Crystal and Molecular Structure of 1,2,4-Triazolium Chloride and its Salt with Antimony Trichloride - Bis(1,2,4-triazolium) pentachloroantimonate(III)-1,2,4-triazolium Chloride

2002 ◽  
Vol 57 (2) ◽  
pp. 157-164 ◽  
Author(s):  
Maciej Bujak ◽  
Jacek Zaleski
Keyword(s):  
Hydrogen Bonds ◽  
Crystal And Molecular Structure ◽  
Antimony Trichloride ◽  
Organic Cations ◽  
Orthorhombic Space Group ◽  
Monoclinic System ◽  
Space Group ◽  
Anionic Sublattice ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

The structures of 1,2,4-triazolium chloride (C2H4N3)Cl and its derivative with antimony trichloride - (C2H4N3)2[SbCl5] · (C2H4N3)Cl containing unsubstituted 1,2,4-triazolium cations were determined. (C2H4N3)Cl crystallizes in the monoclinic system, space group P21/n with the unit cell dimensions at 86 K: a = 9.425(2), b = 8.557(2), c = 11.158(2)Å , β = 95.87(3)°; V = 895.2(3)Å3, Z=8, dc = 1.566, dm = 1.56(2) g·cm-3.At roomtemperature, crystals of (C2H4N3)2- [SbCl5] · (C2H4N3)Cl are orthorhombic, space group P212121, a = 8.318(2), b = 11.381(2), c = 19.931(4) Å, V = 1886.8(7) Å3, Z = 4, dc = 1.917, dm = 1.91(2) g·cm-3. In both crystals the 1,2,4-triazole rings are planar. The anionic sublattice of (C2H4N3)2[SbCl5]·(C2H4N3)Cl consists of polymeric [SbCl5]n 2- zig-zag chains composed of distorted [SbCl6]3- octahedra connected via their vertices and the single Cl- anions. The cavities between the inorganic chains are filled by 1,2,4-triazolium cations. The nature of the distortion of the [SbCl6]3- polyhedra has been studied by examining correlations between the Sb-Cl bond lengths and the strength of hydrogen bonds, which join the anionic sublattice and the organic cations. This study confirms that the deformation of the [SbCl6]3- octahedra is caused by hydrogen bonds.

scholarly journals The crystal and molecular structure of the bis(N,N,N′,N′-tetramethylethanediamine) adduct of I(Br)InInBr2, In2Br3I•2C6H16N2, an indium–indium bonded molecule

1984 ◽  
Vol 62 (3) ◽  
pp. 601-605 ◽  
Author(s):  
Masood A. Khan ◽  
Clovis Peppe ◽  
Dennis G. Tuck
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Crystal And Molecular Structure ◽  
Heavy Atom ◽  
Orthorhombic Space Group ◽  
Trigonal Bipyramidal ◽  
Cell Dimensions ◽  
Unit Cell Dimensions ◽  
Heavy Atom Method ◽  
Distorted Trigonal Bipyramidal

The crystal structure of the title compound has been determined by the heavy atom method. The crystals are orthorhombic, space group Pbca, with unit cell dimensions a = 22.795(3) Å, b = 17.518(2) Å, c = 12.396(3) Å, Z = 8; R = 0.0409 for 1527 unique "observed" reflections. The structure is disordered, with each halogen site (X) occupied by 75% Br, 25% I. The molecule consists of two X2(tmen)In units (tmen = N,N,N′,N′-tetramethylethanediamine) with distorted trigonal bipyramidal geometry, joined by an In—In bond 2.775(2) Å in length.

scholarly journals Synthesis and Characterization of [2-CH3CH2C6H4NH3]6P6O18⋅4H2O

2011 ◽  
Vol 2011 ◽  
pp. 1-6 ◽  
Author(s):  
Houda Marouani ◽  
Salem Slayyem Al-Deyab ◽  
Mohamed Rzaigui
Keyword(s):  
Hydrogen Bonds ◽  
Electrostatic Interactions ◽  
Three Dimensional ◽  
Spectroscopic Studies ◽  
Monoclinic System ◽  
Dimensional Network ◽  
Cell Dimensions ◽  
Unit Cell Dimensions ◽  
Ir Spectroscopic

