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

Interaction of the Components in the {Ce, Gd}-{Ti, Zr}-Sb Systems

2019 ◽  
Vol 289 ◽  
pp. 3-11
Author(s):  
Oleksandr Senchuk ◽  
Roman E. Gladyshevskii
Keyword(s):  
Crystal Structure ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Ternary Systems ◽  
The Other ◽  
Powder Diffraction Data ◽  
Isothermal Sections ◽  
X Ray ◽  
Ternary Compounds ◽  
New Compounds

The phase equilibria in the ternary systems {Ce, Gd}–{Ti, Zr}–Sb were investigated by means of X-ray powder diffraction and energy-dispersive X-ray spectroscopy. The isothermal sections of the phase diagrams at 600°C were constructed. The formation of three ternary compounds (Ce2Ti7Sb12, Ce3TiSb5, and Gd2Ti11Sb14) was confirmed in the {Ce, Gd}–Ti–Sb systems and no more ternaries were found. The investigation of the {Ce, Gd}–Zr–Sb systems revealed several new ternary compounds and confirmed the known ones. The crystal structure of the new compound Ce0.08(3)Zr1.92(3)Sb was determined from X-ray powder diffraction data. The other new compounds in the Ce–Zr–Sb system were found to have compositions close to ~CeZrSb4and ~Ce2Zr3Sb5. In the Gd–Zr–Sb system the existence of a large homogeneity range was established for the GdZrSb compound along the isoconcentrate 33.3 at.% Sb: Gd1-xZr1+xSb (x= 00.905(18) at 600°C), and a new compound, ~Gd3Zr3Sb14, was discovered. The crystal structures at the boundary compositions of the Gd1-xZr1+xSb phase were refined from X-ray powder diffraction data.

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.

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.

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.

Beiträge zur Chemie des 4,5-Benzo-3-methyl-1,3,2-oxazaphosphorinan- 6-on Ringsystems: Röntgenstrukturanalysen an einem Bis(2-chlorethyl)amino- und einem Acetamido-substituierten Derivat / Chemistry of the 4,5-Benzo-3-methyl-1,3,2-oxazaphosphorinan-6-one Ring System: X-Ray Crystal Structure Analysis of a Bis(2-chloroethyl)amino- and of an Acetamido-Substituted Derivative

1994 ◽  
Vol 49 (7) ◽  
pp. 939-949 ◽  
Author(s):  
Axel Fischer ◽  
Ion Neda ◽  
Thomas Kaukorat ◽  
Ralf Sonnenburg ◽  
Peter G. Jones ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Hydrogen Peroxide ◽  
Elemental Sulfur ◽  
Crystal Structure Analysis ◽  
Ring System ◽  
Molecular Structures ◽  
X Ray ◽  
Spectrometric Data ◽  
Structure Determinations ◽  
Phosphoryl Compound

Abstract The reaction of 4,5-benzo-2-chloro-3-methyl-1,3,2-oxazaphosphorinan-6-one 1 with 1,2-bis- (trimethylsiloxy)ethane led to the bisphosphoryl species 2a and to the isomeric bisphosphite derivative 2b. The reaction of 1 with heptamethyldisilazane furnished the expected diphos­phorus compound 3, with two λ3P(III) atoms linked by a methylamino group. Substitution of the chlorine atom of 1 by the 2-chloroethylamino and bis(2-chloroethyl)amino group led to the oxazaphosphorinanones 4 and 6. By oxidation of 4 with the hydrogen peroxide/urea 1:1-adduct, the phosphoryl compound 5 was formed. Oxidation of 4,5-benzo-2-diethyl- amino-3-methyl-1,3,2-oxazaphosphorinan-6-one 7 [1] with hydrogen peroxide, sulfur and se­lenium led to the corresponding phosphoryl, thiophosphoryl and selenophosphoryl com­pounds 8-10. Analogously, the reaction of the dimethylamino- and acetamido-substituted derivatives 11 and 13 [1] with elemental sulfur furnished the thiophosphoryl compounds 12 and 14. X-ray crystal structure determinations of 4 and 14 confirmed the molecular structures, proposed in accord with NMR spectroscopic and mass spectrometric data. The heterocyclic rings are essentially planar. In 14 a hydrogen bond N-H···O (amide) is observed.

NMR Studies and Crystal Structure Determinations of CF3 Group-containing Bicyclic Phenolates

2009 ◽  
Vol 64 (4) ◽  
pp. 423-426 ◽  
Author(s):  
Constantin Mamat ◽  
Helmut Reinke ◽  
Peter Langer
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Hydrogen Bonding ◽  
Ir Spectroscopy ◽  
Elemental Analysis ◽  
Nmr Studies ◽  
Enol Ethers ◽  
X Ray ◽  
Silyl Enol Ethers ◽  
Structure Determinations

Three new CF3-substituted bicyclic salicylate derivatives were synthesized by the TiCl4-mediated cyclization of trifluoromethyl-containing ketones with 1,3-bis(silyl enol ethers) and characterized by NMR and IR, spectroscopy, mass spectrometry and elemental analysis. The crystal structures of the bicyclic derivatives have been determined by single crystal X-ray analysis. All structures exhibit hydrogen bonding.

