Structural and vibrational studies of 1,1,3,3-tetracyanopropane and 2,2,4,4,6-pentacyanocyclohexenamine

1987 ◽  
Vol 65 (2) ◽  
pp. 261-270 ◽  
Author(s):  
R. A. Bell ◽  
B. E. Brown ◽  
M. Duarte ◽  
H. E. Howard-Lock ◽  
C. J. L. Lock
Keyword(s):  
Unit Cell ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
New Methods ◽  
Cell Dimensions ◽  
Cell Data ◽  
Unit Cell Data ◽  
Monoclinic Cell ◽  
C Nmr

1,1,3,3-Tetracyanopropane, 1, was prepared in low yields by a literature method with 2,2,4,4,6-pentacyanocyclohexenamine, 2, as a major by-product. The products were examined by X-ray crystallography. 1 has an orthorhombic space group, Pbcn (No. 60) with cell dimensions, a = 7.158(2), b = 10.510(3), c = 9.733(2) Å and has four formula units in the unit cell. 2 has a monoclinic cell, P21/c (No. 14) with cell dimensions a = 14.368(3), b = 6.626(1), c = 12.300(2) Å, β = 115.60(1)° and has 4 formula units in the unit cell. Data were collected with use of MoKα radiation and a Nicolet P3 diffractometer. The crystal structures were determined by standard methods and refined to Rw = 0.037 (1) and Rw = 0.040 (2) on the basis of 782 and 2108 unique reflections. Bond lengths and angles in the two compounds are normal. 2 has what has been considered to be the less likely tautomeric structure. Both compounds were examined by 1H, 13C nmr, vibrational spectroscopy, and mass spectroscopy. For 2 there was no evidence of the alternative tautomeric structure. New methods were developed for the preparation of both compounds and the mechanism of the original reaction rationalized.

The reaction of chloro(triphenylphosphine)gold(I) with 1-methylthymine

1987 ◽  
Vol 65 (7) ◽  
pp. 1568-1575 ◽  
Author(s):  
R. Faggiani ◽  
H. E. Howard-Lock ◽  
C. J. L. Lock ◽  
M. A. Turner
Keyword(s):  
Aqueous Methanol ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Cell Dimensions ◽  
Cell Data ◽  
Unit Cell Data ◽  
Related Compounds ◽  
C Nmr

1-Methylthyminato-N3-triphenylphosphinegold(I) was prepared by reacting chloro(triphenylphosphine)gold(I) with 1-methylthymine in aqueous methanol at pH 11. The product was examined by X-ray crystallography and was found to have the orthorhombic space group C2221 (no. 20) with cell dimensions a = 12.760(7) Å, b = 11.530(2) Å, c = 31.893(5) Å, and eight formula units in the unit cell. Data were collected with use of MoKα radiation and a Syntex P21, diffractometer. The crystal structure was determined by standard methods and refined to R = 0.112 and Rw = 0.076 on the basis of 4760 unique reflections. Bond lengths and bond angles are normal. Packing in the crystal lattice is dominated by the triphenylphosphine rings which arrange roughly as blades of a propellor and are the source of the crystal's chirality. The title and related compounds were also examined by 1H nmr, 13C nmr, and vibrational spectroscopy.

X-Ray structure of tris(acetonitrile)tricarbonylrhenium(I) tetrafluoroborate

1977 ◽  
Vol 55 (1) ◽  
pp. 111-114 ◽  
Author(s):  
Lillian Y. Y. Chan ◽  
E. E. Isaacs ◽  
W. A. G. Graham
Keyword(s):  
Least Squares ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Cell Dimensions ◽  
The Mean ◽  
Unit Cell Dimensions ◽  
Cell Data ◽  
Unit Cell Data

Reaction of [n-Bu4N]2[Re4(CO)16] with AgBF4 in acetonitrile affords the compound [(CH3CN)3Re(CO)3][BF4]. The latter crystallizes in monoclinic space group P21/c with unit cell dimensions a = 11.021(5) Å, b = 11.136(5) Å, c = 12.980(6) Å, β = 96.906(25)°, and four molecules per unit cell. Data were collected by counter methods and the structure was refined using least-squares procedures to give R = 0.041. The rhenium cation is approximately octahedrally coordinated by six facially arranged ligands. The mean rhenium–nitrogen distance is 2.13 Å, and the mean rhenium–nitrogen–carbon angle in the coordinated acetonitrile is 174.7°.

