scholarly journals Crystal structure ofcis-anti-cis-dicyclohexane-18-crown-6 acetonitrile disolvate

2015 ◽  
Vol 71 (7) ◽  
pp. o472-o473
Author(s):  
Alexander Nazarenko
Keyword(s):  
Crown Ether ◽  
Metal Ion ◽  
Three Dimensional ◽  
Acetonitrile Solution ◽  
Average Deviation ◽  
Torsion Angles ◽  
Acetonitrile Molecule ◽  
Methyl Group ◽  
The Mean ◽  
Ether Molecule

The title compound (systematic name:cis-anti-cis-2,5,8,15,18,21-hexaoxatricyclo[20.4.0.09,14]hexacosane acetonitrile disolvate), C20H36O6·2CH3CN, crystallizes from an acetonitrile solution of dicyclohexane-18-crown-6 on evaporation. The molecule is arranged around a center of symmetry with half the crown ether molecule and one molecule of acetonitrile symmetry independent. All O—C—C—O torsion angles aregauchewhile all C—O—C—C angles aretrans. The sequence of torsion angles is [(tg+t)(tg−t)]3; the geometry of oxygen atoms is close to pseudo-D3dwith three atoms below and three atoms above the mean plane, with an average deviation of ±0.16 (1) Å from the mean plane. This geometry is identical to that observed in metal ion complexes of dicyclohexane-18-crown-6 but differs significantly from the conformation of a free unsolvated molecule. Each acetonitrile molecule connects to a crown ether moleculeviatwo of its methyl group H atoms (C—H...O). Weaker interactions exist between the third H atom of the acetonitrile methyl group and an O atom of a neighbouring crown ether molecule (C—H...O); and between the N atom of the acetonitrile molecule and a H atom of another neighbouring crown ether molecule. All these intermolecular interactions create a three-dimensional network stabilizing the disolvate.

Synthese und Kristallstruktur von [VCl2(15-Krone-5)]+[VOCl4]- / Synthesis and Crystal Structure of [VCl2(15-Crown-5)]+[VOCl4]-

1990 ◽  
Vol 45 (10) ◽  
pp. 1393-1397 ◽  
Author(s):  
Gerlinde Frenzen ◽  
Werner Massa ◽  
Thilo Ernst ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Crown Ether ◽  
Single Crystals ◽  
Structure Determination ◽  
Acetonitrile Solution ◽  
Tetragonal Symmetry ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Ether Molecule

[VCl2(15-crown-5)]+[VOCl4]- has been prepared by the reaction of VCl4 with 15-crown-5 in acetonitrile solution in the presence of water, forming black-brown single crystals. They were characterized by IR spectroscopy as well as by an X-ray structure determination. Space group Pnma, Z = 4, 1530 observed unique reflexions, R = 0.052. Lattice dimensions at -120°C: a = 1128.5(4), b = 1063.3(3), c = 1680(1) pm. The compound forms ions, in which the cation contains vanadium(+III), which is seven coordinate by the five oxygen atoms of the crown ether molecule and by two chlorine atoms in axial positions of a pentagonal bipyramide. The [VOCl4]- anion contains vanadium (+V) with approximately tetragonal symmetry

Synthesen und Kristallstrukturen der Kronenether-Komplexe (18-Krone-6) · 2CH3CN, [Na-15-Krone-5][ReO4] · CH3CN und [Na-15-Krone-5]PF6 / Syntheses and Crystal Structures of the Crown Ether Complexes (18-Crown-6) · 2 CH3CN, [Na-15-Crown-5][ReO4] · CH3CN, and [Na-15-Crown-5]PF6

1989 ◽  
Vol 44 (12) ◽  
pp. 1524-1530 ◽  
Author(s):  
Frank Weller ◽  
Harald Borgholte ◽  
Harald Stenger ◽  
Stefan Vogler ◽  
Kurt Dehnicke
Keyword(s):  
Crown Ether ◽  
Sodium Fluoride ◽  
Ion Pairs ◽  
Sodium Atom ◽  
Acetonitrile Solution ◽  
Space Group ◽  
Crown Ether Complexes ◽  
Water Space ◽  
Ether Molecule ◽  
Oxygen Atoms

