Foreword to the special virtual issue on Modern approaches and tools for teaching crystallography
(Source: Acta Crystallographica Section E)
Source: Acta Crystallographica Section E - August 1, 2023 Category: Chemistry Authors: D í az de Delgado, G. Parkin, S. Tags: crystallographic teaching space-group symmetry crystal growing twinning validation criteria disorder electron diffraction editorial Source Type: research
Synthesis and crystal structures of (E)-N ′ -(4-chloro-3-nitrobenzylidene)acetohydrazide and (E)-2-(4-chlorobenzylidene)-1-(quinolin-8-yl)hydrazine
The syntheses of two benzylidenehydrazine derivatives, namely, (E)-N ′ -(4-chloro-3-nitrobenzylidene)acetohydrazide, C9H8ClN3O3, and (E)-2-(4-chlorobenzylidene)-1-(quinolin-8-yl)hydrazine, C16H12ClN3, are reported. The molecules have been characterized using IR, 1H NMR, 13C NMR and mass spectroscopic and elemental analysis techniques, and their structures have been determined by single-crystal X-ray diffraction. (Source: Acta Crystallographica Section E)
Source: Acta Crystallographica Section E - July 28, 2023 Category: Chemistry Authors: Nasr, T. Kariuki, B.M. Elansary, M.M. Elhaggar, R. Zaghary, W. Tags: synthesis crystal structure benzylidene hydrazine research communications Source Type: research
Synthesis, optical properties and crystal structure of (E,E)-1,3-(3,4:9,10-dibenzododeca-1,11-diene-5,7-diyne-1,12-diyl)benzene
The dehydrobenzannulene (E,E)-1,3-(3,4:9,10-dibenzododeca-1,11-diene-5,7-diyne-1,12-diyl)benzene, C26H16, was successfully synthesized via photocatalyst-assisted stereoselective reductive desulfonylation of 1,3-bis{1-phenylsulfonyl-2-[2-(trimethylsilylethynyl)phenyl]ethenyl}benzene, C44H42O4S2Si2, and subsequent desilylative cyclization of the resulting (E,E)-bis-silyl-protected dienyne, C32H34Si2. The structure of the dehydrobenzannulene thus obtained was confirmed by single-crystal X-ray analysis; three benzene rings are connected to one another by a 1,3-butadiynylene and a pair of ethenylene arrays. Although the π -sys...
Source: Acta Crystallographica Section E - July 28, 2023 Category: Chemistry Authors: Watanabe, H. Sato, T. Sumita, M. Shiroyama, M. Sugawara, D. Tokuyama, T. Okuda, Y. Wakamatsu, K. Akashi, H. Orita, A. Tags: crystal structure expanded π -system dehydrobenzannulene reductive desulfonylation research communications Source Type: research
N-Cyclohexyltryptamine: freebase, bromide and fumarate
The solid-state structures of N-cyclohexyltryptamine (I) {systematic name: N-[2-(1H-indol-3-yl)ethyl]cyclohexanamine}, C16H22N2, and two of its salts, N-cyclohexyltryptammonium bromide (II) {systematic name: N-[2-(1H-indol-3-yl)ethyl]cyclohexanaminium bromide}, C16H23N2+ · Br − , and N-cyclohexyltryptammonium fumarate (III) (systematic name: bis{N-[2-(1H-indol-3-yl)ethyl]cyclohexanaminium} (2E)-but-2-enedioate), 2C16H23N2+ · C4H2O42 − , were determined by single-crystal X-ray diffraction. The freebase compound forms infinite chains along [010] through N — H...N hydrogen bonds. The bromide salt is held together by N...
