J. B. Li ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Structure Type ◽  
Crystal Structure Analysis ◽  
Monoclinic Space Group ◽  
Chemical Formula ◽  
X Ray Diffraction ◽  
Calculated Density ◽  
Synthesis And Crystal Structure ◽  
X Ray

A novel hexaborate, Na2ZnB6O11, has been successfully synthesized by solid-state reaction and ab initio crystal-structure analysis has been completed using powder X-ray diffraction data. The compound crystallizes in the monoclinic space group Cc with lattice parameters a=10.7329(2) Å b=7.4080(3) Å, c=11.4822(2) Å, and β=112.16(2)°. The number of chemical formula per unit cell is Z=4 and the calculated density is 2.768(3) g/cm3. It represents a new structure type in which double-bridge-ring [B6O11]4− groups were found as fundamental building units. The infrared spectrum confirms the presence of both [BO3]3− groups and [BO4]5− groups.

Synthesis and crystal structure of a new microporous silicate with a mixed octahedral-tetrahedral framework: Cs3ScSi8O19

2004 ◽  
Vol 68 (4) ◽  
pp. 677-686 ◽  
Author(s):  
U. Kolitsch ◽  
E. Tillmanns
Keyword(s):  
Crystal Structure ◽  
Structure Type ◽  
Framework Structure ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Tetrahedral Framework ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Open Framework ◽  
Area Detector

AbstractDuring investigations of the system Sc2O3-Al2O3-TiO2-SiO2, a new, unusual microporous compound, Cs3ScSi8O19, was synthesized as colourless plates from a CsF-MoO3 flux. The crystal structure was determined from single-crystal X-ray diffraction data (Mo-Kα radiation, CCD area detector). The compound is orthorhombic, space group Pnma, with a = 11.286(2), b = 7.033(1), c = 26.714(5) Å, and Z = 4 (R1(F) = 2.6% and wR2all(F2) = 7.3%, using 3066 ‘observed’ reflections with Fo > 4σ(Fo)). The crystal structure of Cs3ScSi8O19 represents a new microporous framework structure type (‘MCV-1’), and the compound is exceptional in being the first representative of a mixed octahedral-tetrahedral framework structure, in which the [TO4]:[MO6] ratio is >6:1. The structure is based on isolated, nearly regular ScO6 octahedra [dav(Sc—O) = 2.112 Å] sharing corners with SiO4 tetrahedra to form an open framework with four-, six- and eight-membered rings; the latter are formed by SiO4 tetrahedra only. Two fully occupied Cs positions are located in large framework voids close to the six-membered rings, whereas four partly occupied and disordered Cs positions are close to very large framework voids bordered by the puckered eight-membered rings. The cavities are linked into channels parallel to [100] and [010]. The structure is compared with that of Cs2TiSi6O15 and related microporous scandium-, REE-, titano- and zirconosilicate minerals and compounds. Cs3ScSi8O19 or derivatives may be important in the context of immobilization of radioactive 137Cs waste, cationic conductivity or catalysis.

Tetraphenylphosphonium-hexachloroarsenat, PPh4[AsCl6]; Synthese und Kristallstruktur / Tetraphenylphosphonium Hexachloroarsenate, PPh4[AsCl6]; Synthesis and Crystal Structure

1990 ◽  
Vol 45 (7) ◽  
pp. 927-930 ◽  
Author(s):  
Joachim Bebendorf ◽  
Ulrich Müller
Keyword(s):  
Crystal Structure ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Positional Disorder ◽  
Rotation Axes

When ozone is passed through a solution of (PPh4)2[As2Cl8] in dichloromethane at –40 °C, first an instable red compound forms, then intense yellow PPh4[AsCl6] is obtained. The latter can also be obtained by introducing chlorine instead of ozone. The crystal structure of PPh4[AsCl6] was determined by X-ray diffraction (844 observed unique reflexions, R = 5,9%). Crystal data: tetragonal, space group P4/n, a = 1305.6(3), c = 752.2(4) pm, Z = 2. The structure is isotypic with that for other PPh4[MCl6] compounds, the octahedral AsCl6- ions being situated on fourfold rotation axes and showing a well-known positional disorder in that they are somewhat tilted against the symmetry axes due to packing strain.

scholarly journals High-pressure synthesis and crystal structure of the mixed-cation borate Ga4In4B15O33(OH)3

2019 ◽  
Vol 74 (4) ◽  
pp. 357-363
Author(s):  
Daniela Vitzthum ◽  
Hubert Huppertz
Keyword(s):  
Crystal Structure ◽  
High Pressure ◽  
High Temperature ◽  
Diffraction Data ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Mixed Cation ◽  
High Pressure High Temperature ◽  
Pressure Synthesis

AbstractThe mixed cation triel borate Ga4In4B15O33(OH)3 was synthesized in a Walker-type multianvil apparatus at high-pressure/high-temperature conditions of 12.5 GPa and 1300°C. Although the product could not be reproduced in further experiments, its crystal structure could be reliably determined via single-crystal X-ray diffraction data. Ga4In4B15O33(OH)3 crystallizes in the tetragonal space group I41/a (origin choice 2) with the lattice parameters a = 11.382(2), c = 15.244(2) Å, and V = 1974.9(4) Å3. The structure of the quaternary triel borate consists of a complex network of BO4 tetrahedra, edge-sharing InO6 octahedra in dinuclear units, and very dense edge-sharing GaO6 octahedra in tetranuclear units.