scholarly journals 4-vinylpyridine derivatives: Protonation, methylation and silver(I) coordination chemistry

2021 ◽  
pp. 174751982198965
Author(s):  
Guoqi Zhang
Keyword(s):  
Mass Spectrometry ◽  
Schiff Base ◽  
Coordination Chemistry ◽  
Elemental Analysis ◽  
Silver Complex ◽  
Spectroscopic Techniques ◽  
X Ray ◽  
X Ray Crystallography ◽  
Pyridine Moiety ◽  
New Compounds

( E)-4-[2-(Pyridin-4-yl)vinyl]benzaldehyde, containing both a 4-vinylpyridine and an aldehyde functionality, is utilized to develop new, highly conjugated chalcone compounds and a bis-Schiff base azine compound. The chalcone-containing compounds are further explored for their protonation, methylation and silver(I) coordination chemistry using the pyridine moiety. In parallel, a cyano-containing analogue, ( E)-4-[2-(pyridin-4-yl)vinyl]benzonitrile is also synthesized and studied for its silver(I) coordination chemistry. These new compounds are fully characterized by mass spectrometry, elemental analysis and spectroscopic techniques. The methylated product of ( E)-1-(9-anthryl)-3-{4-[2-(pyridin-4-yl)vinyl]phenyl}prop-2-en-1-one and a silver complex of ( E)-4-[2-(pyridin-4-yl)vinyl]benzonitrile are structurally determined by X-ray crystallography.

scholarly journals Exploring the Structural Chemistry of Pyrophosphoramides: N,N′,N″,N‴-Tetraisopropylpyrophosphoramide

Chemistry ◽  
2021 ◽  
Vol 3 (1) ◽  
pp. 149-163
Author(s):  
Duncan Micallef ◽  
Liana Vella-Zarb ◽  
Ulrich Baisch
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nuclear Magnetic Resonance ◽  
Hydrogen Bonding ◽  
Nmr Spectroscopy ◽  
Ir Spectroscopy ◽  
Room Temperature ◽  
Intermolecular Hydrogen Bonding ◽  
X Ray Diffraction ◽  
X Ray

N,N′,N″,N‴-Tetraisopropylpyrophosphoramide 1 is a pyrophosphoramide with documented butyrylcholinesterase inhibition, a property shared with the more widely studied octamethylphosphoramide (Schradan). Unlike Schradan, 1 is a solid at room temperature making it one of a few known pyrophosphoramide solids. The crystal structure of 1 was determined by single-crystal X-ray diffraction and compared with that of other previously described solid pyrophosphoramides. The pyrophosphoramide discussed in this study was synthesised by reacting iso-propyl amine with pyrophosphoryl tetrachloride under anhydrous conditions. A unique supramolecular motif was observed when compared with previously published pyrophosphoramide structures having two different intermolecular hydrogen bonding synthons. Furthermore, the potential of a wider variety of supramolecular structures in which similar pyrophosphoramides can crystallise was recognised. Proton (1H) and Phosphorus 31 (31P) Nuclear Magnetic Resonance (NMR) spectroscopy, infrared (IR) spectroscopy, mass spectrometry (MS) were carried out to complete the analysis of the compound.

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.

High-pressure Syntheses and Characterization of the Rare-earth Fluoride Borates RE2(BO3)F3 (RE=Tb, Dy, Ho)

2013 ◽  
Vol 68 (11) ◽  
pp. 1198-1206 ◽  
Author(s):  
Ernst Hinteregger ◽  
Michael Enders ◽  
Almut Pitscheider ◽  
Klaus Wurst ◽  
Gunter Heymann ◽  
...  
Keyword(s):  
Crystal Structure ◽  
High Pressure ◽  
Rare Earth ◽  
Monoclinic Space Group ◽  
Rare Earth Fluoride ◽  
Earth Fluoride ◽  
Structure Determinations ◽  
New Compounds ◽  
Rare Earth Fluorides

The new rare-earth fluoride borates RE2(BO3)F3 (RE=Tb, Dy, Ho) were synthesized under highpressure/ high-temperature conditions of 1:5 GPa=1200 °C for Tb2(BO3)F3 and 3:0 GPa=900 °C for Dy2(BO3)F3 and Ho2(BO3)F3 in a Walker-type multianvil apparatus from the corresponding rareearth sesquioxides, rare-earth fluorides, and boron oxide. The single-crystal structure determinations revealed that the new compounds are isotypic to the known rare-earth fluoride borate Gd2(BO3)F3. The new rare-earth fluoride borates crystallize in the monoclinic space group P21/c (Z = 8) with the lattice parameters a=16:296(3), b=6:197(2), c=8:338(2) Å , b =93:58(3)° for Tb2(BO3)F3, a= 16:225(3), b = 6:160(2), c = 8:307(2) Å , b = 93:64(3)° for Dy2(BO3)F3, and a = 16:189(3), b = 6:124(2), c = 8:282(2) Å , β= 93:69(3)° for Ho2(BO3)F3. The four crystallographically different rare-earth cations (CN=9) are surrounded by oxygen and fluoride anions. All boron atoms form isolated trigonal-planar [BO3]3- groups. The six crystallographically different fluoride anions are in a nearly planar coordination by three rare-earth cations.

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