Single crystals of (18-crown-6) · 2 CH3CN were obtained by cooling a solution of 18-crown-6 in acetonitrile to 4 °C. Space group P21/n, Z = 2, 629 observed independent reflexions, R = 0.062. Lattice dimensions at 19°C: a = 911.7(1), b = 852.0(1), c = 1370.0(2) pm; β = 104.61(1)°. The compound forms a molecular structure with approximate D3d symmetry of the crown ether molecule, and C—H ··· O interactions of the acetonitrile molecules with the crown ether, the Η···Ο distances being 243, 253, and 267 pm, respectively.[Na-15-crown-5][ReO4] · CH3CN is formed as a by-product of the reaction of ReNCl4 with sodium fluoride in acetonitrile in the presence of 15-crown-5 and traces of water. Space group Ρ 1̄ , Ζ = 2, 3107 observed independent reflexions, R = 0.045. Lattice dimensions at 19°C: a = 823.4(1), b = 1078.8(1), c = 1204.0(1) pm; α = 112.40(1)°, β = 94.35(1)°, γ = 104.63(1)°. The compound forms ion pairs, in which the sodium atom is sixfold coordinated by the five oxygen atoms of the crown ether molecule, as well as by one oxygen atom of the ReO4- ion, which is only slightly distorted. The bond length Na—OReO3 is 237.8(8) pm, the bond angle NaORe is 164.3(5)°.[Na-15-crown-5]PF6 is formed in the reaction of [ReCl3(NSCl)2 · POC13] with sodium fluoride in acetonitrile solution in the presence of 15-crown-5. Space group Pna21, Ζ = 4, 1130 observed independent reflexions, R = 0.123. The high R value is due to disorder of the skeletal atoms of the crown ether molecule. The compound forms ion pairs, in which the sodium atom is sevenfold coordinated by the five oxygen atoms of the crown ether molecule, as well as by two fluorine atoms of the PF6- ion with Na—F bond lengths of 240(2), and 246(2) pm, respectively.

scholarly journals Ethyl 3-(9-chloro-10-oxo-9,10-dihydroanthracen-9-yl)-5-methylisoxazole-4-carboxylate

2014 ◽  
Vol 70 (3) ◽  
pp. o315-o316 ◽  
Author(s):  
Nathan S. Duncan ◽  
Howard D. Beall ◽  
Alison K. Kearns ◽  
Chun Li ◽  
Nicholas R. Natale
Keyword(s):  
Three Dimensional ◽  
Dihedral Angles ◽  
Boat Conformation ◽  
Asymmetric Unit ◽  
Torsion Angles ◽  
Isoxazole Ring ◽  
Compound C ◽  
Dimensional Network ◽  
Π Stacking Interaction ◽  
The Mean

The asymmetric unit of the title compound, C21H16ClNO4, contains two independent molecules (AandB), each adopting a conformation wherein the isoxazole ring is roughly orthogonal to the anthrone ring. The dihedral angle between the mean plane of the isoxazole (all atoms) and the mean plane of the anthrone (all atoms) is 88.48 (3)° in one molecule and 89.92 (4)° in the other. The ester is almost coplanar with the isoxazole ring, with mean-plane dihedral angles of 2.48 (15) and 8.62 (5)°. In both molecules, the distance between the ester carbonyl O atom and the anthrone ketone C atom is about 3.3 Å. The anthrone ring is virtually planar (r.m.s. deviations of 0.070 and 0.065 Å) and adopts a shallow boat conformation in each molecule, as evidenced by the sum of the six intra-B-ring torsion angles [41.43 (15) and 34.38 (15)° for moleculesAandB, respectively]. The closest separation between the benzene moieties of anthronesAandBis 5.1162 (7) Å, with an angle of 57.98 (5)°, consistent with an edge-to-face π-stacking interaction. In the crystal, weak C—H...O and C—H...N interactions link the molecules, forming a three-dimensional network.

scholarly journals Crystal structure and Hirshfeld surface analysis of a new dithioglycoluril: 1,4-bis(4-methoxyphenyl)-3a-methyltetrahydroimidazo[4,5-d]imidazole-2,5(1H,3H)-dithione

