Lewis-Base Adducts of Group 1B Metal(I) Compounds. XXII. Crystal Structure of 'Bis(pyridine)silver(I) Perchlorate

1985 ◽  
Vol 38 (9) ◽  
pp. 1325 ◽  
Author(s):  
JC Dyason ◽  
PC Healy ◽  
LM Engelhardt ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Complex Cation ◽  
Lewis Base ◽  
X Ray ◽  
Ray Methods

Determination of the crystal structure of 'bis (pyridine)silver(I) perchlorate' by single-crystal X-ray methods shows it to be of 2.4:1 pyridine:silver (I) perchlorate stoichiometry , the structure being refined by least squares to a residual of 0.054 for 1142 'observed' reflections. Crystals are tetragonal, I4, a 21.95(1), c 7.684(3) Ǻ. The structure comprises perchlorate anions of two types of I and 4 symmetry, together with two types of complex cation: [Ag( py )2]+, with 1 symmetry, and [Ag( py )4]+ with 4 symmetry. For the two types of cation Ag-N are 2.15(1), 2.16(1) and 2.30(1) Ǻ.

Studies of the rhenium–oxygen bond. II. The crystal and molecular structure of µ-oxobis(cis-dichloro-cis-di(pyridine)-trans-oxorhenium(V)), ORe(C5H5N)2Cl2ORe(C5H5N)2Cl2O

1978 ◽  
Vol 56 (2) ◽  
pp. 179-188 ◽  
Author(s):  
Colin James Lyne Lock ◽  
Graham Turner
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
The Other ◽  
Full Matrix ◽  
X Ray ◽  
Ray Methods ◽  
Oxygen Bond

The crystal structure of µ-oxobis(cis-dichloro-cis-di(pyridine)-trans-oxorhenium(V)), ORe(C5H5N)2Cl2•O•Re(C5H5N)2Cl2O bas been studied by single crystal X-ray methods. The crystals were orthorhombic with lattice parameters a = 15.367(2), b = 10.283(2), c = 16.685(2) Å. The space group was Pna21 and there were four formula weights per unit cell. A total of 3339 reflections, of which 2990 were observed, were examined, and the structure refined by full matrix least squares (treating the pyridine rings as groups) to an R2 value of 0.0449. The dimer had a roughly rectilinear O—Re—O—Re—O backbone with pairs of chlorine atoms and pyridine molecules arranged cis in each half of the dimer. The two halves of the dimer were arranged such that the pairs of cis atoms in one half were rotated about the Re(1)–Re(2) axis almost 113 ° when compared to the corresponding pair in the other half. Important bond lengths (Re—O(terminal), 1.715(16), 1.764(16); Re—O(bridging), 1.943(16), 1.903(16); Re—Cl, 2.356(5)–2.390(5); Re—N, 2.116(16)–2.180(16)) were close to previously observed values. The molecule was markedly disturbed from the idealized structure and this was caused by intramolecular non-bonded interactions.

Crystal structure of Bis(tri-2-pyridylamine)iron(II) diperchlorate

1978 ◽  
Vol 31 (1) ◽  
pp. 53 ◽  
Author(s):  
ES Kucharski ◽  
WR McWhinnie ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Metal Atom ◽  
Title Compound ◽  
Complex Cation ◽  
X Ray Diffraction ◽  
Tridentate Ligands ◽  
X Ray ◽  
The One

The crystal structure of the title compound, [Fe((C5H4N)3N)2] (ClO4)2, has been determined by single-crystal X-ray diffraction at 295 K and refined by least squares to a residual of 0.059 (1995 'observed' reflections). Crystals are monoclinic, P21/a, a 12.815(4), b 17.503(7), c 8.318(3) Ǻ, β 121.38(3)°, Z 2. The complex cation lies with the metal atom on a centre of symmetry, the metal being six-coordinate, so that only one of the tridentate ligands is crystallographically independent. The geometry about the metal atom deviates only trivially from octahedral, <N-Fe-N> within the one ligand being 88.1°. <Fe-N> is 1.982 Ǻ.

Lewis-Base Adducts of Main Group 1 Metal-Compounds. XII. Synthesis and Crystal Structure of (2,2′-Bipyridine)(bromo)(propan-2-ol)lithium(I)

1990 ◽  
Vol 43 (4) ◽  
pp. 755 ◽  
Author(s):  
BW Skelton ◽  
CR Whitaker ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Title Compound ◽  
Main Group ◽  
Lewis Base ◽  
Metal Compounds ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Ray Methods ◽  
Group 1

The title compound is readily crystallized from a 1 : 1 mixture of 2,2′-bipyridine and lithium(I) bromide in propan-2-ol; its structure has been established by single-crystal X-ray methods at c. 295 K. Crystals are monoclinic, P21/c, a 10.942(3), b 15.060(4), c 9.359(3)Ǻ, β 108.57(2)°, Z = 4; R was 0.050 for 1820 'observed' reflections. In the four-coordinate LiBrN2O environment, Li- Br,O are 2.47(1), 1.94(1)Ǻ, and Li-N are 2.05(1), 2.07(1)Ǻ.