Crystal data and X-ray powder diffraction data of 2,4-diiodo-4-nitrophenol (disophenol), C6H3I2NO3. More precise X-ray powder diffraction data of p-nitrophenol, C6H5NO3

1996 ◽  
Vol 11 (4) ◽  
pp. 301-304
Author(s):  
Héctor Novoa de Armas ◽  
Rolando González Hernández ◽  
José Antonio Henao Martínez ◽  
Ramón Poméz Hernández
Keyword(s):  
Powder Diffraction ◽  
Diffraction Data ◽  
Unit Cell ◽  
Crystal Data ◽  
Powder Diffraction Data ◽  
Space Group ◽  
X Ray ◽  
Cell Dimensions ◽  
Unit Cell Dimensions ◽  
Monoclinic Cell

p-nitrophenol, C6H5NO3, and disophenol, C6H3I2NO3, have been investigated by means of X-ray powder diffraction. The unit cell dimensions were determined from diffractometer methods, using monochromatic CuKα1 radiation, and evaluated by indexing programs. The monoclinic cell found for p-nitrophenol was a=6.159(2) Å, b=8.890(2) Å, c=11.770(2) Å, β=103.04(2)°, Z=4, space group P21 or P2l/m, Dx=1.469 Mg/m3. The monoclinic cell found for disophenol has the dimensions a=8.886(1) Å, b=14.088(2) Å, c=8.521(1) Å, β=91.11(1)°, Z=4, space group P2, P2, Pm or P2/m, Dx=2.438 Mg/m3.

Demicheleite-(I), BiSI, a new mineral from La Fossa Crater, Vulcano, Aeolian Islands, Italy

2010 ◽  
Vol 74 (1) ◽  
pp. 141-145 ◽  
Author(s):  
F. Demartin ◽  
C. M. Gramaccioli ◽  
I. Campostrini
Keyword(s):  
Unit Cell ◽  
Crystal Habit ◽  
New Mineral ◽  
Orthorhombic Space Group ◽  
Medium Temperature ◽  
Synthetic Compound ◽  
Calculated Density ◽  
Cell Data ◽  
Unit Cell Data ◽  
Fossa Crater

AbstractDemicheleite-(I), ideally BiSI, is the iodine-dominant analogue of demicheleite-(Br) and demicheleite-(Cl). It was found in an active medium-temperature intracrateric fumarole at La Fossa crater, Vulcano Island, Aeolian archipelago, Sicily, Italy. The mineral is the first bismuth sulphoiodide so far discovered in a wholly natural environment, and corresponds to the already known synthetic compound. It occurs as acicular to stout, translucent crystals up to 0.25 mm long in an altered pyroclastic breccia, together with demicheleite-(Br), bismoclite, bismuthinite, godovikovite, panichiite, aiolosite, brontesite, adranosite and other new phases under study. The colour is dark red to black, the lustre submetallic. The unit cell is orthorhombic, space group Pnam, with a = 8.4501(7) Å, b = 10.1470(9) Å , c = 4.1389(4) Å , V = 354.88(4) Å3, and Z = 4. The crystal habit is prismatic, with the main forms {110} and {111} inferred from analogy with demicheleite-(Br). Twinning was not observed. The strongest 6 lines in the X-ray powder diffraction pattern [dobs.(Å) (I/I0) (hkl)] are: 6.490 (100) (110); 4.346 (94) (120); 3.896 (90) (210); 2.709 (60) (310); 2.161 (38) (330); 3.243 (22) (220). The chemical analysis obtained by WDS electron microprobe gave: Bi 58.32, S 9.43, I 23.69, Br 5.66, Cl 1.01, totalling 98.11 wt.%, corresponding to an empirical formula (based on 3 a.p.f.u.) of: Bi0.97S1.03(I0.65Br0.25Cl0.10)Σ1.00. The unit-cell data are close to those of the synthetic compound, whose crystal structure is already known. The calculated density is 6.411 g cm–3.

