Masking of Lewis acidity trends in the solid-state structures of trichlorido- and tribromido(2,2′:6′,2′′-terpyridine-κ3N,N′,N′′)gallium(III)

2014 ◽  
Vol 70 (3) ◽  
pp. 312-314 ◽  
Author(s):  
Igor V. Kazakov ◽  
Michael Bodensteiner ◽  
Alexey Y. Timoshkin

The molecular structures of trichlorido(2,2′:6′,2′′-terpyridine-κ3N,N′,N′′)gallium(III), [GaCl3(C15H11N3)], and tribromido(2,2′:6′,2′′-terpyridine-κ3N,N′,N′′)gallium(III), [GaBr3(C15H11N3)], are isostructural, with the GaIIIatom displaying an octahedral geometry. It is shown that the Ga—N distances in the two complexes are the same within experimental error, in contrast to expected bond lengthening in the bromide complex due to the lower Lewis acidity of GaBr3. Thus, masking of the Lewis acidity trends in the solid state is observed not only for complexes of group 13 metal halides with monodentate ligands but for complexes with the polydentate 2,2′:6′,2′′-terpyridine donor as well.

2012 ◽  
Vol 51 (21) ◽  
pp. 11602-11611 ◽  
Author(s):  
Alexey Y. Timoshkin ◽  
Michael Bodensteiner ◽  
Tatiana N. Sevastianova ◽  
Anna S. Lisovenko ◽  
Elena I. Davydova ◽  
...  

Author(s):  
K. Chandra Mohan ◽  
K. Ravikumar ◽  
M. M. Shetty ◽  
D. Velmurugan

AbstractThe solid-state structures of three calcium channel antagonists viz. 1,4-dihydro-6-methyl-5-N-methyl-carbamoyl-4-(3′,4′-dichlorophenyl)-2(3 H)-pyrimidinethione, C


1986 ◽  
Vol 41 (9) ◽  
pp. 1112-1116 ◽  
Author(s):  
Dietmar Schomburg ◽  
Armand Blaschette ◽  
Elke Wieland

Abstract The crystal and molecular structures of two dimesylamine derivatives, RN(SO2CH3)2, (R = Si(CH3)3 (1a), R-CH3 (1b)) were determined. Com pound 1a displays a very long Si-N bond which is well outside the range normally found in comparable com pounds (185.1 pm, mean value for two crystallographically independent m olecules). The unusually large bond length can be explained by the absence of (d -p)π interactions between silicon and nitrogen. In both com pounds the bonding geometry around the nitrogen atoms is essentially planar


2017 ◽  
Vol 73 (11) ◽  
pp. 960-967 ◽  
Author(s):  
Franc Perdih

Copper(II) bis(4,4,4-trifluoro-1-phenylbutane-1,3-dionate) complexes with pyridin-2-one (pyon), 3-hydroxypyridine (hpy) and 3-hydroxypyridin-2-one (hpyon) were prepared and the solid-state structures of (pyridin-2-one-κO)bis(4,4,4-trifluoro-3-oxo-1-phenylbutan-1-olato-κ2 O,O′)copper(II), [Cu(C10H6F3O2)2(C5H5NO)] or [Cu(tfpb-κ2 O,O′)2(pyon-κO)], (I), bis(pyridin-3-ol-κO)bis(4,4,4-trifluoro-3-oxo-1-phenylbutan-1-olato-κ2 O,O′)copper(II), [Cu(C10H6F3O2)2(C5H5NO)2] or [Cu(tfpb-κ2 O,O′)2(hpy-κO)2], (II), and bis(3-hydroxypyridin-2-one-κO)bis(4,4,4-trifluoro-3-oxo-1-phenylbutan-1-olato-κ2 O,O′)copper(II), [Cu(C10H6F3O2)2(C5H5NO2)2] or [Cu(tfpb-κ2 O,O′)2(hpyon-κO)2], (III), were determined by single-crystal X-ray analysis. The coordination of the metal centre is square pyramidal and displays a rare example of a mutual cis arrangement of the β-diketonate ligands in (I) and a trans-octahedral arrangement in (II) and (III). Complex (II) presents the first crystallographic evidence of κO-monodentate hpy ligation to the transition metal enabling the pyridine N atom to participate in a two-dimensional hydrogen-bonded network through O—H...N interactions, forming a graph-set motif R 2 2(7) through a C—H...O interaction. Complex (III) presents the first crystallographic evidence of monodentate coordination of the neutral hpyon ligand to a metal centre and a two-dimensional hydrogen-bonded network is formed through N—H...O interactions facilitated by C—H...O interactions, forming the graph-set motifs R 2 2(8) and R 2 2(7).


