4-Hydroxy-2-vinyl-2,3,4,5-tetrahydro-1-benzazepine and its 7-fluoro and 7-chloro analogues are isomorphous but not strictly isostructural

2009 ◽  
Vol 65 (3) ◽  
pp. o92-o96 ◽  
Author(s):  
Lina M. Acosta ◽  
Ali Bahsas ◽  
Alirio Palma ◽  
Justo Cobo ◽  
Michael B. Hursthouse ◽  
...  
Keyword(s):  
Hydrogen Bond ◽  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Intermolecular Interactions ◽  
Unit Cell ◽  
Cell Dimensions ◽  
Sufficient Variation ◽  
Unit Cell Dimensions ◽  
Atomic Coordinates

4-Hydroxy-2-vinyl-2,3,4,5-tetrahydro-1-benzazepine, C12H15NO, (I), and its 7-fluoro and 7-chloro analogues, namely 7-fluoro-4-hydroxy-2-vinyl-2,3,4,5-tetrahydro-1-benzazepine, C12H14FNO, (II), and 7-chloro-4-hydroxy-2-vinyl-2,3,4,5-tetrahydro-1-benzazepine, C12H14ClNO, (III), are isomorphous, but with variations in the unit-cell dimensions which preclude in compound (III) one of the weaker intermolecular interactions found in compounds (I) and (II). Thus the compounds are not strictly isostructural in terms of the structurally significant intermolecular interactions, although the corresponding atomic coordinates are very similar. The azepine rings adopt chair conformations. The molecules are linked by a combination of N—H...O and O—H...N hydrogen bonds into chains of edge-fusedR33(10) rings, which in compounds (I) and (II) are further linked into sheets by a single C—H...π(arene) hydrogen bond. The significance of this study lies in its observation of isomorphism in compounds (I)–(III), and its observation of a sufficient variation in one of the cell dimensions effectively to alter the range of significant hydrogen bonds present in the crystal structures.

(2RS,4RS)-7-Fluoro-2-(2-phenylethyl)-2,3,4,5-tetrahydro-1H-1,4-epoxy-1-benzazepine and (2RS,4RS)-7-chloro-2-(2-phenylethyl)-2,3,4,5-tetrahydro-1H-1,4-epoxy-1-benzazepine are isomorphous but not strictly isostructural

2012 ◽  
Vol 68 (5) ◽  
pp. o195-o198 ◽  
Author(s):  
Maria C. Blanco ◽  
Alirio Palma ◽  
Justo Cobo ◽  
Christopher Glidewell
Keyword(s):  
Hydrogen Bonds ◽  
Intermolecular Interactions ◽  
Unit Cell ◽  
Molecular Conformations ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

(2RS,4RS)-7-Fluoro-2-(2-phenylethyl)-2,3,4,5-tetrahydro-1H-1,4-epoxy-1-benzazepine, C18H18FNO, (I), and (2RS,4RS)-7-chloro-2-(2-phenylethyl)-2,3,4,5-tetrahydro-1H-1,4-epoxy-1-benzazepine, C18H18ClNO, (II), are isomorphous but not strictly isostructural, as the slight differences in the unit-cell dimensions and molecular conformations are sufficient to preclude, in the structure of (I), the direction-specific intermolecular interactions present in the structure of (II), where the molecules are linked into sheets by a combination of C—H...N and C—H...π(arene) hydrogen bonds.

scholarly journals The crystal structures of two polyamides (‘nylons’)

1947 ◽  
Vol 189 (1016) ◽  
pp. 39-68 ◽  
Keyword(s):  
Crystal Structures ◽  
Unit Cell ◽  
Chain Molecule ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cell Dimensions ◽  
C Fibre ◽  
Diffraction Patterns ◽  
Unit Cell Dimensions ◽  
Crystalline Forms

Detailed interpretations of the X -ray diffraction patterns of fibres and sheets of 66 and 6.10 polyamides (polyhexam ethylene adipamide and sebacamide respectively) are proposed. The crystal structures of the two substances are completely analogous. Fibres of these two polyam ides usually contain two different crystalline forms, α and β, which are different packings of geometrically similar molecules; most fibres consist chiefly of the α form. In the case of the 66 polymer, fibres have been obtained in which there is no detectable proportion of the β form. Unit cell dimensions and the indices of reflexions for the α form were determined by trial, using normal fibre photographs, and were checked by using doubly oriented sheets set at different angles to the X -ray beam. The unit cell of the a form is triclinic, with a — 4·9 A, b = 5·4 A, c (fibre axis) = 17·2A, α = 48 1/2º, β = 77º, γ = 63 1/2º for the 66 polymer; a = 4·95A, b = 5·4A, c (fibre axes) = 22·4A, α = 49º, β = 76 1/2º, γ = 63 1/2º for the 6.10 polymer. One chain molecule passes through the cell in both cases. Atomic coordinates in occrystals were determined by interpretation of the relative intensities of the reflexions. The chains are planar or very nearly so; the oxygen atoms appear to lie a little off the plane of the chain. The molecules are linked by hydrogen bonds between C = 0 and NH groups, to form sheets. A simple packing of these sheets of molecules gives the α arrangement.

