4-Substituted 3,6-Bis(2-pyridyl)pyridazines: Silver(I) Complexes of 4-Cyano- and 4-(4-Bromophenyl)-3,6-bis(2-pyridyl)pyridazine and Pseudopolymorphs of 1,3,5-Tris{3,6-bis(2-pyridyl)pyridazin-4-yl}benzene

2008 ◽  
Vol 61 (11) ◽  
pp. 847 ◽  
Author(s):  
Edwin C. Constable ◽  
Catherine E. Housecroft ◽  
Markus Neuburger ◽  
Sébastien Reymann ◽  
Silvia Schaffner
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Crystal Structures ◽  
Model Structure ◽  
State Structure ◽  
Ligand Environment ◽  
Solid State Structure ◽  
Single Crystal Structures

Metal:ligand complexes are crystallized from reaction mixtures of equimolar amounts of 4-cyano-3,6-bis(2-pyridyl)pyridazine 2 or 4-(4-bromophenyl)-3,6-bis(2-pyridyl)pyridazine 3 and silver(i) triflate. In [Ag2(2)2]2+, the two ligands adopt a head-to-tail arrangement, while a head-to-head motif is confirmed for the solid state structure of [Ag2(3)2]2+. In solution, one ligand environment is observed in each case. Silver(i) reacts with 1,3,5-tris{3,6-bis(2-pyridyl)pyridazin-4-yl}benzene 4 to give highly insoluble powders. The single crystal structures of the pseudopolymorphs (4)·Et2O and 2(4)·2MeCN·H2O are reported; in each structure, the ligand adopts the same conformation, derived from a Cs rather than C3v model structure.

Synthesis and structural characterization of a magnesium phthalocyanine(3–) anion

2012 ◽  
Vol 16 (01) ◽  
pp. 154-162 ◽  
Author(s):  
Edwin W.Y. Wong ◽  
Daniel B. Leznoff
Keyword(s):  
Absorption Spectrum ◽  
Solid State ◽  
Single Crystal ◽  
Structural Characterization ◽  
Heterometallic Complex ◽  
State Structure ◽  
Solid State Structure ◽  
X Ray ◽  
X Ray Crystallography

The reduction of magnesium phthalocyanine (MgPc) with 2.2 equivalents of potassium graphite in 1,2-dimethoxyethane (DME) gives [K2(DME)4]PcMg(OH)(1) in 67% yield. Compound 1 was structurally characterized using single crystal X-ray crystallography and was found to be a monomeric, heterometallic complex consisting of a μ3-OH ligand that bridges a [MgIIPc3-]- anion to two potassium cations solvated by four DME molecules. An absorption spectrum of 1 confirms the Pc ligand is singly reduced and has a 3–charge. The solid-state structure of 1 does not indicate breaking of the aromaticity of the Pc ligand. Compound 1 is only the second Pc3- complex and the first reduced MgPc to be isolated and structurally characterized.

Structural Study of an Acyclic Diterpene From Eremophila Species

1996 ◽  
Vol 49 (6) ◽  
pp. 701 ◽  
Author(s):  
YM Syah ◽  
EL Ghisalberti ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Structural Study ◽  
Room Temperature ◽  
State Structure ◽  
Solid State Structure ◽  
X Ray

The solid-state structure of the semicarbazone derivative (3) of the aldehyde diacid (1), an acyclic diterpene isolated from Eremophila species, has been determined by a single-crystal room-temperature X-ray study. Crystals of (3) are triclinic, Pī , a 14.642(7), b 14.371(6), c 12.823(6) Ǻ, α 76.59(4), β 66.09(4), γ 72.97(4)°, Z = 4; R was 0.052 for 2265 independent 'observed' (I > 3σ(I)) diffractometer reflections.

scholarly journals Switching the Conformation of 3,2′:6′,3″-tpy Domains in 4′-(4-n-Alkyloxyphenyl)-3,2′:6′,3″-Terpyridines

Molecules ◽  
2020 ◽  
Vol 25 (14) ◽  
pp. 3162 ◽  
Author(s):  
Dalila Rocco ◽  
Alessandro Prescimone ◽  
Edwin C. Constable ◽  
Catherine E. Housecroft
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Crystal Structures ◽  
Dominant Role ◽  
Van Der Waals Interactions ◽  
Single Crystal Structures ◽  
Solid State Structures ◽  
Packing Interactions ◽  
Adjacent Sheet

