An X-Ray Structure Determination of the Twinned Crystals of Dinitrato-2,2′-dipyridylsilver(II)

1972 ◽  
Vol 50 (3) ◽  
pp. 315-323 ◽  
Author(s):  
G. W. Bushnell ◽  
M. A. Khan

The crystal structure of dinitrato-2,2′-dipyridylsilver(II) has been solved and refined to an R-value of 0.070. Four circle diffractometer measurements were obtained from the twinned triclinic crystals. The unit cell dimensions at 22 °C are: a = 697.5 ± 0.2 pm, b = 999.4 ± 0.2 pm, c = 1032.2 ± 0.2 pm, α = 113.46 ± 0.02°, β = 100.71 ± 0.02°, γ = 95.28 ± 0.02°. The space group is [Formula: see text] (No. 2) with two molecules per unit cell. The density is 2.06 ± 0.04 g cm−3 (measured), 2.02 g cm−3 (calculated). The four shortest bond lengths to silver are: Ag—O(1), 214.8 ± 1.5 pm; Ag—O(4), 213.6 ± 1.5 pm; Ag—N(1), 212.4 ± 1.6 pm; Ag—N(2), 220.7 ± 1.6 pm. These four bonds are distorted from square planar geometry with the silver atom lying 19.90 ± 0.17 pm out of the mean plane of the other four atoms. There are also long bonds to the nitrato groups of neighboring molecules: Ag—O(1′), 275.3 ± 1.3 pm; Ag—O(2″), 276.3 ± 1.6 pm. Inclusion of these bonds gives a distorted octahedral silver coordination. Though predominantly unidentate, there is a slight tendency toward bidentate bonding in both nitrato ligands: Ag—O(2), 305.8 ± 1.4 pm; Ag—O(5), 295.0 ± 1.7 pm. O(2) and O(5) approach the convex side of the distorted square planar coordination. The deviation from planarity of the closely bonded square, and angular distortions in the above mentioned octahedral coordination can be rationalized by considering the silver as eight coordinate. The bonds to silver may be grouped 4:2:2 by length or 4:3:1 by angular disposition.

1977 ◽  
Vol 55 (1) ◽  
pp. 111-114 ◽  
Author(s):  
Lillian Y. Y. Chan ◽  
E. E. Isaacs ◽  
W. A. G. Graham

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°.


Author(s):  
L. W. Labaw

Crystals of a human γGl immunoglobulin have the external morphology of diamond shaped prisms. X-ray studies have shown them to be monoclinic, space group C2, with 2 molecules per unit cell. The unit cell dimensions are a = 194.1, b = 91.7, c = 51.6Å, 8 = 102°. The relatively large molecular weight of 151,000 and these unit cell dimensions made this a promising crystal to study in the EM.Crystals similar to those used in the x-ray studies were fixed at 5°C for three weeks in a solution of mother liquor containing 5 x 10-5M sodium phosphate, pH 7.0, and 0.03% glutaraldehyde. They were postfixed with 1% osmium tetroxide for 15 min. and embedded in Maraglas the usual way. Sections were cut perpendicular to the three crystallographic axes. Such a section cut with its plane perpendicular to the z direction is shown in Fig. 1.This projection of the crystal in the z direction shows periodicities in at least four different directions but these are only seen clearly by sighting obliquely along the micrograph.


