Derivatives of the triaminoguanidinium ion, 6. Aminal-forming reactions with aldehydes and ketones

2020 ◽  
Vol 75 (3) ◽  
pp. 317-326
Author(s):  
Jan Szabo ◽  
Gerhard Maas
Keyword(s):  
Crystal Structure ◽  
The Other ◽  
Guanidinium Chloride ◽  
X Ray ◽  
Other Hand ◽  
Aldehydes And Ketones ◽  
Structure Determinations ◽  
Derivatives Of

AbstractCyclic aminals (N,N-acetals) could be prepared by the reaction of N,N′,N″-triaminoguanidinium sulfate, N,N′,N″-tris(benzylamino)guanidinium chloride or N,N′,N″-tris(benzylamino)guanidine with formaldehyde or acetone. In all cases, 1,2,4,5-tetrazinane derivatives were obtained, which were structurally confirmed by X-ray crystal structure determinations. In two cases, 1:1 cocrystals of two different tetrazinane products were isolated. On the other hand, the reaction of N,N′,N″-tris(benzylamino)guanidinium chloride with benzaldehyde yielded a 3-(2-benzylidenehydrazin-1-yl)-1H-1,2,4-triazole.

scholarly journals On the interpretation of X-ray, single crystal, rotation photographs

1926 ◽  
Vol 113 (763) ◽  
pp. 117-160 ◽  
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
The Other ◽  
X Rays ◽  
X Ray ◽  
Powder Method ◽  
Convenient Form ◽  
Other Hand ◽  
Rotation Method ◽  
Laue Method

In the development of the study of crystals by X-rays the methods used divide themselves naturally into four types : the Bragg Ionisation Spectrometer method, the Laue method, the Powder method of Debye and Scherrer, and the Rotating Crystal method of Rinne, Schiebold and Polyani. The techniques of the first three of these methods are fully explained in such books as ‘ X-Rays and Crystal Structure,’ by W. H. and W. L. Bragg, ‘ The Structure of Crystals,’ by Wyckoff, and ‘ Krystalle und Rontgenstrahlen,’ by Ewald, as well as in original papers. On the other hand, the rotation method is only slightly touched on in these works, the literature is scattered in a great number of papers, and the technique has not so far been described at any length in a convenient form. Particularly in English, references to it are scanty. In this paper the author has tried to give a concise account of the method, together with various types of charts and tables as it is used in the Davy Faraday Laboratory. The methods described differ in certain respects from those used on the Continent,* but they have been found to be rapid and sufficiently accurate.

Die Kristallstrukturen von Tetraphenylphosphonium- octahalogenodiarsenat( III) und -diantimonat(III) mit Acetonitril, (PPh4)2[E2X8] · CH3CN (E = As, Sb; X = CI, Br)/The Crystal Structures of Tetraphenylphosphonium Octahalogenodiarsenate (III) and Diantimonate (III) with Acetonitrile, (PPh4)2[E2X8]·CH3CN(E=As, Sb; X=Cl, Br)

1999 ◽  
Vol 54 (2) ◽  
pp. 288-290 ◽  
Author(s):  
Wolfgang Czado ◽  
Susanne Rabe ◽  
Ulrich Müller
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
The Other ◽  
Space Group ◽  
X Ray ◽  
Structure Determinations ◽  
Cl Atoms

(PPh4)2[As2Cl8] · CH3CN was obtained from PPh4Cl and S2Cl2 with As or As4S4 or AsCl3 in acetonitrile. PPh4Cl, S2Cl2 and Sb2S3 yielded (PPh4)[Sb2Cl8] CH3CN. PPh4Br and AsBr3 gave (PPh4)2[Sb2Br8]-CH3CN. AsCl2OPh (from AsCl3 and NaOPh) reacted with Ph4Br in acetonitrile in the presence of Na2Se, selenium, and HCl, affording (PPh4)2[As2Br4,2Cl3,8] · CH3CN. According to their X-ray crystal structure determinations, all products are isotypic (space group C2/c, Z=4). The centrosymmetric anions consist of two ψ octahedra sharing an edge. In the [As2Br4,2Cl3,8]2- ion the bridging positions are taken solely by bromine atoms, whereas Br and Cl atoms occupy the other halogen positions randomly.

