Carbacylamidophosphates: Synthethis and Structure of N,N'-Tetramethyl-NM-benzoylphosphoryltriamide and Dimorpholido-N-benzoylphosphorylamide

2000 ◽  
Vol 55 (6) ◽  
pp. 495-498 ◽  
Author(s):  
Katerina E. Gubina ◽  
Vladimir A. Ovchynnikov ◽  
Vladimir M. Amirkhanov ◽  
Viktor V. Skopenkoa ◽  
Oleg V. Shishkinb
Keyword(s):  
Nmr Spectroscopy ◽  
Hydrogen Bonds ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
Sodium Salts ◽  
Space Group ◽  
X Ray ◽  
Centrosymmetric Dimers ◽  
Oxygen Atoms

N,N′-Tetramethyl-N"-benzoylphosphoryltriamide (I) and dimorpholido-N-benzoylphosphorylamide (II), and their sodium salts Nal, Nall were synthesized and characterized by means of IR and 1H, 31P NMR spectroscopy. The structures of I, II were determined by X-ray diffraction: I monoclinic, space group P2i/c with a = 10.162(3), b= 11.469(4), c = 12.286(4) Å , β = 94.04°, V = 1428.4(8) A 3, Z = 4, p(calcd) = 1.187 g/cm3; II monoclinic, space group C2/c with a = 15.503(4), b = 10.991(3), c = 22.000(6) Å, β = 106.39°, V = 3596.3(17) Å3, Z = 8, p(calcd.) = 1.253 g/cm3. The refinement of the structures converged at R = 0.0425 for I, and R = 0.068 for II. In both structures the molecules are connected into centrosymmetric dimers via hydrogen bonds formed by the phosphorylic oxygen atoms and hydrogen atoms of amide groups.

Carbacylamidophosphates: Synthethis and Structure of N,N'-Tetramethyl-N''-p-chlorobenzoyIphosphoryltriamide and N,N'-Tetramethyl-NM-o-fluorobenzoylphosphoryltriamide

2000 ◽  
Vol 55 (11) ◽  
pp. 1015-1019 ◽  
Author(s):  
Katerina E. Gubina ◽  
Vladimir M. Amirkhanov
Keyword(s):  
Nmr Spectroscopy ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
Centrosymmetric Dimer ◽  
Triclinic Space Group ◽  
Sodium Salts ◽  
Space Group ◽  
X Ray ◽  
Independent Molecules

N,N′-Tetramethyl-N″-p-chlorobenzoylphosphoryltriamide (I), N,N′-tetramethyl-N″-o-fluorobenzoylphosphoryltriamide (II) and their sodium salts were synthesized and characterized by means of IR and 1H , 31P NMR spectroscopy. The structures of both compounds were determined by X-ray diffraction (I triclinic, space group P1̄ with a = 12.073(2), b = 12.869(3), c = 12.854(4) Å, α = 56.93(2), β = 62.45(2), γ = 66.34(2)° V = 1453.7(6)Å3, ρ(caled.) = 1.324 mg/cm3, Z = 4 and R = 0.0545, wR2 = 0.1425; II monoclinic, space group P2(1)/n with a = 10.051(2), b = 13.093(2), c = 10.856(2) Å, β = 108.36(2)°, V = 1355.9(4) Å3, ρ(caled.) = 1.339 mg/cm3, Z = 4 and R = 0.0533, wR2 = 0.1263). In both structures the molecules are associated into dimers via hydrogen bonds formed by the phosphorylic oxygen atoms and hydrogen atoms of amide groups. In I the unit cell consists of two independent molecules connected into non-symmetric dimers, in II of centrosymmetric dimer molecules.