Single crystals of [2-CH3CH2C6H4NH3]6P6O18⋅4H2O are synthesized in aqueous solution by the interaction of cyclohexaphosphoric acid and 2-ethylaniline. This compound crystallizes in the monoclinic system with P21/c space group the unit cell dimensions are: a=16.220(4) Å, b=10.220(5) Å, c=20.328(4) Å, β=113.24(3)∘, Z=2, and V=3096.5(18) Å3. The atomic arrangement can be described by layers formed by cyclohexaphosphate anions P6O186− and water molecules connected by hydrogen bonds O–H⋯O. These inorganic layers are developed around bc planes at x=1/2 and are interconnected by the H-bonds created by ammonium groups of organic cations. All the hydrogen bonds, the van der Waals contacts and electrostatic interactions between the different entities give rise to a three-dimensional network in the structure and add stability to this compound. The thermal behaviour and the IR spectroscopic studies of this new cyclohexaphosphate are discussed.

scholarly journals X-ray Crystallographic Study of Ranaconitine

2011 ◽  
Vol 6 (11) ◽  
pp. 1934578X1100601
Author(s):  
Yang Li ◽  
Jun-Hui Zhou ◽  
Gui-Jun Han ◽  
Min-Juan Wang ◽  
Wen-Ji Sun ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Diffraction Analysis ◽  
Critical Role ◽  
X Ray Diffraction ◽  
Monoclinic System ◽  
X Ray ◽  
Crystallographic Study ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

The crystal structure of natural diterpenoid alkaloid ranaconitine isolated from Aconitum sinomontanum Nakai has been determined by single crystal X-ray diffraction analysis. The crystal presents a monoclinic system, space group C2 with Z = 4, unit cell dimensions a = 30.972(19) Å, b = 7.688(5) Å, and c = 19.632(12) Å. Moreover, the intermolecular O–H···O hydrogen bonds and weak π-π interactions play a critical role in expanding the dimensionality.

The crystal and molecular structure of tris-butyl-tin(IV)-(1-pyrrolidinecarbodithioato)-3-propionate

1989 ◽  
Vol 54 (3) ◽  
pp. 684-690 ◽  
Author(s):  
Jan Lokaj ◽  
Viktor Vrábel ◽  
Eleonóra Kellö ◽  
Vladimír Ratay
Keyword(s):  
Molecular Structure ◽  
Structural Analysis ◽  
Least Squares ◽  
Least Squares Method ◽  
Crystal And Molecular Structure ◽  
Analysis Method ◽  
Monoclinic System ◽  
X Ray ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

The crystal and molecular structure of Bu3Sn(pyrn-dtc-prop) was solved by the X-ray structural analysis method and refined by the block diagonal least squares method to R = 0.053 for 1 930 observed reflections. The compound crystallizes in the monoclinic system with a space group of P21/c, Z = 4, F(000) = 1 056, with unit cell dimensions of a = 1.4758(5), b = 0.9970(3), c = 1.9166(6) nm; β = 113.90(2)°. The measured and calculated crystal densities were Dm = 1.32 and Dc = 1.31.103 kg m-3. The tin atom is coordinated by three carbon atoms at distances of Sn-C 0.2117(8), 0.2133(8), 0.2158(11) nm and two oxygen atoms O(1) and O(2) at distances of Sn-O 0.2210(5) and 0.2399(5) nm. The coordination polyhedron is a deformed trigonal bipyramid. The S2CN ligand is approximately planar.

scholarly journals Comparison of the C—H...O bonding in two crystalline phases of 1,4-dithiane 1,1,4,4-tetraoxide

2019 ◽  
Vol 75 (5) ◽  
pp. 576-579
Author(s):  
Richard L. Harlow ◽  
Allen G. Oliver ◽  
Jonathan M. Baker ◽  
William J. Marshall ◽  
Michael P. Sammes
Keyword(s):  
Hydrogen Bonds ◽  
Phase 1 ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Nmr Spectrum ◽  
Crystalline Phases ◽  
Space Group ◽  
H Nmr ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

The crystal structures of two crystalline phases of 1,4-dithiane 1,1,4,4-tetraoxide, C4H8O4S2, have been determined in order to examine the nature of possible intermolecular hydrogen bonds. Phase 1 is monoclinic, space group C2/m, with unit-cell dimensions of a = 9.073 (8), b = 7.077 (6), c = 5.597 (5) Å and β = 105.89 (1)°. The molecule adopts 2/m symmetry and all of the molecules are related by translation and thus have the same orientation. Phase 2 is also monoclinic but in space group P21/n with unit-cell dimensions of a = 7.1305 (5), b = 5.7245 (4), c = 8.3760 (6) Å and β = 91.138 (2)°. In this phase, the molecule sits on an inversion center and the molecules within the unit cell adopt quite different orientations. In both phases, examination of the potential C—H...O hydrogen bonds around each of the independent oxygen atoms (one axial and the other equatorial) shows the general O...H patterns to be quite similar with each oxygen atom in contact with four neighboring H atoms, and each H atom contacting two neighboring O atoms. While none of the H...O contacts is particularly short (all are greater than 2.5 Å), each molecule has 32 such contacts that form an extensive intermolecular network. A 1H NMR spectrum of the compound dissolved in DMSO shows a singlet of 8H at δ 3.677 which indicates that the C—H bonds are only moderately polarized by the single adjacent –SO2– moiety: strongly polarized C—H bonds have δ values in the 5–6 range [Li & Sammes (1983). J. Chem. Soc. Perkin Trans. 1, pp. 1303–1309]. The phase 1 crystal studied was non-merohedrally twinned.

