Adamantane derivatives of sulfonamide molecular crystals: structure, sublimation thermodynamic characteristics, molecular packing, and hydrogen bond networks

CrystEngComm ◽  
2015 ◽  
Vol 17 (4) ◽  
pp. 753-763 ◽  
Author(s):  
German L. Perlovich ◽  
Alex M. Ryzhakov ◽  
Valery V. Tkachev ◽  
Alexey N. Proshin
Keyword(s):  
Hydrogen Bond ◽  
Crystal Structures ◽  
Molecular Crystals ◽  
Thermodynamic Characteristics ◽  
Molecular Packing ◽  
Adamantane Derivatives ◽  
X Ray Diffraction ◽  
X Ray ◽  
Hydrogen Bond Networks ◽  
Derivatives Of

The crystal structures of six adamantane derivatives of sulfonamides have been determined by X-ray diffraction and their sublimation and fusion processes have been studied.

scholarly journals Disordered sodium alkoxides from powder data: crystal structures of sodium ethoxide, propoxide, butoxide and pentoxide, and some of their solvates

2021 ◽  
Vol 77 (1) ◽  
pp. 68-82
Author(s):  
Maurice Beske ◽  
Stephanie Cronje ◽  
Martin U. Schmidt ◽  
Lukas Tapmeyer
Keyword(s):  
Hydrogen Bond ◽  
Crystal Structures ◽  
Sodium Ethoxide ◽  
Amyl Alcohol ◽  
X Ray Diffraction ◽  
Oh Groups ◽  
Space Group ◽  
X Ray ◽  
Alkyl Groups ◽  
Hydrogen Bond Networks

The crystal structures of sodium ethoxide (sodium ethanolate, NaOEt), sodium n-propoxide (sodium n-propanolate, NaO n Pr), sodium n-butoxide (sodium n-butanolate, NaO n Bu) and sodium n-pentoxide (sodium n-amylate, NaO n Am) were determined from powder X-ray diffraction data. NaOEt crystallizes in space group P 421 m, with Z = 2, and the other alkoxides crystallize in P4/nmm, with Z = 2. To resolve space-group ambiguities, a Bärnighausen tree was set up, and Rietveld refinements were performed with different models. In all structures, the Na and O atoms form a quadratic net, with the alkyl groups pointing outwards on both sides (anti-PbO type). The alkyl groups are disordered. The disorder becomes even more pronounced with increasing chain length. Recrystallization from the corresponding alcohols yielded four sodium alkoxide solvates: sodium ethoxide ethanol disolvate (NaOEt·2EtOH), sodium n-propoxide n-propanol disolvate (NaO n Pr·2 n PrOH), sodium isopropoxide isopropanol pentasolvate (NaO i Pr·5 i PrOH) and sodium tert-amylate tert-amyl alcohol monosolvate (NaO t Am· t AmOH, t Am = 2-methyl-2-butyl). Their crystal structures were determined by single-crystal X-ray diffraction. All these solvates form chain structures consisting of Na+, –O− and –OH groups, encased by alkyl groups. The hydrogen-bond networks diverge widely among the solvate structures. The hydrogen-bond topology of the i PrOH network in NaO i Pr·5 i PrOH shows branched hydrogen bonds and differs considerably from the networks in pure crystalline i PrOH.

Phase behaviour and crystal structures of 2′,3′-difluorinated p-terphenyl derivatives

2021 ◽  
Vol 77 (7) ◽  
Author(s):  
Sakuntala Gupta ◽  
Partha Pratim Das ◽  
Przemysław Kula ◽  
Emmanuele Parisi ◽  
Roberto Centore
Keyword(s):  
Crystal Structures ◽  
Crystal Packing ◽  
Phase Behaviour ◽  
Dsc Analysis ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Space Group ◽  
X Ray ◽  
Independent Molecules ◽  
Derivatives Of

