Convenient Synthesis and Molecular Structure of the Cyclometallated Complex [IrCl(H)(C6H4PPh2)(PPh3)2]

2014 ◽  
Vol 69 (11-12) ◽  
pp. 1237-1240 ◽  
Author(s):  
Hans-Christian Böttcher ◽  
Peter Mayer

Abstract The reaction of [{Ir(μ-Cl)(coe)2}2] (coe=cis-cyclooctene) with triphenylphosphane (molar ratio of Ir to P=1 : 3) in dichloromethane at room temperature afforded after a short reaction time the cyclometallated complex [IrCl(H)(C6H4PPh2)(PPh3)2] (1) in almost quantitative yield. The molecular structure of the title compound 1 was determined by an X-ray diffraction study.

2014 ◽  
Vol 69 (3) ◽  
pp. 376-378 ◽  
Author(s):  
Hans-Christian Böttcher ◽  
Peter Mayer

The reaction of hydrated rhodium(III) chloride with formic acid in refluxing ethoxyethanol afforded in a convenient way the known rhodium carbonyl chlorido complex anion cis-[RhCl2(CO)2]-. This species was formed in good yield and was characterized as its PPN salt (PPN+ = bis(triphenylphosphane)iminium cation). The molecular structure of the title compound PPN[RhCl2(CO)2] was confirmed by X-ray diffraction and shown to be isomorphous to PPN[IrCl2(CO)2]


2018 ◽  
Vol 6 (2) ◽  
pp. 132-136
Author(s):  
Pramod Kumar Yadav

The title compound azobenzene-4, 4′-dicarbonyl chloride has been synthesized in distilled dichlomethane and characterized by elemental analysis (C, H, N), IR and NMR (1H & 13C) studies. The crystal and molecular structure was further confirmed using single crystal X-ray diffraction analysis. It was crystallized in triclinic crystal system with space group P-1. The centrosymmetrically related molecules held together via C–H---O secondary interaction result in molecular aggregation of the compound.  Int. J. Appl. Sci. Biotechnol. Vol 6(2): 132-136


1977 ◽  
Vol 55 (2) ◽  
pp. 333-339 ◽  
Author(s):  
Colin James Lyne Lock ◽  
Graham Turner

The crystal and molecular structure of the title compound has been examined by single crystal X-ray diffraction. The crystals are monoclinic with a = 28.045(10), b = 8.766(3), c = 12.376(5) Å, β = 91.14(3)°. The space group is C2/c and there are eight molecules per unit cell. A total of 5053 independent reflections, of which 2860 were observed, were examined on a Syntex [Formula: see text] diffractometer. The structure was refined by full matrix least squares to an R2 value of 0.0449. The ligands form a very rough octahedron around the rhenium atom with Re—Cl(1), 2.441(3); Re—Cl(2), 2.366(3), Re—O(1), 1.684(7); Re—O(2), 1.896(6); Re—N(1), 2.144(7); Re—N(2), 2.132(7) Å. The pyridine rings are a dominant factor in determining the details of the molecular structure.


1997 ◽  
Vol 52 (2) ◽  
pp. 256-258 ◽  
Author(s):  
Evgeni V. Avtomonov ◽  
Rainer Grüning ◽  
Jörg Lorberth

Abstract The crystal structure of the title compound has been determined by X-ray diffraction methods. Due to the Lewis acidic character of the iodine substituent a “zig-zag” chain is formed via intermolecular interactions (2.933(4) A) between iodine and oxygen atoms of theocarbamate moiety. A three-dimensional network is formed through hydrogen-bridging (2.04 A) between NH-groups and the oxygen atoms of the neighbouring carbamate group of the next molecule.


1984 ◽  
Vol 39 (2) ◽  
pp. 145-148 ◽  
Author(s):  
Ulf Thewalt ◽  
Konrad Holl

The compound S2N2 • 2AlBr3 has been prepared by reaction of S4N4 with AlBr3 in 1,2-dibromoethane at room temperature. Its crystal and molecular structure have been determined by X-ray diffraction; R = 0.068. Crystal data: monoclinic, P 21/n, a = 9.594(5), b = 9.975(4), c = 7.528(4) Å , β = 111.36(5)°. The S2N2 ring of the centrosymmetrical complex is bonded via its nitrogen atoms to two AlBr3 units thus completing coordination tetrahedra around the Al atoms. Bond distances and angles within the S2N2 ring are d(S-N) = 1.629(13) and 1.651(13) Å, ∢ (S-N-S) = 95.8, and ∢ (N-S-N) - 84.2°. Whereas the S-N bond lengths agree closely with those of free S2N2, the angle at N is enlarged by ca. 5° and the angle at S is decreased by ca. 5°. The sulfur atoms form two close S···Br contacts of length 3.149 (intramolecular) and 3.193 (intermolecular) Å , respectively. The intermolecular attractive nonbonded S···Br interactions tie the complexes together in a way that leads to infinite chains which run parallel to the crystallographic z axis


