scholarly journals Crystal structures and Hirshfeld surface analyses of bis(4,5-dihydrofuran-2-yl)dimethylsilane and (4,5-dihydrofuran-2-yl)(methyl)diphenylsilane

2022 ◽  
Vol 78 (1) ◽  
Author(s):  
Annika Schmidt ◽  
Anna Krupp ◽  
Eva Rebecca Barth ◽  
Carsten Strohmann
Keyword(s):  
Crystal Structures ◽  
Building Blocks ◽  
Hirshfeld Surface ◽  
Polymeric Chain ◽  
Triclinic Crystal System ◽  
Space Group ◽  
Axis Direction ◽  
Crystal System ◽  
Hirshfeld Surfaces ◽  
Interconnected Structure

The title compounds, C10H16O2Si (1) and C17H18OSi (2), are classified as dihydrofurylsilanes, which show great potential as building blocks for various functionalized silanes. They both crystallize in the space group P\overline{1} in the triclinic crystal system. Analyses of the Hirshfeld surfaces show packing-determining interactions for both compounds, resulting in a polymeric chain along the [011] for silane 1 and a layered-interconnected structure along the b-axis direction for silane 2.

scholarly journals Crystal Structure, Spectral Studies, and Hirshfeld Surfaces Analysis of 5-Methyl-5H-dibenzo[b,f]azepine and 5-(4-Methylbenzyl)-5H-dibenzo[b,f]azepine

2014 ◽  
Vol 2014 ◽  
pp. 1-9
Author(s):  
Madan Kumar Shankar ◽  
Basavapattana C. Manjunath ◽  
Koravangala Shivakumar Vinay Kumar ◽  
Kudigana J. Pampa ◽  
Marilinganadoddi P. Sadashiva ◽  
...  
Keyword(s):  
Diffraction Method ◽  
Spectral Studies ◽  
Boat Conformation ◽  
Orthorhombic Crystal System ◽  
Orthorhombic Crystal ◽  
Space Group ◽  
Cell Parameters ◽  
Crystal System ◽  
Hirshfeld Surfaces ◽  
Short Contacts

The compounds, 5-methyl-5H-dibenzo[b,f]azepine (1) and 5-(4-methylbenzyl)-5H-dibenzo[b,f]azepine (2), were synthesized and characterized by spectral studies, and finally confirmed by single crystal X-ray diffraction method. The compound 1 crystallizes in the orthorhombic crystal system in Pca21 space group, having cell parameters a=11.5681 (18) Å, b=11.8958 (18) Å, c=8.0342 (13) Å, and Z=4 and V=1105.6 (3) Å3. And the compound 2 crystallizes in the orthorhombic crystal system and space group Pbca, with cell parameters a=16.5858 (5) Å, b=8.4947 (2) Å, c=23.1733 (7) Å, and Z=8 and V=3264.92 (16) Å3. The azepine ring of both molecules 1 and 2 adopts boat conformation with nitrogen atom showing maximum deviations of 0.483 (2) Å and 0.5025 (10) Å, respectively. The C–H⋯π short contacts were observed. The dihedral angle between fused benzene rings to the azepine motif is 47.1 (2)° for compound 1 and 52.59 (6)° for compound 2, respectively. The short contacts were analyzed and Hirshfeld surfaces computational method for both molecules revealed that the major contribution is from C⋯H and H⋯H intercontacts.

Investigation of the crystal structures and Hirshfeld surfaces of three closely related N-(2-fluorobenzoyl)-arylsulfonamides

2016 ◽  
Vol 231 (6) ◽  
Author(s):  
Parameshwar Adimule Suchetan ◽  
Gundagallu Madanagopala Reddy Supriya ◽  
Kalavala Shivaprakash Srivishnu ◽  
Hanumanahalli Nagaraju Lakshmikantha ◽  
Shivalingegowda Naveen ◽  
...  
Keyword(s):  
Crystal Structures ◽  
Three Dimensional ◽  
Hirshfeld Surface ◽  
Compound I ◽  
One Dimensional ◽  
Π Interactions ◽  
Hirshfeld Surfaces ◽  
3D Network ◽  
2D Arrays ◽  
2D Network