The crystal structures of difluorine derivatives of p-terphenyls (nTm) have been determined by single-crystal X-ray diffraction. For the unsymmetrical substituted compounds 2′,3′-difluoro-4-methyl-p-terphenyl (1T0, C19H14F2) and 4-ethyl-2′,3′-difluoro-4′′-methyl-p-terphenyl (1T2, C21H18F2), the crystal structure is disordered, with molecules statistically entering the crystal in up and down orientations, with full superposition of all the atoms, except for those of the terminal groups (H/methyl for 1T0 and methyl/ethyl for 1T2). For triclinic 2′,3′-difluoro-4,4′′-dimethyl-p-terphenyl (1T1, C20H16F2), with the space group P\overline{1}, the two crystallographically independent molecules have the same conformation, which is different from monoclinic 1T0 (space group C2) and 1T2 (space group C2/c). A common feature of the conformation of the three compounds is the noncoplanar twisted arrangement of the three rings of the p-terphenyl moiety. Two-dimensional (2D) Hirshfeld fingerprint plots are consistent with H...H and C...H contacts in the crystal packing. For the three compounds, the phase behaviour has been investigated by POM (Petra/Osiris/Molinspiration) and differential scanning calorimetry (DSC) analysis. 1T2 is mesogenic, with enantiotropic nematic behaviour.

Metallkomplexe mit biologisch wichtigen Liganden, CIV [1]. ortho-Palladierte Komplexe von N,N-Dimethyl-C-phenyl-glycinmethylester. Synthese von α-Aminosäure-Derivaten durch Insertion von Isocyaniden, CO, Alkenen und Alkinen in die Pd-C-Bindung / Metal Complexes of Biologically Important Ligands, CIV [ 1]. ortho-Palladated Complexes of N,N-Dimethyl-C-phenylglycine-methylester. Synthesis of α-Amino Acid Derivatives by Insertion of Isocyanides, CO, Alkenes, and Alkynes into the Pd-C Bond

1998 ◽  
Vol 53 (4) ◽  
pp. 448-458 ◽  
Author(s):  
Andreas Böhm ◽  
Kurt Polborn ◽  
Karlheinz Sünkel ◽  
Wolfgang Beck
Keyword(s):  
Acetic Acid ◽  
Amino Acid ◽  
Metal Complexes ◽  
Crystal Structures ◽  
Trinuclear Complex ◽  
Amino Acid Derivatives ◽  
X Ray Diffraction ◽  
X Ray ◽  
Derivatives Of ◽  
Amine Ligand

Abstract N,N-Dimethyl-C-phenylglycinemethylester reacts with Pd(OAc)2 in acetic acid to give the orthopalladated, acetato bridged complex 1. Treatment of 1 with sodium halide affords the chloro, bromo, and iodo bridged compounds [Me2NC(H)(CO2Me)C6H4PdX]2 (2a -c) (X = halide). From 2a and 1,1′-bis(diphenylphosphino)ferrocene the phosphine bridged trinuclear complex 3 is obtained. Substitution of the amine ligand of 2a by the phosphino group is observed for the reaction of 2a with Ph2PC(Me)C(Me)PPh2. Insertion of 2,6-dimethyl-phenylisocyanide, CO, alkyl-vinyl-ketones, and diphenylacetylene into the Pd-C bond o f 2a -c provides the orthosubstituted organic and organometallic derivatives of phenylglycine 6a -c, 7, 8a -b and 9a -c. The crystal structures of 1, 4a, 6a, 7 and 9a were determined by X-ray diffraction.

Structural studies in the iron(III)/chloride/α,α'-diimine system. II. Ionic derivatives of stoichiometry FeCl3(phen,bpy)1,1.5

1983 ◽  
Vol 36 (10) ◽  
pp. 2043 ◽  
Author(s):  
BN Figgis ◽  
JM Patrick ◽  
PA Reynolds ◽  
BW Skelton ◽  
AH White ◽  
...  
Keyword(s):  
Single Crystal ◽  
Least Squares ◽  
Crystal Structures ◽  
Acetonitrile Solution ◽  
Structural Studies ◽  
X Ray Diffraction ◽  
X Ray ◽  
Structure Determinations ◽  
Derivatives Of

