Efficient S-Acylation of Thiourea

Acid Chlorides ◽

X Ray

Efficient S-acylation of thiourea using a variety of acid chlorides is reported. Structurally diverse aryl and alkyl substrates are compatible with this methodology. Confirmation that acylation occurs exclusively on the sulfur atom of thiourea is provided by single-crystal X-ray crystallographic analysis.

Chemical Bonding and the Sulfur K X-Ray Spectrum

Advances in X-ray Analysis ◽

10.1154/s0376030800003670 ◽

1965 ◽

Vol 9 ◽

pp. 354-364 ◽

Cited By ~ 5

Author(s):

D. W. Wilbur ◽

J. W. Gofman

Keyword(s):

Electronic Structure ◽

Single Crystal ◽

Organic Compounds ◽

Sulfur Atom ◽

Chemical Bonding ◽

Proportional Counter ◽

Pulse Height ◽

X Ray ◽

Pulse Height Analysis ◽

Chemical States

AbstractAn investigation has been made of the relative Kβ intensities in different chemical states of the sulfur atom using the Kα lines, with appropriate corrections, to provide the intensity standards. Both inorganic and organic compounds were included in the study. The data for each compound appear to be reliable to about ± 0.5%, while the whole series of compounds shows a variation greater than 20% in the corrected Kβ/Kα ratios. Energies were also measured, particularly the Kα energies, and their shifts were studied relative to the Kβ, intensity shifts. The work was done with a plane, single-crystal, helium-path spectrometer with proportional counter and pulse-height analysis for detection. The results are indicative of the usefulness of the method both in clarifying an uncertain chemical state and in studying the electronic structure of the bonded atom.

Single Crystal X-Ray Structural Characterization of [BiX2(S2CNEt2)]Infinity∞, X=Cl, Br

10.1071/ch9940405 ◽

1994 ◽

Vol 47 (2) ◽

pp. 405 ◽

Cited By ~ 4

Author(s):

PK Bharadwaj ◽

AM Lee ◽

BW Skelton ◽

BR Srinivasan ◽

AH White

Keyword(s):

Single Crystal ◽

Sulfur Atom ◽

Structural Characterization ◽

Structure Determination ◽

Room Temperature ◽

X Ray ◽

Structure Determinations

Single-crystal room-temperature X-ray structure determinations of the title compounds have been carried out. The two compounds are isomorphous, and isomorphous with the previously determined iodide analogue, being monoclinic, P 21/c, a ≈ 10.0, b ≈ 14.9, c ≈ 7.8 Ǻ, β ≈ 92°, Z = 4 formula units; residuals were 0.037, 0.036 for 2197, 1654 'observed' reflections for X = Cl , Br respectively. As in the iodide, the complexes are infinite polymers, with successive bismuth atoms bridged by the two halides and one sulfur atom of the ligand , which also chelates each bismuth. The structure determination of C5H5NCONEt2]2 [Cl5Bi(NC5H5)], isostructural with its thiocarbamoyl analogue, is also recorded.

Revised Absolute Configurations of Latifolic Acid and the Pyrrolizidine Alkaloid Latifoline

10.1071/ch9881781 ◽

1988 ◽

Vol 41 (11) ◽

pp. 1781 ◽

Cited By ~ 3

Author(s):

JN Roitman ◽

RY Wong

Keyword(s):

Carboxylic Acid ◽

Single Crystal ◽

Pyrrolizidine Alkaloid ◽

Side Chain ◽

X Ray ◽

The Absolute ◽

Absolute Stereochemistry

The absolute stereochemistry of (+)- latifolk acid has been determined by single-crystal X-ray crystallographic analysis to be (2S,3R,4R)-3- hydroxy-2,4-dimethyl-5-oxotetrahydrofuran-3-carboxylic acid. The configuration of the three chiral centres is opposite to that presently recorded in the literature. Accordingly, the configuration of the pyrrolizidine alkaloid, latifoline, which includes a latifolic acid side chain, must be revised.

Stereoselective synthesis and X-ray crystallographic analysis of mixed 6,6-dihalo penicillanates

Canadian Journal of Chemistry ◽

10.1139/v85-525 ◽

1985 ◽

Vol 63 (11) ◽

pp. 3177-3181 ◽

Cited By ~ 9

Author(s):

Diego U. Belinzoni ◽

Oreste A. Mascaretti ◽

Pedro M. Alzari ◽

Graciela Punte ◽

Carlos Faerman ◽

...

