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.

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.

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)).

Solvothermal Synthesis and Crystal Structure Determination of Tris- (ethyleneamine-ammonium) Tetraselenoantimonat: Non-Centrosymmetry Mediated by an Extended Unusual N-H···N Hydrogen Bonded Network?

1998 ◽  
Vol 53 (10) ◽  
pp. 1144-1148 ◽  
Author(s):  
Frank Wendland ◽  
Christian Näther ◽  
Michael Schur ◽  
Wolfgang Bensch
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Solvothermal Synthesis ◽  
Amino Nitrogen ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Ammonium Hydrogen ◽  
Solvothermal Conditions

AbstractThe title compound has been synthesized under solvothermal conditions by the reaction of elemental chromium, antimony and selenium in a solution of 40% 1,2-ethanediamine (en) in methanol. The crystal structure consists of tetrahedral SbSe43- anions which are connected by monoprotonated 1,2-ethanediamine (enH+) cations via N-H--Se hydrogen bonding. The enH+ cations are joined via strong N-H -N hydrogen bonds between the ammonium hydrogen and the amino nitrogen atom forming four distinct chains, each built up of three crystallographically independent enH+ cations. Two of these chains are running parallel to [100], the other two are parallel to [010]. Based on this arrangement different centrosymmetric or non-centrosymmetric hydrogen bonding patterns are possible, but only in one chain the sequence of NH2 and NH3+ groups was determined by X-ray diffraction

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.

scholarly journals Synthese und Kristallstruktur von [Na(15-Krone-5)]2S6 / Synthesis and Crystal Structure of [Na(15-crown-5)]2S6

1992 ◽  
Vol 47 (8) ◽  
pp. 1063-1066 ◽  
Author(s):  
Alfred-Dirk Bacher ◽  
Ulrich Müller
Keyword(s):  
Crystal Structure ◽  
Crown Ether ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
X Ray ◽  
Ether Molecule

[Na(15-crown-5)]2S6 was obtained from Na2S4 und 15-crown-5 in acetonitrile. Its crystal structure was determined by X-ray diffraction with 2968 observed reflexions, R = 0.119. Crystal data: a = 861.4(9), b = 1006(1), c = 2097(1) pm, α = 89.7(1), β = 100.20(8), γ = 114.6(1)°, Ζ = 2, space group Ρ 1̄. The chain-like S62- ion has transoid conformations, each of its terminal atoms is in contact with one Na+ ion which in turn is coordinated with one crown ether molecule.

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).

scholarly journals Crystal structure of bis{(S)-1-[2-(diphenylphosphanyl)ferrocenyl]-(R)-ethyl}ammonium bromide dichloromethane monosolvate

2017 ◽  
Vol 73 (2) ◽  
pp. 152-154
Author(s):  
Afrooz Zirakzadeh ◽  
Berthold Stöger ◽  
Karl Kirchner
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Hydrogen Bonding ◽  
The Other ◽  
Ammonium Bromide ◽  
X Ray Diffraction ◽  
Interplanar Angle ◽  
X Ray ◽  
The Mean ◽  
Protonated Ligand

During the synthesis of an FeBr2complex with the PNP ligand (R,R,SFc,SFc)-[Fe2(C5H5)2(C38H35NP2)] (1), single crystals of the dichloromethane monosolvate of the Br−salt of the protonated ligand1H+were obtained serendipitously,i.e.[Fe2(C5H5)2(C38H36NP2)]Br·CH2Cl2. The crystal structure of1H·Br·CH2Cl2was determined by single-crystal X-ray diffraction. The mean bond lengths in the ferrocene units are Fe—C = 2.049 (3) Å and C—C = 1.422 (4) Å within the cyclopentadienyl rings. The mean C—N bond length is 1.523 (4) Å. The interplanar angle between the two connected cyclopentadienyl rings is 49.2 (2)°. One ferrocene moiety adopts a staggered conformation, whereas the other is between staggered and eclipsed. The Br−ions and the CH2Cl2molecules are located in channels extending along <100>. One ammonium H atom forms a hydrogen bond with the Br−ion [H...Br = 2.32 (4) Å and C—H...Br = 172 (3)°]. The second ammonium H atom is not involved in hydrogen bonding.