AbstractThe investigation of the crystal structures of three closely related sulfonamides, namely N-(2-fluorobenzoyl)-2-methylbenzenesulfonamide (I), N-(2-fluorobenzoyl)-4-methylbenzenesulfonamide (II) and N-(2-fluorobenzoyl)-2-chlorobenzenesulfonamide (III) by analysing intermolecular interactions and the packing patterns, and also by Hirshfeld surface analyses is presented. Compound (I) has a three-dimensional (3D) network, in which N–H···O and C–H···F chains build up two-dimensional (2D) arrays, which are extended into a 3D network through C–H···π interactions. In (II), alternating N–H···O and C–H···O rings form one-dimensional (1D) ribbons, which are interconnected by C–H···π interactions to build a 2D network. In (III), 2D sheets comprising N–H···O rings, C–H···π chains, Cl···F and F···F contacts are stacked by π···π interactions to form a 3D network. Hirshfeld surface analyses, comprising d

Understanding metal–ligand interactions in coordination polymers using Hirshfeld surface analysis

2019 ◽  
Vol 75 (6) ◽  
pp. 707-716 ◽  
Author(s):  
Camila B. Pinto ◽  
Leonardo H. R. Dos Santos ◽  
Bernardo L. Rodrigues
Keyword(s):  
Surface Analysis ◽  
Coordination Polymers ◽  
Building Blocks ◽  
Shape Index ◽  
Hirshfeld Surface ◽  
Hirshfeld Surface Analysis ◽  
Joint Analysis ◽  
Hirshfeld Surfaces ◽  
Ligand Interactions ◽  
Metal Ligand

Properties related to the size and shape of Hirshfeld surfaces provide insight into the nature and strength of interactions among the building blocks of molecular crystals. In this work, we demonstrate that functions derived from the curvatures of the surface at a point, namely, shape index (S) and curvedness (C), as well as the distances from the surface to the nearest external (d e) and internal (d i) nuclei, can be used to help understand metal–ligand interactions in coordination polymers. The crystal structure of catena-poly[[[(1,10-phenanthroline-κ2 N,N′)copper(II)]-μ-4-nitrophthalato-κ2 O 1:O 2] trihydrate], {[Cu(C8H3NO6)(C12H8N2)]·3H2O} n , described here for the first time, was used as a prototypical system for our analysis. Decomposition of the coordination polymer into its metal centre and ligand molecules followed by joint analysis of the Hirshfeld surfaces generated for each part unveil qualitative and semi-quantitative information that cannot be easily obtained either from conventional crystal packing analysis or from Hirshfeld surface analysis of the entire polymeric units. The shape index function S is particularly sensitive to the coordination details and its mapping on the surface of the metallic centre is highly dependent on the nature of the ligand and the coordination bond distance. Correlations are established between the shape of the Hirshfeld surface of the metal and the geometry of the metal–ligand contacts in the crystals. This could be applied not only to estimate limiting coordination distances in metal–organic compounds, but also to help establish structure–property relationships potentially useful for the crystal engineering of such materials.

scholarly journals Crystal Structures, Hirshfeld Surfaces, and Thermal Study of Isostructural Polymeric Ladders of La(III) and Sm(III) Coordination Compounds with 4,4’-Bipyridine and Dibromoacetates

Materials ◽  
2020 ◽  
Vol 13 (19) ◽  
pp. 4274
Author(s):  
Agnieszka Czylkowska ◽  
Anna Pietrzak ◽  
Małgorzata Szczesio ◽  
Bartłomiej Rogalewicz ◽  
Jakub Wojciechowski
Keyword(s):  
Crystal Structures ◽  
Coordination Compounds ◽  
Central Atom ◽  
Thermal Study ◽  
Hirshfeld Surface ◽  
Mixed Ligand ◽  
Enrichment Ratio ◽  
X Ray Diffraction ◽  
X Ray ◽  
Hirshfeld Surfaces

Two novel mixed ligand complexes with general formula [M2(4,4′-bpy)1.5(CBr2HCOO)6(H2O)2]n (where 4,4′-bpy = 4,4′-bipyridine) were synthesized. Thermal analysis was used to describe a solid intermediate and final products of thermolysis. A coupled TG-MS system was used to monitor principal volatile fragments evolved during pyrolysis. Crystal structures of the complexes were determined. Cationic dinuclear M2 (M(III) = La, Sm) coordination cores were obtained. Both crystal structures are isostructural. Single crystal X-ray diffraction analysis revealed that investigated structures of 1D coordination polymers assembled in ladder-like systems. The central atom replacement resulted in unit cell identity parameter П = 0.0091. Additionally, the isostructurality of the reported La(III) and Sm(III) complexes was revealed using Hirshfeld Surface analysis supported by Enrichment Ratio calculations.