New Phosphorus-Containing Polycylic Large-Ring Systems Involving Heteroatoms

2002 ◽  
Vol 57 (9) ◽  
pp. 1008-1016
Author(s):  
Yingzi Lu ◽  
Matthias Freytag ◽  
Peter G. Jones ◽  
Reinhard Schmutzler
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Elemental Sulfur ◽  
Trimethylsilyl Ether ◽  
The Other ◽  
X Ray ◽  
Phosphorus Containing ◽  
Structure Determinations ◽  
New Compounds ◽  
Moderate Yield

The [1+1] cyclocondensation of the bis-PCl species 1,2-bis(benzo-1-methyl-2-chloro- 1,3,2-diazaphosphorin-4-on-3-yl)ethane 1 and 1,3-bis(benzo-1-methyl-2-chloro-1,3,2-diazaphosphorin- 4-on-3-yl)propane 2 with the 1,2-benzenediol bis(trimethylsilyl) ether 3a and 2,3- naphthalenediol bis(trimethylsilyl) ether 3b gave the symmetrical phosphorus-containing largering systems 4 - 7 in moderate yield. The phosphoryl compounds 8 - 11 were obtained by the oxidation of 4 - 7 with (H2N)2C(:O) H2O2. Oxidation of 6 and 7 with elemental sulfur furnished the thiophosphoryl compounds (12 and 13). All new compounds formed in the reactions were characterized unambiguously by NMR spectroscopy, mass spectrometry, and elemental analysis. For compounds 6, 9, 10, 11 and 12, X-ray crystal structure determinations were conducted. The compounds with ten-membered rings show approximate (6, 12) or exact (10) twofold symmetry. In each of the compounds 9 and 11 the two six-membered heterocycles are appreciably different; one is approximately planar, whereas in the other, phosphorus lies outside the plane of the other five atoms

Tris(ethyldimethylphenylammonium) nonahalogenodibismuthates(III)

1999 ◽  
Vol 54 (3) ◽  
pp. 305-313 ◽  
Author(s):  
H. Eickmeier ◽  
Bernd Jaschinski ◽  
A. Hepp ◽  
Jürgen Nuß ◽  
Hans Reuter ◽  
...  
Keyword(s):  
Crystal Structure ◽  
High Temperature ◽  
Powder Diffraction ◽  
Lattice Parameters ◽  
The Other ◽  
Temperature Dependent ◽  
X Ray ◽  
Dsc Measurements ◽  
Structure Determinations ◽  
High Temperature Modification

The halogenobismuthates Q3Bi2X9 (Q = EtMe2PhN; X = Cl, Br, I) were prepared by reaction of BiX3 with EtMe2PhNX in ethanol. Single crystal structure determinations yielded: [EtMe2PhN]3[Bi2Cl9], S.G. P212121, Nr. 19, a = 952.5(3), b = 1184.1(4), c = 3726.4(9 pm, Z = 2;[EtMe2PhN]3[Bi2Br9] S.G .P21/c , No. 14, a= 1839.4(4),b= 1329.5(3), c = 1817.3(6)pm, β = 92.68(3)°, Z = 4, [EtMe2PhN]3[Bi2l9], ], S.G . P21/c, No. 14, a = 1915.3(2), b = 1379.0(3), c = 1890.9(5) pm, β = 92.48(1)°, Z = 4. The thermal behaviour was investigated with the aid of DSC measurements and temperature dependent X-ray powder diffraction. All compounds undergo a transition into a high temperature modification which could be obtained in case of [EtMe2PhN]3[Bi2Br9-xIx] in form of single crystals: S.G . P21/c, Nr. 14, a = 1002.7(5), b = 1278.7 (8), c = 3584.3(5) pm, β = 90.12(2)°, Z = 4. Surprisingly in this compound the iodine atoms are not statistically distributed over all possible bromine positions, but occupy only one position. Lattice parameters of the other high temperature modifications and enthalpies of transition of the compounds are given. In addition a second iodobismuthate was isolated:[EtMe2PhN]4[Bi6l22], S.G . P1̄, Nr. 2 , with lattice parameters of a = 1343.4(3), b = 1554.3(3), c = 2262.5(6) pm, a = 100.89(3)°, β = 96.63(1)°, 7 = 98.94(2)° and Z = 2.

