Preparation and structure of mer-trichloro(acetonitrile)bis-(triphenylphosphine)osmium(III)

1980 ◽  
Vol 58 (10) ◽  
pp. 1042-1045 ◽  
Author(s):  
R. L. Parkes ◽  
N. C. Payne ◽  
E. O. Sherman
Keyword(s):  
Three Dimensional ◽  
Phosphine Ligands ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Distorted Octahedral Coordination Geometry ◽  
Distorted Octahedral ◽  
Cell Dimensions ◽  
The Mean ◽  
Bond Trans

An air-stable, red, crystalline, N-bonded acetonitrile complex of Os(III), OsCl3(NCCH3)(P(C6H5)3)2, has been prepared and characterized by elemental analysis, magnetic susceptibility, and a single crystal X-ray structure determination. Crystals are monoclinic, space group P21/c, cell dimensions a = 10.029(2), b = 15.233(2), c = 25.246(4) Å, β = 113.65(1)°, and Z = 4. Three dimensional X-ray diffraction intensity data were collected on an automatic four circle diffractometer using Cu radiation. Full-matrix least-squares refinement on F converged at R = 0.038 for 4384 unique observations. The Os atom has a slightly distorted octahedral coordination geometry, with trans phosphine ligands, mean Os—P 2.406(2) Å. The acetonitrile ligand is σ-bonded through the N atom, Os—N 2.038(6) Å. The bond trans to the acetonitrile ligand. Os—Cl(1) 2.364(2) Å, is not significantly different from the mean of the cisOs—Cl bonds, 2.361(2) Å.

Poly[[μ-(1-azaniumylethane-1,1-diyl)bis(hydrogen phosphonato)]sodium]: a powder X-ray diffraction study

2013 ◽  
Vol 69 (8) ◽  
pp. 815-818 ◽  
Author(s):  
Mwaffak Rukiah ◽  
Thaer Assaad
Keyword(s):  
Hydrogen Bonding ◽  
Rietveld Method ◽  
Three Dimensional ◽  
Coordination Geometry ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
X Ray ◽  
Dimensional Network ◽  
Distorted Octahedral Coordination Geometry ◽  
Distorted Octahedral

The title two-dimensional coordination polymer, [Na(C2H8NO6P2)]n, was characterized using powder X-ray diffraction data and its structure refined using the Rietveld method. The asymmetric unit contains one Na+cation and one (1-azaniumylethane-1,1-diyl)bis(hydrogen phosphonate) anion. The central Na+cation exhibits distorted octahedral coordination geometry involving two deprotonated O atoms, two hydroxy O atoms and two double-bonded O atoms of the bisphosphonate anion. Pairs of sodium-centred octahedra share edges and the pairs are in turn connected to each other by the biphosphonate anion to form a two-dimensional network parallel to the (001) plane. The polymeric layers are connected by strong O—H...O hydrogen bonding between the hydroxy group and one of the free O atoms of the bisphosphonate anion to generate a three-dimensional network. Further stabilization of the crystal structure is achived by N—H...O and O—H...O hydrogen bonding.<!?tpb=18.7pt>

A new three-dimensional CdIIsupramolecular framework constructed from the 1-[(1H-tetrazol-5-yl)methyl]-1,4-diazoniabicyclo[2.2.2]octane ligand

2015 ◽  
Vol 71 (2) ◽  
pp. 93-96 ◽  
Author(s):  
Qiang Li ◽  
Hui-Ting Wang ◽  
Lin Zhou
Keyword(s):  
Crystal Packing ◽  
Three Dimensional ◽  
Supramolecular Network ◽  
Stacking Interactions ◽  
X Ray Diffraction ◽  
One Dimensional ◽  
X Ray ◽  
Distorted Octahedral Coordination Geometry ◽  
Distorted Octahedral ◽  
Cl Atoms

