Syntheses and Characterization of Chemically Flexible, Water-Soluble Dithio−Bis(phosphine) Compounds:  (HOH2C)2P(CH2)2S(CH2)3S(CH2)2P(CH2OH)2, (HOH2C)2PCH2CH2S(CH2)4SCH2CH2P(CH2OH)2, and (HOH2C)2PCH2CH2CH2S(CH2)3SCH2CH2CH2P(CH2OH)2. Systematic Investigation of the Effect of Chain Length on the Coordination Chemistry of Rhenium(V). X-ray Crystal Structures of [ReO2(HOH2C)2P(CH2)2S(CH2)3S(CH2)2P(CH2OH)2]2(Cl)2, [ReO2(HOH2C)2P(CH2)2S(CH2)4S(CH2)2P-(CH2OH)2]2(ReO4-)2, and [ReO2(HOH2C)2P(CH2)3S(CH2)3S(CH2)3P(CH2OH)2](Cl)

1997 ◽  
Vol 36 (18) ◽  
pp. 3928-3935 ◽  
Author(s):  
C. Jeffrey Smith ◽  
Kattesh V. Katti ◽  
Wynn A. Volkert ◽  
Leonard J. Barbour
Keyword(s):  
Coordination Chemistry ◽  
Crystal Structures ◽  
Chain Length ◽  
Systematic Investigation ◽  
Water Soluble ◽  
X Ray

scholarly journals A Versatile Approach to Access Trimetallic Complexes Based on Trisphosphinite Ligands

Molecules ◽  
2020 ◽  
Vol 25 (3) ◽  
pp. 593
Author(s):  
Juan Miranda-Pizarro ◽  
Macarena G. Alférez ◽  
M. Dolores Fernández-Martínez ◽  
Eleuterio Álvarez ◽  
Celia Maya ◽  
...  
Keyword(s):  
Coordination Chemistry ◽  
Late Transition Metal ◽  
X Ray Diffraction ◽  
X Ray ◽  
Full Characterization ◽  
Metal Precursors ◽  
Straightforward Method ◽  
One Step ◽  
Late Transition

A straightforward method for the preparation of trisphosphinite ligands in one step, using only commercially available reagents (1,1,1-tris(4-hydroxyphenyl)ethane and chlorophosphines) is described. We have made use of this approach to prepare a small family of four trisphosphinite ligands of formula [CH3C{(C6H4OR2)3], where R stands for Ph (1a), Xyl (1b, Xyl = 2,6-Me2-C6H3), iPr (1c), and Cy (1d). These polyfunctional phosphinites allowed us to investigate their coordination chemistry towards a range of late transition metal precursors. As such, we report here the isolation and full characterization of a number of Au(I), Ag(I), Cu(I), Ir(III), Rh(III) and Ru(II) homotrimetallic complexes, including the structural characterization by X-ray diffraction studies of six of these compounds. We have observed that the flexibility of these trisphosphinites enables a variety of conformations for the different trimetallic species.

Distorted chiolite crystal structures of α-Na5M3F14 (M=Cr,Fe,Ga) studied by X-ray powder diffraction

2003 ◽  
Vol 18 (2) ◽  
pp. 128-134 ◽  
Author(s):  
A. Le Bail ◽  
A.-M. Mercier
Keyword(s):  
Crystal Structures ◽  
Powder Diffraction ◽  
Room Temperature ◽  
Rietveld Refinements ◽  
Space Group ◽  
X Ray ◽  
Precise Characterization

The crystal structures of the chiolite-related room temperature phases α-Na5M3F14 (MIII=Cr,Fe,Ga) are determined. For all of them, the space group is P21/n, Z=2; a=10.5096(3) Å, b=7.2253(2) Å, c=7.2713(2) Å, β=90.6753(7)° (M=Cr); a=10.4342(7) Å, b=7.3418(6) Å, c=7.4023(6) Å, β=90.799(5)° (M=Fe), and a=10.4052(1) Å, b=7.2251(1) Å, c=7.2689(1), β=90.6640(4)° (M=Ga). Rietveld refinements produce final RF factors 0.036, 0.033, and 0.035, and RWP factors, 0.125, 0.116, and 0.096, for MIII=Cr, Fe, and Ga, respectively. The MF6 polyhedra in the defective isolated perovskite-like layers deviate very few from perfect octahedra. Subtle octahedra tiltings lead to the symmetry decrease from the P4/mnc space group adopted by the Na5Al3F14 chiolite aristotype to the P21/n space group adopted by the title series. Facile twinning precluded till now the precise characterization of these compounds.

