The Bayer-Villiger oxidation of diamantanone and the structure of 11-oxo-10-oxapentacyclo[7,4,1,14,13,02,7,06,12]-pentadecane

1989 ◽  
Vol 54 (12) ◽  
pp. 3260-3266 ◽  
Author(s):  
Jan Ondráček ◽  
Josef Janků ◽  
Jiří Novotný ◽  
Luděk Vodička ◽  
László Csordás ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
General Position ◽  
Direct Methods ◽  
Inverse Image ◽  
Unit Cell ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
C Nmr ◽  
Villiger Oxidation

The studied substance was prepared by the Bayer-Villiger oxidation of diamantanone and identified by 1H and 13C NMR spectroscopy. The structure of the compound was solved by direct methods and refined to the value R = 0.052 for 845 observed reflections (I > 1.96σ(I)). The substance crystallizes in the orthorhombic space group Pnnm; a = 23.595(4), b = 10.284(2), c = 6.676(1) Å. The unit cell of the crystal structure of 11-oxo-10-oxapentacyclo[7,4,1,14,13,02,7,06,12]pentadecane contains four ordered and two disordered molecules. The disordered molecule is described by averaging the image of the ordered molecule and its inverse image. Thus, the unit cell contains 6 formula units (part of the atoms have fractional occupation factors) even though the multiplicity of the general position in the Pnnm group is 8.

Crystal Structure and NMR Study of Tetrakis(acetonitrile)silver(I) Fluorosulfonate [Ag(CH3CN)4]+[SO3F]–

2014 ◽  
Vol 69 (3) ◽  
pp. 373-375 ◽  
Author(s):  
Can-Carlo Dörtbudak ◽  
Karin Lux ◽  
Andreas Kornath
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Title Compound ◽  
Unit Cell ◽  
Fluorosulfonic Acid ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Nmr Study

The title compound [Ag(CH3CN)4]+[SO3F]- crystallizes in the orthorhombic space group Pna21, a = 24:383(24), b = 8:632(11), c = 20:755(17) Å, V = 4368(6) Å3, Z = 12, with three independent formula units in the unit cell. A comparison with the isostructural compound [Ag(CH3CN)4]+ [ClO4]- is given. The salt has also been characterized by solution 1H and 19F NMR spectroscopy and the data compared to that of fluorosulfonic acid

Methansulfinylchlorid-Lewissäure-Addukte CH3S(Cl)OMF5 (M = As, Sb) und Kristallstruktur von CH3S(Cl)OSbCl5 [1] / Methanesulfinylchloride Lewis Acid Adducts CH3S(Cl)OMF5 (M = As, Sb) and Crystal Structure of CH3S(Cl)OSbCl5 [1]

1996 ◽  
Vol 51 (1) ◽  
pp. 133-138 ◽  
Author(s):  
Rolf Minkwitz ◽  
Ulrike Lohmann ◽  
Hans Preut
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Lewis Acid ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Space Group ◽  
New Compounds ◽  
Lewis Acid Adducts

Abstract CH3S(0)C1 reacts in HF as solvent with MF5 (M = As, Sb) to give products CH3S(Cl)OMF5 (M = As, Sb). The new compounds are stable below 253 K and were charac­ terized by Raman and NMR spectroscopy.In addition, the crystal structure of CH3S(Cl)OSbCl5 has been determinated. The complex crystallizes in the monoclinic space group P21/n with a = 644.3(5), b = 1905.9(14), c = 900.0(7) pm, β = 99.27(6)° with four formula units per unit cell.

Notizen: The Synthesis and Crystal Structure of (R *,R *)-(±)-[(η5-C5H5){1,2-C6H4(PMePh)2}Fe(PCl3)]Cl ··2 MeCN

1989 ◽  
Vol 44 (5) ◽  
pp. 615-618 ◽  
Author(s):  
Evamarie Hey ◽  
S. Bruce Wild ◽  
Simon G. Bott ◽  
Jerry L. Atwood
Keyword(s):  
Crystal Structure ◽  
Unit Cell ◽  
Racemic Compound ◽  
Orthorhombic Space Group ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
Solvent Molecules ◽  
Opposite Helicity

The unit cell of (R*,R*)-(±)-[(η5-C5H5){1.2-C6H4(PMePh)2}Fe(PCl3)]Cl · 2 MeCN is orthorhombic, space group Pccn, with a = 1531.2(3). b = 2202.7(20). c = 1874.6(16) pm, and Z = 8. The salt crystallizes as a racemic compound with four pairs of asymmetric cations of opposite helicity and associated anions and solvent molecules in each unit cell.