A new tetrazole–metal supramolecular compound, di-μ-chlorido-bis(trichlorido{1-[(1H-tetrazol-5-yl-κN2)methyl]-1,4-diazoniabicyclo[2.2.2]octane}cadmium(II)), [Cd2(C8H16N6)2Cl8], has been synthesized and structurally characterized by single-crystal X-ray diffraction. In the structure, each CdIIcation is coordinated by five Cl atoms (two bridging and three terminal) and by one N atom from the 1-[(1H-tetrazol-5-yl)methyl]-1,4-diazoniabicyclo[2.2.2]octane ligand, adopting a slightly distorted octahedral coordination geometry. The bridging bicyclo[2.2.2]octane and chloride ligands link the CdIIcations into one-dimensional ribbon-like N—H...Cl hydrogen-bonded chains along thebaxis. An extensive hydrogen-bonding network formed by N—H...Cl and C—H...Cl hydrogen bonds, and interchain π–π stacking interactions between adjacent tetrazole rings, consolidate the crystal packing, linking the poymeric chains into a three-dimensional supramolecular network.

X-Ray Structure of a Nickel(II) Complex of the Tetra-N-methylated Macrocycle Dibenzocyclam with a Folded Ligand Configuration

1984 ◽  
Vol 39 (7) ◽  
pp. 903-906 ◽  
Author(s):  
Horst Elias ◽  
Rüdiger Grewe ◽  
Dirk-Detlev Klaehn ◽  
Helmut Paulus
Keyword(s):  
Three Dimensional ◽  
Bidentate Ligand ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Nitrate Ion ◽  
Light Blue ◽  
X Ray ◽  
Mild Conditions ◽  
Distorted Octahedral ◽  
R Value

Under mild conditions nickel(II) nitrate reacts with the macrocyclic N4 ligand TMBC ( = 1,4 ,8,11-tetramethyl-1,4,8,11-tetraazadibenzo[b,i]cyclotetradecane) to form the light blue-green complex Ni (TMBC) (NO3)2. A three-dimensional X-ray diffraction study shows that the complex crystallizes in the monoclinic space group P21/c with a = 896.1(3) pm, b = 2059.9(7) pm , c = 1298.6(6) pm, β = 91.37(1)° and Z = 4. The nickel is six-coordinate. The distorted octahedral N4O2 arrangement of donor atoms around the nickel is formed by the tetradentate N4 macrocycle TMBC in an unexpected folded form and by a nitrate ion as a bidentate ligand occupying two depositions. The structure could be refined to the final R-value of 0.045 only by assuming disorder for the second, noncoordinated nitrate ion.

A New POM-Based Supramolecular Compound: Synthesis, Structure and Adsorptive Property of [Cu(phen)2]3[W6O19]

2014 ◽  
Vol 919-921 ◽  
pp. 2013-2016 ◽  
Author(s):  
Ya Bing Liu ◽  
Hong Jie Wang ◽  
Hong Kai Zhao
Keyword(s):  
Three Dimensional ◽  
Building Blocks ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Hybrid Compound ◽  
Adsorptive Property ◽  
X Ray ◽  
Hydrogen Bonding Interactions ◽  
Compound Synthesis ◽  
Metal Organic

A POM - based organice - inorganic hybrid compound with the chemical formula of[Cu (phen)2]3[W6O19] (phen = 1,10-phenanthroline) (1) has been hydrothermally synthesized andstructurally characterized by the elemental analysis, and single crystal X-ray diffraction. Compound 1 crystallizes in the monoclinic space groupC2/c witha=18.319(4) Å,b= 17.311(4) Å,c= 22.248(4) Å,β= 112.40(3) o,V= 6523(2) Å3,Z= 4, R1= 0.0448, andwR2=0.1218. Compound 1 consists of the [W6O19]3-building blocks and [Cu (phen)2]+metal organic cationic moieties, which are packed together via the extensive hydrogen-bonding interactions to form a three-dimensional supramolecular framework. The adsorption of methylene blue (MB) under UV irradiation with 1 as the heterogeneous adsorbent has been investigated, showing a good adsorptive property of 1 for MB degradation.