Clay Minerals ◽  
1990 ◽  
Vol 25 (4) ◽  
pp. 507-518 ◽  
Author(s):  
M. H. Ebinger ◽  
D. G. Schulze

AbstractMn-substituted iron oxides were synthesized at pH 4, 6, 8, and 10 from Fe-Mn systems with Mn mole fractions (Mn/(Mn + Fe)) of 0, 0·2, 0·4, 0·6, 0·8, and 1·0, and kept at 50°C for 40 days. The Mn mole fraction in goethite was <0·07 at pH 4 but increased to ∼0.47 at pH 6. Goethite and/or hematite formed in Fe and Fe + Mn syntheses at pH 4 and pH 6 at Mn mole fractions ≤0·8, and at Mn mole fractions ≤0·2 at pH 8 and pH 10. Hausmannite and jacobsite formed at pH 8 and pH 10 at Mn mole fractions ≥0·4. In the pure Mn syntheses, manganite (γ-MnOOH) formed at pH 4 and pH 6, whereas hausmannite (Mn3O4) formed at pH 8 and pH 10. As the Mn substitution increased, the unit-cell dimensions of goethite shifted toward those of groutite, and the mean crystallite dimensions of goethite decreased.


1996 ◽  
Vol 11 (4) ◽  
pp. 301-304
Author(s):  
Héctor Novoa de Armas ◽  
Rolando González Hernández ◽  
José Antonio Henao Martínez ◽  
Ramón Poméz Hernández

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.


1999 ◽  
Vol 55 (2) ◽  
pp. 539-541
Author(s):  
Palangpon Kongsaeree ◽  
Jun Liang ◽  
Roy A. Jensen ◽  
Jon Clardy

The title protein has been crystallized in a new crystal form. The crystals belong to the cubic space group P4132 (or P4332) with unit-cell dimensions a = b = c = 126.1 Å at 100 K and typically diffract beyond 1.6 Å at the Cornell High Energy Synchotron Source (CHESS) A1 beamline.


Author(s):  
Robert Heimann

X-ray powder diffraction (XRPD) is an important tool to determine the phase composition of archaeological ceramics. In principle, a thin beam of X-rays incident to a lattice plane of crystalline matter is scattered in specific directions and angles depending on the distances of atoms. This allows determination of characteristic unit cell dimensions and serves to unambiguously identify crystalline phases in the ceramics. In this chapter, generation of X-rays and the theory of diffraction will be briefly discussed as well as equipment, focusing conditions, and sample preparation procedures of common XRPD methods. The X-ray pattern obtained will provide an analytical fingerprint that can be matched against the Powder Diffraction File of the International Centre for Diffraction Data. Examples will be given of application of this analytical technique to archaeological clays and ceramics.


1992 ◽  
Vol 45 (11) ◽  
pp. 1933 ◽  
Author(s):  
PR Traill ◽  
AG Wedd ◽  
ERT Tiekink

The characterization of two MoVI complexes, cis -[MoO2(2-pymS)2] and cis -[MoO2(2-pyS)2] (where 2-pymSH is pyrimidine-2-thiol and 2-pySH is pyridine-2-thiol), and their reaction with Ph3P are reported. The X-ray structure of cis -[MoO2(2-pymS)2] shows the molybdenum atom to exist in a distorted octahedral geometry defined by two mutually cis oxygen atoms and two chelating 2-pymS ligands so that the two sulfur atoms occupy approximate trans positions. Crystals of cis -[MoO2(2-pymS)2] are monoclinic, space group P 21/n, with unit cell dimensions: a 9.301(3), b 12.121(2), c 11.303(3) �, β 112.62(3)�, V 1176.3 �3, Z 4. The structure was refined by a full-matrix least-squares procedure to R 0.067 for 1858 reflections with I ≥ 2.5 (I).


1976 ◽  
Vol 31 (9) ◽  
pp. 1175-1178 ◽  
Author(s):  
Kurt Walenta

A new compound having the same composition as zircon, ZrSiO4, but differing from it in its structure has been obtained by heating zircon particles to a temperature of 5000 to 10000°K. According to X-ray powder diffraction data the structure and within limits of error also the unit-cell dimensions are identical with that of monoclinic baddeleyite, ZrO2. This suggests that the baddeleyite lattice can not only accommodate 10 molecular % SiO2 as is already known for some time, but substantially more, unless it is assumed that some kind of submicroscopic exsolution of amorphous SiO2 has taken place.


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