The crystal structures of the 1 : 1 adducts of FeCl3 with 2,2'-bipyridine (bpy) (1) and 1,10-phenanthroline (phen) (2), as recrystallized from nitromethane, have been determined by single-crystal X-ray diffraction methods at 295 K, being refined by least squares to residuals of 0.038 and 0.032 for 1341 and 3968 'observed' reflections; the result for (2) is a redetermination. Crystals of (1) are orthorhombic, Pbnb, a 15.013(4), b 13.510(5), c 12.471(3) Ǻ, Z 4. Crystals of (2) are triclinic, P1, a 15.823(5), b 11.021(5), c 8.200(3) Ǻ, α 80.27(3), β 76.78(3), γ 89.64(3)°, Z 2. Both complexes haw the stoichiometry (FeCl3)1(bpy,phen)1, but are formulated as cis-[Fe(bpy,phen)2Cl2] [FeCl4]; in both compounds, the Fe-N distance is c. 2.20, (trans to Cl), 2.1, Ǻ(cis to Cl), while Fe-Cl, c. 2.2, Ǻ, is short. The structure determinations of Fe2Cl6(phen,bpy)3 as [Fe(phen)2Cl2]+ [Fe(phen)Cl4]- (3) and [Fe(bpy)2Cl2]+ [Fe(bpy)Cl4]- (4) are also reported. Compound (3) (from acetonitrile solution) is triclinic, P1, a 16.502(5), b 11.857(3), c 10.653(3) Ǻ, α 84.92(2), β 72.66(2), γ 74.80(2)°, Z 2, and was refined to a residual of 0.034 for 5540 'observed' reflections. The cation geometry is similar to that of (2); in the anion, the two Fe-CI bonds trans to each other are long [2.377(1) and 2.365(1) Ǻ] while those trans to the Fe-N bonds are short [2.287(1) and 2.318(1) Ǻ]. Fe-N distances are 2.216(3) and 2.220(3) A. Compound (4) (as its nitromethane solvate) is also triclinic, P1, a 14.480(7), b 12.645(5), c 10.678(4) Ǻ, α 95.68(3), β 109.21(3), γ 9258(3)°, Z 2; a residual of 0.042 was obtained for 4962 'observed' reflections. Cation and anion metal geometries are similar to those of (3).

X-ray and NQR studies of bromoindate(III) complexes: [C2H5NH3]4InBr7, [C(NH2)3]3InBr6, and [H3NCH2C(CH3)2CH2NH3]InBr5

2017 ◽  
Vol 72 (2) ◽  
pp. 141-151 ◽  
Author(s):  
Takeharu Iwakiri ◽  
Hiromitsu Terao ◽  
Enno Lork ◽  
Thorsten M. Gesing ◽  
Hideta Ishihara
Keyword(s):  
Thermal Analysis ◽  
Hydrogen Bond ◽  
Differential Thermal Analysis ◽  
Crystal Structures ◽  
The Other ◽  
Positive Temperature ◽  
X Ray ◽  
Hydrogen Bond Networks ◽  
Quadrupole Resonance ◽  
Nuclear Quadrupole

AbstractThe crystal structures of [C2H5NH3]4InBr7(1), [C(NH2)3]3InBr6(2), and [H3NCH2C(CH3)2CH2NH3]InBr5(3) were determined at 100(2) K: monoclinic, P21/n, a=1061.94(3), b=1186.40(4), c=2007.88(7) pm, β= 104.575(1)°, Z=4 for 1; monoclinic, C2/c, a=3128.81(12), b=878.42(3), c=2816.50(10) pm, β=92.1320(10)°, Z=16 for 2; orthorhombic, P212121, a=1250.33(5), b=1391.46(6), c=2503.22(9) pm, Z=4 for 3. The structure of 1 contains an isolated octahedral [InBr6]3− ion and a Br− ion. The structure of 2 contains three different isolated octahedral [InBr6]3− ions. The structure of 3 has a corner-shared double-octahedral [In2Br11]5− ion and an isolated tetrahedral [InBr4]− ion. The 81Br nuclear quadrupole resonance (NQR) lines of the terminal Br atoms of the compounds are widely spread in frequency, and some of them show unusual positive temperature dependence. These observations manifest the N−H···Br−In hydrogen bond networks developed between the cations and anions to stabilize the crystal structures. The 81Br NQR and differential thermal analysis (DTA) measurements have revealed the occurrence of unique phase transitions in 1 and 3. When the bond angles were estimated from the electric field gradient (EFG) directions calculated by the molecular orbital (MO) methods, accurate values were obtained for [InBr6]3− of 1 and for [In2Br11]5− and [InBr4]− of 3, except for several exceptions in those for the latter two ions. On the other hand, the calculations of 81Br NQR frequencies have produced up to 1.4 times higher values than the observed ones.

