Polysulfonylamine, LXV [1] Eine neue zentrosymmetrische Festkörper-Konformation von 18-Krone-6: Darstellung und Kristallstrukturen der monomeren Supramoleküle (CH2CH2O) 6 · 2 HN (SO2-2-Naphthyl)2 und (CH2CH2O) 6 · 2 iPrOH · 2 HN(SO2Ph)2 / Polysulfonylamines, LXV [1] A Novel Centrosymmetric Solid-State Conformation of 18-Crown-6: Synthesis and Crystal Structures of the Monomeric Supramolecules (CH2CH2O) 6 · 2 HN (SO2-2-Naphthyl)2 and (CH2CH2O) 6 · 2 iPrOH · 2 HN(SO2Ph)2

1995 ◽  
Vol 50 (6) ◽  
pp. 913-922 ◽  
Author(s):  
Dagmar Henschel ◽  
Martina Näveke ◽  
Thomas Hamann ◽  
Armand Blaschette ◽  
Peter G. Jones
Keyword(s):  
Solid State ◽  
Inversion Symmetry ◽  
Triclinic Space Group ◽  
Space Group ◽  
Ether Oxygen ◽  
O 175 ◽  
O 193 ◽  
Solid State Structures ◽  
Solid State Conformation ◽  
Oxygen Atoms

The complexes 18 C 6 · 2 HN (SO2-2 -Naphthyl)2 (2a) and 18 C 6 · 2 iPrOH · 2 HN (SO2Ph)2 (3e) were obtained by co-crystallization of 18-crown-6 (18 C 6) with the appropriate di(arenesulfonyl) amine from isopropanol solutions at temperatures ≥20 °C (for 2a) or at - 20 °C (for 3e). Both structures contain isolated formula units displaying crystallographic inversion symmetry. The conformation of the crown rings is characterized by the torsion angle sequence g+g+aag−g+ag+ag−g−aag+g−ag−a, unprecedented in solid-state structures of 18C 6 complexes. The six ether oxygen atoms and four out of twelve carbon atoms of the ring are coplanar within ± 7 pm. In 2a (triclinic, space group P 1̄) , the disulfonylamine molecules are linked to the oxygen atoms of the g±g∓g∓ units via N -H ··· O hydrogen bonds ( H ··· O 201 pm, N - H ··· O 161°). In 3e (triclinic, space group P 1̄ ) , each amine is N - H ··· O bonded to an isopropanol molecule (H ··· O 193 pm , N - H ··· O 175°) that is connected to a crown oxygen atom of the same conformational type as indicated above for 2a (H ··· O 198 pm, O - H ··· O 166°).

Polysulfonylamine, LXIII [1] / Polysulfonylamines, LXIII [1]

1995 ◽  
Vol 50 (1) ◽  
pp. 128-138 ◽  
Author(s):  
Dagmar Henschel ◽  
Armand Blaschette ◽  
Peter G. Jones
Keyword(s):  
Hydrogen Bond ◽  
Phenyl Group ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
Amine Molecule ◽  
Chain Sequence ◽  
O 193 ◽  
Oxygen Atoms

Complexes of Uncharged Molecules, Crystal StructureThe thermally labile ternary complexes 18C6 · 2MeOH · 2 HN(SO2Ph)2 (2a), 18C6 · 2MeOH · 2HN(SO2–C6H4-4-Cl)2 (2b) and 18C6 · 3 MeOH · HN(SO2Me)(SO2Ph) (3) were obtained by co-crystallization of 18-crown-6 (18C6) and the appropriate di(organosulfonyl)amine from methanolic solutions and characterized by low-temperature X-ray diffraction. The crystal structures of 2a (monoclinic, space group P21/n) and 2b (triclinic, space group P1̄) consist of monomeric, centrosymmetric formula units. Each di(arenesulfonyl)-amine molecule is connected to a methanol molecule by an N-Η ··· O hydrogen bond (H ··· O 203 pm in 2a, 190 pm in 2b). The methanol molecules are linked to three alternate crown oxygen atoms via one O-Η ··· O(crown) hydrogen-bond and two weaker C-Η ··· O(crown) interactions (OH ··· O 201 pm in 2a, 186 pm in 2b; CH ··· O 236 and 247 pm in 2a, 240 and 254 pm in 2b); two symmetry-related oxygen atoms of the crown are involved in O-Η ··· O and the other four in C-Η ··· O interactions. The structure of complex 3 (monoclinic, space group P21) is built of infinite chains parallel to [101]. The methyl group of the di(organosulfonyl)amine is bonded by C-Η ··· O(crown) interactions to a set of three alternate oxygen atoms of the cyclic polyether (H ··· O 228, 245 and 247 pm). Starting from the acidic NH function, a sequence of three methanol molecules catenated by hydrogen bonds curves around the bulky phenyl group and links with its terminal MeOH through one O-H ··· O(crown) and two C-Η ··· O(crown) bonds to the second set of alternate oxygen atoms in the adjacent symmetry-equivalent crown (OH ··· O 193 pm, CH ··· O 248 and 250 pm). Within the chain sequence N-H ··· O′(Me)H′ ··· O″(Me)H″ ··· O‴(Me)H, the H ··· O distances are H ··· O′ 184, H′ ··· O″ 189 and H″··· O‴ 183 pm. In the structures of 2a, 2b and 3, the crown rings adopt the frequently observed D3d pseudosymmetry.

