Synthese und Kristallstruktur des Bromdifluormethyl-triphenyl- phosphoniumbromids, [(C6H5)3PCF2Br]+ Br- / Synthesis and Crystal Structure of Bromodifluoromethyl-triphenylphosphonium Bromide, [(C6H5)3PCF2Br]+ Br-

2000 ◽  
Vol 55 (2) ◽  
pp. 167-170 ◽  
Author(s):  
C. Bender ◽  
D. Wulff-Molder ◽  
H. Vogt ◽  
F. Ritschl ◽  
M. Meisel
Keyword(s):  
Crystal Structure ◽  
Chloride Solution ◽  
Methylene Chloride ◽  
Monoclinic Space Group ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Methylene Chloride Solution ◽  
Mndo Calculations ◽  
Triphenylphosphonium Bromide ◽  
Good Agreement

Abstract Difluorobromomethyl-triphenylphosphonium bromide [(C6H5)3PCF2Br]+ Br- (1) has been prepared by the reaction of triphenylphosphine with dibromodifluoro-methane in acetonitrile or methylene chloride. The colorless crystals are monoclinic, space group P 21/n, Z=4, a = 1067.1(2), b = 1488,5(2), c = 1178,2(2) pm, β = 95,67(3)°. The lattice contains Br- anions and [(C6H5)3PCF2Br]+ cations with a Br-Br distance of 322,33(11) pm.. For the title compound the results of AM 1, PM 3 ,and MNDO calculations are in good agreement with corresponding values determined by the X-ray analysis only in the case of PM 3.The yellow-red [(C6H5)3PCF2Br]+ Br3- (2) has been obtained by treating 1 with equimolar quantities of elemental bromine in methylene chloride solution.

Synthese und Kristallstruktur der Benzyltriphenylphosphonium-bromide: [C6H5-CH2P(C6H5)3]+Br-CH2Cl2 und [C6H5-CH2P(C6H5)3]+Br3- / Synthesis and Crystal Structures of (Benzyl)triphenylphosphonium Bromides, [C6H5-CH2P(C6H5)3]+Br-CH2Cl2 and [C6H5-CH2P(C6H5)3]+Br3-

1997 ◽  
Vol 52 (11) ◽  
pp. 1321-1324 ◽  
Author(s):  
J. Hübner ◽  
D. Wulff-Molder ◽  
H. Vogt ◽  
M. Meisel
Keyword(s):  
Crystal Structures ◽  
Chloride Solution ◽  
Methylene Chloride ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
Methylene Chloride Solution ◽  
Triphenylphosphonium Bromide

(Benzyl)triphenylphosphonium bromide, [C6H5-CH2P(C6H5)3]+Br- (CH2Cl2) (1) has been prepared by the reaction of triphenylphosphine with benzylbromide and its structure determined. The colorless crystals are triclinic, space group P1̄, Z = 2, a = 976.0(3), b = 1069.0(3), c = 1226.1(4) pm, α = 94.13(3), β = 104.70(3), γ = 100.14(3)°. The lattice contains Br- anions and [C6H5-CH2P(C6H5)3]+ cations. [C6H5-CH2P(C6H5)3]Br3 (2) has been obtained by treating compound 1 with equimolar quantities of elemental bromine in methylene chloride solution. The red crystals of 2 are monoclinic, space group P21/c, Z = 4, a = 917.9(2), b = 1022.6(2), c = 2573.6(5) pm, β = 99.11(2)°, and comprise[C6H5-CH2P(C6H5)3]+ cations and linear, slightly asymmetrical Br3- anions with bromine-bromine distances of 246.19(11) and 263.69(11) pm.