X-Ray Crystal Structure Determination of Some Sodium Anthraquinone Sulfonate Derivatives

1993 ◽  
Vol 46 (10) ◽  
pp. 1595 ◽  
Author(s):  
e Gamag ◽  
e Gamag ◽  
BM Peake ◽  
BM Peake ◽  
J Simpson ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Structure Determination ◽  
X Ray Diffraction ◽  
Molecular Mechanics Calculations ◽  
X Ray ◽  
Photochemical Behaviour ◽  
Sufficient Magnitude ◽  
Ray Methods

The crystal structures of sodium 9,10-dioxo-9,10-dihydroanthracene-2-sulfonate hydrate (1) and sodium 9,10-dioxo-9,10-dihydroanthracene-1,5-disulfonate trihydrate (2) have been determined by single-crystal X-ray diffraction at 253 K and refined to R 0.03 for (1) (1535 reflections) and R 0.04 for (2) (1409 reflections). Crystals of (1) are monoclinic, P21, a 17.395(5), b 6.625(2), c 5.537(1)Ǻ, β 91.87(2)°, Z 2, and those of (2) are orthorhombic, Pnma, a 11.332(4), b 20.048(5), c 7.634(3)Ǻ, Z 4. The results of molecular mechanics calculations on these two molecules were in general agreement with those determined by X-ray methods. The effect of sulfonate substitution in the 1-position compared with that in the 2-position include a small lengthening of the C-S bond and a displacement of the sulfur and quinone oxygen atoms to opposite sides of the plane of the substituted aromatic ring. However, these differences do not appear to be of sufficient magnitude to account for the much greater differences in the electrochemical and photochemical behaviour of these two classes of anthraquinone sulfonate derivatives.

Lewis-Base Adducts of Group-11 Metal(I) Compounds. XXIX. Crystal Structures of Bis(Pyridine-4-carbonitrile)silver(I) Nitrate and Bis(4-benzoylpyridine)Silver(I) Nitrate Monohydrate

1987 ◽  
Vol 40 (9) ◽  
pp. 1603 ◽  
Author(s):  
S Gotsis ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Least Squares ◽  
Crystal Structures ◽  
Complex Cation ◽  
Lewis Base ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
Silver Atoms ◽  
Close Contacts

The crystal structures of the title compounds, [Ag(C6H4N2),] (NO3), (I), and [Ag(C12H9NO)2] (NO3).H2O, (2), have been determined by single-crystal X-ray diffraction methods at ~295 K, being refined by full-matrix least-squares methods to residuals of 0.042 and 0.044 for 1814 and 3434 independent 'observed' reflections respectively. Crystals of (1) and (2) are triclinic P1; for (1) a, 27.954(7), b 6.354(2), c 3.710(1)�, α 87.55(3), β 86.21(2), γ 89.35(2)�, Z 2; for (2), a 17.036(5), b 8.691(3), c 7.849(3) �, α � 107.74(2), β 97 53(2), γ 91 .11(2)�, Z 2. In both structures the formulation is basically a linearly coordinated complex cation/anion as shown above: in (I), Ag-N are 2.214(4), 2.203(4) � with N-Ag-N, 162.2(2)"; in (2), Ag-N are 2.146(3), 2.147(3) �, N-Ag-N, 175.3(1)�. The shortest Ag-O contact is found in (1) at 2.693(4)�. No close contacts are found between the silver atoms and cyano or ketonic ligand substituents.

Studies of β-Diketone Complexes of Rhenium. VII. The Crystal and Molecular Structure of Oxodichloropentane-2,4-dionatotriphenylphosphinerhenium(V)

1975 ◽  
Vol 53 (11) ◽  
pp. 1548-1553 ◽  
Author(s):  
C. J. L. Lock ◽  
Che'ng Wan
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Rhenium Atom ◽  
Full Matrix ◽  
X Ray ◽  
Bonding Interaction ◽  
Ray Methods

The crystal structure of oxodichloropentane-2,4-dionatotriphenylphosphinerhenium(V) has been studied by single crystal X-ray methods. The crystals are triclinic with lattice parameters a = 11.023(8) Å, b = 13.523(8) Å, c = 9.360(7) Å, α = 90.2(1)°, β = 114.1(1)°, γ = 67.7(2)°. The space group is [Formula: see text] and there are two formula weights per unit cell. A total of 2891 reflections, of which 2447 were observed, were examined, and the structure was refined by full matrix least squares to an R2 value of 0.0782. The ligands are arranged around the rhenium atom such that the nearest six atoms are at the corners of a very distorted octahedron. Most of this distortion appears to be caused by nonbonding repulsive interactions. The short oxo–phosphine distance, 2.85(1) Å, suggests the possibility of a weak bonding interaction. Observed bond distances (Re—Cl, 2.35 Å av; Re—O(oxo), 1.69(1) Å; Re—O(diketone), 1.99(1), 2.10(1) Å; Re—P, 2.431(4) Å) are close to those observed previously in similar compounds.

