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.

Oxide, Sulfide, Selenide, and Borane Derivatives of Indenylphosphines

2003 ◽  
Vol 56 (11) ◽  
pp. 1153 ◽  
Author(s):  
Julian J. Adams ◽  
David E. Berry ◽  
Owen J. Curnow ◽  
Glen M. Fern ◽  
Michelle L. Hamilton ◽  
...  
Keyword(s):  
Solid State ◽  
13C Nmr Spectroscopy ◽  
State Structure ◽  
Solid State Structure ◽  
X Ray ◽  
X Ray Crystallography ◽  
Isolation And Characterization ◽  
Linear Relationships ◽  
Derivatives Of

We report the preparation, isolation and characterization of oxide, sulfide, selenide, and borane derivatives of a series of indenylphosphines. Some members of the series had already been prepared, and we have completed the series. We have prepared (indenyl)xPh3-xPO (x = 1–3) for the oxide series, (indenyl)xPh3-xPS (x = 3) for the sulfides, (indenyl)xPh3-xPSe (x = 1,2) for the selenides, and (indenyl)xPh3-xPBH3 (x = 1–3) for the boranes. Linear relationships of the 31P NMR chemical shift with the number of indenyl groups were observed. The compounds were also characterized by 1H and 13C NMR spectroscopy and mass spectrometry. The solid-state structure of diindenylphenylphosphine selenide was determined by X-ray crystallography and found to be isomorphous with diindenylphenylphosphine sulfide. The solid-state structure of triindenylphosphine sulfide was also determined by X-ray crystallography and the indenyl groups were confirmed to all be the inden-3-yl isomer. Additionally, pentacarbonyl(triindenylphosphine)molybdenum(0), 1,3-bis(diphenylphosphino)indene diborane, and rac-bis(1-(diphenylphosphino)indenyl)ironII) diborane were prepared, isolated, and 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.

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.

Solid-state structure of NH-pyrazolium hydrochlorides and hydrobromides by X-ray crystallography and CPMAS NMR

1997 ◽  
Vol 415 (1-2) ◽  
pp. 81-92 ◽  
Author(s):  
Concepción Foces-Foces ◽  
Lourdes Infantes ◽  
Rosa Marı́a Claramunt ◽  
Concepción López ◽  
Nadine Jagerovic ◽  
...  
Keyword(s):  
Solid State ◽  
State Structure ◽  
Solid State Structure ◽  
X Ray ◽  
X Ray Crystallography

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.

scholarly journals Bleaching the Record: After 200 Years, Single Crystal X-Ray Crystallography Reveals the Structure and Hydrogen-Bonding Properties of Hypochlorite and Hypobromite Ions in the Solid State

2021 ◽  
Author(s):  
Filip Topic ◽  
Joseph Marrett ◽  
Tristan Borchers ◽  
Hatem M. Titi ◽  
Christopher J. Barrett ◽  
...  
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Gas Phase ◽  
X Ray ◽  
X Ray Crystallography ◽  
Single Crystal Structures ◽  
Hypohalous Acids ◽  
Bonding Properties ◽  
Insight Into

<div>We report the first single crystal structures of hypochlorite and hypobromite salts, including hydrated sodium hypochlorite - a ubiquitous bleaching and disinfection agent in use for almost 200 years. The structures represent the first characterization of fundamentally important hypochlorite and hypobromite anions in the solid state, by X-ray crystallography and are supported by Raman spectroscopy on individual crystals. The structural analysis provides insight into supramolecular chemistry of the hypohalite ions in the hydrated environment of the NaOCl<sup>.</sup>5H<sub>2</sub>O and NaOBr<sup>.</sup>5H<sub>2</sub>O solid salts, and reveals measured Cl-O and Br-O bond lengths of 1.69 A and 1.82 A, respectively, which are significantly longer than those for corresponding higher-valence oxoanions, and in agreement with the values spectroscopically determined for hypohalous acids and corresponding oxides in the gas phase.<br></div>

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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