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8. Cobalt-complexed conjugated diyne salts: A family of rigid masked dielectrophiles. Syntheses, structures, and double nucleophilic substitutions

Author

Amouri, H., Malezieux, B., Andres, R., Vaissermann, J., Gruselle, M., and Silva, C. Da

Subjects
X-rays -- Research, Electrophiles -- Chemical properties, Chemistry
Abstract

Three X-ray structures belonging to family of rigid masked dielectrphiles were ascertained by X-ray analysis. The X-ray structures provide valuable information on the arrangement of the CO(sub 2)-alkyne units, which have a cis geometry and are in sharp contrast to that observed for diyne - tetracobalt compounds.

Published
2000

9. Potentiometric and multinuclear NMR study of the binary and ternary uranium(VI)-L- fluoride systems. where L is alpha-hydroxycarboxylate or glycine

Author

Szabo, Zoltan, Grenthe, Ingmar, Krausz, Elmars, Vaissermann, J., and Gruselle, M.

Subjects
Fluorides -- Chemical properties, Uranium dioxide -- Chemical properties, Nuclear magnetic resonance spectroscopy -- Usage, Chemistry
Abstract

The rates and mechanisms of inter-and intramolecular ligand-exchange reactions in dioxouranium(VI) complexes are discussed. The complex formation and equilibrium dynamics are studied by potentiometry and multinuclear NMR spectroscopy for the binary and ternary uranium(VI)-alpha-hydroxycarxylate-fluoride systems.

Published
2000

14. Strong magneto-chiral dichroism in enantiopure chiral ferromagnets

Author

Train, C., Gheorghe, R., Krstic, V., L.M., Chamoreau, Ovanesyan, N., G.L.J.A., Rikken, Gruselle, M., Verdaguer, M., Laboratoire National des Champs Magnétiques Pulsés (LNCMP), Centre National de la Recherche Scientifique (CNRS)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA), Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Université Toulouse III - Paul Sabatier (UT3), and Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS)

Subjects
[PHYS.COND.CM-S]Physics [physics]/Condensed Matter [cond-mat]/Superconductivity [cond-mat.supr-con], ComputingMilieux_MISCELLANEOUS
Abstract

International audience

Published
2008

15. A new family of mono- and dicarboxylic ruthenium complexes [Ru(DIP)(2)(L-2)](2+) (DIP=4,7-diphenyl-1,10-phenanthroline): Synthesis, solution behavior, and X-ray molecular structure of trans-[Ru(DIP)(2)(MeOH)(2)][OTf](2)

Author

Caspar, R., Cordier, C., Waern, Jb., Guyard-Duhayon, Carine, Gruselle, M., Le Floch, Pascal, Amouri, Hani, Laboratoire de Chimie Inorganique et Matériaux Moléculaires (CIM2), Université Pierre et Marie Curie - Paris 6 (UPMC)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Interfaces, Traitements, Organisation et Dynamique des Systèmes (ITODYS (UMR_7086)), Université Paris Diderot - Paris 7 (UPD7)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Laboratoire Hétéroéléments et Coordination (DCPH), École polytechnique (X)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Centre National de la Recherche Scientifique (CNRS)-Université Pierre et Marie Curie - Paris 6 (UPMC), Centre National de la Recherche Scientifique (CNRS)-Université Paris Diderot - Paris 7 (UPD7), and Centre National de la Recherche Scientifique (CNRS)-École polytechnique (X)

Subjects
ligands, hexafluorophosphate, [CHIM.COOR]Chemical Sciences/Coordination chemistry, dynamics, recognition, dna-binding, crystal
Abstract

