Hydrate formation at extreme conditions
(Source: Acta Crystallographica Section C)
Source: Acta Crystallographica Section C - December 8, 2022 Category: Chemistry Authors: Parsons, S. Tags: salt hydrate high pressure intercalation crystal structure potassium chloride scientific commentaries Source Type: research
FeIII in the high-spin state in dimethylammonium bis[3-ethoxysalicylaldehyde thiosemicarbazonato(2 – )- κ 3O2,N1,S]ferrate(III)
The synthesis and crystal structure (100 K) of the title compound, [(CH3)2NH2][Fe(C10H11O2N3S)2], are reported. The asymmetric unit consists of an octahedral [FeIII(L)2] − fragment, where L2 − is 3-ethoxysalicylaldehyde thiosemicarbazonate(2 − ), and a dimethylammonium cation. Each L2 − ligand binds with the thiolate S, the imine N and the phenolate O atoms as donors, resulting in an FeIIIS2N2O2 chromophore. The ligands are orientated in two perpendicular planes, with the O and S atoms in cis positions, and mutually trans N atoms. The FeIII ion is in the high-spin state at 100 K. The variable-temperature ma...
Source: Acta Crystallographica Section C - December 7, 2022 Category: Chemistry Authors: Powell, R.E. Lees, M.R. Tizzard, G.J. Coles, S.J. Yuan, Q. Koningsbruggen, P.J. van Tags: FeIII complex high-spin crystal structure thiosemicarbazone salicylaldehyde magnetic susceptibility research papers Source Type: research
Synthesis, crystal structure and biological properties of a fluorophore-labelled mixed-ligand copper(II) complex incorporating N-hydroxynaphthalene-1,8-dicarboximide
The mixed-ligand fluorophore-labelled copper(II) complex aqua[2,4-dioxo-3-azatricyclo[7.3.1.05,13]trideca-1(12),5,7,9(13),10-pentaen-3-olato- κ 2O2,O3](1,10-phenanthroline- κ 2N,N ′ )copper(II) nitrate, [Cu(C12H6NO3)(C12H8N2)(H2O)]NO3 · CH3OH or [Cu(L)(phen)(H2O)]NO3 · CH3OH (where phen is 1,10-phenanthroline and HL is N-hydroxynaphthalene-1,8-dicarboximide), (1), was synthesized and structurally characterized. The structure of (1) was confirmed by single-crystal X-ray structure determination. The complex crystallized in the triclinic space group P\overline{1}. The geometry around the copper centre is distorted squar...
Source: Acta Crystallographica Section C - November 28, 2022 Category: Chemistry Authors: Bhat, S.S. Kawade, V.A. Revankar, V.K. Kumbar, V. Bhat, K. Tags: crystal structure fluorophore labelled copper(II) anticancer activity cellular uptake phenanthroline naphthalenedicarboximide research papers Source Type: research
Crystal structure of potassium chloride monohydrate: water intercalation into the B1 structure of KCl under high pressure
A new hydrate form of potassium chloride, KCl · H2O, is identified for the first time by in situ single-crystal X-ray diffraction under high pressure. It has a monoclinic structure with lattice parameters of a = 5.687 (7), b = 6.3969 (3), c = 8.447 (3) Å and β = 107.08 (8) ° at 2.23 (4) GPa and 295 K. The structure of this hydrate has K — Cl alignments similar to the B1 phase of anhydrous KCl, while water molecules intercalate among the ionic species. The coordination structures of the K and Cl atoms can be regarded as the intermediate states between the B1 and B2 phases of...
Source: Acta Crystallographica Section C - November 25, 2022 Category: Chemistry Authors: Yamashita, K. Komatsu, K. Kagi, H. Tags: salt hydrate high pressure intercalation crystal structure potassium chloride research papers Source Type: research
Rearrangement of hydrogen bonds in dehydrated raffinose tetrahydrate: a time-of-flight neutron diffraction study
Structural changes of the raffinose crystal on dehydration from the pentahydrate to the tetrahydrate were investigated by single-crystal time-of-flight neutron diffraction. It was revealed that during the dehydration, rearrangement occurs in the hydrogen bonds related to the lost water molecule, while the symmetry of the crystal structure is retained. The hydrogen-bonding status of raffinose pentahydrate and tetrahydrate were discussed comprehensively according to Jeffrey's hydrogen-bonding classification. It was shown that the water molecules are hydrogen bonded to the surrounding molecules by moderate O — H...O hydroge...