Carbacylamidophosphates: Synthesis, Properties, and Structure of Dimorfolido-N-trichloroacetylphosphorylamide

1998 ◽  
Vol 53 (4) ◽  
pp. 481-484 ◽  
Author(s):  
Vladimir A Ovchynnikov ◽  
Vladimir M Amirkhanov ◽  
Taras P Timoshenko ◽  
Tadeusz Glowiak ◽  
Henryk Kozlowskib
Keyword(s):  
Ir Spectroscopy ◽  
Hydrogen Bonds ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
Space Group ◽  
X Ray ◽  
Synthesis Properties ◽  
First Time ◽  
Centrosymmetric Dimers ◽  
Ir Bands

Abstract Dimorpholido-N-trichloroacetylphosphorylamide: CCl3C(O)NHP(O)[N(CH2CH2)2O]2 [HL] and its sodium [NaL] and morpholine [HN(CH2-CH2)2O•HL] salts were synthesized for the first time. The compounds were studied by IR spectroscopy and assignments of the characteristic IR bands have been made. The structure of [HL] was determined by X-ray diffraction. Crystals are monoclinic, a = 11.412(2) Å, b = 16.056(3) Å, c = 9.622(2) Å, β = 108.55(3)°, space group P21/c; Z = 4. The refinement of the structure converged at R = 0.066. The molecules are connected into centrosymmetric dimers via hydrogen bonds formed by the phosphorylic oxygen atoms and hydrogen atoms of amide groups.

Silver(I)-Saccharinato Complexes with 2-(Aminomethyl)pyridine and 2-(2-Aminoethyl)pyridine Ligands: [Ag(sac)(ampy)] and [Ag2(sac)2(μ-aepy)2]

2005 ◽  
Vol 60 (9) ◽  
pp. 978-983 ◽  
Author(s):  
Sevim Hamamci ◽  
Veysel T. Yilmaz ◽  
William T. A. Harrison
Keyword(s):  
Thermal Analysis ◽  
Hydrogen Bonds ◽  
Monoclinic Space Group ◽  
Stacking Interactions ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Pyridine Ligands

Two new saccharinato-silver(I) (sac) complexes, [Ag(sac)(ampy)] (1), and [Ag2(sac)2(μ-aepy)2] (2), [ampy = 2-(aminomethyl)pyridine, aepy = 2-(2-aminoethyl)pyridine], have been prepared and characterized by elemental analysis, IR spectroscopy, thermal analysis and single crystal X-ray diffraction. Complexes 1 and 2 crystallize in the monoclinic space group P21/c and triclinic space group P1̄, respectively. The silver(I) ions in both complexes 1 and 2 exhibit a distorted T-shaped AgN3 coordination geometry. 1 consists of individual molecules connected into chains by N-H···O hydrogen bonds. There are two crystallographically distinct dimers in the unit cell of 2 and in each dimer, the aepy ligands act as a bridge between two silver(I) centers, resulting in short argentophilic contacts [Ag1···Ag1 = 3.0199(4) Å and Ag2···Ag2 = 2.9894(4) Å ]. Symmetry equivalent dimers of 2 are connected by N-H···O hydrogen bonds into chains, which are further linked by aromatic π(py)···π(py) stacking interactions into sheets.

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.

1,3,5-Triphosphorinane. Synthese und Struktur der Isomeren des 1,3,5-Triphenyl-1,3,5-triphosphorinans/ 1,3,5-Triphosphorinanes. Synthesis and Structure of the Isomers of 1,3,5-Triphenyl-1,3,5-triphosphorinane

2006 ◽  
Vol 61 (5) ◽  
pp. 577-582 ◽  
Author(s):  
Manfred Fild ◽  
Peter G. Jones ◽  
Michael Lorms ◽  
Stefan Jäger
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Column Chromatography ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray

The reaction of lithiated Ph(H)PCH2P(H)Ph with (ClCH2)2PPh yields 1,3,5-Triphenyl-1,3,5- triphosphorinane (1) as a mixture of two isomers. The isomers have been separated by column chromatography and characterized by NMR spectroscopy and single crystal X-ray diffraction as the eq-eq-eq (1a) and eq-eq-ax-isomers (1b). (1a) crystallizes with a = 1326.9(3) pm and c = 933.4(3) pm in the rhombohedral space group R3 and displays 3-fold symmetry, showing an eq-eq-eq conformation. (1b) crystallizes in the monoclinic space group P21/c with a = 984.09(12) pm, b = 1757.5(2) pm, c = 1083.13(12) pm, β = 93.329(2)° and displays an ax-eq-eq conformation.