9 pages; A new family of ruthenium complexes of general formula [Ru(DIP)(2)(L-2)](2+), where DIP) 4,7-diphenyl-1,10-phenanthroline,a bidentate ligand with an extended aromatic system, was prepared and fully characterized. When L is a monodentate ligand, the following complexes were obtained: L = CF3SO3-1 (2), CH3CN (3), and MeOH (4). When L-2 is a bidentate ligand, the compounds [Ru(DIP)(2)(Hcmbpy)][Cl](2) (5) and [Ru(DIP)(2)(H(2)dcbpy)][Cl](2) ( 6) were prepared (Hcmbpy = 4-carboxy-4'-methyl-2,2-bipyridine, H(2)dcbpy = 4,4'-dicarboxy-2,2'-bipyridine). Complex [Ru(DIP)(2)(MeOH)(2)][OTf](2) (4) displayed a trans configuration of the DIP ligands, which is rare for octahedral complexes featuring DIP bidentate ligands. DFT calculations carried out on 4 showed that the cis isomer is more stable by 12.2 kcal/ mol relative to the trans species. The solution behaviors of monocarboxylic complex [ Ru( DIP) 2( Hcmbpy)][Cl](2) ( 5) and dicarboxylic complex [Ru(DIP)(2)(H(2)dcbpy)][Cl](2) (6) were investigated by H-1 NMR spectroscopy. VT-NMR, concentration dependence, and reaction with NaOD allowed us to suggest that aggregation of the cationic species in solution, especially for 6, originates mainly from hydrogen bonding interactions.

Published
2006
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32. Electronic and steric factors for elimination reactions in carbenium ions derived from (17.beta.-ethynylestradiol)M2L6 complexes (M2L6 = Co2(CO)6, Mo2Cp2(CO)4. X-ray structure of [Mo2Cp2(CO)4(.mu.-CH.tplbond.CC19H25O)]+BF-4 [Erratum to document cited in CA113(23):212426v]

Author

Gruselle, M., primary, Cordier, C., additional, Salmain, M., additional, El Amouri, H., additional, Guerin, C., additional, Vaissermann, J., additional, and Jaouen, G., additional

Published
1991
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37. Thermoanalytical study of acetylacetonate-modified titanium(IV) isopropoxide as a precursor for TiO2 films.

Author

Krunks, M., Oja, I., Tõnsuaadu, K., Es-Souni, M., Gruselle, M., and Niinistö, L.

Subjects
TITANIUM dioxide, FOURIER transform infrared spectroscopy, THERMOCHEMISTRY, TITANIUM ores, TITANIUM group, THERMAL analysis
Abstract

Thermal decomposition of dried TiO2 gel, obtained by hydrolysing acetylacetonate-modified titanium(IV) isopropoxide, was monitored by simultaneous TG/DTA/EGA-FTIR measurements in dynamic air up to 900°C. XRD and FTIR were employed to identify the solid reaction products. Thermal degradation of the TiO2 gel consists of five distinct mass loss steps, the total mass loss being 43.8%. EGA by FTIR revealed the release of H2O below 120°C; followed by acetone, isopropyl acetate and 1-propanol around 200-300°C, and finally CO and CO2 up to 550°C. Highly exothermic reaction at 410-550°C is caused by the combustion of carbon residues. Crystalline TiO2-anatase is formed around 500°C and TiO2-rutile close to 800°C. [ABSTRACT FROM AUTHOR]

Published
2005
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39. Unexpected formation of chiral single crystals of {NH( n- C 3 H 7 ) 3 [Mn II Cr III (C 2 O 4 ) 3 ]}, A 2D oxalate-based material.

Author

Shilov, G.V., Ovanesyan, N.S., Aldoshin, S.M., Gruselle, M., Train, C., and Guyard-Duhayon, C.