Source: Acta Crystallographica Section C - November 18, 2022 Category: Chemistry Authors: Kawasaki, T. Takahashi, M. Kiyanagi, R. Ohhara, T. Tags: raffinose hydrate hydrogen bonding dehydration neutron diffraction time-of-flight research papers Source Type: research
Competition between chalcogen and halogen bonding assessed through isostructural species
The amino group of 2-amino-5-(4-halophenyl)-1,3,4-chalcogenadiazole has been replaced with bromo/iodo substituents to obtain a library of four compositionally related compounds. These are 2-iodo-5-(4-iodophenyl)-1,3,4-thiadiazole, C8H4I2N2S, 2-bromo-5-(4-bromophenyl)-1,3,4-selenadiazole, C8H4Br2N2Se, 2-bromo-5-(4-iodophenyl)-1,3,4-selenadiazole, C8H4BrIN2Se, and 2-bromo-5-(4-iodophenyl)-1,3,4-thiadiazole, C8H4BrIN2S. All were isostructural and contained bifurcated Ch...N (Ch is chalcogen) and X...X (X is halogen) interactions forming a zigzag packing motif. The noncovalent Ch...N interaction between the chalcogen-bond dono...
Source: Acta Crystallographica Section C - November 9, 2022 Category: Chemistry Authors: De Silva, V. Magueres, P.L. Averkiev, B.B. Aaker ö y, C.B. Tags: halogen bonding chalcogen bonding Hirshfeld surfaces isostructural molecular electrostatic potential energy framework interaction energies crystal structure research papers Source Type: research
Halogen, chalcogen, and hydrogen bonding in organoiodine cocrystals of heterocyclic thiones: imidazolidine-2-thione, 2-mercaptobenzimidazole, 2-mercapto-5-methylbenzimidazole, 2-mercaptobenzoxazole, and 2-mercaptobenzothiazole
Through the combination of heterocyclic thiones with variation in the identity of the heterocyclic elements, namely, imidazolidine-2-thione, 2-mercaptobenzimidazole, 2-mercapto-5-methylbenzimidazole, 2-mercaptobenzoxazole, and 2-mercaptobenzothiazole with the common halogen-bond donors 1,2-, 1,3-, and 1,4-diiodotetrafluorobenzene, 1,3,5-trifluorotriiodobenzene, and tetraiodoethylene, a series of 18 new crystalline structures were characterized. In most cases, N — H...S hydrogen bonding was observed, with these interactions in imidazole-containing structures typically resulting in two-dimensional motifs (i.e. ribbons). La...
Source: Acta Crystallographica Section C - November 9, 2022 Category: Chemistry Authors: Watts, S. Peloquin, A.J. Bandara, M. McMillen, C.D. Pennington, W.T. Tags: crystal structure halogen bonding organoiodine chalcogen bonding hydrogen bonding thione research papers Source Type: research
Bending properties in the 4-halobenzonitrile crystals and C – halogen...N[triple-bond]C halogen bonds
The single crystal of 4-iodobenzonitrile (C7H4IN) is brittle, whereas those of 4-bromobenzonitrile (C7H4BrN) and one of the two forms of 4-chlorobenzonitrile (C7H4ClN) are compliant in nature. The chloro crystal exhibits elastic bending, but in spite of having stronger halogen bonds, the bromo crystal exhibits plastic bending. Crystal structures have been analyzed to understand the different bending properties of these three crystals. In all three cases, the molecules form C — X...N[triple-bond]C (X = halogen) halogen-bonded chains in their respective crystal structures. Statistical analyses and DFT calculations on th...