The preparation and characterization of 4′-(4-n-octyloxyphenyl)-3,2′:6′,3″-terpyridine (8) and 4′-(4-n-nonyloxyphenyl)-3,2′:6′,3″-terpyridine (9) are reported. The single crystal structures of 4′-(4-n-hexyloxyphenyl)-3,2′:6′,3″-terpyridine (6), 4′-(4-n-heptyloxyphenyl)-3,2′:6′,3″-terpyridine (7), and compounds 8 and 9 have been determined. The conformation of the 3,2′:6′,3″-tpy unit is trans,trans in 6 and 7, but switches to cis,trans in 8 and 9. This is associated with significant changes in the packing interactions with a more dominant role for van der Waals interactions between adjacent n-alkyloxy chains and C–Hmethylene... π interactions in 8 and 9. The solid-state structures of 6 and 7 with the n-hexyloxy and n-heptyloxy chains feature interwoven sheets of supramolecular assemblies of molecules, with pairs of n-alkyloxy chains threaded through cavities in an adjacent sheet.

N–O Bond Cleavage During the Deprotonation of N,O-Bis(trimethylsilyl)hydroxylamine

2008 ◽  
Vol 63 (3) ◽  
pp. 339-341 ◽  
Author(s):  
Ajay Venugopal ◽  
Alexander Willner ◽  
Norbert W. Mitzel
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Elemental Analysis ◽  
Bond Cleavage ◽  
State Structure ◽  
X Ray Diffraction ◽  
Solid State Structure ◽  
X Ray ◽  
Potassium Hydride ◽  
Oxygen Atoms

The reaction of N,O-bis(trimethylsilyl)hydroxylamine with potassium hydride in pentane affords a product of the formula {K6[OSiMe3]4[ON(SiMe3)2]2}, resulting from deprotonation followed by N-O bond cleavage and 1,2-silylshift. The compound was characterised by elemental analysis and by single crystal X-ray diffraction. The aggregate consists of a K3O3 bis-cubane core, with N(SiMe3)2 groups at the oxygen atoms shared by the two cubes, andMe3Si groups attached to the four O vertices. Two weak K···N interactions are also detected in the solid state structure.

Notizen: Solid State Structure of N,N-Dibenzylhydroxylamine

1995 ◽  
Vol 50 (4) ◽  
pp. 699-701 ◽  
Author(s):  
Norbert W. Mitzel ◽  
Jürgen Riede ◽  
Klaus Angermaier ◽  
Hubert Schmidbaur
Keyword(s):  
Solid State ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
State Structure ◽  
X Ray Diffraction ◽  
Space Group ◽  
Solid State Structure ◽  
X Ray

The solid-state structure of N,N-dibenzylhydroxylamine (1) has been determined by single crystal X-ray diffraction. The compound crystallizes in the monoclinic space group P 21/n with four formula units in the unit cell. N,N-dibenzylhydroxylamine dimerizes to give N2O2H2 sixmembered rings as a result of the formation of two hydrogen bonds O - H ··· N in the solid state.

Synthesis of Diferrocenylethyne by Molybdenum-Catalyzed Metathesis of 1-Ferrocenylprop-1-yne

2003 ◽  
Vol 68 (10) ◽  
pp. 1897-1903 ◽  
Author(s):  
Martin Kotora ◽  
David Nečas ◽  
Petr Štěpnička
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
State Structure ◽  
X Ray Diffraction ◽  
Catalytic Systems ◽  
Solid State Structure ◽  
X Ray

Diferrocenylethyne (1) was synthesized by metathesis of 1-ferrocenylprop-1-yne using various catalytic systems based on [Mo(CO)6] (5 mole %) and a chlorophenol (30 mole %) in toluene. The yields varied for different chlorophenols; the best conversions were obtained with 2,5-dichlorophenol (66%) and 4-chlorophenol (55%). Alkyne 1 was further reduced to the known (E)-1,2-diferrocenylethene and 1,2-diferrocenylethane, and its solid-state structure determined by single-crystal X-ray diffraction.

Structural Study of Dehydrocurvularin, an Inhibitor of Microtubule Assembly

1994 ◽  
Vol 47 (6) ◽  
pp. 1193 ◽  
Author(s):  
F Almassi ◽  
EL Ghisalberti ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Structural Study ◽  
Room Temperature ◽  
Microtubule Assembly ◽  
State Structure ◽  
Fungal Metabolite ◽  
Solid State Structure ◽  
X Ray ◽  
Opposite Helicity

The solid-state structure of the fungal metabolite E-dehydrocurvularin (2), an inhibitor of microtubule assembly, has been determined by a single-crystal room-temperature X-ray study for comparison with curvularin (1). Crystals of (2) are orthorhombic, P212121, a 17.757(9), b 10.031(6), c 8.069(4) Ǻ, Z = 4; R was 0.060 for 988 independent 'observed' [I > 3σ(I)] diffractometer reflections. The results of this study show that (1) and (2) adopt opposite helicity in the solid state.

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