2019 ◽  
Vol 75 (9) ◽  
pp. 1297-1300 ◽  
Author(s):  
Jonnie N. Asegbeloyin ◽  
Kenechukwu J. Ifeanyieze ◽  
Obinna C. Okpareke ◽  
Ebube E. Oyeka ◽  
Tatiana V. Groutso
Keyword(s):  
Hydrogen Bonds ◽  
Surface Analysis ◽  
Steric Effect ◽  
Bond Angle ◽  
Three Dimensional ◽  
Hirshfeld Surface ◽  
Hirshfeld Surface Analysis ◽  
Supramolecular Network ◽  
Torsion Angles ◽  
Methyl Group

In the title dithioglycoluril derivative, C19H20N4O3S2, there is a difference in the torsion angles between the thioimidazole moiety and the methoxyphenyl groups on either side of the molecule [C—N—Car—Car = 116.9 (2) and −86.1 (3)°, respectively]. The N—C—N bond angle on one side of the dithioglycoluril moiety is slightly smaller compared to that on the opposite side, [110.9 (2)° cf. 112.0 (2)°], probably as a result of the steric effect of the methyl group. In the crystal, N—H...S hydrogen bonds link adjacent molecules to form chains propagating along the c-axis direction. The chains are linked by C—H...S hydrogen bonds, forming layers parallel to the bc plane. The layers are then linked by C—H...π interactions, leading to the formation of a three-dimensional supramolecular network. Hirshfeld surface analysis and two-dimensional fingerprint plots were used to investigate the molecular interactions in the crystal.

scholarly journals Crystal structure of bis[4′-(1,4,7,10-tetraoxa-13- azacyclopentadecan-13-yl)-2,2′:6′,2′′-terpyridine]cobalt(III) tris(perchlorate) methanol monosolvate monohydrate

2015 ◽  
Vol 71 (8) ◽  
pp. 997-999
Author(s):  
Hitomi Ohmagari ◽  
Manabu Nakaya ◽  
Ryo Ohtani ◽  
Masaaki Nakamura ◽  
Shinya Hayami
Keyword(s):  
Crystal Structure ◽  
Crown Ether ◽  
Complex Cation ◽  
Three Dimensional ◽  
Dimensional Network ◽  
Centroid Distance ◽  
Π Stacking Interaction ◽  
Terpyridine Ligands ◽  
The Mean ◽  
Solvent Molecules

In the title compound, [Co(C25H30N4O4)2](ClO4)3·CH3OH·H2O, the metal atom is coordinated by two tridentate crown ether terpyridine ligands, forming a distorted CoN6octahedron. The three pyridine rings in each crown–terpyridine ligand are approximately coplanar [maximum deviations = 0.088 (12) and 0.102 (15) Å] and the mean planes through the three pyridine rings are perpendicular to each other, making a dihedral angle of 89.95 (17)°. An intramolecular C—H...π interaction is observed between the two terpyridine ligands. In the crystal, O—H...O and C—H...O hydrogen bonds, a π–π stacking interaction [centroid–centroid distance = 3.923 (7) Å] and a C—H...π interaction connect the complex cation, the perchlorate anions and the two types of solvent molecules, forming a three-dimensional network.

Synthese und Kristallstruktur von [Na-15-Krone-5][MoF5 (NCl)]

1988 ◽  
Vol 43 (9) ◽  
pp. 1125-1129 ◽  
Author(s):  
Dieter Fenske ◽  
Karin Völp ◽  
Kurt Dehnicke
Keyword(s):  
Crown Ether ◽  
Nmr Spectra ◽  
Bond Angle ◽  
Ion Pairs ◽  
Sodium Ion ◽  
Acetonitrile Solution ◽  
Crystal Data ◽  
X Ray ◽  
Data Space ◽  
Ether Molecule

Abstract [Na-15-Crown-5][MoF5(NCl)] has been prepared as yellow crystals by the reaction of NaF with MoF4(NCl) in the presence of 15-crown-5 in acetonitrile solution. The compound was charac­terized by its IR and 19F NMR spectra as well as by an X-ray structure determination. Crystal data: space group P21/n, Z = 4 (3736 observed, independent reflexions, R = 0.034). Lattice dimensions at -70 °C: a = 823.5(4). b = 1612.2(9), c = 1383.4(8), β = 99.35(3)°. The compound forms ion pairs, in which the sodium ion is seven-coordinated by the oxygen atoms of the crown ether molecule and by two fluorine ligands of the [MoF5(NCl)]- unit with Na-F distances of 228.3 and 249.6 pm. The Mo=N-Cl group of the anion is nearly linear (bond angle 175.8°) with bond lengths MoN = 172.9 and NCl = 161.8 pm.