scholarly journals White Dwarf Masses and Accretion Rates of Recurrent Novae: an X-ray Perspective

2011 ◽  
Vol 7 (S281) ◽  
pp. 186-189
Author(s):  
Koji Mukai ◽  
Jennifer L. Sokoloski ◽  
Thomas Nelson ◽  
Gerardo J. M. Luna
Keyword(s):  
White Dwarf ◽  
Cataclysmic Variables ◽  
The Other ◽  
X Ray ◽  
Other Hand ◽  
Accretion Rates

AbstractWe present recent results of quiescent X-ray observations of recurrent novae (RNe) and related objects. Several RNe are luminous hard X-ray sources in quiescence, consistent with accretion onto a near Chandrasekhar mass white dwarf. Detection of similar hard X-ray emissions in old novae and other cataclysmic variables may lead to identification of additional RNe candidates. On the other hand, other RNe are found to be comparatively hard X-ray faint. We present several scenarios that may explain this dichotomy, which should be explored further.

PHASE TRANSITION IN LAYERED PEROVSKITE LIKE MANGANATE Ca3Mn2O7 UNDER HIGH PRESSURE

2001 ◽  
Vol 15 (18) ◽  
pp. 2491-2497 ◽  
Author(s):  
J. L. ZHU ◽  
L. C. CHEN ◽  
R. C. YU ◽  
F. Y. LI ◽  
J. LIU ◽  
...  
Keyword(s):  
Crystal Structure ◽  
High Pressure ◽  
Diamond Anvil Cell ◽  
The Other ◽  
Layered Perovskite ◽  
X Ray Diffraction ◽  
Two Phase ◽  
X Ray ◽  
Diamond Anvil

In situ high pressure energy dispersive X-ray diffraction measurements on layered perovskite-like manganate Ca 3 Mn 2 O 7 under pressures up to 35 GPa have been performed by using diamond anvil cell with synchrotron radiation. The results show that the structure of layered perovskite-like manganate Ca 3 Mn 2 O 7 is unstable under pressure due to the easy compression of NaCl-type blocks. The structure of Ca 3 Mn 2 O 7 underwent two phase transitions under pressures in the range of 0~35 GPa. One was at about 1.3 GPa with the crystal structure changing from tetragonal to orthorhombic. The other was at about 9.5 GPa with the crystal structure changing from orthorhombic back to another tetragonal.

Preparations, X-ray crystal structure determinations, and base strength measurements of substituted tritylamines

2000 ◽  
pp. 85-92 ◽  
Author(s):  
Moisés Canle L. ◽  
William Clegg ◽  
Ibrahim Demirtas ◽  
Mark R. J. Elsegood ◽  
Howard Maskill
Keyword(s):  
Crystal Structure ◽  
X Ray ◽  
Structure Determinations ◽  
Base Strength

scholarly journals II. Compounds isomeric with the sulphocyanic ethers.—I. On the mustard oil of the ethyl series

1868 ◽  
Vol 16 ◽  
pp. 254-258
Keyword(s):  
Royal Society ◽  
The Other ◽  
Mustard Oil ◽  
Other Hand ◽  
Derivatives Of

The results of my researches on the chloroform-derivatives of the primary monamines, which, as I have shown, are isomeric with the nitriles, could not fail to direct my attention to allied groups of bodies, with the view of discovering similar isomerisms. In a note communicated to the Royal Society some months ago, I expressed the expectations which even then appeared to be justified in the following manner:—“In conclusion, I may be permitted to announce as everv probable the existence of a series of bodies isomeric with the sulphocyanides. Already M. Cloëz has shown that the action of chloride of cyanogen on ethylate of potassium gives rise to the formation of an ethylic cyanate possessing properties absolutely different from those belonging to the cyanate discovered by M. Wurtz. On comparing, on the other hand the properties of the methylic and ethylic sulphocyamdes with those of the sulphocyanides of allyl and phenyl, it can scarcely be doubted that we have here the representatives of two groups entirely different, and that the terms of the methyl- and ethyl-series which correspond to oil of mustard, and to the sulphocyanide of phenyl, still remain to be discovered. Experiments with which I am now engaged will show whether these bodies cannot be obtained by the action of the iodides of methyl and ethyl on sulphocyanide of silver."