Bis(trifluormethyl)disulfan und -trisulfan: Molekülgeometrie im festen Zustand [1] / Bis(trifluoromethyl)disulfane and Trisulfane: Molecular Geometry in the Solid State [1]

1997 ◽  
Vol 52 (1) ◽  
pp. 69-71 ◽  
Author(s):  
Christian Meyer ◽  
Dietrich Mootz ◽  
Birgit Bäck ◽  
Rolf Minkwitz
Keyword(s):  
Solid State ◽  
Electron Diffraction ◽  
Molecular Geometry ◽  
Monoclinic Space Group ◽  
Trans Conformation ◽  
Gaseous State ◽  
Triclinic Space Group ◽  
Space Group ◽  
Solid State Structures ◽  
State 1

The solid-state structures of the low-melting compounds bis(trifluoromethyl)disulfane (CF3SSCF3, triclinic, space group P 1̄, Z = 2) and bis(trifluoromethyl)trisulfane (CF3SSSCF3, monoclinic, space group C2/c, Z = 4) have been determined on single crystals with MoK α radiation at -160°C. The trisulfane has trans conformation. The geometry of both molecules agrees well with results of electron diffraction on the gaseous state. A comparison is made also with the crystal structures of the related molecules CF3TeTeCF3 and CF3OOOCF3

Calixcrown Binding to Alkali Metal Cations—Comparison of Two 1,3-Alternate Calix[4]arenebiscrown-5 Ligands

1996 ◽  
Vol 49 (2) ◽  
pp. 183 ◽  
Author(s):  
R Abidi ◽  
Z Asfari ◽  
JM Harrowfield ◽  
AN Sobolev ◽  
J Vicens
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Alkali Metal ◽  
Chloroform Solution ◽  
Metal Cations ◽  
Alkali Metal Cations ◽  
Triclinic Space Group ◽  
Space Group ◽  
Solid State Conformation

While determination of the crystal structure of 1,3;2,4-biscrown-5-calix[4] arene (chloroform solvate, triclinic. space group Pī, a 11.151(4), b 16.832(6), c 21.929(8) Ǻ, α 98.78(3), β 92.02(3), γ 92.12(3)°, Z = 4 f.u ., conventional R on |F| 0.085 for 4699 'observed', I > 2σ(I), reflections) shows that this ligand has a closely similar solid state conformation to that of its previously characterized, substituted analogue, 1,3;2,4-biscrown-5-p-t-butylcalix[4] arene, the two ligands do differ significantly in their interactions with alkali metal picrates in chloroform solution. Most obviously, the t-butyl substituents of the latter ligand appear to inhibit caesium binding. changing the nature of the interactions to a form similar to that of both ligands with Li+ and Na+, for which 1H n.m.r. spectroscopy indicates weak exocyclic binding to some of the polyether oxygen atoms. 1H n.m.r. spectroscopy also provides evidence of picrate binding to the metals in isomeric forms.

Synthese und Kristallstruktur von l,13-Bis(8-chinolyl)- 1,4,7,10,13-pentaoxatridecan-diquecksilber(I)-diperchlorat

1991 ◽  
Vol 46 (1) ◽  
pp. 1-4 ◽  
Author(s):  
Klaus Brodersen ◽  
Jörg Zimmerhackl
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
R Value ◽  
Torsional Angles ◽  
L 13 ◽  
Oxygen Atoms

1,13-Bis(8-quinolyl)-1,4,7,10,13-pentaoxatridecane-dimercury(I)-diperchlorate is formed by the reaction of 1,13-bis(8-quinolyl)-1,4,7,10,13-pentaoxatridecane in ethanol with an aqueous solution of dimercury(I)-diperchlorate.It crystallizes in the triclinic space group P Ī with a = 1020.6(2), b = 1200.6(8), c = 1441.1(6) pm , α = 69.60(5)°, β = 83.04(13)°, y = 66.53(4)° and Z = 2. The crystal structure was determined by X -ray diffraction and refined to an R-value o f 0.079. The Hg22+ -ion is coordinated to both nitrogen atoms and four oxygen atoms of one molecule of the ligand. By changing four C - O torsional angles from trans to gauche, the ligand adopts a helical, chiral configuration around the Hg22+-ion. The CIO4--ions are not coordinated to the Hg22+-ion.