Barium Rare Earth Titanates: X-Ray Characterization of BaR2Ti3O10 and BaR2Ti4O12: R = Lanthanide

1992 ◽  
Vol 7 (3) ◽  
pp. 176-178 ◽  
Author(s):  
X. Jing ◽  
C. Zheng ◽  
A.R. West
Keyword(s):  
Rare Earth ◽  
Solid State ◽  
Unit Cell ◽  
Lanthanide Ion ◽  
X Ray ◽  
Ion Size ◽  
Cell Data ◽  
Unit Cell Data ◽  
Cell Volumes

AbstractThe compounds, BaR2Ti3O10: R = La, Pr, Nd and Sm; BaR2Ti4O12: R = La, Pr, Sm, Gd, Eu have been prepared by solid state reaction and characterized by X-ray powder diffraction. Unit cell data are summarised; lattice parameters and unit cell volumes increase approximately linearly with lanthanide ion size.

Electron Microscopy of Alcohol Oxidase Crystals from Pichia Pastoris

1990 ◽  
Vol 48 (1) ◽  
pp. 108-109
Author(s):  
Janet Vonck ◽  
Ernst F.J. van Bruggen
Keyword(s):  
Pichia Pastoris ◽  
Hansenula Polymorpha ◽  
Alcohol Oxidase ◽  
Unit Cell ◽  
Electron Microscopic ◽  
X Ray ◽  
X Ray Crystallography ◽  
Cell Dimensions ◽  
Microscopic Studies ◽  
Unit Cell Dimensions

Several yeast species are able to grow on methanol. When they are grown in a methanol-restricted culture, their peroxisomes contain large crystalline inclusions, consisting of alcohol oxidase (AOX). A monomer of AOX has a molecular weight of ca. 74,000. Inside the peroxisome, AOX occurs as octamers.Electron microscopic studies of AOX from Hansenula polymorpha have revealed that the eight subunits are slightly elongated and form two layers of four, which are twisted relative to each other. The molecule measures ca. 12 nm in all directions.Recently, crystals suitable for x-ray diffraction have been formed of AOX from Pichia pastoris . The space group is P21, with unit cell dimensions a=157.3Å, b=171.45Å, c=231.6Å, β=94°. These dimensions indicate that the unit cell contains four octamers, too much to solve by x-ray crystallography alone. Therefore, we have started an EM study of the crystals, to get information about the organization of the molecules in the crystal lattice.

Powder Diffraction Data of Potassium Calcium Phosphate KCa PO4.H2O

1987 ◽  
Vol 2 (4) ◽  
pp. 253-254 ◽  
Author(s):  
D. Louër ◽  
F. Deneuve ◽  
N. Ouillon
Keyword(s):  
Calcium Phosphate ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Unit Cell ◽  
Powder Diffraction Data ◽  
X Ray ◽  
Cell Dimensions ◽  
Unit Cell Dimensions ◽  
Monoclinic Cell

AbstractPotassium calcium phosphate, KCa PO4.H2O, has been investigated by means of X-ray powder diffraction. Unit cell dimensions were determined from diffractometer data obtained with strictly monochromatized Cu Kα1 radiation, by indexing programs. A C-centered monoclinic cell was found: a =7.5834(9) Å, b = 8.1568(11) Å, c = 7.6541(8) Å, β= 102.975 (9)°.