Synthesis and Crystal Structure of the Flexible Ligand Coordination Polymer [Co3(bpd)5.5(NCS)6(NH3)]n⋅2H2O(bpd= 1,4-bis (4-pyridyl)-2,3-diaza-1,3-butadiene)

2013 ◽  
Vol 803 ◽  
pp. 80-84
Author(s):  
Yu Qi Liu ◽  
Yong Yang ◽  
Rui Yang ◽  
Xiao Jun Xu
Keyword(s):  
Crystal Structure ◽  
Infrared Spectroscopy ◽  
Coordination Polymer ◽  
Single Crystal ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Elemental Analyses ◽  
Ligand Coordination ◽  
Point Symbol

A novel metalorganic coordination polymer, namely [Co3(bpd)5.5(NCS)6(NH3)]n2H2O (1) (bpd=1,4-bis (4-pyridyl)-2,3-diaza-1,3-butadiene), has been synthesized and characterized by elemental analyses, infrared spectroscopy, and single-crystal X-ray diffraction. Compound 1 presents 2D[3,4,-connected 3-nodal net with the point symbol (4268210)(4462)(8210). In addition, four identical 2D single nets is interlocked with each other in parallel, thus directly leading to the formation of a polycatenated layer (2D2D).

scholarly journals Redetermination of Sr2PdO3 from single-crystal X-ray data

2019 ◽  
Vol 75 (1) ◽  
pp. 30-32
Author(s):  
Gohil S. Thakur ◽  
Hans Reuter ◽  
Claudia Felser ◽  
Martin Jansen
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Diffraction Data ◽  
Structure Refinement ◽  
Structure Type ◽  
X Ray Diffraction ◽  
High Quality ◽  
X Ray ◽  
Cell Parameters ◽  
Anisotropic Displacement Parameters

The crystal structure redetermination of Sr2PdO3 (distrontium palladium trioxide) was carried out using high-quality single-crystal X-ray data. The Sr2PdO3 structure has been described previously in at least three reports [Wasel-Nielen & Hoppe (1970). Z. Anorg. Allg. Chem. 375, 209–213; Muller & Roy (1971). Adv. Chem. Ser. 98, 28–38; Nagata et al. (2002). J. Alloys Compd. 346, 50–56], all based on powder X-ray diffraction data. The current structure refinement of Sr2PdO3, as compared to previous powder data refinements, leads to more precise cell parameters and fractional coordinates, together with anisotropic displacement parameters for all sites. The compound is confirmed to have the orthorhombic Sr2CuO3 structure type (space group Immm) as reported previously. The structure consists of infinite chains of corner-sharing PdO4 plaquettes interspersed by SrII atoms. A brief comparison of Sr2PdO3 with the related K2NiF4 structure type is given.

scholarly journals Redetermination of the crystal structure of RhPb2 from single-crystal X-ray diffraction data, revealing a rhodium deficiency

2021 ◽  
Vol 77 (12) ◽  
Author(s):  
Takashi Mochiku ◽  
Yoshitaka Matsushita ◽  
Nikola Subotić ◽  
Takanari Kashiwagi ◽  
Kazuo Kadowaki
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Diffraction Data ◽  
Structure Type ◽  
Site Symmetry ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cell Parameters ◽  
Anisotropic Displacement Parameters ◽  
Slight Deficiency

RhPb2 (rhodium dilead) is a superconductor crystallizing in the CuAl2 structure type (space group I4/mcm). The Rh and Pb atoms are located at the 4a (site symmetry 422) and 8h (m.2m) sites, respectively. The crystal structure is composed of [RhPb8] antiprisms, which share their square faces along the c axis and the edges in the direction perpendicular to the c axis. We have succeeded in growing single crystals of RhPb2 and have re-determined the crystal structure on basis of single-crystal X-ray diffraction data. In comparison with the previous structure studies using powder X-ray diffraction data [Wallbaum (1943). Z. Metallkd. 35, 218–221; Havinga et al. (1972). J. Less-Common Met. 27, 169–186], the current structure analysis of RhPb2 leads to more precise unit-cell parameters and fractional coordinates, together with anisotropic displacement parameters for the two atoms. In addition and likewise different from the previous studies, we have found a slight deficiency of Rh in RhPb2, leading to a refined formula of Rh0.950 (9)Pb2.

scholarly journals Rubidium tetrafluoridobromate(III): redetermination of the crystal structure from single-crystal X-ray diffraction data

IUCrData ◽  
2019 ◽  
Vol 4 (11) ◽  
Author(s):  
Artem V. Malin ◽  
Sergei I. Ivlev ◽  
Roman V. Ostvald ◽  
Florian Kraus
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Diffraction Data ◽  
Structure Type ◽  
X Ray Diffraction ◽  
X Ray ◽  
Square Planar ◽  
Atomic Coordinates

Single crystals of rubidium tetrafluoridobromate(III), RbBrF4, were grown by melting and recrystallizing RbBrF4 from its melt. This is the first determination of the crystal structure of RbBrF4 using single-crystal X-ray diffraction data. We confirmed that the structure contains square-planar [BrF4]− anions and rubidium cations that are coordinated by F atoms in a square-antiprismatic manner. The compound crystallizes in the KBrF4 structure type. Atomic coordinates and bond lengths and angles were determined with higher precision than in a previous report based on powder X-ray diffraction data [Ivlev et al. (2015). Z. Anorg. Allg. Chem. 641, 2593–2598].

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