Eine unerwartete Synthese des Triphenyphosphazenium-chlorids, [(C6H5)3PNH2]+CI– und eine Neubestimmung seiner Kristallstruktur / An Unaspected Synthesis of Triphenylphosphazenium Chloride, [(C6H5)3PNH2]+Cl– , and a Redeterm ination of its Crystal Structure

1996 ◽  
Vol 51 (6) ◽  
pp. 865-868 ◽  
Author(s):  
H. Vogt ◽  
A. Fischer ◽  
P. G. Jones
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Tetrahedral Geometry ◽  
Triclinic Space Group ◽  
Space Group

Abstract Triphenylphosphazenium chloride has been prepared by the reaction of triphenylphosphine with trimethylsilylazide in impure, wet dichloromethane. Yields are improved as stoichiometric quantities of water are added. Colourless crystals are obtained by recrystallization from the same solvent. The crystals are triclinic, space group P1̅, Z=2, a = 894,6(3), b - 979,8(3), c = 1142,9(4) pm, α = 107,27(3), β = 93,70(3), y = 92,97(3)°. In the solid state the compound exists as [(C6H5)3PNH2]+ cations, and Cl- anions. Dimeric units are formed by H-bonding. The crystal structure contains one molecule CH2Cl2 per one molecule (C6H5)3PNH2Cl. The cation has a slightly irregular tetrahedral geometry around the P-atom with a relatively short P-N bond

Die Kristallstruktur von Gadolinium (III)-sulfit Trihydrat Gd2(S03)3∙ 3H2O / Crystal Structure of Gadolinium(III)-sulfite Trihydrate Gd2(SO3)3 ∙3H2O

1994 ◽  
Vol 49 (1) ◽  
pp. 60-62 ◽  
Author(s):  
Hans-Ulrich Hummel ◽  
Petra Joerg ◽  
Gerhard Pezzei ◽  
Alexander Wolski
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Room Temperature ◽  
Triclinic Space Group ◽  
Space Group ◽  
Bond Lengths ◽  
Clear Solution ◽  
Oxygen Atoms

Abstract Gd2(SO3)3 • 3 H20 is obtained by passing gaseous SO2 through a suspension of Gd2O3 in H2O at room temperature until a clear solution is formed. Single crystals are obtained by heating to 70(2) °C for 6 days. The compound crystallizes in the triclinic space group P 1 with a = 6.499(6), b = 6.621(3), c = 6.954(3) Å, α = 110.71(5), β = 90.54(3), γ = 106.05(1)° and Z = 1. The two crystallographically different gadolinium atoms are both coordinated by eight oxygen atoms forming distorted square antiprisms. Gd(l) is coordinated by six O atoms of sulfite ligands and two O atoms of water, while Gd(2) is surrounded by seven O atoms of SO3 and one of H2O. Gd-O-bond lengths vary between 2.31(3) and 2.50(3) Å.

Mono- and difunctional furan-based 1,2,3,5-dithiadiazolyl radicals; preparation and solid state structures of 2,5-[(S2N2C)OC4H2(CN2S2)] and 2,5-[(S2N2C)OC4H2(CN)]

1992 ◽  
Vol 70 (3) ◽  
pp. 919-925 ◽  
Author(s):  
A. Wallace Cordes ◽  
Charles M. Chamchoumis ◽  
Robin G. Hicks ◽  
Richard T. Oakley ◽  
Kelly M. Young ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
The Mean ◽  
Solid State Structures ◽  
Solid State Characterization

The preparation and solid state characterization of the bifunctional radical furan-2,5-bis(1,2,3,5-dithiadiazolyl) 2,5-[(S2N2C)OC4H2(CN2S2)] and the related monofunctional radical 2-cyanofuran-5-(1,2,3,5-dithiadiazolyl) 2,5-[(S2N2C)OC4H2(CN)] are described. The crystal structure of 2,5-[(S2N2C)OC4H2(CN2S2)] is orthorhombic, space group Pna21, and consists of interleaved arrays of dimers, for which the mean interannular [Formula: see text] contact is 3.137 Å. The crystal structure of the monofunctional radical 2,5-[(S2N2C)OC4H2(CN)] is monoclinic, space group P21/n, and consists of a ribbon-like network of dimers (mean interannular [Formula: see text] interconnected by close head-to-tail [Formula: see text] contacts. The dimer units form stacks parallel to z, with a mean interdimer [Formula: see text] separation of 3.956 Å. The similarities and differences between these two crystal structures and those of related benzene-substituted systems are discussed. Keywords: dithiadiazolyl radicals, furan-based diradicals, cyanofuran-based radicals, radical dimers, crystal structures.