Synthese und Kristallstruktur von Iodmethyltriphenylphosphonium-iodid (C6H5)3PCH2I+I- / Synthesis and Crystal Structure of Iodomethyltriphenylphosphonium Iodide (C6H5)3PCH2I+I-

1993 ◽  
Vol 48 (12) ◽  
pp. 1760-1766 ◽  
Author(s):  
H. Vogt ◽  
K. Lauritsen ◽  
L. Riesel ◽  
M. von Löwis ◽  
G. Reck
Keyword(s):  
Crystal Structure ◽  
Title Compound ◽  
Colourless Needle ◽  
Molecular Structures ◽  
Orthorhombic Space Group ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Mndo Calculations ◽  
Good Agreement

Iodomethyltriphenylphosphonium iodide, (C6H5)3PCH2I+I-, has been prepared by the reaction of (C6H5)3P with CH2I2 in dichloromethane forming colourless needle like crystals. The crystal and molecular structures have been determined by an X-ray structure analysis. The crystals are orthorhombic, space group Pca21, Z = 8; a = 1478,8(3) pm, b = 1249,3(3) pm, c = 2053,2(3) pm. R = 0.050 for 3219 observed reflections with I ≥ 2 σ(Ι). In the solid state the title compound exists as two discrete monomeric units, (C6H5)3PCH2I+I-. In both symmetry independent units the I-I distances are surprisingly short with 346,5(1) pm and 356,3(1) pm. For the title compound the results of AM 1, PM 3, and MNDO calculations are in good agreement with corresponding values determined by the X-ray analysis.

Notizen: Eine neue bicyclische Zinn-Selen-Verbindung. Synthese und Kristallstruktur von [{Cp(CO)2Fe}3ClSn3Se4] / A New Bicyclic Tin Selenium Compound. Synthesis and Crystal Structure of [{Cp(CO)2Fe}3ClSn3Se4]

1993 ◽  
Vol 48 (7) ◽  
pp. 1009-1012 ◽  
Author(s):  
Kurt Merzweiler ◽  
Harald Kraus
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Synthesis And Crystal Structure ◽  
Selenium Compound ◽  
Space Group ◽  
X Ray ◽  
Lattice Constants ◽  
Compound Synthesis

[{Cp(CO)2Fe}SnCl3] reacts with Na2Se in THF to form the compound [{Cp(CO)2Fe}3ClSn3Se4] 1. 1 crystallizes in the monoclinic space group P21/n with 4 formula units per unit cell. The lattice constants are α = 1435.2(7), b = 1124.4(4), c = 1972.7(12) pm, β = 94.59(4)°. According to the X-ray structure determination 1 contains a bicyclic Sn3Se4 framework.

Synthesis and Crystal Structure Determination of Cyclosporin H

2000 ◽  
Vol 65 (8) ◽  
pp. 1317-1328 ◽  
Author(s):  
Alexandr Jegorov ◽  
Ladislav Cvak ◽  
Aleš Husek ◽  
Petr Šimek ◽  
Anna Heydová ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Amino Acids ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Acid Catalyzed ◽  
Products Of Reaction ◽  
Cyclosporin H

Acid-catalyzed degradation of cyclosporin A was studied in various solvents and products of reaction were monitored by HPLC. Identification of amino acids and their chirality were determined after hydrolysis and derivatization by GC-MS. Cyclosporin H was isolated as the principal product and its structure was determined by X-ray diffraction: Cyclosporin H- diethyl ether-water (1 : 0.5 : 1) crystallizes in the monoclinic space group I2 with a = 12.338(2) Å, b = 18.963(2) Å, c = 34.074(3) Å, β = 96.47(2)°, Z = 4, and V = 7 921.4(17) Å3.

The reactions of [Pd2Cl2(μ-PP)2] (PP = dppm, dmpm) with Et2NC≡CNEt2 in methylene chloride solution: X-ray crystal structures of [Pd2Cl2(μ-CH2)(μ-dppm)2] and hexakis(diethylamino)benzene, C6(NEt2)6

1996 ◽  
Vol 74 (11) ◽  
pp. 2331-2339 ◽  
Author(s):  
Sean R. Klopfenstein ◽  
Constanze Kluwe ◽  
Kristin Kirschbaum ◽  
Julian A. Davies
Keyword(s):  
Key Words ◽  
Crystal Structures ◽  
Chloride Solution ◽  
Methylene Chloride ◽  
X Ray ◽  
Methylene Chloride Solution ◽  
Methylene Group