scholarly journals X-ray spectroscopy characterization of self-assembled monolayers of nitrile-substituted oligo(phenylene ethynylene)s with variable chain length

2012 ◽  
Vol 3 ◽  
pp. 12-24 ◽  
Author(s):  
Hicham Hamoudi ◽  
Ping Kao ◽  
Alexei Nefedov ◽  
David L Allara ◽  
Michael Zharnikov
Keyword(s):  
Chain Length ◽  
Photoelectron Spectroscopy ◽  
Self Assembled Monolayers ◽  
Phenylene Ethynylene ◽  
X Ray ◽  
Molecular Length ◽  
Assembled Monolayers ◽  
Self Assembled ◽  
Gold Thiolate

Self-assembled monolayers (SAMs) of nitrile-substituted oligo(phenylene ethynylene) thiols (NC-OPEn) with a variable chain length n (n ranging from one to three structural units) on Au(111) were studied by synchrotron-based high-resolution X-ray photoelectron spectroscopy and near-edge absorption fine-structure spectroscopy. The experimental data suggest that the NC-OPEn molecules form well-defined SAMs on Au(111), with all the molecules bound to the substrate through the gold–thiolate anchor and the nitrile tail groups located at the SAM–ambient interface. The packing density in these SAMs was found to be close to that of alkanethiolate monolayers on Au(111), independent of the chain length. Similar behavior was found for the molecular inclination, with an average tilt angle of ~33–36° for all the target systems. In contrast, the average twist of the OPEn backbone (planar conformation) was found to depend on the molecular length, being close to 45° for the films comprising the short OPE chains and ~53.5° for the long chains. Analysis of the data suggests that the attachment of the nitrile moiety, which served as a spectroscopic marker group, to the OPEn backbone did not significantly affect the molecular orientation in the SAMs.

Coordination Chemistry ofN,N,N′,N′-Tetraethylpyridine-2,6-dithiocarboxamide (S-dept) - X-ray Crystal Structures and Magnetic Properties of [Co(S-dept)X2] (X = Br, I, and NCS)

2005 ◽  
Vol 2005 (19) ◽  
pp. 3884-3893 ◽  
Author(s):  
Ramesh Kapoor ◽  
Ashok Kataria ◽  
Paloth Venugopalan ◽  
Pratibha Kapoor ◽  
Geeta Hundal ◽  
...  
Keyword(s):  
Magnetic Properties ◽  
Coordination Chemistry ◽  
Crystal Structures ◽  
X Ray

scholarly journals The preparation and characterization of SeCl3SbF6, improved syntheses of MCl3(As/Sb)F6 (M = S, Se), and the X-ray crystal structure determination of SeCl3AsF6 and a new phase of SBr3SbF6

1996 ◽  
Vol 74 (9) ◽  
pp. 1671-1681 ◽  
Author(s):  
Jack Passmore ◽  
Paul D. Boyle ◽  
Gabriele Schatte ◽  
Todd Way ◽  
T. Stanley Cameron
Keyword(s):  
Crystal Structure ◽  
Raman Spectroscopy ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
X Ray ◽  
Ft Raman Spectroscopy ◽  
New Phase ◽  
Ft Raman

Alternative and, in some cases, improved syntheses of the salts MX3(As/Sb)F6 (M = S, Se) and SCl3(SbCl6/AlCl4) are described. In addition, the synthesis of SeCl3SbF6 is reported. The compounds were characterized by FT–Raman spectroscopy and the X-ray crystal structures of SeCl3AsF6 (also 77Se NMR) and a new phase of SBr3SbF6 were determined. Crystals of SeCl3AsF6 and SBr3SbF6 are monoclinic, space group P21/c with [values for SBr3SbF6 in brackets] a = 7.678(1) [8.137(1)] Å, b = 9.380(3) [9.583(2)] Å, c = 11.920(3) [12.447(2)] Å, β = 98.19(2)° [97.36(1)]°, V = 849.72(3) [962.6(3)] Å3,z = 4, Dx = 2.925 [3.502] Mg m−3, R = 0.0525 [0.055], and Rw = 0.0554 [0.060] for 1151 [1472] observed reflections. Key words: MX3+ salts, FT–Raman spectroscopy, X-ray crystal structures of SeCl3AsF6, SBr3SbF6, and preparation of SeCl3SbF6.

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