Source: Acta Crystallographica Section E - July 25, 2023 Category: Chemistry Authors: Naeem, M. Le, A.N. Bauer, B.E. Chadeayne, A.R. Golen, J.A. Manke, D.R. Tags: crystal structure tryptamines indoles hydrogen bonds research communications Source Type: research
Crystal structure and Hirshfeld surface analysis of 4-cyano-N-[(4-cyanophenyl)sulfonyl]-N-[2-(5-methylfuran-2-yl)phenyl]benzenesulfonamide
In the title compound, C25H17N3O5S2, intramolecular π – π interactions [centroid-to-centroid distance = 3.5640 (9) Å ] are observed between the furan and benzene rings of the 4-cyanophenyl group. In the crystal, molecules are connected via C — H...O and C — H...N hydrogen bonds, forming layers parallel to the (100) plane. These layers are interconnected by C — H... π interactions and weak van der Waals interactions. Hirshfeld surface analysis indicates that H...H (30.2%), N...H/H...N (22.3%), C...H/H...C (17.9%) and O...H/H...O (15.4%) interactions make the most significant contributions to the crystal ...
Source: Acta Crystallographica Section E - July 21, 2023 Category: Chemistry Authors: Mammadova, G.Z. Yakovleva, E.D. Burkin, G.M. Khrustalev, V.N. Akkurt, M. Ç elikesir, S.T. Bhattarai, A. Tags: crystal structure sulfonamides hydrogen bonds — H... π interactions – Hirshfeld surface analysis research communications Source Type: research
Crystal-structure determination and Hirshfeld surface analysis of two new thiophene derivatives: (E)-N-{2-[2-(benzo[b]thiophen-2-yl)ethenyl]-5-fluorophenyl}benzenesulfonamide and (E)-N-{2-[2-(benzo[b]thiophen-2-yl)ethenyl]-5-fluorophenyl}-N-(but-2-yn-1-yl)benzenesulfonamide
In the title compounds, C22H16FNO2S2 (I) and C26H20FNO2S2 (II), the benzothiophene rings are essentially planar with maximum deviations of 0.009 (1) and 0.001 (1) Å for the carbon and sulfur atom in compounds I and II, respectively. In I, the thiophene ring system is almost orthogonal to the phenyl ring attached to the sulfonyl group, with a dihedral angle of 77.7 (1) ° . In compound I, the molecular structure is stabilized by weak C — H...O intramolecular interactions formed by the sulfone oxygen atoms, which generate two S(5) ring motifs. In the crystal of I, N — H...O hydrogen bonds link the molecu...
Source: Acta Crystallographica Section E - July 21, 2023 Category: Chemistry Authors: Madhan, S. NizamMohideen, M. Pavunkumar, V. MohanaKrishnan, A.K. Tags: crystal structure thiophene benzothiophene flurophenyl phenylsulfonamide hydrogen bonding Hirshfeld surface analysis research communications Source Type: research
Crystal structure and Hirshfeld surface analysis of (E)-1-(2,4-dimethylfuran-3-yl)-3-phenylprop-2-en-1-one
The title compound, C15H14O2, adopts an E configuration about the C=C double bond. The furan ring is inclined to the phenyl ring by 12.03 (9) ° . In the crystal, pairs of molecules are linked by C — H...O hydrogen bonds, forming dimers with R22(14) ring motifs. The molecules are connected via C — H... π interactions, forming a three dimensional network. No π – π interactions are observed. (Source: Acta Crystallographica Section E)
Source: Acta Crystallographica Section E - July 14, 2023 Category: Chemistry Authors: Khalilov, A.N. Khrustalev, V.N. Samigullina, A.I. Akkurt, M. Rzayev, R.M. Bhattarai, A. Mamedov, İ .G. Tags: crystal structure 2,4-dimethylfuran chalcones hydrogen bond — H... π interactions Hirshfeld surface analysis research communications Source Type: research
Crystal structures of four organic salts of trihexyphenidyl at 90 K
The syntheses and crystal structure studies of four organic salts of trihexyphenidyl, viz., trihexyphenidylium [1-(3-cyclohexyl-3-hydroxy-3-phenylpropyl)piperidin-1-ium] 4-nitrobenzoate, C20H32NO+ · C7H4NO4 − (I), trihexyphenidylium 4-hydroxybenzoate, C20H32NO+ · C7H5O − (II), trihexyphenidylium 4-bromobenzoate, C20H32NO+ · C7H4BrO2 − (III), and trihexyphenidylium thiophene-2-carboxylate hemihydrate, 2C20H32NO+ · 2C5H3O2S − · H2O (IV), conducted at 90 K are described. Structures I, II, and III are solvent free with one cation – anion pair per asymmetric unit, while IV crystallizes as a hemihydrate, havin...