The binuciear palladium(I) complex, [Pd2Cl2(μ-dppm)2] (dppm = bis(diphenylphosphino)methane), has been shown to react with bis(diethylamino)acetylene, Et2NC≡CNEt2, in methylene chloride solution to yield two isolable products, the known methylene-bridged complex, [Pd2Cl2(μ-CH2)(μ-dppm)2], and hexakis(diethylamino)benzene, C6(NEt2)6, both of which have been characterized crystallographically. The source of the bridging methylene group in [Pd2Cl2(μ-CH2)(μ-dppm)2] has been shown to be the methylene chloride solvent. A mechanism that accounts for the formation of the two isolable products is proposed. The complex, [Pd2Cl2(μdmpm)2] (dmpm = bis(dimethylphosphino)methane), was similarly found to react with Et2NC≡NEt2 in methylene chloride solution to yield [Pd2Cl2(μ-CH2)(μ-dmpm)2], which was identified spectroscopically. Key words: acetylene, palladium, cyclooligomerization, aminoacetylene, hexakis(diethylamino)benzene.

Synthesis and Crystal Structure of a Fe(II,III) Complex with 2-(4΄-Chlorine-benzoyl)-benzoic acid and 3-(2-Pyridyl)pyrazole

2013 ◽  
Vol 634-638 ◽  
pp. 2592-2595
Author(s):  
Qing Wei Wang ◽  
Ting Feng Lu ◽  
Jia Guo ◽  
Xiu Mei Li
Keyword(s):  
Crystal Structure ◽  
Benzoic Acid ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Organic Complex ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Elemental Analyses ◽  
Metal Organic Complex ◽  
Metal Organic

A new metal-organic complex FeII2FeIII2(cbba)4(L)6 (Hcbba = 2-(4΄-chlorine-benzoyl) benzoic acid, L = 3-(2-pyridyl)pyrazole) 1 has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction, elemental analyses, TG and IR spectroscopy. The compound crystallizes in monoclinic, space group Cc with a = 17.729(5), b = 15.919(5), c = 33.650(5) Å, β = 92.058(5)°, V = 9491(4) Å3, C104H68Cl4Fe4N18O12, Mr = 2126.96, Dc = 1.489 g/cm3, μ(MoKα) = 0.786 mm1, F(000) = 4344, Z = 4, the final R = 0.0559 and wR = 0.1122 for 12093 observed reflections (I > 2(I)).

Synthese und Kristallstruktur von [Hg2(p-SC6H4NO2)]NO3 / Synthesis and Crystal Structure of [Hg2(p-SC6H4NO2)]NO3

1990 ◽  
Vol 45 (8) ◽  
pp. 1193-1196 ◽  
Author(s):  
Klaus Brodersen ◽  
Axel Knörr
Keyword(s):  
Crystal Structure ◽  
Chain Structure ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Nitrate Ions ◽  
R Value ◽  
A Chain

[Hg2(p-SC6H4NO2)]NO3 is formed by the reaction of p-nitrothiophenol with dimercury(I)-dinitrate in methanol. It crystallizes in the monoclinic space group P21/n with a = 1175.5(9) pm, b = 1079.8(8) pm, c = 876.2(8) pm, β = 110.74(4)° and Z = 4. The crystal structure has been determined by X-ray diffraction and refined to an R-value of 0.052. The results show that the compound exists as a chain structure of [—®S(C6H4NO2)— Hg— Hg—]n with nitrate ions connecting the chains.

Synthesis and Crystal Structure of a Caesium Hydrogen Benzoylcyanoximate Complex with 18-Crown-6: Cs(18-Crown-6){H(L)2}

1997 ◽  
Vol 52 (8) ◽  
pp. 901-905 ◽  
Author(s):  
Vera V Ponomareva ◽  
Victor V Skopenko ◽  
Konstantin V Domasevitch ◽  
Joachim Sieler ◽  
Thomas Gelbrich
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Crown Ether ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
The Mean ◽  
Cyano Groups ◽  
Oxygen Atoms