Novel hydrogen bonding in crystalline tetra-n-butylammonium salts of catechol halides

1985 ◽  
Vol 63 (8) ◽  
pp. 2119-2122 ◽  
Author(s):  
Masood A. Khan ◽  
Archibald W. McCulloch ◽  
A. Gavin McInnes
Keyword(s):  
Hydrogen Bonding ◽  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Halide Anions ◽  
Cell Dimensions

The crystal structures of [N(n-C4H9)4] [catechol … Cl] (1) and [N(n-C4H9)4] [catechol … Br] (2) have been determined by X-ray analysis which showed that the two structures are isomorphous, with the orthorhombic space group Pbca, Z = 8. The cell dimensions and final R-values are: (1) a = 15.323(2), b = 16.166(2), c = 19.713(2) Å, R = 0.048 for 1361 observed reflections; (2) a = 15.432(1), b = 16.244(2), c = 19.824(1) Å, R = 0.041 for 1958 observed reflections. The crystal structures consist of discrete tetra-n-butylammonium cations and catechol halide anions. Catechol forms two strong hydrogen bonds to a single halide ion giving a pattern of hydrogen bonding unique for such systems.

Crystalline complexes of 18-crown-6 with methyl sulfonates

1993 ◽  
Vol 71 (8) ◽  
pp. 1225-1235 ◽  
Author(s):  
Robert Chênevert ◽  
René Gagnon ◽  
Daniel Chamberland ◽  
Michel Simard
Keyword(s):  
Crystal Structure ◽  
Unit Cell ◽  
Monoclinic System ◽  
Guest Molecules ◽  
Space Group ◽  
Cell Dimensions ◽  
Unit Cell Dimensions ◽  
Crystalline Complexes Of

The macrocyclic polyether 18-crown-6 forms crystalline complexes with methyl sulfonates. Most complexes have a 2:1 (sulfonate:crown) stoichiometry whereas small aliphatic sulfonates give a 1:1 ratio. In the 2:1 ratio complexes, the guest molecules are coordinated above and below the crown in such a way that the dipoles are compensated. In the 1:1 ratio complexes, there is a polymeric type association with the two ends of the sulfonate interacting with different crown molecules. A crystal structure is reported for each type of complex. The complex 18-crown-6•CH3SO3CH3 (7) crystallizes in the monoclinic system, space group P21/c with Z = 4. The unit cell dimensions are as follows: a = 8.525(4), b = 16.401(7), c = 15.071(6) Å, β = 113.92(3)°. Final Rw = 0.064 for 3650 reflections. The complex 18-crown 6•(C6H5SO3Me)2 (1) crystallizes in the monoclinic system, space group P21/c with Z = 2. The unit cell dimensions are as follows: a = 8.101(3), b = 17.136(5), c = 12.990(5) Å, β = 121.30(3)°. Final Rw = 0.048 for 2913 reflections.

Crystal and molecular structure of two C-phenyl pentitol derivatives

1978 ◽  
Vol 56 (23) ◽  
pp. 2915-2921 ◽  
Author(s):  
Douglas C. Rohrer ◽  
Jean-Claude Fischer ◽  
Derek Horton ◽  
Wolfgang Weckerle
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Direct Methods ◽  
Coupling Constants ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Cell Dimensions ◽  
Palladium Catalyzed ◽  
Discrepancy Index