Subjects
CHIRALITY, CRYSTAL whiskers, OXALATES, BIMETALLISM, OPTICAL isomers, ENANTIOMERS
Abstract

In an attempt to obtain chiral single crystals of a two-dimensional (2D) bimetallic oxalate-based material by enantioselective auto-assembling of Mn 2+ and ( rac )-[Cr(C 2 O 4 ) 3 ] 3- templated by the optically active complex (+)-( Rp )-[1-CH 2 ( n- C 3 H 7 ) 3 -2-CH 3 (C 5 H 3 )Fe(C 5 H 5 )] + , we obtained the unexpected 2D network species {NH( n- C 3 H 7 ) 3 [MnCr(C 2 O 4 ) 3 ]}. X-ray diffraction determination of the structure reveals that the complex crystallizes in the enantiomorphous space group P 6 3 . The interlayer spacing of 7.93 Å is the lowest found so far for 2D, bimetallic, oxalate-bridged compounds. [ABSTRACT FROM AUTHOR]

Published
2004
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41. Chiral Templating Activity of Tris(bipyridine)ruthenium(II) Cation in the Design of Three-Dimensional (3D) Optically Active Oxalate-Bridged {[Ru(bpy)<INF>3</INF>][Cu<INF>2</INF><INF>x</INF><INF></INF>Ni<INF>2(1</INF><INF>-</INF><INF>x</INF><INF></INF><INF>)</INF>(C<INF>2</INF>O<INF>4</INF>)<INF>3</INF>]}<INF>n</INF> (0 ≤ x ≤ 1; bpy = 2,2‘-bipyridine): Structural, Optical, and Magnetic Studies

Author

Pointillart, F., Train, C., Gruselle, M., Villain, F., Schmalle, H. W., Talbot, D., Gredin, P., Decurtins, S., and Verdaguer, M.

Abstract

Three-dimensional oxalate-based {[Ru(bpy)3][Cu2xNi2(1-x)(ox)3]}n (0≤ x ≤ 1, ox = C2O42-, bpy = 2,2‘bipyridine) were synthesized. The structure was determined for x = 1 by X-ray diffraction on single crystal. The compound crystallizes in the cubic space group P4132. It shows a three-dimensional 10-gon 3-connected (10,3) anionic network where copper(II) has an unusual tris(bischelated) environment. X-ray powder diffraction patterns and their Rietveld refinement show that all the compounds along the series are isostructural and single-phased. According to X-ray absorption spectroscopy, copper(II) and nickel(II) have an octahedral environment, respectively elongated and trigonally distorted. As shown by natural circular dichroism, the optically active forms of {[Ru(bpy)3][CuxNi2(1-x)(ox)3]}n are obtained starting from resolved Δ- or Λ-[Ru(bpy)3]2+. The Curie−Weiss temperatures range between −55 (x = 1) and −150 K (x = 0). The antiferromagnetic exchange interaction thus decreases when the copper contents increases in agreement with the crystallographic structure of the compounds and the electronic structure of the metal ions. At low temperature, the compounds exhibit complex long-range ordered magnetic behavior.

Published
2004

45. A General Route to Prochiral and Chiral Dicationic Molybdenum−Cobalt Acetylenic Complexes:  Synthesis, Structures, and Reactivity

Author

Gruselle, M., Malezieux, B., Vaissermann, J., and Amouri, H.