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.

Short-range order, thermal vibration and expansion, and other properties of pseudosymmetric and mixed crystals of small organic molecules - Mixed crystals of phenzaine and n -oxyphenazine: refinement of crystal structures

1970 ◽  
Vol 266 (1180) ◽  
pp. 593-622 ◽  
Keyword(s):  
Unit Cell ◽  
Mixed Crystals ◽  
X Ray Diffraction ◽  
Small Organic Molecules ◽  
Anisotropic Temperature ◽  
Cell Dimensions ◽  
Average Unit ◽  
Unit Cell Dimensions ◽  
Temperature Factors ◽  
Atomic Coordinates

Compositions (accurate to about 1%) of mixed crystals of phenazine (P) and N -oxyphenazine (NOP) were determined from their u.v. absorption spectra. Densities, habit and unit-cell dimensions were found at 20 °C for crystals containing respectively 0, 8, 52, 81 and 100 mole % NOP relative to P; and X-ray diffraction data (F obs ) were obtained for all these and also at — 90 °C for NOP. All are isostructural (NOP being pseudocentrosymmetric) in P2 1 / a with two molecules per average unit cell. Atomic coordinates, bond lengths and anisotropic temperature factors are listed, site-occupation factors for the oxygen atoms being used for the 8, 52 and 81 mole % compositions. A qualitative explanation, in terms of structure, is offered for the anisotropic thermal expansion of NOP.

scholarly journals Isomorphous Crystals Formed by the Similar Supramolecular Motifs in Sorafenib Hydrochloride and Regorafenib Hydrochloride Salts

Crystals ◽  
2019 ◽  
Vol 9 (12) ◽  
pp. 649 ◽  
Author(s):  
Chi Uyen Phan ◽  
Jie Shen ◽  
Jiyong Liu ◽  
Jianming Mao ◽  
Xiurong Hu ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Crystal Structures ◽  
Pyridinium Cation ◽  
Supramolecular Motifs ◽  
Solubility Profile ◽  
Cell Dimensions ◽  
Unit Cell Dimensions ◽  
Similar Unit ◽  
Similar Crystal Structure

Sorafenib and regorafenib (or fluoro-sorafenib) are multikinase inhibitors active in the treatment of various human cancers, but their solubilities are very poor. To improve their solubilities, in this study, sorafenib hydrochloride (Sor·HCl, I) and regorafenib hydrochloride (Reg·HCl, II) have been prepared and their crystal structures were characterized. Their solubility properties in water were evaluated. Intriguingly, they are isomorphous crystal structures with the same space group and the similar unit cell dimensions, which were caused by the similar supramolecular patterns resulted by the formation of N–H···Cl− hydrogen bond instead of hydrogen bond between the protonated pyridinium cation and counterion. Moreover, the solubility properties displayed identical profiles. It may be concluded that a similar crystal structure leads to a comparable solubility profile.

Structures of three inclusion compounds of cholanamide with either (S)-enantiomer, (R)-enantiomer or an optically resolved mixture of butan-2-ol

1996 ◽  
Vol 52 (4) ◽  
pp. 728-733 ◽  
Author(s):  
P. Briozzo ◽  
T. Kondo ◽  
K. Sada ◽  
M. Miyata ◽  
K. Miki
Keyword(s):  
Crystal Structures ◽  
Inclusion Compounds ◽  
Unit Cell Volume ◽  
Optical Resolution ◽  
Unit Cell ◽  
Molar Ratio ◽  
Hydrogen Bond Network ◽  
Cell Dimensions ◽  
Bond Network ◽  
Unit Cell Dimensions

The three types of inclusion compounds of cholanamide (CAM, 3α, 7α, 12α-trihydroxy-5β-cholan-24-amide) have been crystallized from the solutions of (S)-butan-2-ol (CAMSB), (R)-butan-2-ol (CAMRB) and racemic butan-2-ol (CAMSRB), respectively. The crystal structures have been determined. The three crystal structures are isomorphous to each other and revealed that the host CAM molecules form the same layered arrangements, providing channel spaces for the guest butan-2-ol molecules. As expected, the CAMSB and CAMRB crystals include the pure (S)- and (R)-enantiomers of butan-2-ol, whereas the (S)-enriched mixture of enantiomers is accommodated in CAMSRB with a molar ratio between the host CAM and guest butan-2-ol molecules of 1:1. The hydrogen-bond network is rigidly formed between the CAM molecules and also between CAM and butan-2-ol molecules. CAMSB and CAMRB have slightly different unit-cell dimensions: the channels in CAMRB have a larger section, resulting in a larger unit-cell volume. In CAMSRB, although both enantiomers of the guest alcohol are included, the (S)-enantiomer is more abundant, indicating that the optical resolution occurs during the crystallization step.