scholarly journals Crystal structure of bis{μ-(E)-2-[(2-oxidophenylimino)methyl]quinolin-8-olato-κ4O,N,N′,O′}bis[dibutyltin(IV)]

2017 ◽  
Vol 73 (1) ◽  
pp. 4-7
Author(s):  
Camacho-Camacho Carlos ◽  
Ortiz-Pastrana Naytzé ◽  
Garza-Ortiz Ariadna ◽  
Rojas-Oviedo Irma
Keyword(s):  
Crystal Structure ◽  
Schiff Base ◽  
Metal Atom ◽  
Title Complex ◽  
Unit Cell ◽  
Type Structure ◽  
Triclinic Space Group ◽  
Space Group ◽  
Centrosymmetric Dimers ◽  
Oxygen Atoms

Condensation of 8-hydroxyquinoline-2-carbaldehyde with 2-aminophenol gave the (E)-2-[(2-hydroxyphenylimino)methyl]quinolin-8-ol derivative that reacted with di-n-butyltin oxide with release of H2O to yield the chelate title complex, [Sn2(C4H9)4(C16H10N2O2)2]. The compound crystallizes in the triclinic space groupP-1, with two independent centrosymmetric dimers in the unit cell. Each features a typical pincer-type structure where the dianionic ligand is tetradentate, coordinating to the central tin atom through both phenolate oxygen atoms, as well as through the quinoline and imine N atoms. Each metal atom adopts a distorted pentagonal–bipyramidal SnC2N2O3coordination arising from theN,N′,O,O′-tetradentate deprotonated Schiff base, one bridging phenolate O atom of the neighbouring ligand and two butyl groups in the axial sites.

Synthesis and Structure of (17-Hydroxy-4,4,9,9,11- pentamethyl-5,8,12,13,15-pentaazaheptadec- 11-en-2-one hydrazone)nickel(II) Perchlorate; a Compound with a Hexadentate gem-Diamine Ligand

1997 ◽  
Vol 50 (1) ◽  
pp. 69 ◽  
Author(s):  
Neil F. Curtis ◽  
Olga P. Gladkikh
Keyword(s):  
Oxygen Atom ◽  
Secondary Amine ◽  
Ground State ◽  
Starting Material ◽  
Octahedral Coordination ◽  
Triplet Ground State ◽  
Triclinic Space Group ◽  
Space Group ◽  
Oxygen Atoms

(4,4,9,9-Tetramethyl-5,8-diazadodecane-2,11-dione dihydrazone)nickel(II) perchlorate reacts with 2- aminoethanol and methanal to form blue-violet (17-hydroxy-4,4,9,9,11-pentamethyl-5,8,12,13,15- pentaazaheptadec-11-en-2-one hydrazone)nickel(II) perchlorate. The structure of a methanol solvate was determined [C18H43Cl2N7NiO10, Mr 647·2, triclinic, space group P -1, a 8·992(7), b 10·86(2), c 15·02(1) Å, α 79·95(2), β 76·85(5), γ 78·83(2)°, Z 2, R 0·0637 for 2992 reflections]. The ligand has one terminal hydrazone function of the starting material linked to the 2-aminoethanol residue by a gem-diamine function derived from methanal. The ligand is hexadentate, with the triplet ground state nickel(II) ion in octahedral coordination by three secondary amine and two hydrazone nitrogen atoms and a hydroxy oxygen atom, with the terminal hydrazone nitrogen and the hydroxy oxygen atoms coordinated trans.

Conformation of a Fluorochrome from Aniline Blue

1997 ◽  
Vol 50 (10) ◽  
pp. 987
Author(s):  
Maureen F. Mackay, ◽  
Michael J. McTigue ◽  
Maruse Sadek
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Dimethyl Sulfoxide ◽  
Chemical Shifts ◽  
Deuterium Oxide ◽  
Sodium Ion ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
Solid State Conformation

The solid-state conformation of the fluorochrome sodium 4,4′-[carbonylbis(benzene-4,1-diyl)bis(imino)]-bisbenzenesulfonate has been defined by single-crystal X-ray crystallography. Monoclinic crystals belong to the space group C 2/c with a 11·732(1), b 6·185(1), c 37·179(3) Å, β 94·40(1)° and Z 8. The structure was refined to a final R0·042 for all 2271 unique terms. In the crystal six oxygen atoms form an octahedral grouping around the sodium ion and these octahedra are linked into layers sandwiched between the layers of organic anions which adopt an extended conformation. The n.m.r. spectra indicate that in solution the fluorochrome is flexible and averages to an extended structure that maintains symmetry about its longitudinal and carbonyl axes. Chemical shifts have been measured in water, deuterium oxide and (D6)dimethyl sulfoxide

Sign in / Sign up

Export Citation Format

Share Document