Source: Acta Crystallographica Section C - November 9, 2022 Category: Chemistry Authors: Veluthaparambath, R.V.P. Krishna G, V. Pancharatna, P.D. Saha, B.K. Tags: elastic bending plastic bending halogen bonding statistical analysis 4-halobenzonitrile research papers Source Type: research
N-Cycloamino substituent effects on the packing architecture of ortho-sulfanilamide molecular crystals and their in silico carbonic anhydrase II and IX inhibitory activities
In the search for new `sulfa drugs' with therapeutic properties, o-nitrosulfonamides and N-cycloamino-o-sulfanilamides were synthesized and characterized using techniques including 1H NMR, 13C NMR and FT – IR spectroscopy, and single-crystal X-ray diffraction (SC-XRD). The calculated density functional theory (DFT)-optimized geometry of the molecules showed similar conformations to those obtained by SC-XRD. Molecular docking of N-piperidinyl-o-sulfanilamide and N-indolinyl-o-sulfanilamide supports the notion that o-sulfanilamides are able to bind to human carbonic anhydrase II and IX inhibitors (hCA II and IX; PDB entrie...
Source: Acta Crystallographica Section C - November 8, 2022 Category: Chemistry Authors: Kolade, S.O. Izunobi, J.U. Gordon, A.T. Hosten, E.C. Olasupo, I.A. Ogunlaja, A.S. Asekun, O.T. Familoni, O.B. Tags: sulfanilamide nitrosulfonamide cycloamino SC-XRD DFT crystal structure packing architecture inhibitory activity research papers Source Type: research
Zwitterionic versus neutral molecules of fluoroquinolones: crystal structure of danofloxacin dihydrate
The crystal structure of danofloxacin (DFX) as a zwitterionic dihydrate [systematic name: (1S,4S)-5-(3-carboxylato-1-cyclopropyl-6-fluoro-4-oxo-1,4-dihydroquinolin-7-yl)-2-methyl-2,5-diazabicyclo[2.2.1]heptan-2-ium dihydrate], C19H20FN3O3 · 2H2O, has been determined for the first time. The stability of the crystal structure is ensured by N — H...O and O — H...O hydrogen bonds, some of which are assisted by charge. The zwitterionic molecules of DFX are packed in stacks and this structural motif can be defined as a basic one from a supramolecular and energetic point of view. Hirshfeld surface analysis was used for an ad...
Source: Acta Crystallographica Section C - November 8, 2022 Category: Chemistry Authors: Felczak, A. Kalinowska-Lis, U. Kusz, J. Ch ę ci ń ska, L. Tags: danofloxacin dihydrate zwitterionic structure Hirshfeld surface analysis destabilizing interactions stacking interactions crystal structure antibacterial agent antibiotic fluoroquinolone research papers Source Type: research
A new heteroleptic cuprous polymer constructed by a cyanopyridine ligand exhibiting a supramolecular framework structure and luminescence
Luminescent cuprous complexes are of great importance among coordination compounds due to their relative abundance, low cost and ability to display excellent luminescence. The title heteroleptic cuprous polymer solvate, catena-poly[[[(9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphane)- κ 2P,P ′ ]( μ -pyridine-3-carbonitrile- κ 2N1:N3)copper(I)] hexafluorophosphate dichloromethane trisolvate], {[Cu(C6H4N2)(C39H32OP2)]PF6 · 3CH2Cl2}n, conventionally abbreviated as {[Cu(3-PyCN)(Xantphos)]PF6 · 3CH2Cl2}n, where Xantphos and 3-PyCN represent (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphane) and pyridine-3-c...
Source: Acta Crystallographica Section C - October 28, 2022 Category: Chemistry Authors: Kong, Y.-J. Wang, J.-T. Song, L. Tags: heteroleptic cuprous polymer helical chain crystal structure supramolecular metal – organic framework Xantphos luminescence cyanopyridine research papers Source Type: research
Synthesis, crystal structure and Hirshfeld analysis of triphenylphosphine – (4-bromophenyl)borane
The title compound, alternatively called (4-bromophenyl)dihydrido(triphenylphosphanyl)boron, C24H21BBrP, crystallizes in the space group P\overline{1} with one symmetry-independent molecule in the asymmetric unit. The B and P atoms both adopt the expected tetrahedral geometry. A possible intramolecular B — H δ − ... δ +H — C dihydrogen bond exists between an arene group on phosphorus and the borane center. In the solid state, the title molecule is connected to its neighbors by intermolecular C — H... π interactions, with the arene rings on the P atom acting as hydrogen-bond donors and the arene ring of the boran...