The Crystal Structure of KIO3.HIO3

1971 ◽  
Vol 49 (3) ◽  
pp. 468-476 ◽  
Author(s):  
Lilian Y. Y. Chan ◽  
F. W. B. Einstein
Keyword(s):  
Crystal Structure ◽  
Three Dimensional ◽  
Monoclinic Space Group ◽  
X Ray ◽  
R Factor ◽  
Octahedral Environment ◽  
Distorted Octahedral ◽  
Potassium Hydrogen ◽  
A Cell ◽  
Least Squares Techniques

The crystal structure of potassium hydrogen di-iodate (bi-iodate) KIO3.HIO3 was determined from three dimensional X-ray data collected by counter methods. The structure was refined by full-matrix least-squares techniques to a conventional R factor of 5.0 % for the 1392 observed reflexions. The salt crystallizes in the monoclinic space group P21/c with eight formula units in a cell of dimension a = 7.028(1) Å, b = 8.203(1) Å, c = 21.841(3) Å, β = 98.03(1)°.The iodate units are all basically pyramidal; weak interionic I—O contacts complete a very distorted octahedral environment around three iodine atoms. There is a capped octahedral (7-coordinate) environment around the remaining iodine atom. The I—O bonds are in the range 1.75–1.82 Å and the I—OH bonds are 1.91 and 1.95 Å, variations in length can be correlated with differences in the degree of involvement in (a) hydrogen bonding and (b) interaction with adjacent iodine atoms.

Structure and Fluorescence Properties of a Novel Supramolecular Zinc Complex

2008 ◽  
Vol 63 (12) ◽  
pp. 1357-1360 ◽  
Author(s):  
Gang Chen
Keyword(s):  
Hydrothermal Reaction ◽  
Three Dimensional ◽  
Free Ligand ◽  
Distorted Octahedral Geometry ◽  
Monoclinic Space Group ◽  
Ligand Complex ◽  
Complex Molecules ◽  
Hydrogen Bonding Interactions ◽  
Distorted Octahedral ◽  
Cell Dimensions

Hydrothermal reaction of Zn(NO3)2 · 6H2O and 2-hydroxypyridine-3-carboxylic acid afforded a novel supramolecular complex, [Zn(C6H4NO3)2(H2O)2] (1). The complex has been characterized by macroanalysis, IR spectra, and thermogravimetric and differential thermal analysis (TG/DTA). Single crystal X-ray analysis shows that complex 1 crystallizes in the monoclinic space group P21/c with the cell dimensions a = 7.534(6), b = 12.289(1), c = 7.534(6) Å, β = 100.51°, V = 685.85(1) Å3, and Z = 2. The six-coordinated Zn atom is in a severely distorted octahedral geometry. The complex molecules are assembled via strong O-H· · ·O and N-H· · ·O hydrogen bonding interactions into a three-dimensional supramolecular framework. Compared with the free ligand, complex 1 exhibits strong fluorescence in the solid state at room temperature.

Synthesis and Characterization of the Manganese Pyroarsenate Mn2As2O7 · 2H2O

2001 ◽  
Vol 56 (4-5) ◽  
pp. 359-363 ◽  
Author(s):  
N. Stock ◽  
G. D. Stucky ◽  
A. K. Cheetham
Keyword(s):  
Three Dimensional ◽  
Spectroscopic Studies ◽  
Mean Value ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Raman Spectroscopic ◽  
Distorted Octahedral ◽  
Ir And Raman ◽  
Hydrothermal Methods

Abstract The manganese pyroarsenate hydrate, Mn2As2O7 · 2 H2O, has been obtained as a single phase product using hydrothermal methods and the structure has been determined by single crystal X-ray diffraction. The title compound crystallizes in the monoclinic space group P21/n with a = 6.6576(4), b = 14.555(1), c = 7.8147(5) Å, β = 94.935(1)°, V = 754.46(8) Å3 and Z = 4. The manganese ions are each coordinated to five oxygen atoms and a water molecule in a distorted octahedral arrangement. Edge-sharing MnO6 octahedra form chains which are connected to a three-dimensional framework by As2O74- ions. The pyroarsenate anion, which attains a nearly eclipsed conformation, has a mean As-O distance for the terminal As-O bonds of 1.669(2) Å, while for the bridging oxygen atom a mean value of 1.757(2) Å is observed. Magnetic susceptibility measurements indicate the presence of high-spin Mn2+ ions. Thermogravimetric as well as IR and Raman spectroscopic studies of Mn2As2O7 · 2 H2O are presented.