Structure of Tl(18-crown-6){Cl3CC(O)N P(O)(OCH3)2}: Coordination of the Ionic Multidentate Weakens the Interaction of the Metal Atom with the Crown Ether

1999 ◽  
Vol 54 (4) ◽  
pp. 451-455 ◽  
Author(s):  
Victor A. Trush ◽  
Konstantin V. Domasevitch ◽  
Vladimir M. Amirkhanov ◽  
Joachim Sieler
Keyword(s):  
Ir Spectroscopy ◽  
Crown Ether ◽  
Metal Atom ◽  
Central Atom ◽  
Carbonyl Groups ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
The Mean ◽  
Oxygen Atoms

The thallium(I) dimethyl-N-trichloroacetylamidophosphate complex with a 18-crown-6 of the composition Tl(18-crown-6){L} (L = {Cl3CC(O)NP(O)(OCH3)2} -) has been prepared and characterized by means of IR spectroscopy and X-ray diffraction (orthorhombic, space group P212121 with a = 8.660( 1), b = 11.557(2), c =26.296(3) Å, Z = 4, V = 2631.8(6) Å3; R1 = 0.0285 and wR2 = 0.0558 for 4314 unique reflections). It was shown that (L-) is coordinated to the central atom in a bidentate manner via oxygen atoms of phosphoryl [Tl-O(l) 2.678(4) Å] and carbonyl groups [Tl-O(2) 3.012(6) Å.The Tl( 18-crown-6)+ moiety adopts a typical “sunrise” coordination with the metal atom laying 1.134(2) Å above the mean plane of the oxygen atoms of the macrocycle. This deviation is the highest value of the structurally examined Tl( 18- crown-6 )+ complexes. The Tl-O (etheric) separations are in the range 2.913(4) - 3.198(5) Å (av. 3.030(6) Å).

scholarly journals Synthesis and Crystal Structure of a Sandwich-type Transition Metal Complex with Tungstobismutate and Triethanolamine

2009 ◽  
Vol 64 (7) ◽  
pp. 821-825 ◽  
Author(s):  
Xiuhong Xu ◽  
Ling Zhang ◽  
Yi Zhang ◽  
Bin Qi ◽  
Fang Luo
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Transition Metal Complex ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Hydrogen Bonding Interactions ◽  
Type Complex ◽  
Sandwich Type

The sandwich-type complex Na(H2O)6(C6H16O3N)2[Na2(H2O)7(C6H16O3N)]2[(Na(H2O)2)3- (Cu(H2O))3(BiW9O33)2]・14H2O (1) (C6H16O3N+ = protonated triethanolamine) has been synthesized and structurally characterized by single-crystal X-ray diffraction, IR spectroscopy and TG analysis. The basic framework of 1 is built from a sandwich-type [(Na(H2O)2)3- (Cu(H2O))3(BiW9O33)2]9− anion, two [Na2(H2O)7(C6H16O3N)]3+ cations, a free Na(H2O)6+ cation, and two free C6H16O3N+ units. In compound 1, the [(Na(H2O)2)3(Cu(H2O))3- (BiW9O33)2]9− anion links two bi-nuclear units [Na2(H2O)7(C6H16O3N)]3+ to form a [Na2- (H2O)7(C6H16O3N)]2[(Na(H2O)2)3(Cu(H2O))3(BiW9O33)2]3− cluster, and a new 3D supramolecular structure is further constructed by hydrogen bonding interactions among this cluster, the free Na(H2O)6+ cation, and the free C6H16O3N+ cations. Crystal data: Cu3Na8Bi2W18C24H150O121N4, monoclinic, C2/c, a = 14.5668(13), b = 23.0405(13), c = 37.412(2) Å , β = 91.569(10)° , Z = 4.

Synthesis and Crystal Structure of (1E,2E)-1,2-Di (-3-Nitrobenzylidene) Hydrazine under Micromave Irradiation

2013 ◽  
Vol 787 ◽  
pp. 205-207
Author(s):  
Hong Yan Zhou
Keyword(s):  
Crystal Structure ◽  
Microwave Irradiation ◽  
Monoclinic Space Group ◽  
Stacking Interactions ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
H Nmr ◽  
The Stability ◽  
High Yields

A compound of (1E,2E)-1,2-di (-3-nitrobenzylidene) hydrazine was synthesized under microwave irradiation (500 w), giving high yields of products (93%). Its structure was determined IR, 1H NMR, MS, elemental analysis and X-ray diffraction. The crystal of the compound is Monoclinic, space group P2(1)/n with a = 6.9611(18), b = 7.823(2), c = 12.999(3) Å, α = 90, β = 105.215(4), γ = 90o, V= 683.1(3) Å3, Z=4, Dc=1.450g/cm3,μ=0.110 mm-1, F(000)=308, R=0.0401 and wR = 0.1131 for 1273 observed reflection with I>2σ (I). π-π stacking interactions contribute to the stability of the structure.

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