2001 ◽  
Vol 05 (09) ◽  
pp. 702-707 ◽  
Author(s):  
LI CHEN ◽  
JESSE B. FOX ◽  
GEUN-BAE YI ◽  
MASOOD A. KHAN ◽  
GEORGE B. RICHTER-ADDO

Para-aminosubstituted nitrosoarenes react with Ru ( CO )( OEP ) or [ Co ( TPP )( THF )2] SbF 6 (OEP2- = 2,3,7,8,12,13,17,18-octaethylporphyrinato dianion, TPP2- = 5,10,15,20-tetraphenylporphyrinato dianion) to generate Ru ( OEP )( ONC 6 H 4 NMe 2)2 and [ Co ( TPP )( ONC 6 H 4 NR 2)2] SbF 6 ( R = Me , Et ), respectively, in fair to high yields. These N -bound nitrosoarene complexes have been characterized by spectroscopic methods. The complexes Ru ( OEP )( ONC 6 H 4 NMe 2)2 and [ Co ( TPP )( ONC 6 H 4 NMe 2)2] ClO 4 have also been characterized by single-crystal X-ray crystallography. Their structures represent the first reported solid-state structures of Ru and Co porphyrins containing C-nitroso ligands.


2001 ◽  
Vol 79 (5-6) ◽  
pp. 607-612 ◽  
Author(s):  
Man-Kit Lau ◽  
Joyce LC Chim ◽  
Wing-Tak Wong ◽  
Ian D Williams ◽  
Wa-Hung Leung

Reaction of [OsO4] with C7H7MgBr (C7H7 = 2-methylphenyl) followed by column chromatography afforded the reported osmium tetraaryl [Os(C7H7)4] along with the oxo-osmium(VI) ([OsO(C7H7)4]) (1) (13%) and the dioxo-osmium(VI) ([OsO2(C7H7)2]) (2) (25%) complexes. Treatment of [OsO4] with C8H9MgBr (C8H9 = 2,5-dimethylphenyl) gave a mixture of [Os(C8H9)4] (3) (34%) and [OsO(C8H9)4] (4) (4%) while that with C8H9OMgBr (C8H9O = 4-methoxy-2-methylphenyl) afforded [OsO(C8H9O)4] (5) in 20% yield. Oxidation of 3 with 3-chloroperoxybenzoic acid afforded 4 in good yield. The solid-state structures of 1 and 4 have been established by X-ray crystallography. Crystals of 1 are tetragonal with a = 13.080(1) and c = 6.6506(5) Å, V = 1137.9(1) Å3, Z = 2, and space group of P4/n; while those of 4 are tetragonal with a = 13.593(2) and c = 7.377(2) Å, V = 1363.0(5) Å3, Z = 4, and space group of P4/n. The geometry around osmium in both complexes is square pyramidal with the oxo ligand occupying apical position. The Os—O and Os—C distances in 1 are 1.652(2) and 2.084(1) Å, respectively, while those in 4 are 1.688(7) and 2.088(4) Å, respectively. The cyclic voltammograms of the monooxo aryl osmium(VI) compounds show reversible Os(VI/V) couple at around –1.4 V vs. ferrocene/ferrocenium couple.Key words: osmium(VI), oxo aryl complexes.


2016 ◽  
Vol 45 (14) ◽  
pp. 6149-6158 ◽  
Author(s):  
David-R. Dauer ◽  
Melchior Flügge ◽  
Regine Herbst-Irmer ◽  
Dietmar Stalke

On the basis of the deprotonated bis-(4-methylbenzoxazol-2-yl)-methane ligand 1 a series of group 13 metal complexes was synthesised and fully characterised. A detailed comparison of solid state structures demonstrates clearly the similarity of methanide and the omnipresent nacnac ligand.


CrystEngComm ◽  
2019 ◽  
Vol 21 (21) ◽  
pp. 3295-3303 ◽  
Author(s):  
Rüdiger W. Seidel ◽  
Richard Goddard ◽  
Nils Nöthling ◽  
Christian W. Lehmann

The crystal and molecular structures of the bio-based platform chemical furfural (1) and its derivatives furfurylamine (2), 2-furonitrile (3) and 2-methylfuran (4), which are all liquid at ambient temperature, have been determined by in situ cryocrystallography.


2011 ◽  
Vol 66 (12) ◽  
pp. 1255-1260 ◽  
Author(s):  
Sebastian Leitner ◽  
Manuela List ◽  
Uwe Monkowius

1-(2,2ʹ-Diethoxyethyl)-3-methyl-imidazolium bromide, 1, has been prepared and used as a precursor for the synthesis of the corresponding silver bromide complex [(NHC)2Ag][AgBr2], 2. Transmetallation of 2 with (tht)AuBr (tht = tetrahydrothiophene) yields (NHC)AuBr, 3. The solid-state structures of 2 and 3 have been determined by single-crystal X-ray diffraction revealing a loose aggregation of the complexes by weak metal-metal interactions. Due to the presence of these contacts, both complexes are emissive in the solid state.


2011 ◽  
Vol 40 (34) ◽  
pp. 8598 ◽  
Author(s):  
Oleksandr Hietsoi ◽  
Alexander S. Filatov ◽  
Cristina Dubceac ◽  
Marina A. Petrukhina

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