Source: Acta Crystallographica Section C - October 27, 2022 Category: Chemistry Authors: Allen, C.J. Olden, A.M. Yates, J.L. Wheeler, K.A. Abbey, E.R. Tags: Lewis acid Lewis base phosphine-borane NMR crystal structure research papers Source Type: research
Quantitative insights into noncovalent interactions involving halogen and tetrel bonds in 2,4,6-trimethylpyrylium tetrafluoroborate
The crystal and molecular structure of an organic salt, in which a 2,4,6-trimethylpyrylium cation forms a salt with a tetrafluoroborate anion, namely, 2,4,6-trimethylpyrylium tetrafluoroborate, C8H11O+ · BF4 − , has been experimentally realized. The compound crystallizes in the orthorhombic centrosymmetric space group Pnma. The crystal packing is stabilized via a subtle interplay of [F3 — B — F] − ...O+ — C fluorine/oxygen-centred halogen/chalcogen bonds and C δ +...F δ − tetrel-bonded contacts. Although the O centre has a formal charge of +1, the estimation of the partial negative charges on O is in accorda...
Source: Acta Crystallographica Section C - October 25, 2022 Category: Chemistry Authors: Mandal, K. Sarkar, S. Ghosh, P. Hathwar, V.R. Chopra, D. Tags: crystal structure noncovalent interactions halogen bond tetrel bond trimethylpyrylium tetrafluoroborate research papers Source Type: research
Synthesis, and spectroscopic and structural characterization of three new styrylquinoline – benzimidazole hybrids
Three new 4-styrylquinoline – benzimidazole hybrids have been synthesized using a reaction sequence in which 2-methylquinoline precursors first undergo selective oxidation by selenium dioxide to form the corresponding 2-formylquinoline intermediates, followed by oxidative cyclocondensation reactions with benzene-1,2-diamine to yield the hybrid products. The formyl intermediates and the hybrid products have all been fully characterized using a combination of IR, 1H and 13C NMR spectroscopy, and high-resolution mass spectrometry, and the structures of the three hybrid products have been determined using single-crystal X-ra...
Source: Acta Crystallographica Section C - October 25, 2022 Category: Chemistry Authors: Ardila, D.M. Rodr í guez, D.F. Palma, A. D í az, I. Cobo, J. Glidewell, C. Tags: synthesis oxidative cyclocondensation styrylquinoline benzimidazole molecular hybrids molecular structure molecular conformation hydrogen bonding supramolecular assembly crystal structure research papers Source Type: research
Complexes of 2,4,6-trihydroxybenzoic acid: effects of intramolecular hydrogen bonding on ligand geometry and metal binding modes
This article describes a series of more than 20 new compounds formed by the combination of 2,4,6-trihydroxybenzoic acid (H4thba) with metal ions in the presence of a base, with structures that include discrete molecular units, chains, and two- and three-dimensional networks. As a result of the presence of two ortho-hydroxy groups, H4thba is a relatively strong acid (pKa1 = 1.68). The carboxylate group in H3thba − is therefore considerably less basic than most carboxylates with intramolecular hydrogen bonds, conferring a rigid planar geometry upon the anion. These characteristics of H3thba − significantly impact upon...
Source: Acta Crystallographica Section C - October 25, 2022 Category: Chemistry Authors: Abrahams, B.F. Commons, C.J. Hudson, T.A. Arlt, R.S. Ahl, R. Carajias, E.D. Chan, J.W.K. Guo, Z. Hill, R.E. McGinty, A. Peters, N.L. Poon, J.Y.P. Qu, J. Qu, J. Rochette, E.E. Walkear, C. Wang, H. Wu, H. Xu, C. Zhang, J. Tags: carboxylate crystal engineering crystallographic education crystal structure 2,4,6-trihydroxybenzoic acid intramolecular hydrogen bonds coordination polymers research papers Source Type: research