Crystal structure and topological affinities of magbasite, KBaFe3+Mg7Si8O22(OH)2F6: a trellis structure related to amphibole and carpholite

2014 ◽  
Vol 78 (1) ◽  
pp. 29-45 ◽  
Author(s):  
M. D. Welch ◽  
R. H. Mitchell ◽  
A. R. Kampf ◽  
A. R. Chakhmouradian ◽  
D. Smith ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Unit Cell ◽  
Unit Cell Parameters ◽  
Carbonatite Complex ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Cell Parameters ◽  
Structural Relations ◽  
Final Agreement

AbstractThe crystal structure of magbasite from the Eldor carbonatite complex, Quebec, Canada, has been determined and indicates that the currently accepted formula should be revised to KBaFe3+Mg7Si8O22(OH)2F6. Magbasite is orthorhombic, space group Cmme (Cmma), with unit-cell parameters a 18.9506(3) Å, b 22.5045(3) Å, c 5.2780(1) Å, V 2250.93(6) Å3 (Z = 4). The structure has been solved and refined to final agreement indices R1 = 0.026, wR2 = 0.052, GooF = 1.116 for a total of 2379 unique reflections, and is a new kind of trellis motif related to amphibole and carpholite topologies. An amphibole-like I-beam ‖(100) of edge-sharing octahedrally-coordinated M(1,2,3) sites, which are filled by Mg, is sandwiched between double-chains of SiO4 tetrahedra ‖c. This I-beam is connected to side-ribbons ‖(010) of edge-sharing (Mg,Fe2+)O4(OH,F)2 and Fe3+O4(OH)2 octahedra to form a tunnelled box or trellis structure very like that of carpholite, for which the I-beams are pyroxene-like. K occupies a tunnel site analogous to the A site of amphibole. Ba occupies a cavity site at the corners where the I-beam and side-ribbon meet, and corresponds to the A site of carpholite. The structural relations between magbasite and carpholite are discussed.

Crystal structure of 1,6-anhydro-1(6)-thio-β-D-glucopyranose S-oxide

1991 ◽  
Vol 56 (10) ◽  
pp. 2169-2174 ◽  
Author(s):  
Jiří Novotný ◽  
Jaroslav Podlaha ◽  
Miloslav Černý
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Title Compound ◽  
Direct Methods ◽  
Orthorhombic Space Group ◽  
Space Group

The crystals of the title compound are orthorhombic, space group P212121, a = 6.193(1), b = 6.3734(7), c = 38.553(6)Å, Z = 8. The structure was solved by direct methods and refined to R = 0.035 for 1 460 independent reflections. It is composed of two crystallographically independent but chemically almost identical molecules. The structure is stabilized by hydrogen bonding characterized by strong participation of the sulfoxide groups. A comparison with the structure of the thio derivative demonstrates that the exo-sulfoxide oxygen influences very little the overall conformation of the bicyclic skeleton.

scholarly journals Crystal structure of chain silicate Cs3LuSi3O9

2021 ◽  
Vol 77 (12) ◽  
Author(s):  
Hiromitsu Kimura ◽  
Hisanori Yamane
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Title Compound ◽  
Three Dimensional ◽  
Unit Cell ◽  
Single Chain ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Chain Silicate ◽  
A Chain

A caesium lutetium(III) silicate, Cs3LuSi3O9, was synthesized by heating a pelletized mixture of Cs2CO3, Lu2O3 and SiO2 at 1273 K. Single crystals of the title compound were grown in a melted area of the pellet. Cs3LuSi3O9 is a single-chain silicate (orthorhombic space group Pna21) with a chain periodicity of six and is isostructural with Cs3 RE IIIGe3O9 (RE = Pr, Nd and Sm–Yb). The two symmetry-dependent [Si6O18]12− chains in the unit cell lie parallel to the [011] direction. The Lu3+ ions are octahedrally coordinated by O atoms of the silicate chains, generating a three-dimensional framework. Cs+ ions are located in the voids in the framework.

The crystal structure of Cu2GeSe3 and the structure-types of the I2-IV-VI3 family of semiconducting compounds

2021 ◽  
Vol 77 (1) ◽  
pp. 158-167
Author(s):  
Analio Dugarte-Dugarte ◽  
Nahum Ramírez Pineda ◽  
Luis Nieves ◽  
José Antonio Henao ◽  
Graciela Díaz de Delgado ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Unit Cell Parameters ◽  
Orthorhombic Space Group ◽  
Initial Report ◽  
Space Group ◽  
Cell Parameters ◽  
Semiconducting Compounds ◽  
Bond Valence Model