Structural studies of (N-phenylthioureidoalkyl- and -aryl)phosphonates

2004 ◽  
Vol 60 (2) ◽  
pp. 211-218 ◽  
Author(s):  
Lilianna Chęcińska ◽  
László Fábián ◽  
Zbigniew H. Kudzin
Keyword(s):  
Crystal Structures ◽  
Molecular Packing ◽  
Structural Studies ◽  
X Ray Diffraction ◽  
X Ray

The crystal structures of three (N-phenylthioureidoalkyl- and -aryl)phosphonates, i.e. diphenyl [(3-phenylthioureido)phenylpropyl]phosphonate, diphenyl [1-(3-phenylthioureido)benzyl]phosphonate and diphenyl [2,2-dimethyl-1-(3-phenylthioureido)propyl]phosphonate, have been determined by X-ray diffraction. The conformations of the title molecules, the geometry of the thioureide fragments and molecular packing arrangements are analyzed and compared with literature data.

Hydrogen-bond directionality and symmetry in [C(O)NH](N)2P(O)-based structures: a comparison between X-ray crystallography data and neutron-normalized values, and evaluation of reliability

2021 ◽  
Vol 77 (3) ◽  
Author(s):  
Maryam Taherzadeh ◽  
Mehrdad Pourayoubi ◽  
Banafsheh Vahdani Alviri ◽  
Samad Shoghpour Bayraq ◽  
Maral Ariani ◽  
...  
Keyword(s):  
Hydrogen Bond ◽  
Crystal Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Maximum Percentage ◽  
Bond Lengths ◽  
X Ray Crystallography ◽  
Percentage Difference ◽  
Structural Database

For [C(O)NH](N)2P(O)-based structures, the magnitude of the differences in the N—H...O, H...O=P and H...O=C angles has been evaluated when the N—H bond lengths, determined by X-ray diffraction, were compared to the neutron normalized values and the maximum percentage difference was obtained, i.e. about 3% for the angle even if the N—H bond lengths have a difference of about 30% (0.7 Å for the X-ray and 1.03 Å for the neutron-normalized value). The symmetries of the crystals are discussed with respect to the symmetry of the molecules, as well as to the symmetry of hydrogen-bonded motifs, and the role of the most directional hydrogen bond in raising the probability of obtaining centrosymmetric crystal structures is investigated. The work was performed by considering nine new X-ray crystal structures and 204 analogous structures retrieved from the Cambridge Structural Database.

scholarly journals Novel Quaternary Ammonium Derivatives of 4-Pyrrolidino Pyridine: Synthesis, Structural, Thermal, and Antibacterial Studies

Crystals ◽  
2020 ◽  
Vol 10 (5) ◽  
pp. 339 ◽  
Author(s):  
Rusi Rusew ◽  
Vanya Kurteva ◽  
Boris Shivachev
Keyword(s):  
Crystal Structures ◽  
Quaternary Ammonium ◽  
Antibacterial Properties ◽  
Bacterial Strains ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Orthorhombic Crystal ◽  
One Pot ◽  
X Ray ◽  
Derivatives Of

Six novel quaternary ammonium derivatives of 4-pyrrolidino pyridine were prepared and isolated via a facile one-pot synthesis and a simple purification procedure. The purity and the molecular structure of the 4-pyrrolidino pyridine derivatives were confirmed with 1H and 13C NMR spectroscopy and powder X-ray diffraction techniques. The crystal structures of the compounds were characterized by single crystal X-ray diffraction (SCXRD) and their thermal properties were studied by Differential Scanning Calorimetry (DSC) analyses. The antibacterial properties of the title compounds against five bacterial strains were evaluated using Kirby–Bauer disk diffusion susceptibility test. The compounds crystallize in the monoclinic or orthorhombic crystal systems (space groups: P21/c, P21/n, or P212121) and their crystal structures are stabilized by a combination of intra- and intermolecular halogen bonding interactions, short contacts and π-π interactions. Above interactions, they contribute to the thermal stability and lack of phase transition effects up to 350 °C. Two of the compounds possess antibacterial effect against E. coli or S. aureus bacterial strains—similar or better than the kanamycin reference.

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