THE CRYSTAL STRUCTURES OF SOME INTERMETALLIC COMPOUNDS OF PLUTONIUM

1956 ◽  
Vol 34 (2) ◽  
pp. 133-145 ◽  
Author(s):  
O. J. C. Runnalls
Keyword(s):  
Crystal Structures ◽  
Intermetallic Compounds ◽  
Unit Cell ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

The crystal structures of the following binary intermetallic compounds of plutonium are reported: PuAl2, PuAl3, PuAl4, PuBe13, PuCo2, PuFe2, PuMn2, PuNi2, PuNi5, and Pu2Ni17. In addition, the unit cell dimensions are reported for PuAg3.

Notizen: Refinement of the Crystal Structures of CuTe2Br and CuTe2I

1989 ◽  
Vol 44 (8) ◽  
pp. 990-992 ◽  
Author(s):  
Wolfgang Milius
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Unit Cell ◽  
Lattice Parameters ◽  
Crystal Data ◽  
Space Group ◽  
Cell Dimensions ◽  
Unit Cell Dimensions

The crystal structures of CuTe2Br and CuTe2I have been refined on the basis of single crystal data. Both compounds crystallize monoclinically in space group P21/c. The structures are isotypic with that of CuTe2Cl. The lattice parameters of CuTe2Br are a = 834.5(8) pm, b = 492.8(4) pm, c = 1573.3(5) pm and β = 135.3(2)°. The unit cell dimensions of CuTe2I are a = 866.5(8) pm, b = 491.4(4) pm, c = 1649.6(3) pm and β = 135.1(2)°.

Die Kristall- und Molekülstrukturen von π-C7Η7Μο(CO)2Cl und π-C7H7Mo(CO)2Br / The Crystal Structures of π-C7Η7Μο(CO)2Cl and π-C7H7Mo(CO)2Br

1975 ◽  
Vol 30 (1-2) ◽  
pp. 26-29 ◽  
Author(s):  
M. L. Ziegler ◽  
H. E. Sasse ◽  
B. Nuber
Keyword(s):  
Least Squares ◽  
Crystal Structures ◽  
Three Dimensional ◽  
Unit Cell ◽  
Fourier Methods ◽  
X Ray ◽  
Cell Dimensions ◽  
Unit Cell Dimensions ◽  
Group D ◽  
Chlorine Bond

The structures of the title compounds have been determined from three dimensional X-ray data by Patterson and Fourier methods. The crystals of both are orthorombic with the space group D42-P 212121. The chloride (2) and the bromide (3) are isomorphous, they have unit cell dimensions a = 642,76 pm, b =1187,27 pm, c =1311,14 pm (2) and 644,59 pm, 1183,78 pm, c = 1321,83 pm (3) and Z = 4. Least squares refinement by use of 1179 (2) and 1037 (3) independent reflections measured on a diffractometer has reached R = 12,5% and R = 7,4% respectively. The molybdenum-bromine bond in 3 is relatively shorter than the molybdenum-chlorine bond in 2, due to greater dπ-dπ interaction.

The External Shape of Human γ GI Immunoglobulin from Crystal Sections

1971 ◽  
Vol 29 ◽  
pp. 428-429
Author(s):  
L. W. Labaw
Keyword(s):  
Molecular Weight ◽  
Sodium Phosphate ◽  
Osmium Tetroxide ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
X Ray ◽  
Large Molecular Weight ◽  
Cell Dimensions ◽  
Unit Cell Dimensions ◽  
Crystallographic Axes

Crystals of a human γGl immunoglobulin have the external morphology of diamond shaped prisms. X-ray studies have shown them to be monoclinic, space group C2, with 2 molecules per unit cell. The unit cell dimensions are a = 194.1, b = 91.7, c = 51.6Å, 8 = 102°. The relatively large molecular weight of 151,000 and these unit cell dimensions made this a promising crystal to study in the EM.Crystals similar to those used in the x-ray studies were fixed at 5°C for three weeks in a solution of mother liquor containing 5 x 10-5M sodium phosphate, pH 7.0, and 0.03% glutaraldehyde. They were postfixed with 1% osmium tetroxide for 15 min. and embedded in Maraglas the usual way. Sections were cut perpendicular to the three crystallographic axes. Such a section cut with its plane perpendicular to the z direction is shown in Fig. 1.This projection of the crystal in the z direction shows periodicities in at least four different directions but these are only seen clearly by sighting obliquely along the micrograph.

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