Almost 50 years after the initial report, the crystal structure of Cu2GeSe3, a I2-IV-VI3 semiconductor, has been revised using modern single-crystal X-ray diffraction data. The structure of this material can be properly described in the monoclinic space group Cc (No. 9) with unit-cell parameters a = 6.7703 (4) Å, b = 11.8624 (5) Å, c = 6.7705 (4) Å, β = 108.512 (6)°, V = 515.62 (5) Å3, Z = 4, rather than in the orthorhombic space group Imm2 (No. 44) with unit-cell parameters a = 11.860 (3), b = 3.960 (1), c = 5.485 (2) Å, V = 257.61 Å3, Z = 2, as originally proposed [Parthé & Garín (1971). Monatsh. Chem. 102, 1197–1208]. Contrary to what was observed in the orthorhombic structure, the distortions of the tetrahedra in the monoclinic structure are consistent with the distortions expected from considerations derived from the bond valence model. A brief revision of the structures reported for the I2-IV-VI3 family of semiconducting compounds (I: Cu, Ag; IV: Si, Ge, Sn; and VI: S, Se, Te) is also presented.

Powder and single-crystal X-ray diffraction study of the structure of [Y(H2O)]2(C2O4)(CO3)2

2000 ◽  
Vol 56 (6) ◽  
pp. 998-1002 ◽  
Author(s):  
Thierry Bataille ◽  
Daniel Louër
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Diffraction Pattern ◽  
Powder Diffraction ◽  
Direct Methods ◽  
Unit Cell ◽  
Powder Pattern ◽  
Orthorhombic Symmetry ◽  
Direction Parallel ◽  
Space Group

From powder pattern indexing it has been demonstrated that [Y(H2O)]2(C2O4)(CO3)2, yttrium oxalate carbonate, crystallizes with orthorhombic symmetry, space group C2221, a = 7.8177 (7), b = 14.943 (1), c = 9.4845 (7) Å, V = 1108.0 (1) Å3, Z = 4. This unit cell displays a doubling of the c parameter, arising from weak diffraction lines observed in the powder diffraction pattern, with respect to results reported in the literature. The crystal structure has been solved ab initio using direct methods from powder data and has been confirmed by additional single-crystal data collected with a CCD area detector. The overall crystal structure is similar for both unit cells, except that an alternation of the carbonate groups in the direction parallel to the screw axis is displayed in the larger cell, while with the suggested half unit cell (space group C2mm) the carbonate groups would show only one orientation. The unit-cell determination strategy from single-crystal diffraction, collected with Nonius CAD-4 and Nonius Kappa CCD diffractometers, is discussed with respect to the results extracted from the powder diffraction pattern. The study demonstrates the power and usefulness of the full trace of a powder pattern for the detection of subtle structure details.

Crystal structure of semiorganic antimony thiourea bromide monohydrate crystals: a redetermination

2009 ◽  
Vol 87 (4) ◽  
pp. 345-348 ◽  
Author(s):  
Mahesha K. Upadhya ◽  
N. K. Udayashankar
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Room Temperature ◽  
Direct Methods ◽  
Unit Cell ◽  
Unit Cell Parameters ◽  
Orthorhombic Space Group ◽  
Cell Parameters ◽  
Evaporation Technique ◽  
R Value

The growth of antimony thiourea bromide monohydrate (ATBM) single crystals by evaporation technique at room temperature is reported here. Antimony thiourea bromide monohydrate crystallizes in the orthorhombic space group Cmca with unit cell parameters a = 12.320(7) Å, b = 11.668(7) Å, c = 18.615(11), and z = 8. The structure has been solved by direct methods and refined to a final R value of 0.0239.

The molecular and crystal structure of 4,4-dimethyl-6,6-diphenyl-tetrahydro-2H-pyran-2-one

1989 ◽  
Vol 54 (6) ◽  
pp. 1661-1665
Author(s):  
Jiří Novotný ◽  
Jan Ondráček ◽  
Marián Schwarz ◽  
Bohumil Kratochvíl
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Least Squares ◽  
Heterocyclic Compound ◽  
Least Squares Method ◽  
Lactone Ring ◽  
Direct Methods ◽  
Molecular And Crystal Structure ◽  
Boat Conformation ◽  
C Nmr

The molecular and crystal structure of 4,4-dimethyl-6,6-diphenyl-tetrahydro-2H-pyran-2-one was solved by direct methods and anisotropically refined by the least squares method. The final R-factor value was 0.065 for 2 181 observed reflections (I > 1.96σ (I)) and 272 refined parameters. The symmetry of the structure corresponds to the P21/c space group with lattice parameters a = 11.207(2), b = 8.168(1), c = 16.896(3) Å, β = 90.05(1)°. The unit cell contains four formula units. A lactone structure was found for this geminally substituted heterocyclic compound and was also demonstrated by 1H and 13C NMR spectroscopy. The lactone ring assumes the boat conformation.

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