Crystal structures and Hirshfeld surface analyses of a des-A-B-aromatic steroidal compound, and two of its derivatives, having a trans-2,3,4,5-tetrahydro-3a-methyl-7-methoxybenz[e]indane skeleton – structural comparisons with reported tetrahydrobenz[e]indene derivatives

2019 ◽  
Vol 74 (9) ◽  
pp. 649-663
Author(s):  
Ligia R. Gomes ◽  
John N. Low ◽  
Alan B. Turner ◽  
Alexander W. Nowicki ◽  
Thomas C. Baddeley ◽  
...  
Keyword(s):  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Intermolecular Interactions ◽  
Hirshfeld Surface ◽  
Dimensional Structure ◽  
Monoclinic Space Group ◽  
Asymmetric Unit ◽  
Space Group ◽  
Π Interactions ◽  
Independent Molecules

AbstractThe crystal structures and Hirshfeld surface analyses of the des-A-B-aromatic steroid derivative, (3a,9b)-1,2,3a,4,5,9b-hexahydro-7-methoxy-3a-methyl-3H-benz[e]-inden-3-one (or 5-methoxy-des-A-estra-5,7,9-triene-17-one) 1, its acetohydrazide derivative, 2, and its hydrazone derivative, 3, are reported. All three compounds crystallize in chiral space groups: compounds 1 and 2 in the orthorhombic space group P212121 each with one molecule in the asymmetric unit, and compound 3 in the monoclinic space group P21 with two similar but independent molecules, Mol A and Mol B, in the asymmetric unit. Both the five-membered and six-membered non-aromatic rings in all three compounds have envelope or near envelope shapes. In compounds 2 and 3 the N=N units have (E)-arrangements. The intermolecular interactions in crystals of compound 1 are C–H · · · O hydrogen bonds and C–H · · · π interactions, in compound 2 N–H · · · O and C–H · · · O hydrogen bonds and C–H · · · π interactions are present, while in compound 3 there are just C–H · · · π interactions. An important substructure in 1 is a sheet of molecules, composed of ${\rm{R}}_6^6(44)$ rings, formed from C–H · · · O(methoxy) and C–H · · · O(carbonyl) hydrogen bonds, the molecules of which form columns linked via the B and D rings, i.e. in a head-to-tail fashion. Compound 2 is an acylhydrazonyl compound, in which the two independent molecules are linked into asymmetric dimers via strong classical N–H · · · O hydrogen bonds, with the formation of ${\rm{R}}_2^2(8)$ rings. In both 1 and 2, further intermolecular interactions result in 3-dimensional structures, while compound 3 has a 1-dimensional structure arising from C–H · · · O interactions generating spiral chains. The results have been compared with existing data.

Preparation and Crystal Structures of the Isotypic Compounds CdXO4 · 2 HgO (X = S, Se)

2004 ◽  
Vol 59 (3) ◽  
pp. 281-285 ◽  
Author(s):  
Matthias Weil
Keyword(s):  
Single Crystals ◽  
Crystal Structures ◽  
Diffraction Data ◽  
Building Blocks ◽  
Data Sets ◽  
X Ray Diffraction ◽  
Hydrothermal Conditions ◽  
Space Group ◽  
X Ray ◽  
Structure Factors

Colourless single crystals of the compounds CdXO4 · 2 HgO (X = S, Se) were obtained under hydrothermal conditions (250 °C, 5 d), starting from stoichiometric amounts of HgO, CdSO4 ·7H2O and CdSeO4 ·2H2O, respectively. The crystal structures were determined from X-ray diffraction data sets. The CdXO4 · 2HgO compounds crystallise isotypically with two formula units in space group P1̅ (# 2) [CdSO4 · 2HgO (CdSeO4 · 2HgO): a = 6.793(2) (6.9097(5)) Å , b = 7.205(2) (7.1786(6)) Å , c=7.359(2) (7.4556(6)) Å ,α =73.224(6) (74.586(2))°, β =66.505(6) (68.229(1))°, γ =63.054(5) (63.886(1))°, 1670 (1786) structure factors, 92 parameters, R[F2 > 2σ(F2)] = 0.0379 (0.0244)] and are made up from zig-zag [O-Hg-O]∞ chains with very short bonds of d̅(Hg-O) 2.025 Å , distorted [CdO6] octahedra (d̅(Cd-O)= 2.297 Å ), and XO4 tetrahedra (d̅(S-O)= 1.458 Å , d̅(Se-O)= 1.633 Å ) as the main building blocks. The CdXO4 ·2HgO compounds reveal no structural relationship with the corresponding HgXO4 ·2HgO phases