Abstract

Several [Co−Co]−alkyne adducts [Co2(CO)6)(μ-η2,η2-HOCR1R2-C&tbd1;C−CR1R2OH)] were prepared (R1 = R2 = H (1); R1 = H, R2 = CH3 (2); R1 = R2 = CH3 (3)) and their X-ray molecular structures determined, showing that the μ-alkyne unit adopts a specific geometry depending on the nature of the alkyne unit. The prochiral [Mo−Co]−alkyne adduct [CpMoCo(CO)5(μ-η2,η2-HOCH2−C&tbd1;C−CH2OH)] (4), identified by X-ray analysis, was obtained from [Co2(CO)6)(μ-η2,η2-HOCH2−C&tbd1;C−CH2OH)] (1) via replacement of a −Co(CO)3 vertex by the isolobal moiety −CpMo(CO)2. Complex 4 reacts with aqueous HBF4 to produce the dicationic tetranuclear species [{CpMoCo(CO)5(μ-η2,η3-CH2−C&tbd1;C−CH2-)}2O][BF4]2 (5), which reacts further with nucleophiles to give a new dicationic tetranuclear species [{CpMoCo(CO)5(μ-η2,η2-Nu1−CH2−C&tbd1;C−CH2−)}2O][BF4]2 (Nu1 = pyridine (6), 3-picoline (7), triphenylphosphine (8)), where the nucleophile has been introduced to the carbenium center (−CH2+). Subsequent treatment of these dications in acidic medium produces the carbenium ions [CpMoCo(CO)5(μ-η2,η3-Nu1−CH2−C&tbd1;C−CH2)][BF4]2 (Nu1 = pyridine (9), 3-picoline (10), triphenylphosphine (11)), which further react with nucleophile Nu2 to produce dications [CpMoCo(CO)5(μ-η2,η2-Nu1−CH2−C&tbd1;C−CH2−Nu2)][BF4]2 {Nu1 = Nu2 = pyridine (13); Nu1 = pyridine, Nu2 = triphenylphosphine (14); Nu1 = Nu2 = triphenylphosphine (15); Nu1 = Nu2 = 3-picoline (16); Nu1 = pyridine = Nu2 = 3-picoline (17)). This synthetic approach is unprecedented because it allows the placement of the same or different types of nucleophiles in a stepwise fashion at the two terminal carbon atoms of the acetylenic complex, yielding, for instance, the chiral dicationic [Mo−Co] cluster [CpMoCo(CO)5(μ-η2,η2-C6H5N−CH2−C&tbd1;C−CH2−NC6H4(CH3))][BF4]2 (17). The X-ray molecular structures of 13, 16, and 17 belonging to this family were determined, including the first chiral [Mo−Co] complex (17) possessing two different functional groups. Further, the structure shows that the coordinated functionalized alkyne can adopt a specific geometry, whereby the two positively functionalized groups are situated on the same side of the cluster unit, available to bind molecules of opposite charge.

Published
1998

47. Synthesis, NMR, and X-ray Molecular Structure of a Unique Chiral Propeller-Like Cobalt Complex [(Co<INF>2</INF>(CO)<INF>4</INF>)μ,η<SUP>2</SUP>,η<SUP>2</SUP>-(−H<INF>2</INF>CC&tbd1;CCH<INF>2</INF>−)(−dppm)<INF>2</INF>][BF<INF>4</INF>]<INF>2</INF> and Differentiation of Its Enantiomers by the Trisphat Anion

Author

Amouri, H., Thouvenot, R., Gruselle, M., Malezieux, B., and Vaissermann, J.

Abstract

The unusual chiral two-bladed propeller cobalt complex [(Co2(CO)4)μ,η2,η2-(−H2CC&tbd1;CCH2−)(−dppm)2][BF4]2 (3) has been prepared and its X-ray structure determined. Addition of the trisphat anion to a CD2Cl2 solution of 3 has led to the NMR nonequivalency of the two enantiomers 3a,b. This is the first example in which a chiral propeller transition metal complex with C2-symmetry has been differentiated by the trisphat anion.

Published
2001

48. Cobalt-Induced C−N and C−C Bond Formation via Metal-Stabilized α-CF<INF>3</INF> Carbenium Ion

Author

Amouri, H., Begue, J.-P., Chennoufi, A., Bonnet-Delpon, D., Gruselle, M., and Malezieux, B.

Abstract

An α-CF3-carbenium ion stabilized by a bimetallic [Co−Co] cluster was prepared and isolated in good yield, starting from the corresponding alcohol by action of HBF4/Et2O. C−N and C−C bonds with nitrogen and carbon nucleophiles could be easily formed. Subsequent decomplexation gave the free substituted β-CF3 alkynes in good yields.

Published
2000

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