Reaction Pathways in Solid-State Processes. 1. Carbon-13 NMR and X-ray Crystallography of Fluorobullvalene

The mixed-metal mixed-halide complex [CuPbBrlL2]2 has been prepared by the direct interaction of zerovalent copper with lead halides and 2-dimethylaminoethanol (HL) in dmso and has been characterized by X-ray crystallography; the structure shows a layer arrangement of the tetranuclear metal units through the μ3-halogen bridging.

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Bis(1-phenyl-1-propyne) complexes of tungsten(II): crystal structures of [WI2(CO)(NCR)(η2-MeC2Ph)2] (R = Me, Et, or Ph)

Canadian Journal of Chemistry ◽

10.1139/v01-028 ◽

2001 ◽

Vol 79 (3) ◽

pp. 263-271

Author(s):

Paul K Baker ◽

Michael GB Drew ◽

Deborah S Evans

Keyword(s):

Carbon Monoxide ◽

Solid State ◽

Crystal Structures ◽

Octahedral Geometry ◽

X Ray ◽

X Ray Crystallography ◽

Alkyne Complexes ◽

First Time

Reaction of [WI2(CO)3(NCMe)2] with two equivalents of 1-phenyl-1-propyne (MeC2Ph) in CH2Cl2, and in the absence of light, gave the bis(1-phenyl-1-propyne) complex [WI2(CO)(NCMe)(η2-MeC2Ph)2] (1) in 77% yield. Treatment of equimolar quantities of 1 and NCR (R = Et, i-Pr, t-Bu, Ph) in CH2Cl2 afforded the nitrile-exchanged products, [WI2(CO)(NCR)(η2-MeC2Ph)2] (2-5) (R = Et (2), i-Pr (3), t-Bu (4), Ph (5)). Complexes 1, 2, and 5 were structurally characterized by X-ray crystallography. All three structures have the same pseudo-octahedral geometry, with the equatorial sites being occupied by cis and parallel alkyne groups, which are trans to the cis-iodo groups. The trans carbon monoxide and acetonitrile ligands occupy the axial sites. In structures 1 and 2, the methyl and phenyl substituents of the 1-phenyl-1-propyne ligands are cis to each other, whereas for the bulkier NCPh complex (5), the methyl and phenyl groups are trans to one another. This is the first time that this arrangement has been observed in the solid state in bis(alkyne) complexes of this type.Key words: bis(1-phenyl-1-propyne), carbonyl, nitrile, diiodo, tungsten(II), crystal structures.

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

Journal of Porphyrins and Phthalocyanines ◽

10.1142/s1088424611004440 ◽

2012 ◽

Vol 16 (01) ◽

pp. 154-162 ◽

Cited By ~ 24

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.

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Simultaneous use of solution, solid-state NMR and X-ray crystallography to study the conformational landscape of the Crh protein during oligomerization and crystallization

Advances and Applications in Bioinformatics and Chemistry ◽

10.2147/aabc.s8715 ◽

2010 ◽

pp. 25

Author(s):

Malliavin

Keyword(s):

Solid State ◽

Solid State Nmr ◽

X Ray ◽

X Ray Crystallography ◽

Conformational Landscape ◽

Simultaneous Use

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Simple Methylcadmium Alkoxides

Zeitschrift für Naturforschung B ◽

10.1515/znb-2007-1018 ◽

2007 ◽

Vol 62 (10) ◽

pp. 1339-1342 ◽

Cited By ~ 6

Author(s):

Surajit Jana ◽

Tania Pape ◽

Norbert W. Mitzel

Keyword(s):

Mass Spectrometry ◽

Solid State ◽

Molecular Formula ◽

Equimolar Ratio ◽

X Ray ◽

X Ray Crystallography ◽

Elemental Analyses ◽

Solid State Structures ◽

Structural Aspects ◽

C Nmr

The reaction of dimethylcadmium with alcohols R-OH in equimolar ratio leads to the formation of tetrameric methylcadmium alkoxides with molecular formula [(MeCd)4 (OR)4] [R = Me (1), Et (2) and iPr (3)]. These compounds have been characterised by 1H, 13C NMR and IR spectroscopy, by mass spectrometry, elemental analyses and by X-ray crystallography (for 2 and 3). The solid state structures show distorted cubane-type aggregates with Cd4O4 cores. The structural aspects and the spectroscopic characterisations of these compounds are discussed.

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Synthesis and characterization of the binuclear diamido titanium chalcogenides [(Ar)NCH2CH2CH2N(Ar)]2Ti(µ-E)2 (E = Se, Te)

Canadian Journal of Chemistry ◽

10.1139/v02-052 ◽

2002 ◽

Vol 80 (11) ◽

pp. 1524-1529 ◽

Cited By ~ 2

Author(s):

Tianle Zhang ◽

Warren E Piers ◽

Masood Parvez

Keyword(s):