2009 ◽  
Vol 152-153 ◽  
pp. 205-208 ◽  
Author(s):  
H. Arabi ◽  
S. Nateghi ◽  
S. Sadeghi

Iron oxide nanoparticles were synthesis by reverse micelle method. X-ray diffraction technique and vibration sample magnetometer were applied to characterize the produced samples at different conditions and parameters for synthesis route. There is no significant difference between samples prepared at 5°C and room temperature except a better crystalline at room temperature. The molar ratio of water to surfactant (w parameter) and concentration of the salt solution on size and magnetic properties of nanoparticles have been investigated. Increasing w leads to producing particles with larger size i.e. for w=16.83, 11.22, and 5.6, particles size are 15.22, 11.66 and 10.5 nm, respectively. The size of nanoparticles are in the range of 9 to 20 nanometers


2018 ◽  
Vol 2018 ◽  
pp. 1-7 ◽  
Author(s):  
Tanat Chokpanyarat ◽  
Vittaya Punsuvon ◽  
Supakit Achiwawanich

The novel three-dimensionally ordered macroporous (3DOM) CaO/SiO2, 3DOM CaO/Al2O3, and 3DOM Ca12Al14O32Cl2 catalysts for biodiesel transesterification were prepared by sol-gel method. The 3DOM catalysts were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FTIR). The hierarchical porous structure was achieved; however, only 3DOM CaO/Al2O3 and 3DOM Ca12Al14O32Cl2 catalysts were used for transesterification due to high amount of active CaO. Various parameters such as methanol to oil molar ratio, catalyst concentration, reaction time, and their influence on the biodiesel production were studied. The result showed that 99.0% RPO conversion was achieved using the 3DOM Ca12Al14O33Cl2 as a catalyst under the optimal condition of 12 : 1 methanol to oil molar ratio and 6 wt.% catalyst with reaction time of 3 hours at 65°C.


1980 ◽  
Vol 58 (8) ◽  
pp. 777-779 ◽  
Author(s):  
T. Stanley Cameron ◽  
Christine Chan ◽  
David G. Morris ◽  
Alistair G. Shepherd

The crystals belong to the orthorhombic space group C222, with a = 9.226, b = 12.092, c = 16.513 Å, Z = 4. A single crystal X-ray diffraction analysis has shown that the title compound, in which all carbon atoms are sp2 hybridized, exists with the ten membered ring in a slightly twisted tub conformation. The 13C nmr spectrum is also reported.


1989 ◽  
Vol 44 (1) ◽  
pp. 5-8
Author(s):  
Michel Mégnamisi-Bélombé

Abstract trans-Dichloro(ethanedial-dioximato)(ethanediaI-dioxime)rhodium (III), RhCl2(GH)(GH2), has been synthesized and its structure determined by single crystal X-ray diffraction at room temperature. C4H7Cl2N4O4Rh, Mr = 348.94. monoclinic space group P21/ɑ; a = 10.543(3), b = 8.363(2), c = 11.512(3)Å ; β = 92.79(2)°; V = 1024Å3; Z = 4; Dc = 2.26 Mg m-3. Final Rw = 0.075 for 2035 reflections and 139 parameters. The coordination geometry around Rh is a dis­torted (4+2) octahedron, with four chelating N atoms lying in the equatorial plane and the two Cl atoms in the apical positions. The H atoms of the oxime groups are involved in relatively weak intramolecular O-H-O bridgings, as well as in very strong intermolecular bridgings which extend throughout the crystal structure and propagate nearly parallel to the [101] crystallographic direction.


1998 ◽  
Vol 53 (5-6) ◽  
pp. 634-636 ◽  
Author(s):  
Martina Näveke ◽  
Armand Blaschette ◽  
Peter G. Jones

Abstract The crystal structure of the known title compound was determined by low-temperature X-ray diffraction (orthorhombic, space group Pbcn, Z = 4). The molecule displays an unusually short O-N bond, a relatively long C-O bond and a moderately pyramidal O-NS2 skeleton (O-N 133.1, C-O 148.5 pm, sum of bond angles at N: 347.4°).


Sign in / Sign up

Export Citation Format

Share Document