Keyword(s):

Single Crystal ◽

Crystal Structures ◽

Stereoselective Synthesis ◽

Displacement Reaction ◽

X Ray ◽

Single Crystal Analysis

The pivaloyloxy methyl 6,6-dihalo penicillanates 1a, 1b, and 1c have been stereoselectively prepared from the reaction of pivaloyloxy methyl 6-diazo penicillanate 2 with either N-halosuccinimide/halide or the interhalogens Xl (X = Cl, Br). The crystal structures of 3S,5R,6R pivaloyloxy methyl 6-bromo, 6-chloro penicillanate1a; 3S,5R,6R pivaloyloxy methyl 6-iodo, 6-bromo penicillanate 1b, and 3S, 5R, 6R pivaloyloxymethyl 6-iodo, 6-chloro penicillanate 1c have been determined by X-ray single crystal analysis. The stereochemistry of the displacement reaction is discussed.

Two- and three-dimensional β,β’-N-heterocycle fused porphyrins: concise construction, singlet oxygen production and electro-catalytic hydrogen evolution reaction

Organic Chemistry Frontiers ◽

10.1039/d1qo01161h ◽

2021 ◽

Author(s):

Jianxin Song ◽

Yan Fan ◽

Zhiming Zeng ◽

Hui Shu ◽

Mingbo Zhou ◽

...

Keyword(s):

Single Crystal ◽

Hydrogen Evolution Reaction ◽

Three Dimensional ◽

Coupling Reaction ◽

Oxygen Production ◽

X Ray ◽

Palladium Catalyzed ◽

Catalytic Hydrogen ◽

Catalytic Hydrogen Evolution

A powerful and concise synthesis of two- and three-dimensional β,β’-N-heterocycle fused porphyrins by palladium-catalyzed C-N coupling reaction of bromoporphyrins with arylamines has been demonstrated. Single crystal X-ray crystallographic analysis revealed...

Molekülstrukturen, Schwingungsspektren und Konformation der Thiooxalsäurederivate CH3S-CO-CONH2, CH3S-CS-CONH2, C2H5O-CO-CSNH2 und K[OSC-CONH2] / Molecular Structure, Vibrational Spectra and Conformation of the Thiooxalic Acid Derivatives CH3S-CO-CONH2, CH3S-CS-CONH2, C2H5O-CO-CSNH2 and K[OSC-CONH2]

Zeitschrift für Naturforschung B ◽

10.1515/znb-1983-0311 ◽

1983 ◽

Vol 38 (3) ◽

pp. 335-340 ◽

Cited By ~ 4

Author(s):

Rainer Mattes ◽

Franz Waldmann

Keyword(s):

Molecular Structure ◽

Hydrogen Bonds ◽

Single Crystal ◽

Crystal Structures ◽

Sulfur Atom ◽

Vibrational Spectra ◽

Torsional Angle ◽

X Ray Diffraction ◽

X Ray ◽

Centrosymmetric Dimers

Abstract The crystal structures of CH3S-CO-CONH2 (1), CH3S-CS-CONH2 (2), C2H5O-CO-CSNH2 (3) and K[OSC-CONH2] (4) have been determined by single crystal X-ray diffraction. The molecules 1, 2 and 3 are nearly planar and form centrosymmetric dimers by N H···O or N-H···S hydrogen bonds with the amidic oxygen or sulfur atom as acceptor atoms. The anion of 4 is not quite planar. The torsional angle around the C-C bond is 18.4°. The conformations of the title compounds are E, Z' (1 and 2), Z, Z' (3) and Z (4). According to the vibrational spectra, which are discussed briefly, 1 and 3 retain their conformation also in solution.

Pigments of Fungi. LVII. Structure and X-Ray Crystallographic Analysis of Dermocanarin 10, a New Naphthalene - Dihydroanthracenone Dimer from an Australian Dermocybe Toadstool

10.1071/ch99078 ◽

1999 ◽

Vol 52 (9) ◽

pp. 881 ◽

Cited By ~ 2

Author(s):

Melvyn Gill ◽

Petra M. Millar ◽

Evelin Raudies ◽

Somphone Phonh-Axa ◽

Jonathan M. White ◽

...