Effect of Meta-Substitution on Solid State Geometry of N-(Aryl)-2,2,2-trichloro-acetamides, 3-XC6H4NH-CO-CCl3 and 3,5-X2C6H3NH-CO-CCl3 (X = Cl, CH3)

2007 ◽  
Vol 62 (1-2) ◽  
pp. 91-100
Author(s):  
Basavalinganadoddy Thimme Gowda ◽  
Jozef Kožíšek ◽  
Ingrid Svoboda ◽  
Hartmut Fuess
Keyword(s):  
Solid State ◽  
Crystal Structures ◽  
Nitro Group ◽  
Room Temperature ◽  
Asymmetric Unit ◽  
Strong Electron ◽  
Space Group ◽  
Lattice Constants ◽  
Crystal System ◽  
Electron Withdrawing Group

The crystal structures of N-(meta-substituted phenyl)-2,2,2-trichloro-acetamides such as N- (3-methylphenyl)-2,2,2-trichloro-acetamide, 3-CH3C6H4NH-CO-CCl3 (3MPTCA); N-(3-chlorophenyl)- 2,2,2-trichloro-acetamide, 3-ClC6H4NH-CO-CCl3 (3CPTCA); N-(3,5-dimethylphenyl)- 2,2,2-trichloro-acetamide, 3,5-(CH3)2C6H3NH-CO-CCl3 (35DMPTCA) and N-(3,5-dichlorophenyl)- 2,2,2-trichloro-acetamide, 3,5-Cl2C6H3NH-CO-CCl3 (35DCPTCA) have been determined at room temperature. The crystal system, space group, formula units and lattice constants (Å ) of the new structures are: 3MPTCA: orthorhombic, Pbca, Z = 8, a = 12.3199(11), b = 8.9719(8), c = 20.2058(15); 3CPTCA: orthorhombic, Fdd2, Z =16, a=19.285(4), b=40.765(8), c=5.5920(11); 35DMPTCA: triclinic, P1̄, Z = 2, a = 8.994(4), b = 9.9890(10), c = 14.760(5), α = 79.56(2)°, β = 73.32(3)°, γ = 86.47(2)°; and 35DCPTCA: orthorhombic, Pbca, Z = 8, a = 22.485(5), b=10.738(2), c=10.028(3). The compound 35DMPTCA has two molecules in its asymmetric unit, similar to o-NO2-, m-NO2- and p-CH3-substituted phenyl-trichloro-acetamides, while 3MPTCA, 3CPTCA and 35DCPTCA have one molecule each in their asymmetric units. The analysis of data indicates that the substitution of a strong electron withdrawing group such as a nitro group into PTCA at ortho or meta positions has a significant effect on the crystal parameters.

scholarly journals Crystal structures of two (±)-exo-N-isobornylacetamides

2015 ◽  
Vol 71 (10) ◽  
pp. 1117-1120 ◽  
Author(s):  
Dmitrijs Stepanovs ◽  
Daniels Posevins ◽  
Maris Turks
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Asymmetric Unit ◽  
Double Chain ◽  
Space Group ◽  
Axis Direction ◽  
Independent Molecules

The title compounds consist of a bornane skeleton with attached acetamide, C12H21NO (±)-(1) {systematic name: (±)-N-[(1RS,2RS,4RS)-1,7,7-trimethylbicyclo[2.2.1]heptan-2-yl]acetamide}, and chloroacetamide, C12H20ClNO (±)-(2) {systematic name: (±)-2-chloro-N-[(1RS,2RS,4RS)-1,7,7-trimethylbicyclo[2.2.1]heptan-2-yl]acetamide}, functionalities to the 2-exo-position. The crystal structure of the first monoclinic polymorph of (±)-(1) has been reported previously [Unget al.(2014).Monatsh. Chem.145, 983–992]. Compound (±)-(1) crystallizes in the space groupP21/nwith two independent molecules in the asymmetric unit, in contrast to the above-mentioned polymorph which crystallized in the space groupC2/cwith one molecule in the asymmetric unit. In the title compounds, the bicyclic bornane moieties have normal geometries. In the crystals of both compounds, molecules are linked by N—H...O hydrogen bonds, reinforced by C—H...O contacts, formingtrans-amide chains propagating along thea-axis direction. In the case of compound (±)-(1), neighbouring chains are linked by further C—H...O contacts, forming double-chain ribbons along [100].