Source: Acta Crystallographica Section E - July 14, 2023 Category: Chemistry Authors: Vinaya Basavaraju, Y.B. Yathirajan, H.S. Parkin, S. Tags: trihexyphenidyl trihexyphenidylium cation crystal structure disorder twinning non-merohedry hydrogen bonding research communications Source Type: research
Crystal structure of poly[(acetonitrile- κ N)( μ 3-7-{[bis(pyridin-2-ylmethyl)amino]methyl}-8-hydroxyquinoline-5-sulfonato- κ 4N,O:O ′ :O ′ ′ )sodium]
In the title compound, [Na(C22H19N4O4S)(CH3CN)]n, the NaI atom adopts a distorted square-pyramidal coordination geometry, formed by one N and one O atom of the qunolinol moiety in the ligand, two O atoms of sulfonate moieties of two adjacent ligands and the N atom of the coordinated acetonitrile solvent. The NaI atom is located well above the mean basal plane of the square-based pyramid. The apical position is occupied by a sulfonate O atom of a neighboring ligand. Three N atoms of the bis(pyridin-2-ylmethyl)amine moiety in the ligand are not coordinated by the sodium atom. The molecule forms an intramolecular bifurcated O...
Source: Acta Crystallographica Section E - July 14, 2023 Category: Chemistry Authors: Kubono, K. Tanaka, R. Kashiwagi, Y. Tani, K. Yokoi, K. Tags: crystal structure coordination polymer sodium complex 8-hydroxyquinoline sulfonato — H...O interactions research communications Source Type: research
Crystal structure and luminescence spectrum of a one-dimensional nickel(II) coordination polymer incorporating 1,4-bis[(2-methylimidazol-1-yl)methyl]benzene and adamantane-1,3-dicarboxylate co-ligands
An NiII coordination polymer, namely, poly[( μ 2-adamantane-1,3-dicarboxylato- κ 4O1,O1 ′ :O3,O3 ′ )[ μ 2-1,4-bis(2-methyl-imidazol-1-ylmethyl)benzene- κ 2N3:N3 ′ ]nickel(II)], [Ni(C12H14O4)(C16H18N4)]n or [Ni(adc)(bmib)]n, (I) [adc = adamantane-1,3-dicarboxylate, C12H14O42 – and bmib = 1,4-bis(2-methyl-imidazol-1-ylmethyl)benzene, C16H18N4] was synthesized and characterized. It exhibits a one-dimensional extended structure built up from alternating [Ni2(bmib)2] 26-membered rings and [Ni2(adc)2] 16-membered rings. The nickel atom lies on a crystallographic twofold axis and both ligands are completed by mirror s...
Source: Acta Crystallographica Section E - July 14, 2023 Category: Chemistry Authors: Zhang, Y. Qin, H. Wu, B. Tags: crystal structure nickel coordination polymer research communications Source Type: research
Crystal structure of K6[Zn(CO3)4]
The crystal structure of K6[Zn(CO3)4], hexapotassium tetracarbonatozincate(II), comprises four unique potassium cations (two located on a general position, and two on the twofold rotation axis of the space group C2/c) and a [Zn(CO3)4]6 − anion. The ZnII atom of the latter is located on the twofold rotation axis and is surrounded in a slightly distorted tetrahedral manner by two pairs of monodentately binding carbonate groups, with Zn — O distances of 1.9554 (18) and 1.9839 (18) Å . Both carbonate groups exhibit a slight deviation from planarity, with the C atom being shifted by 0.008 (2) and 0.006 ...