Solid State ◽

Key Words ◽

Synthesis And Characterization ◽

Catalyst Precursor ◽

Tellurium Atom ◽

Titanium Complex ◽

X Ray ◽

X Ray Crystallography ◽

Atom Source

Reaction of McConville's chelating amido titanium complex [(Ar)NCH2CH2CH2N(Ar)]Ti(CH3)2 (Ar = 2,6-i-Pr2C6H3) with either elemental Se or the tellurium atom source Te=PBu3 resulted in the formation of bis-µ-chalcogenido dimers [(Ar)NCH2CH2CH2N(Ar)]2Ti(µ-E)2 (E = Se, 2; Te, 3) with concommitant loss of EMe2. The dimers 2 and 3 were characterized spectroscopically and via X-ray crystallography. The two compounds are isostructural in the solid state. The tellurido dimer 3 may also be synthesized by reduction of the diamido dichloride [(Ar)NCH2CH2CH2N(Ar)]2TiCl2 with NaHg amalgam followed by treatment with Te=PBu3. This dimer is unreactive toward further Te=PBu3 or stannanes such as HSnBu3. Unlike decamethyltitanocene derivatives, the diamido complex is not an effective catalyst precursor for the heterohydrodecoupling of Te=PBu3 and HSnBu3.Key words: diamido titanium complexes, selenides, tellurides.

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The structure of 1-formyl-3-phenyl-Δ2-pyrazoline in the gas phase (DFT calculations), in solution (NMR) and in the solid state (X-ray crystallography)

Journal of Molecular Structure ◽

10.1016/j.molstruc.2003.10.041 ◽

2004 ◽

Vol 689 (3) ◽

pp. 251-254 ◽

Cited By ~ 14

Author(s):

I. Alkorta ◽

J. Elguero ◽

A. Fruchier ◽

N. Jagerovic ◽

G.P.A. Yap

Keyword(s):

Solid State ◽

Dft Calculations ◽

Gas Phase ◽

Solution Nmr ◽

X Ray ◽

X Ray Crystallography

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1-[N-Methyl-N-(Phenyl)amino]-3- (4-Methylphenyl)Thiourea

Molbank ◽

10.3390/m1052 ◽

2019 ◽

Vol 2019 (1) ◽

pp. M1052 ◽

Cited By ~ 1

Author(s):

Chien Yeo ◽

Edward Tiekink

Keyword(s):

Hydrogen Bond ◽

Solid State ◽

Hydrogen Bonds ◽

Single Crystal ◽

Elemental Analysis ◽

Title Compound ◽

Molecular Conformation ◽

Phenyl Hydrazine ◽

X Ray ◽

X Ray Crystallography

The title compound, 1-[N-methyl-N-(phenyl)amino]-3-(4-methylphenyl)thiourea (1), was synthesized by the reaction of 1-methyl-1-phenyl hydrazine and 4-tolyl isothiocyanate, and was characterized by spectroscopy (1H and 13C{1H} NMR, IR, and UV), elemental analysis as well as by single crystal X-ray crystallography. In the solid state, the molecule exists as the thioamide tautomer and features an anti-disposition of the thioamide–N–H atoms; an intramolecular N–H⋯N hydrogen bond is noted. The molecular conformation resembles that of the letter L. In the molecular packing, thioamide-N1–H⋯S1(thione) hydrogen bonds lead to centrosymmetric eight-membered {⋯HNCS}2 synthons. The dimers are assembled into a supramolecular layer in the bc-plane by phenyl- and methyl-C–H⋯π(phenyl) interactions.

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Probing solid iminobis(diorganophosphine chalcogenide) systems with multinuclear magnetic resonance

Canadian Journal of Chemistry ◽

10.1139/v08-150 ◽

2009 ◽

Vol 87 (1) ◽

pp. 348-360 ◽

Cited By ~ 1

Author(s):

Bryan A Demko ◽

Roderick E Wasylishen

Keyword(s):

Solid State ◽

Chemical Shift ◽

Solid State Nmr ◽

Magnetic Shielding ◽

Chemical Shift Tensors ◽

X Ray ◽

X Ray Crystallography ◽

Shielding Tensor ◽

Nuclear Magnetic Shielding Tensors ◽

Nuclear Magnetic

A 31P and 77Se solid-state NMR investigation of the iminobis(diorganophosphine chalcogenide) HN(R2PE)2 (R = Ph,iPr; E = O, S, Se) systems is presented. The NMR results are discussed in terms of the known HN(R2PE)2 structures available from X-ray crystallography. The phosphorus chemical shift tensors are found to be sensitive to the nature of the alkyl and chalcogen substituents. The nature of the R group also influences the selenium chemical shift tensors of HN(R2PSe)2 (R = Ph, iPr), which are shown to be sensitive to hydrogen bonding in the dimer structure of HN(Ph2PSe)2 and to the presence of disorder in the case of HN(iPr2PSe)2. Scalar relativistic ZORA DFT nuclear magnetic shielding tensor calculations were performed yielding the orientations of the corresponding chemical shift tensors. A theoretical investigation into the effect of the E-P···P-E “torsion” angle on the phosphorus and selenium chemical shift tensors of a truncated HN(Me2PSe)2 system indicates that the electronic effect of the alkyl group on the respective nuclear magnetic shielding tensors are more important than the steric effect of the E-P···P-E torsion angle.Key words: iminobis(diorganophosphine chalcogenide), solid-state NMR, 31P NMR, 77Se NMR, ZORA DFT.

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