Synthese und Kristallstrukturen der ionischen Kronenetherkomplexe [TiCl3(15-Krone-5)(CH3CN)][SbCl6) und [VCI(OH)(18-Krone-6)(CH3CN)2][SbCl6] · ½(18-Krone-6 · CH3CN) / Synthesis and Crystal Structures of the Ionic Crown Ether Complexes [TiCl3(15-Crown-5)(CH3CN)][SbCl6) und [VCI(OH)(18-Crown-6)(CH3CN)2][SbCl6] · ½(18-Crown-6 · CH3CN)

1993 ◽  
Vol 48 (2) ◽  
pp. 149-155 ◽  
Author(s):  
Michael Plate ◽  
Gerlinde Frenzen ◽  
Kurt Dehnicke
Keyword(s):  
Crown Ether ◽  
Chlorine Atom ◽  
Titanium Atom ◽  
Hydroxyl Group ◽  
Acetonitrile Solution ◽  
Antimony Pentachloride ◽  
Space Group ◽  
Structure Determinations ◽  
Ether Molecule ◽  
Oxygen Atoms

AbstractThe title compounds were prepared by the reaction of titanium tetrachloride with 15-crown-5 and antimony pentachloride, and by the reaction of vanadium trichloride with 18-crown-6 and antimony pentachloride in the presence of traces of water in acetonitrile solution, respectively. The complexes were characterized by IR spectroscopy and by X-ray structure determinations.[TiCl3(15-crown-5)(CH3CN)][SbCl6]: Space group Pnma, Z = 4, 1355 observed unique reflections, R = 0.035. Lattice dimensions at -80 °C: a = 1987(1), b = 1742.2(6), c = 111.0(2) pm. The compound consists of SbCl6- anions and cations [TiCl3(15-crown-5)(CH3CN)]+, in which the titanium atom is coordinated octahedrally by three chlorine atoms in facial arrangement, by the nitrogen atom of the acetonitrile molecule, and by two oxygen atoms of the crown ether molecule.[VCl(OH)(18-crown-6 )(CH3CN)2][SbCl6] · ½(18-crown-6 · CH3CN); Space group P 1̄, 3936 observed unique reflections, R = 0.714. Lattice dimensions at -80 °C: a = 1194.2(6), b = 1349.8(6), c = 1365.5(6) pm, α = 93.55(4)°, β = 111.23(4)°, γ = 93.15(4)°. The compound consists of SbCl6- anions, included 18-crown-6 and acetonitrile molecules, and cations [VCl(OH)(18-crown-6)(CH3CN)2]+, in which the vanadium atom is octahedrally coordinated by two nitrogen atoms of the acetonitrile molecules in trans positions, by a chlorine atom and a hydroxyl group in cis position, and by two oxygen atoms of the crown ether molecule. One of the acetonitrile molecules forms weak hydrogen bridges with two oxygen atoms of the included crown ether molecule as well as with one chlorine atom of the SbCl6- ion.

scholarly journals Crystal structure ofN-ethyl-2-(1,2,3,4-tetrahydronaphthalen-1-ylidene)hydrazinecarbothioamide

2017 ◽  
Vol 73 (2) ◽  
pp. 291-295 ◽  
Author(s):  
Adriano Bof de Oliveira ◽  
Johannes Beck ◽  
Christian Landvogt ◽  
Renan Lira de Farias ◽  
Bárbara Regina Santos Feitoza
Keyword(s):  
Crystal Packing ◽  
Site Occupancy ◽  
Hirshfeld Surface ◽  
Asymmetric Unit ◽  
Torsion Angles ◽  
Methyl Group ◽  
Compound C ◽  
The Mean ◽  
Graph Set ◽  
Independent Molecules

There are two crystallographically independent molecules in the asymmetric unit of the title compound, C13H17N3S, one of them being disordered over the methyl group [site-occupancy ratio = 0.705 (5):0.295 (5)]. The maximum r.m.s. deviations from the mean plane of the non-H atoms for the tetralone fragments amount to 0.4572 (17) and 0.4558 (15) Å. The N—N—C—N fragments are not planar and torsion angles are −9.4 (2) and 8.3 (2)°. In the crystal, the molecules are linked by weak N—H...S interactions into chains along [100] with graph-set motifC(4) and connected by weak N—H...S and C—H...S interactions, formingR21(10) rings. The Hirshfeld surface analysis indicates that the most important contributions for the crystal packing are the H...H (64.20%), H...S (12.60%) and H...C (12.00%) interactions. The crystal packing resembles a herringbone arrangement when viewed along [001].