Grignard addition of phenylmagnesium bromide to 3,5-O-benzylidene-1-deoxy-D-erythro-2-pentulose (1) affords C-phenyl branched-chain pentitols having exclusively either the D-arabino (2) or D-ribo (5) stereochemistry according to the mode of substitution of 1. In order to determine the chirality of these products conclusively, the crystal and molecular structure of the unsubstituted pentitol 6 (from 2) has been determined. Crystals of 1-deoxy-2-C-phenyl-D-arabinitol (6; C11H16O4) are orthorhombic, space group P212121, with cell dimensions a = 8.9420(6), b = 18.910(1), c = 6.4263(6) Å, and Z = 4. The structure was solved by multi-solution direct methods and refined to a final discrepancy index of 5.6%. The molecule has an extended, planar zigzag conformation with the phenyl ring nearly perpendicular to this plane. Compound 6 forms one intramolecular (between 2-OH and O-4) and three intermolecular hydrogen bonds. Palladium-catalyzed hydrogenolysis of the 2-phenylcarbamate of 2 results in deoxygenation of the benzylic center with complete-inversion of configuration, as established by crystal-structure determination of the product 7. Crystals of 2(S)-4-O-acetyl-3,5-O-benzylidene-1,2-dideoxy-2-C-phenyl-D-erytro-pentitol (7; C20H22O4) are monoclinic, space group C2, with cell dimensions a = 19.102(1), b = 6.1925(5), c = 16.098(1) Å, β = 108.325(9)°, and Z = 4. The structure was solved by multi-solution direct methods and refined to a final discrepancy index of 5.9%. The molecule has an almost ideal planar, zigzag backbone conformation which incorporates the 1,3-dioxane ring. Comparison of the conformation observed in the crystal with that calculated from proton–proton coupling constants shows good agreement

Crystal and Molecular Structure of 2-Bromo-11-ethyl-5,9-dimethoxytetracyclo[5.4.1.14,12•18,11]tetradecan-3-one, C18H27BrO3

1971 ◽  
Vol 49 (15) ◽  
pp. 2497-2500 ◽  
Author(s):  
R. F. Dunphy ◽  
H. Lynton
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Heavy Atom ◽  
Unit Cell ◽  
Monoclinic System ◽  
Cell Dimensions ◽  
Final Agreement ◽  
Unit Cell Dimensions ◽  
Heavy Atom Method ◽  
Atomic Parameters

The molecular structure of 2-bromo-11-ethyl-5,9-dimethoxytetracyclo[5.4.1.14,12•18,11]tetradecan-3-one, C18H27BrO3, synthesized in an attempt to develop a method of conversion from an advanced relay compound to the alkaloid delphinine, has been determined by the heavy atom method. The compound crystallizes in the monoclinic system, space group P21/c, with unit cell dimensions a = 9.684(9), b = 13.481(15), c = 12.988(14) Å, β = 99.47(7)°, and four molecules in the unit cell. The atomic parameters were refined by block-diagonal least squares using anisotropic thermal parameters. The hydrogen atom positions were established but the parameters were not refined. The final agreement residual for 816 observed reflections is R = 0.044.The stereochemistry of the compound was found to be unsuitable for the delphinine synthesis.

Coordination Chemistry of trans-(NH3)2Pt(II) with Uracil Nucleobases. A Comparison with cis-(NH3)2Pt(II)

1990 ◽  
Vol 45 (6) ◽  
pp. 731-740 ◽  
Author(s):  
Iris Dieter ◽  
Bernhard Lippert ◽  
Helmut Schöllhon ◽  
Ulf Thewalt
Keyword(s):  
Oxidation Products ◽  
Orthorhombic Space Group ◽  
Monoclinic System ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
Cell Dimensions ◽  
Rare Tautomers ◽  
Cis Isomer ◽  
Heteronuclear Complex

Protonated and heteronuclear adducts as well as a series of Pt(IV) oxidation products derived from trans-a2PtL2 (a = NH3, NH2CH3, L = 1-methyluracil anion, C5H5N2O2, or uridine anion, C10HnN2O6) have been prepared and studied by spectroscopic methods and in two cases by X-ray crystallography. trans-(NH3)2Pt(C5H5N2O2)2Ag2(NO3)2H2O · H2O (7) crystallizes in the orthorhombic space group Pna21 with cell dimensions a = 13.206(6), b = 7.238(9), c = 22.051(10) Å, U = 2107.7 Å3, Z = 4. 7 forms a polymeric structure with PtAg2 entities linked via O(4) sites of the 1-methyluracilato ligands. Pt is coordinated through N(3), the Ag centers have a mixed O(2),O(4) coordination, trans,trans,trans-[(NH3)2Pt(OH)2(C5H6N2O2)2](NO3)2 (9) contains two N(3)-bound neutral 1-methyluracil ligands, hence rare tautomers of this model nucleobase. 9 crystallizes in the monoclinic system, space group P21/n with cell dimensions a = 7.098(1), b = 10.395(1), c = 13.295(2) Å, U = 980.4 Å3, Z = 2. While the chemistry leading to Pt(IV) oxidation products from trans-a.2PtL2 is similar to that of the cis-isomer, protonation as well as heteronuclear complex formation of trans-a2PtL2 is more difficult to accomplish than with the cis-isomer. This difference appears to be primarily of steric origin.

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