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.

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.

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.

scholarly journals Synthesis and crystal structure of two new phosphates with Alluaudite type structure: (M, Mn)3Fe(PO4)3 (M= Ca, Cd)

2018 ◽  
Vol 149 ◽  
pp. 01084 ◽  
Author(s):  
Ghaleb Alhakmi ◽  
Abderrazzak Assani ◽  
Mohamed Saadi ◽  
Lahcen El Ammari
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Type Structure ◽  
X Ray Diffraction ◽  
Monoclinic System ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Open Framework ◽  
Bivalent Cations ◽  
The Common

Two new phosphates with alluaudite type structure (M, Mn)3Fe(PO4)3 (M= Ca, Cd), namely Ca1.54Mn1.46Fe(PO4)3 and Cd0.66Mn2.34Fe(PO4)3, has been synthesized by a solid state reaction and characterized by single-crystal X-ray diffraction. The two compounds crystallize in the monoclinic system with C2/c space group. Their open framework results from (Fe1/Mn1)2O10 units of edge-sharing (Fe/Mn)O6 octahedra, which alternate with M(1)O6 octahedra (M(1)=Ca1/Mn2 or Cd1/Mn2) that form infinite chains running along [10-1] direction. These chains are linked together through the common corners of PO4 tetrahedra giving rise to two types of tunnels occupied by bivalent cations Ca2+ or Cd2+ and Mn2+.

High-pressure synthesis and crystal structure of In3B5O12

2017 ◽  
Vol 72 (1) ◽  
pp. 69-76 ◽  
Author(s):  
Daniela Vitzthum ◽  
Michael Schauperl ◽  
Klaus R. Liedl ◽  
Hubert Huppertz
Keyword(s):  
Crystal Structure ◽  
High Pressure ◽  
Room Temperature ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
High Pressure High Temperature ◽  
Pressure Synthesis ◽  
Ir And Raman

AbstractOrthorhombic In3B5O12 was synthesized in a Walker-type multianvil apparatus under high-pressure/high-temperature conditions of 12.2 GPa and 1500°C. Its structure is isotypic to the rare earth analogs RE3B5O12 (RE=Sc, Er–Lu). In the field of indium borate chemistry, In3B5O12 is the third known ternary indium borate besides InBO3 and InB5O9. The crystal structure of In3B5O12 has been determined via single-crystal X-ray diffraction data collected at room temperature. It crystallizes in the orthorhombic space group Pmna with the lattice parameters a=12.570(2), b=4.5141(4), c=12.397(2) Å, and V=703.4(2) Å3. IR and Raman bands of In3B5O12 were theoretically determined and assigned to experimentally recorded spectra.

Synthesis and Crystal Structure of Pergolide Sulfoxide

1998 ◽  
Vol 63 (6) ◽  
pp. 803-812 ◽  
Author(s):  
Jan Čejka ◽  
Zdeněk Horák ◽  
Svetlana Pakhomova ◽  
Bohumil Kratochvíl ◽  
Petr Sedmera ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Hydrogen Peroxide ◽  
Ergot Alkaloids ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray

Pergolide sulfoxide (1), a metabolite of pergolide (2), has been prepared by oxidation of 2 with hydrogen peroxide. Its structure was determined by X-ray diffraction and compared with the structures of related ergot alkaloids. Two molecules of pergolide (S)- and (R)-sulfoxide crystallize with one molecule of water in the orthorhombic space group P212121 with a = 12.216(3) Å, b = 13.733(2) Å, c = 22.186(6) Å, Z = 4, V = 3 722(2) Å3.

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 Oxysulfide Gd6+xTi4 –xS10 – yO6+y (where x ~ 0.04 and y ~ 0.27)

2004 ◽  
Vol 59 (9) ◽  
pp. 963-968 ◽  
Author(s):  
Vincent Meignen ◽  
Alain Meerschaut ◽  
Laurent Cario ◽  
Alain Lafond
Keyword(s):  
Crystal Structure ◽  
Quaternary System ◽  
Fused Silica ◽  
Silica Tube ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Lattice Constants ◽  
New Phase