Dimer oder nicht dimer, das ist hier die Frage: Zwei benachbarte I3–--Ionen eingeschlossen in Hohlr¨aumen einer komplexen Wirtsstruktur

2010 ◽  
Vol 65 (12) ◽  
pp. 1462-1466 ◽  
Author(s):  
Michaela K. Meyer ◽  
Jürgen Graf ◽  
Guido J. Reiß
Keyword(s):  
Nmr Spectroscopy ◽  
Hydrogen Bonds ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Dimensional Network ◽  
Oder Nicht ◽  
Bonding Interaction ◽  
Hydrogen Bonded

[Me(HO)2P-(CH2)10-P(O)OHMe]2[I3]2・MeHO(O)P-(CH2)10-P(O)OHMe (1) was synthesized and characterized by IR, Raman and NMR spectroscopy. Its structure was determined by singlecrystal X-ray diffraction (T = 100 K; space group P1̄). The structure consists of decane-1,10-diyl-bis- (methylphosphinic acid) molecules and the analogous mono-protonated cations in a ratio 1:2 connected with each other by strong O-H···O hydrogen bonds to form a two-dimensional network. Between these hydrogen-bonded layers, there are elongated cavities each containing two triiodide anions. The intermolecular I· · · I distance of the two enclosed triiodide anions is 3.6317(4) Å and should be considered as an interhalogen bonding interaction.

Monomere und dimere Oxotrihalogenoselenate(IV): Darstellung, Struktur und Eigenschaften von [As(C6H5)4]SeOCl3 und [N(C2H5)4]SeOCl3 / Monomerie and Dimeric Oxotrihalogenoselenates(IV): Preparation, Structure and Properties of [As(C6H5)4]SeOCl3 and [N(C2H5)4]SeOCl3

1983 ◽  
Vol 38 (1) ◽  
pp. 20-29 ◽  
Author(s):  
Bernt Krebs ◽  
Marita Hucke ◽  
Michael Hein ◽  
Andreas Schäffer
Keyword(s):  
Polymer Chains ◽  
Monoclinic Space Group ◽  
Structure And Properties ◽  
Reaction Products ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Centrosymmetric Dimers

Abstract The monomeric SeOCl3- ion, which can be prepared as the tetraphenylarsonium salt from SeOCl2 and As(C6H5)4Cl, was structurally characterized by a low-temperature single crystal X-ray diffraction analysis. [As(C6H5)4]SeOCl3 is monoclinic, space group P21/c, with a = 9,332(3), b = 13,761(4), c = 18,985(6) Å, β = 110,97(3)° (at -135 °C), Z = 4; it contains a novel type of ψ-trigonal bipyramidal oxotrichloroselenate(IV) anion which is not associated to dimers or polymer chains as in known structures. The equatorial positions are occupied by doubly bonded oxygen (Se-O 1,601(3) Å) and by one Cl(Se-Cl 2,234(1) Å), the axial Se-Cl bonds (2,430(1) and 2,475(1) Å) being significantly longer. [N(C2H5)4]SeOCl3, which was obtained as crystals by oxidation of trichloroselenate(II), is triclinic, space group P1̄, with a = 10,607(3), b = 8,950(2), c = 8,862(2) Å, α = 119,79(2)°, β = 101,07(2)°, γ = 96,28(2)°, Z = 2. The X-ray structure analysis shows the anions to be present as centrosymmetric dimers Se2O2Cl62- like in the [P(C6H5)4]+ salt, with two tetragonal SeOCl4 pyramids linked through a Cl···Cl edge and the lone pairs trans to the axial Se-O bonds (1,589(4) Å). Se-Cl bond lengths are 2.270(1) and 2,351(2) Å (terminal); 2,698(1) and 2,920(1) Å (bridging). The results show that the nature of the reaction products of the Lewis acid SeOCl2 with halogenides as bases changes very sensitively with small variations in cations and environment. The vibrational spectra are discussed.