Notizen: [K(18-Krone-6)][WF5(NCl)]; Synthese und Kristallstruktur / [K(18-Crown-6)][WF5(NCl)]; Synthesis and Crystal Structure

1992 ◽  
Vol 47 (7) ◽  
pp. 1054-1056 ◽  
Author(s):  
Harald Stenger ◽  
Kurt Dehnicke ◽  
Wolfgang Hiller
Keyword(s):  
Crystal Structure ◽  
Crown Ether ◽  
Structure Determination ◽  
Ir Spectrum ◽  
Bond Angle ◽  
Ion Pairs ◽  
Acetonitrile Solution ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Ether Molecule

[K(18-crown-6)][WF5(NCl)] has been prepared as yellow crystals by the reaction of KF with WCl4(NCl) in the presence of 18-crown-6 in acetonitrile solution. The compound was characterized by its IR spectrum and by an X-ray structure determination. Space group P21/n, Z = 4, 3697 observed unique reflections, R = 0.034. Lattice dimensions at –65 °C: a = 1313.8(3), b = 851.2(1), c = 1842.7(4) pm, β = 95.304(1)°. The compound forms ion pairs, in which the pottassium ion is coordinated by the six oxygen atoms of the crown ether molecule and by two fluorine ligands of the [WF5(NCl)]- unit with K–F distances of 272.4(5) and 288.6(5) pm. The W=N–Cl group of the anion is nearly linear (bond angle 170.7(5)°) with bond lengths of WN = 172.4(7) and NCI = 162.7(7) pm.

scholarly journals Crystal structures of 6a,6b,7,11a-tetrahydro-6H,9H-spiro[chromeno[3′,4′:3,4]pyrrolo[1,2-c]thiazole-11,3′-indoline]-2′,6-dione and 5′-methyl-6a,6b,7,11a-tetrahydro-6H,9H-spiro[chromeno[3′,4′:3,4]pyrrolo[1,2-c]thiazole-11,3′-indoline]-2′,6-dione

2019 ◽  
Vol 75 (2) ◽  
pp. 246-250
Author(s):  
S. Pangajavalli ◽  
R. Ranjithkumar ◽  
N. Srinivasan ◽  
S. Ramaswamy ◽  
S. Selvanayagam
Keyword(s):  
Hydrogen Bonds ◽  
Three Dimensional ◽  
Ring System ◽  
Dimensional Structure ◽  
Dihedral Angles ◽  
Pyrrolidine Ring ◽  
Methyl Group ◽  
Significant Difference ◽  
The Mean ◽  
Compound Ii

The title compounds, C20H16N2O3S, (I), and C21H18N2O3S, (II), differ by the presence of a methyl group in position 5 on the 1H-indole-2-one ring of compound (II). The two compounds have a structural overlap r.m.s. deviation of 0.48 Å. There is a significant difference in the conformation of the thiazolidine ring: it has a twisted conformation on the fused N—C bond in (I), but an envelope conformation in compound (II) with the S atom as the flap. The planar pyrrolidine ring of the indole ring system is normal to the mean plane of the five-membered pyrrolidine ring of the pyrrolothiazole unit in both compounds, with dihedral angles of 88.71 (9) and 84.59 (8)°. The pyran rings in both structures have envelope conformations with the methylene C atom adjacent to the C=O group as the flap. In both compounds, there is a short intramolecular C—H...O contact present. In the crystal of (I), molecules are linked by C—H...O hydrogen bonds forming chains propagating along the b-axis direction. The chains are linked by N—H...π interactions, forming layers parallel to (10\overline{1}). In the crystal of (II), molecules are linked by pairs of N—H...O hydrogen bonds, forming inversion dimers which are linked by C—H...O hydrogen bonds to form a three-dimensional structure.

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