Abstract The caesium hydrogen benzoylcyanoximate (L-) complex with 18-crown-6 of composition Cs(18-crown-6){H(L)2} has been prepared and studied by means of X-ray diffraction [monoclinic, space group P21/n, with a = 9.906(1), b = 18.387(3), c = 18.855(3)Å, β = 90.13(1)°, V = 3434.3(9) Å, Z = 4; final R1 = 0.043 for the 6431 independent reflections used. The lattice consists of Cs(18-crown-6)+ cations and complex hydrogen oximate anions {H(L)2}-, formed via strong hydrogen bonding between the oxygen atoms of nitroso-groups [O - - - O ca. 2.456(5)Å]. The caesium atom deviates by 1.492(3) Å from the mean plane of the oxygen atoms of the macrocyclic ether (dominant orientation of disordered ligand, 60%) and adopts a typical “sunrise coordination” [Cs-O (ether) 3.040(9)-3.312(7) Å]. The hydrogen oximate groups are bonded to the metal center only on one side of the crown ether plane via the oxygen atoms of nitroso-groups and the nitrogen atoms of cyano groups (Cs-O ca. 3.040(9), 3.312(7) Å; Cs-N ca. 3.469(5), 3.679(6) Å). The coordination polyhedron of Cs+ can be described as a distorted bicapped tetragonal prism.

scholarly journals Synthesis and Crystal Structure ofN-Dichloroacetyl-3,4-dihydro-3-methyl-6-chloro-2H-1,4-benzoxazine

2015 ◽  
Vol 2015 ◽  
pp. 1-5
Author(s):  
Shuang Gao ◽  
Hai-Tao Qu ◽  
Fei Ye ◽  
Ying Fu
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Title Compound ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Compound C

A new compound,N-dichloroacetyl-3,4-dihydro-3-methyl-6-chloro-2H-1,4-benzoxazine, was synthesized and characterized. The crystal structure of the title compound (C11H10Cl3NO2,Mr=294.55) has been determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space groupP21/c, witha=6.7619(14),b=24.866(5),c=9.737(3) Å,α=90.00,β=130.982(18),γ=90.00°,V=1235.9(5) Å3,Z=4,Dx=1.583 Mg/cm3,λ(Mo  Ka)=0.71073 Å,F(000)=600,μ=0.729 mm−1,R=0.0476, andwR=0.1274for 2217 reflections withI>2σ(I).

Synthesen und Kristallstrukturen von Tris(di-n-propylamino)-p-brombenzylphosphonium-bromiden: [(C3H7)2N]3PCH2C6H4Br+Br- und [(C3H7)2N]3PCH2C6H4Br+Br3-/Syntheses and Crystal Structures of Tris(di-n-propylamino)-p-bromobenzyl-phosphonium Bromides: [(C3H7)2N]3PCH2C6H4Br+Br- and [(C3H7)2N]3PCH2C6H4Br+Br3-

1999 ◽  
Vol 54 (1) ◽  
pp. 113-116 ◽  
Author(s):  
J. Nolte ◽  
P. Neubauer ◽  
H. Vogt ◽  
M. Meisel
Keyword(s):  
Crystal Structures ◽  
Chloride Solution ◽  
Methylene Chloride ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
Methylene Chloride Solution

Tris(di-n-propylamino)-p-bromobenzylphosphonium bromide [(C3H7)2N]3PCH2C6H4Br+- Br- (1) has been prepared by the reaction of tris(di-n-propylamino)phosphine with p-bromobenzylbromide in methylene chloride. The colorless crystals are monoclinic, space group P21, Z = 2, a = 930.2(3), b = 1501.2(3), c = 1093.5(2) pm, β = 105,97(4)°. The lattice contains Br- anions and [(C3H7)2N]3PCH2C6H4Br+ cations. [(C3H7)2N]3PCH2C6H4Br+Br- (2) has been obtained by treating 1 with equimolar quantities of elemental bromine in methylene chloride solution. The yellow-red crystals of 2 are triclinic, space group P1̄, Z = 2, a = 1069.5(3), b = 1267.7(7), c = 1273.7(3) pm, α= 87.27(3), β = 82,67, γ = 67.15°, and consist of [(C3H7)2N]3PCH2C6H4Br+ cations and linear Br3- anions. The three N atoms in the cations of 2 are planar.

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