A new phase in the quaternary system Gd/Ti/S/O was obtained from a mixture of Gd2O3, Gd2S3, TiO2, TiS2 and Ti by a solid state reaction at 1323 K in a sealed fused-silica tube. The structure of Gd6+xTi4−xS10−yO6+y (where x ~ 0.04, and y ~ 0.27), was solved by single-crystal X-ray diffraction, with R(obs) = 2.69% for 2391 reflections (I > 3σ (I)) and 155 variables. This compound crystallizes with four formula units in the orthorhombic space group Pnma, and the lattice constants (Å ): a = 13.991(1), b = 3.7124(2), c = 34.029(3) Å. The structure is built up from the stacking of ribbons of five Gd-polyhedra alternating with ribbons of five Ti- and Gd/Ti-polyhedra along the a-axis. This is the first example of a rare earth (RE) and titanium oxysulfide compound that shows mixed RE/Ti sites together with pure RE- and Ti-sites. Gd6+xTi4−xS10−yO6+y is a mixed-valent titanium oxysulfide in which half of the Ti cations are Ti3+ and half are Ti4+.

Darstellung und Kristallstruktur von Bis(triphenylphosphin)-decahydro-hypho-hexaboran [(PPh3)2B6H10]·CH2Cl2 / Synthesis and Crystal Structure of Bis(triphenylphosphine)-decahydro-hypho-hexaborane[( PPh3)2B6H10]CH2Cl2

1998 ◽  
Vol 53 (11) ◽  
pp. 1326-1328 ◽  
Author(s):  
T. Schaper ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray

By reaction of [B6H6]2- with (PPh3)3AgCl in dichloromethane the belt-shaped hypho-hexaborane adduct [(PPh3)2B6H10] is formed. The crystal structure of [(PPh3)2B6H10]·CH2Cl2 has been determined by single crystal X-ray diffraction analysis: orthorhombic, space group Pbnb with a = 9.804(3), b = 17.864(4), c = 21.334(2) Å, Z = 4.

The seriesRE5Li2Sn7(RE= Ce, Pr, Nd, Sm) revisited: crystal structure ofRE5Li2−xSn7+x[0 ≤x≤ 0.03 (1)]

2013 ◽  
Vol 70 (1) ◽  
pp. 2-6 ◽  
Author(s):  
Julien P. A. Makongo ◽  
Svilen Bobev
Keyword(s):  
Crystal Structure ◽  
Structure Type ◽  
Intermetallic Phases ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
Pearson Symbol ◽  
High Temperature Reactions ◽  
Compositional Variations

The series ofRE5Li2Sn7(RE= Ce–Sm) compounds were synthesized by high-temperature reactions and structurally characterized by single-crystal X-ray diffraction. The compounds are pentacerium dilithium heptastannide, Ce5Li1.97Sn7.03, pentapreseodymium dilithium heptastannide, Pr5Li1.98Sn7.02, pentaneodymium dilithium heptastannide, Nd5Li1.99Sn7.01, and pentasamarium dilithium heptastannide, Sm5Li2Sn7. All five compounds crystallize in the chiral orthorhombic space groupP212121(No. 19), which is relatively uncommon among intermetallic phases. The structure belongs to the Ce5Li2Sn7structure type (Pearson symboloP56), with 14 unique atoms in the asymmetric unit. Minor compositional variations exist, due to the mixed occupancy of Li and Sn atoms at one of the Li sites. The small occupational disorder is most evident forRE5Li2−xSn7+x(RE= Ce, Pr;x≃ 0.03), while the structure of Nd5Li2Sn7and Sm5Li2Sn7show no apparent disorder.

scholarly journals High-pressure synthesis and crystal structure of the samarium meta-oxoborate γ-Sm(BO2)3

2020 ◽  
Vol 75 (6-7) ◽  
pp. 589-595
Author(s):  
Birgit Fuchs ◽  
Robert O. Kindler ◽  
Gunter Heymann ◽  
Hubert Huppertz
Keyword(s):  
Crystal Structure ◽  
High Pressure ◽  
Rare Earth ◽  
Earth Element ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
High Pressure High Temperature ◽  
Pressure Synthesis

Abstractγ-Sm(BO2)3 was obtained via a high-pressure/high-temperature approach in a multi-anvil apparatus at 10 GPa and 1673 K. It crystallizes in the orthorhombic space group Pca21 (no. 29) with the lattice parameters a = 18.3088(8), b = 4.4181(2), and c = 4.2551(2) Å. The compound was analysed by means of X-ray diffraction and vibrational spectroscopy. The structure is isotypic to that of the already known meta-oxoborates γ-RE(BO2)3 (RE = La−Nd) and built up of a highly condensed borate framework containing three-, four-, six-, and ten-membered rings. Next to neodymium, samarium represents the second rare earth element that forms the α-, β-, and γ-modification of the four known rare earth meta-oxoborate structure types.

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