Keyword(s):

Single Crystal ◽

Structure Analysis ◽

Spectroscopic Data ◽

Fungal Metabolite ◽

X Ray ◽

Absolute Stereochemistry

The structure and absolute stereochemistry of the fungal metabolite dermocanarin 10 (2), which differs from all previous members of the dermocanarin group by virtue of the connectivity between the anthraquinone and dimethoxynaphthol rings, is deduced from spectroscopic data and confirmed by a single-crystal X-ray structure analysis.

Investigation of Isomer Formation of Triorganotin(IV) Complexes Involving Diorganophosphino-N-Phenyl(Thioformamide) Ligands: The Crystal and Molecular-Structure of [Diphenylphosphino-N-Phenyl(Thioformamido)]Triphenyltin, Ph3Sn[Ph2PC(S) NPh ]

10.1071/ch9880195 ◽

1988 ◽

Vol 41 (2) ◽

pp. 195 ◽

Cited By ~ 2

Author(s):

D Dakternieks ◽

BF Hoskins ◽

CL Rolls

Keyword(s):

Molecular Structure ◽

Single Crystal ◽

Sulfur Atom ◽

Crystal And Molecular Structure ◽

Steric Effects ◽

X Ray Diffraction ◽

Similar Compound ◽

Space Group ◽

X Ray ◽

Tetrahedral Environment

The isomer of Ph3Sn[Ph2PC(S) NPh] formed depends on the method of preparation. The crystal and molecular structure of the tin(IV) complex Ph3Sn[Ph2PC(S) NPh ] has been established by single-crystal X-ray diffraction techniques. The crystals are monolinic, space group P21/n, a 12.620(2), b 10.541(2), c 24.292(4)Ǻ, β 96.90(1) with Z 4; R and Rw were 0.031 and 0.034 respectively for 5632 unique reflections with I > 3σ(I). The crystals consist of discrete Ph3Sn[Ph2PC(S) NPh ] molecules. There is a tetrahedral environment about the tin atom formed by the three phenylic carbons and a sulfur atom of the [Ph2PC(S) NPh ]- ligand . Comparisons are made with the structurally similar compound Ph3Sn[(c-C6H11)2PC(S) NPh ]. On the basis of these comparisons and on earlier n.m.r . data, a favoured four-centered mechanism for insertion of dipolar PhNCS into the tin-phosphorus bond of Ph3SnPPh2 is inferred. Differences in reactivity of Ph2PC(S)N(H)Ph and (c-C6H11)2PC(S)N(H)Ph appear to result from electronic rather than steric effects.

Synthesis and characterization of (η5-C5Me5)W(NO)I2, a monomeric, formally 16-electron complex

Canadian Journal of Chemistry ◽

10.1139/v88-335 ◽

1988 ◽

Vol 66 (8) ◽

pp. 2100-2103 ◽

Cited By ~ 8

Author(s):

Neil H. Dryden ◽

Peter Legzdins ◽

Frederick W. B. Einstein ◽

Richard H. Jones

Keyword(s):

Molecular Structure ◽

Molecular Weight ◽

Solid State ◽

Single Crystal ◽

Significant Degree ◽

Synthesis And Characterization ◽

X Ray ◽

Degree Of Association

The compound (η5-C5Me5)W(NO)I2 has been prepared by treating (η5-C5Me5)W(NO)(CO)2 with I2. A single crystal X-ray crystallographic analysis establishes that the formally 16-electron complex possesses a monomeric, three-legged piano stool molecular structure in the solid state. Solution molecular weight measurements also indicate no significant degree of association of the compound.

Detailed example of the identification and crystallographic analysis of a pseudo-merohedrally twinned crystal

Acta Crystallographica Section B Structural Science ◽

10.1107/s0108768112002728 ◽

2012 ◽

Vol 68 (2) ◽

pp. 150-157 ◽

Cited By ~ 7

Author(s):

Ilia Guzei ◽

Regine Herbst-Irmer ◽

Apollinaire Munyaneza ◽

James Darkwa

Keyword(s):

Single Crystal ◽

Structural Determination ◽

Organometallic Complex ◽

X Ray ◽

Positional Disorder ◽

Crystal Structural

A detailed description of the procedures utilized in the non-routine X-ray single-crystal structural determination and refinement of a pseudo-merohedrally twinned crystal of an Fe/Ni organometallic complex is presented. It illustrates to the practitioners of crystallography how to properly handle such cases and describes the logic and concrete steps necessary to account for the twinning, pseudo-symmetry and atomic positional disorder.