Single Crystal Growth of High-Pressure Phases of Ice and Salt Hydrate Far Below the Original Melting Point by Mixing Alcohol: Crystal Structure Determination of Magnesium Chloride Heptahydrate

2020 ◽  
Author(s):  
Keishiro Yamashita ◽  
Kazuki Komatsu ◽  
Hiroyuki Kagi
Keyword(s):  
Crystal Structure ◽  
High Pressure ◽  
Crystal Growth ◽  
Single Crystal ◽  
Room Temperature ◽  
Growth Technique ◽  
Salt Hydrate ◽  
X Ray

An crystal-growth technique for single crystal x-ray structure analysis of high-pressure forms of hydrogen-bonded crystals is proposed. We used alcohol mixture (methanol: ethanol = 4:1 in volumetric ratio), which is a widely used pressure transmitting medium, inhibiting the nucleation and growth of unwanted crystals. In this paper, two kinds of single crystals which have not been obtained using a conventional experimental technique were obtained using this technique: ice VI at 1.99 GPa and MgCl<sub>2</sub>·7H<sub>2</sub>O at 2.50 GPa at room temperature. Here we first report the crystal structure of MgCl2·7H2O. This technique simultaneously meets the requirement of hydrostaticity for high-pressure experiments and has feasibility for further in-situ measurements.

Crystal structure of ab-Bis(3-methylpyridine)-dc,fe-bis(pentane-2,3,4-trione 3-oximato)iron(II)

1978 ◽  
Vol 31 (11) ◽  
pp. 2431 ◽  
Author(s):  
BN Figgis ◽  
CL Raston ◽  
RP Sharma ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Title Compound ◽  
X Ray Diffraction ◽  
X Ray ◽  
Chelate Ligands

The crystal structure of the title compound has been determined at 295 K by single-crystal X-ray diffraction and refined by least squares to a residual of 0.062. Crystals are monoclinic, P2/c, a 19.102(8), b 8.117(4), c 16.610(8) Ǻ, β 111.90(3)°, Z. Unlike the tris(α-oxyimino ketonato)iron(II) complexes which are fac, the present derivative is based upon substitution of the two picoline moieties into a mer derivative, trans to the nitrogen atoms of the chelate ligands. <Fe- N(picoline)> is 2.020; <Fe-N, O(chelate)> 1.880, 1.952 Ǻ.

scholarly journals Magnetically Oriented Powder Crystal to Indexing and Structure Determination

2014 ◽  
Vol 70 (a1) ◽  
pp. C1560-C1560
Author(s):  
Fumiko Kimura ◽  
Wataru Oshima ◽  
Hiroko Matsumoto ◽  
Hidehiro Uekusa ◽  
Kazuaki Aburaya ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Crystal Lattice ◽  
Powder Diffraction ◽  
Diffraction Method ◽  
Lattice Parameters ◽  
X Ray Diffraction ◽  
X Ray ◽  
Crystal Lattice Parameters

In pharmaceutical sciences, the crystal structure is of primary importance because it influences drug efficacy. Due to difficulties of growing a large single crystal suitable for the single crystal X-ray diffraction analysis, powder diffraction method is widely used. In powder method, two-dimensional diffraction information is projected onto one dimension, which impairs the accuracy of the resulting crystal structure. To overcome this problem, we recently proposed a novel method of fabricating a magnetically oriented microcrystal array (MOMA), a composite in which microcrystals are aligned three-dimensionally in a polymer matrix. The X-ray diffraction of the MOMA is equivalent to that of the corresponding large single crystal, enabling the determination of the crystal lattice parameters and crystal structure of the embedded microcrytals.[1-3] Because we make use of the diamagnetic anisotropy of crystal, those crystals that exhibit small magnetic anisotropy do not take sufficient three-dimensional alignment. However, even for these crystals that only align uniaxially, the determination of the crystal lattice parameters can be easily made compared with the determination by powder diffraction pattern. Once these parameters are determined, crystal structure can be determined by X-ray powder diffraction method. In this paper, we demonstrate possibility of the MOMA method to assist the structure analysis through X-ray powder and single crystal diffraction methods. We applied the MOMA method to various microcrystalline powders including L-alanine, 1,3,5-triphenyl benzene, and cellobiose. The obtained MOMAs exhibited well-resolved diffraction spots, and we succeeded in determination of the crystal lattice parameters and crystal structure analysis.

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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