Triazene derivatives of (1,x-)diazacycloalkanes. Part VI. 3-({5,5-Dimethyl-3-[2-aryl-1-diazenyl]-1-imidazolidinyl}methyl)-4,4-dimethyl-1-[2-aryl-1-diazenyl]imidazolidines — Synthesis, characterization, and X-ray crystal structure

2006 ◽  
Vol 84 (10) ◽  
pp. 1294-1300 ◽  
Author(s):  
Keith Vaughan ◽  
Shasta Lee Moser ◽  
Reid Tingley ◽  
M Brad Peori ◽  
Valerio Bertolasi
Keyword(s):  
Crystal Structure ◽  
Significant Degree ◽  
Ion Trapping ◽  
Published Data ◽  
X Ray ◽  
X Ray Crystallography ◽  
Diazonium Ion ◽  
Derivatives Of ◽  
C Nmr

Reaction of a series of diazonium salts with a mixture of formaldehyde and 1,2-diamino-2-methylpropane affords the 3-({5,5-dimethyl-3-[2-aryl-1-diazenyl]-1-imidazolidinyl}methyl)-4,4-dimethyl-1-[2-aryl-1-diazenyl]imidazolidines (1a–1f) in excellent yield. The products have been characterized by IR and NMR spectroscopic analysis, elemental analysis, and X-ray crystallography. The X-ray crystal structure of the p-methoxycarbonyl derivative (1c) establishes without question the connectivity of these novel molecules, which can be described as linear bicyclic oligomers with two imidazolidinyl groups linked together by a one-carbon spacer. This is indeed a rare molecular building block. The molecular structure is corroborated by 1H and 13C NMR data, which correlates with the previously published data of compounds of types 5 and 6 derived from 1,3-propanediamine. The triazene moieties in the crystal of 1c display significant π conjugation, which gives the N—N bond a significant degree of double-bond character. This in turn causes restricted rotation around the N—N bond, which leads to considerable broadening of signals in both the 1H and 13C NMR spectra. The molecular ion of the p-cyanophenyl derivative (1b) was observed using electrospray mass spectrometry (ES + Na). The mechanism of formation of molecules of type 1 is proposed to involve diazonium ion trapping of the previously unreported bisimidazolidinyl methane (13).Key words: triazene, bistriazene, imidazolidine, synthesis, X-ray crystallography, NMR spectroscopy.

Molecular tapes in the structure of isoguaninium chloride

2017 ◽  
Vol 74 (1) ◽  
pp. 108-112 ◽  
Author(s):  
Urszula Anna Budniak ◽  
Paulina Maria Dominiak
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Charge Density ◽  
Interaction Energy ◽  
Electrostatic Interaction ◽  
Electrostatic Interactions ◽  
The Other ◽  
X Ray Diffraction ◽  
X Ray ◽  
Diffraction Structure

Isoguanine, an analogue of guanine, is of intrinsic interest as a noncanonical nucleobase. The crystal structure of isoguaninium chloride (systematic name: 6-amino-2-oxo-1H,7H-purin-3-ium chloride), C5H6N5O+·Cl−, has been determined by single-crystal X-ray diffraction. Structure analysis was supported by electrostatic interaction energy (E es) calculations based on charge density reconstructed with the UBDB databank. In the structure, two kinds of molecular tapes are observed, one parallel to (010) and the other parallel to (50\overline{4}). The tapes are formed by dimers of isoguaninium cations interacting with chloride anions. E es analysis indicates that cations in one kind of tape are oriented so as to minimize repulsive electrostatic interactions.

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