scholarly journals The Crystal Structure of Zineb, 75 years later

2019 ◽  
Author(s):  
Jonathan B Lefton ◽  
Kyle B Pekar ◽  
Tomce Runcevski
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
20Th Century ◽  
Thermal Characteristics ◽  
Structural Features ◽  
Inversion Symmetry ◽  
Triclinic Crystal System ◽  
Space Group ◽  
Crystal System ◽  
Short Summary

Ethylene bis(dithiocarbamates) (EBDTCs) have been used as staple fungicides for over 75 years. The first industrially manufactured EBDTC was zineb, zinc ethylene bis(dithiocarbamate), marketed under the tradename Dithane. Even though zineb has been used as a fungicide since the 1940s, its crystal structure remained unknown. Herein, we describe the crystal structure of zineb (triclinic crystal system, space group P–1, a = 7.5094(9) Å, b = 9.4356(9) Å, c = 7.4120(7) Å, α = 107.945(8) °, β = 100.989(7) °, γ = 105.365(8) °, V = 460.07(10) Å3). The inorganic fragment of the structure consists of two Zn2+ cations, coordinated by the thiocarbamate group. There are four Zn–S bonds with lengths in the range of 2.325 – 2.426 Å, and one rather long Zn–S contact of 2.925(8) Å. Inorganic fragments are linked by organic EBDTC ligands to form extended, polymeric layers. The layers are packed in a ABAB manner, related by the inversion symmetry and held together by hydrogen bonding network. In this article, in addition to describing the crystal structure, we correlate the structural features with the vibrational spectroscopic and thermal characteristics of zineb, and we provide a short summary of the major developments of fungicides in the 20th century<br>

scholarly journals Synthesis, Crystal Structures, and Molecular Properties of Three Nitro-Substituted Chalcones

Crystals ◽  
2021 ◽  
Vol 11 (12) ◽  
pp. 1589
Author(s):  
Alam Yair Hidalgo ◽  
Manuel Velasco ◽  
Eduardo Sánchez-Lara ◽  
Abraham Gómez-Rivera ◽  
Miguel A. Vilchis-Reyes ◽  
...  
Keyword(s):  
Crystal Structures ◽  
Functional Groups ◽  
Direct Effect ◽  
Crystal Packing ◽  
Hirshfeld Surface ◽  
Stacking Interactions ◽  
Orthorhombic Space Group ◽  
Trans Conformation ◽  
Space Group ◽  
X Ray

Three functionalized chalcones containing combinations of nitro functional groups have been synthesized via Claisen-Schmidt condensation between 2-nitroacetophenone and nitrobenzaldehyde, and the crystal structures obtained ((E)-1,3-bis(2-nitrophenyl)prop-2-en-1-one, 1a, (E)-1-(2-nitrophenyl)-3-(3-nitrophenyl)prop-2-en-1-one, 1b and (E)-1-(2-nitrophenyl)-3-(4-nitrophenyl)prop-2-en-1-one, 1c), C15H10N2O5, are reported. Compounds 1a and 1c crystallized in the triclinic centrosymmetric space group P1¯, whereas compound 1b crystallized in the orthorhombic space group Pbca. The X-ray analysis reveals that structures 1a and 1b exhibits s-trans conformation, whereas structure 1c exists in s-cis conformation, concerning the olefinic double bonds. In addition, the results show that the position of the nitro substituent attached to the aromatic B-ring has a direct effect on the molecular coplanarity of these compounds. The Hirshfeld surface analysis suggests that the non-covalent π-π stacking interactions are the most important contributors for the crystal packing of 1a and 1b. In 1c, the crystal packing is mainly stabilized by weak intermolecular C―H···O interactions due to the planar nature of the molecule.

Sign in / Sign up

Export Citation Format

Share Document