Synthesis and Structure of cis-Dioxobis(pyrimidine-2-thiolato-N,S)molybdenum(VI)

1992 ◽  
Vol 45 (11) ◽  
pp. 1933 ◽  
Author(s):  
PR Traill ◽  
AG Wedd ◽  
ERT Tiekink
Keyword(s):  
Least Squares ◽  
Octahedral Geometry ◽  
Distorted Octahedral Geometry ◽  
Monoclinic Space Group ◽  
Full Matrix ◽  
X Ray ◽  
Distorted Octahedral ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

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).

Thyroid Hormone Stereochemistry. II. Molecular Structure of Thyronine HCl Ethyl Ester Monohydrate

1974 ◽  
Vol 52 (17) ◽  
pp. 3042-3047 ◽  
Author(s):  
Arthur Camerman ◽  
Norman Camerman
Keyword(s):  
Ethyl Ester ◽  
Three Dimensional ◽  
Chloride Ion ◽  
Dimensional Structure ◽  
Side Chain ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Ether Linkage ◽  
Cell Dimensions ◽  
Phenyl Rings

The three-dimensional structure of L-thyronine, the non-iodinated physiologically inactive analog of thyroxine, has been determined by single crystal X-ray diffraction and compared to the active thyroid hormones. The compound crystallized as the monohydrate of thyronine hydrochloride ethyl ester in the monoclinic space group P21 with cell dimensions a = 10.502, b = 5.165, c = 17.940 Å, β = 109.74°. The structure was solved by Patterson methods to find the chloride ion and iterative Fourier maps to locate the rest of the atoms. Refinement was by anisotropic full-matrix least squares to convergence at R = 0.048.The two phenyl rings adopt a twisted orientation with respect to each other with angles of −37° and −67° between the plane of the inter-ring ether linkage and the planes of the α- and β-rings, respectively. This orientation differs considerably from that found in the iodinated thyronines. The conformation of the alanine side chain is remarkably similar to that of the alanine in the iodinated thyronines.

scholarly journals The reaction of 3,5-diphenyl-1,2-dithiolium-4-olate with aniline: the crystal structure of 1-phenylimino-2-phenylamino-3-phenylindene

1987 ◽  
Vol 65 (12) ◽  
pp. 2830-2833 ◽  
Author(s):  
David M. McKinnon ◽  
Peter D. Clark ◽  
Robert O. Martin ◽  
Louis T. J. Delbaere ◽  
J. Wilson Quail
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Direct Methods ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

3,5-Diphenyl-1,2-dithiolium-4-olate (1) reacts with aniline to form 1-phenylimino-2-phenylamino-3-phenylindene (3a). Under suitable conditions, 6-phenylbenzo[b]indeno[1,2-e]-1,2-thiazine is also formed. These structures are confirmed by alternative syntheses. The molecular structure of 3a has been determined by single crystal X-ray diffraction. Compound 3a crystallizes in the monoclinic space group C2/c with unit cell dimensions a = 20.777(3) Å, b = 6.130(3) Å, c = 31.327(3) Å, 3 = 99.59(1)°, and Z = 8. The structure was solved by direct methods and refined by least squares to a final R = 0.055. The molecular structure of 3a shows the three phenyl containing substituents to have the planes of their ring systems tilted between 40° and 60° from the plane of the indene system due to steric repulsions.

Sign in / Sign up

Export Citation Format

Share Document