A new polymorph of bis(2-aminopyridinium) fumarate–fumaric acid (1/1) from powder X-ray diffraction

2013 ◽  
Vol 69 (8) ◽  
pp. 896-900 ◽  
Author(s):  
Shuichao Dong ◽  
Yaqiu Tao ◽  
Xiaodong Shen ◽  
Zhigang Pan
Keyword(s):  
Hydrogen Bonds ◽  
Fumaric Acid ◽  
Diffraction Method ◽  
Monoclinic Space Group ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
Acta Cryst ◽  
Space Group ◽  
X Ray ◽  
Hydrogen Bonded

A new polymorph of bis(2-aminopyridinium) fumarate–fumaric acid (1/1), 2C5H7N2+·C4H2O42−·C4H4O4, was obtained and its crystal structure determined by powder X-ray diffraction. The new polymorph (form II) crystallizes in the triclinic system (space groupP\overline{1}), while the previous reported polymorph [form I; Ballabh, Trivedi, Dastidar & Suresh (2002).CrystEngComm,4, 135–142; Büyükgüngör, Odabaşoğlu, Albayrak & Lönnecke (2004).Acta Cryst.C60, o470–o472] is monoclinic (space groupP21/c). In both forms I and II, the asymmetric unit consists of one 2-aminopyridinium cation, half a fumaric acid molecule and half a fumarate dianion. The fumarate dianion is involved in hydrogen bonding with two neighbouring 2-aminopyridinium cations to form a hydrogen-bonded trimer in both forms. In form II, the hydrogen-bonded trimers are interlinked across centres of inversionviapairs of N—H...O hydrogen bonds, whereas such trimers are joinedviasingle N—H...O hydrogen bonds in form I, leading to different packing modes for forms I and II. The results demonstrate the relevance and application of the powder diffraction method in the study of polymorphism of organic molecular materials.

Two crystal structures of 10,10′-(l,4-phenylene-dimethylidene)-bis-9,10-H-anthracenone

1992 ◽  
Vol 200 (3-4) ◽  
Author(s):  
G. Dewald ◽  
M. Hanack ◽  
E.-M. Peters ◽  
L. Walz
Keyword(s):  
Crystal Structures ◽  
Diffraction Data ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
Space Group ◽  
X Ray ◽  
Crystal And Molecular Structures

AbstractThe crystal and molecular structures of dimorphic 10,10′-(1,4-phenylene-dimethylidene)-bis-9,10-H-anthracenone (1) have been determined using X-ray diffraction data. The compound crystallizes either in the monoclinic space groupSince all non-hydrogen atoms are of pure

Two new organic-selenate salts: syntheses and crystal structures of bis(di-iso-propylammonium) selenate and di-n-butylammonium hydrogenoselenate

2017 ◽  
Vol 72 (6) ◽  
pp. 425-432
Author(s):  
Waly Diallo ◽  
Libasse Diop ◽  
Cheikh Abdoul Khadir Diop ◽  
Laurent Plasseraud ◽  
Hélène Cattey
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Hydrogen Bonds ◽  
Single Crystal ◽  
Elemental Analysis ◽  
X Ray Diffraction ◽  
Monoclinic System ◽  
Space Group ◽  
X Ray ◽  
Structural Characterizations

AbstractTwo new dialkyammonium selenate salts [i-Pr2NH2]2[SeO4] (1) and [n-Bu2NH2][HSeO4] (2) have been isolated and characterized by single-crystal X-ray diffraction. Salt 1 crystallizes in the monoclinic system, space group P21/n with a=8.7190(5), b=8.8500(4), c=22.5953(9) Å, β=94.6290(17)°, V=1737.84(14) Å3 and Z=4. Salt 2 crystallizes in the monoclinic system space group P21/n with a=10.9328(9), b=8.1700(6), c=13.8095(11) Å, β=97.130(3)°, V=1223.94(17) Å3 and Z=4. In both salts, dialkylammonium cations and selenate anions are connected through NH···O and OH···O hydrogen bonds. In the crystal structure, 1 and 2 are organized in layer-like arrangements. Structural characterizations were completed by infrared and 1H, 13C{1H} and 77Se NMR spectroscopy and elemental analysis which corroborate the X-ray elucidations.

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