Source: Acta Crystallographica Section E - July 14, 2023 Category: Chemistry Authors: Eder, F. Weil, M. Tags: crystal structure zinc in tetrahedral coordination carbonate research communications Source Type: research
Crystal structure of bis{S-octyl-3-[(thiophen-2-yl)methylidene]dithiocarbazato- κ 2N3,S}nickel(II)
In the title complex, [Ni(C14H21N2S3)2], the nickel(II) atom is located on a crystallographic inversion center and exhibits a square-planar coordination environment, being coordinated by two negatively charged N,S-chelating ligands in a trans configuration. In the crystal, the non-H atoms of the complex are practically coplanar (r.m.s. deviation of fitted atoms = 0.135 Å ), and the angle between the thienyl and the chelating rings is 6.7 (1) ° . The molecules stack at a distance of 3.623 (2) Å along the b-axis direction. (Source: Acta Crystallographica Section E)
Source: Acta Crystallographica Section E - July 11, 2023 Category: Chemistry Authors: Khan, S.S. Howlader, M.B.H. Sheikh, M.C. Miyatake, R. Zangrando, E. Tags: crystal structure nickel(II) complex dithiocarbazato ligand research communications Source Type: research
Synthesis and crystal structures of three Schiff bases derived from 3-formylacetylacetone and benzyl-, tert-butyl- and (S)-methylbenzylamine
Treatment of 3-formylacetylacetone with the amines benzylamine, tert-butylamine and (S)-methylbenzylamine led to the formation of the corresponding Schiff bases 3-[(benzylamino)methylidene]pentane-2,4-dione, C13H15NO2 (1), 3-[(tert-butylamino)methylidene]pentan-2,4-dione, C10H17NO2 (2) and 3-{[(S)-benzyl(methyl)amino]methylidene}pentane-2,4-dione, C14H17NO2 (3). The molecules of all three compounds exist as enamine tautomers that contain a nearly planar amino-methylene-pentane-2,4-dione core with a strong intramolecular N — H...O hydrogen bridge. The R group attached to the enamine N atom has no significant influence on ...
Source: Acta Crystallographica Section E - July 11, 2023 Category: Chemistry Authors: Halz, J.H. Hentsch, A. Wagner, C. Merzweiler, K. Tags: crystal structure enamine 3-formylacetylacetone Schiff base research communications Source Type: research
(NH4)2[UO2Cl4] · 2H2O, a new uranyl tetrachloride with ammonium charge-balancing cations
A new uranyl tetrachloride salt with chemical formula, (NH4)2[UO2Cl4] · 2H2O, namely, diammonium uranyl tetrachloride dihydrate, 1, was prepared and crystallized via slow evaporation from a solution of 2 M hydrochloric acid. As confirmed by powder X-ray diffraction, the title compound crystallizes with an ammonium chloride impurity that formed as a result of the breakdown of a triazine precursor. The (UO2Cl4)2 − dianion is charge balanced by ammonium cations, while an extensive hydrogen-bond network donated from structural water molecules stabilize the overall assembly. Compound 1 adds to the extensive collection of act...
Source: Acta Crystallographica Section E - July 7, 2023 Category: Chemistry Authors: Kohlgruber, T.A. Surbella III, R.G. Tags: ammonium optical properties uranyl tetrachloride X-ray diffraction crystal structure research communications Source Type: research
Synthesis and crystal structure of a bench-stable pyridinium ketene hemiaminal: 1-(1-ethoxyethenyl)-2-[methyl(phenyl)amino]pyridin-1-ium trifluoromethanesulfonate
The novel bench-stable N-quaternized ketene N,O-acetal, C16H19N2O+ · CF3O3S − , was synthesized and its structure determined. The title compound is a rare example of a pyridinium ketene hemiaminal for which a crystal structure has been determined, joining the 2-chloro-1-(1-ethyoxyethenyl)pyridin-1-ium trifluoromethanesulfonate salt from which it was synthesized. The cationic species of the title compound can be defined by three individually planar fragments assembling into a non-coplanar cation. The phenyl substituent extending from the amino nitrogen atom and the ethyoxyvinyl substituent extending from the pyridine N a...
Source: Acta Crystallographica Section E - July 7, 2023 Category: Chemistry Authors: Krevlin, Z.A. Bote, I.C. Crespo, M.C.F. Lam, C.C. McMillen, C.D. Majireck, M.M. Tags: crystal structure ketene hemiaminal N-quaternized ketene N,O-acetal research communications Source Type: research