Aegirine of possible authigenic origin in Middle Devonian sediments in Caithness, Scotland

1978 ◽  
Vol 42 (324) ◽  
pp. 439-442 ◽  
Author(s):  
N. J. Fortey ◽  
U. McL. Michie
Keyword(s):  
River Basin ◽  
Middle Devonian ◽  
Unit Cell ◽  
Green River Formation ◽  
Green River Basin ◽  
Green River ◽  
X Ray ◽  
Orcadian Basin ◽  
Cell Data ◽  
Unit Cell Data

SummaryAn occurrence of aegirine in Middle Devonian lacustrine beds in Caithness is described. The mineral occurs as euhedral to subhedral prismatic crystals within a finely laminated siltstone. Microprobe analyses reveal a remarkably ‘pure’ composition consisting almost entirely of Na, Fe3+, Si, and O. X-ray diffractometry yielded the unit cell data: a 9·657 Å, b 8·800 Å, c 5·296 Å, and β 107·37°. Comparison with other natural aegirine compositions shows marked differences from those of igneous or metamorphic origin but a close similarity to a unique occurrence of authigenic aegirine in the lacustrine Green River Formation of Wyoming, U.S.A. Consideration of the nature of the Caithness occurrence, and comparison of the Devonian Orcadian basin with the Eocene Green River basin indicate similar geological environments. It is suggested that the mineral formed in hypersaline conditions in which sodium may have been derived from contemporaneous alkaline volcanism within the Orcadian basin.

The preparation, characterization, and crystal and molecular structure of oxobis(ethan-1,2-dithiolato-S,µS′)technetium(V)oxo(ethan- 1,2-dithiolato-S,S′)technetium(V) [(TcO)2(SCH2CH2S)3]. A Tc(V) compound containing metal—sulfur—metal bridges

1985 ◽  
Vol 63 (2) ◽  
pp. 319-323 ◽  
Author(s):  
A. Davison ◽  
B. V. DePamphilis ◽  
R. Faggiani ◽  
A. G. Jones ◽  
C. J. L. Lock ◽  
...  
Keyword(s):  
Monoclinic Space Group ◽  
Protecting Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Thiolate Ligands ◽  
Cell Dimensions ◽  
Field Desorption Mass Spectrometry ◽  
New Type ◽  
Cell Data ◽  
Unit Cell Data

As a result of an investigation undertaken to evaluate the acetamidomethyl group (—CH2NHCOCH3) as a water-solubilizing protecting group for thiolate ligands, a new type of oxotechnetium(V) complex was prepared. The compound oxobis(ethan-1,2-dithiolato-S,µS′)technetium(V)oxo(ethan-1,2-dithiolato-S,S′)technetium(V), [(TcO)2(SCH2CH2S)3], 1, was synthesized by the reaction of [TcOCl4]− with either an excess of bis(acetamidomethyl)ethanedithiol or 1.5 equiv. of ethanedithiol. The complex was characterized by field desorption mass spectrometry (m/e = 505(8), 507(2.8)) and its structure determined by single crystal X-ray diffraction. 1 has a monoclinic space group P21/c with cell dimensions a = 8.833(2) Å, b = 15,034(3) Å, c = 11.350(2) Å, and β = 108.17(1)°, and has four formula units in the unit cell. Data were collected with the use of MoKα radiation and a Nicolet P3 diffractometer. The crystal structure was determined by standard methods and refined to R1 = 0.0366 and R2 = 0.0455 on the basis of 3312 independent reflections. The compound contains two technetium atoms. Two sulphur atoms of one square pyramidal TcOS4 core are bonded to another TcOS2 unit forming two square pyramids sharing an edge with an angle of 106.0(1) between the basal planes. TheTc—Tc distance is 3.654(1) Å. There are four distinct types of Tc—S bonds (range 2.256(2)—2.418(2) Å) and the Tc—O distances (1.66 Å) are normal.

X-ray study on egg-yolk lecithin: Unit cell data and electron density profile

1977 ◽  
Vol 117 (1) ◽  
pp. 285-291 ◽  
Author(s):  
I. Sakurai ◽  
S. Iwayanagi ◽  
T. Sakurai ◽  
T. Seto
Keyword(s):  
Electron Density ◽  
Density Profile ◽  
Egg Yolk ◽  
Electron Density Profile ◽  
Unit Cell ◽  
X Ray ◽  
Cell Data ◽  
Unit Cell Data
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