structure Crystal structure of a layered phosphate molybdate K2Gd(PO4)(MoO4) By journals.iucr.org Published On :: 2024-01-05 The title compound dipotassium gadolinium(III) phosphate(V) molybdate(VI), K2Gd(PO4)(MoO4), was synthesized from a high-temperature melt starting from GdF3 as a source of gadolinium. Its structure is isotypic with other MI2MIII(MVIO4)(PO4) compounds, where MI = Na, K or Cs, and MIII = rare-earth cation, MVI = Mo or W. The three-dimensional framework is built up from [Gd(PO4)(MoO4)] anionic sheets, which are organized by adhesion of [GdPO4] layers and [MoO4] tetrahedra stacked above and below these layers. The interstitial space is occupied by K cations having eightfold oxygen coordination. The polyhedron of GdO8 was estimated to be a triangular dodecahedron by the continuous shape measurement method. Full Article text
structure Crystal structure and Hirshfeld surface analysis of (E)-2-[2-(2-amino-1-cyano-2-oxoethylidene)hydrazin-1-yl]benzoic acid N,N-dimethylformamide monosolvate By journals.iucr.org Published On :: 2024-01-05 In the title compound, C10H8N4O3·C3H7NO, the asymmetric unit contains two crystallographically independent molecules A and B, each of which has one DMF solvate molecule. Molecules A and B both feature intramolecular N—H⋯O hydrogen bonds, forming S(6) ring motifs and consolidating the molecular configuration. In the crystal, N—H⋯O and O—H⋯O hydrogen bonds connect molecules A and B, forming R22(8) ring motifs. Weak C—H⋯O interactions link the molecules, forming layers parallel to the (overline{2}12) plane. The DMF solvent molecules are also connected to the main molecules (A and B) by N—H⋯O hydrogen bonds. π–π stacking interactions [centroid-to-centroid distance = 3.8702 (17) Å] between the layers also increase the stability of the molecular structure in the third dimension. According to the Hirshfeld surface study, O⋯H/H⋯O interactions are the most significant contributors to the crystal packing (27.5% for molecule A and 25.1% for molecule B). Full Article text
structure Synthesis and crystal structure of a cadmium(II) coordination polymer based on 4,4'-(1H-1,2,4-triazole-3,5-diyl)dibenzoate By journals.iucr.org Published On :: 2024-01-09 The asymmetric unit of the title compound, catena-poly[[[aquabis(pyridine-κN)cadmium(II)]-μ2-4,4'-(1H-1,2,4-triazole-3,5-diyl)dibenzoato-κ4O,O':O'',O'''] 4.5-hydrate], {[Cd(C16H9N3O4)(C5H5N)2(H2O)]·4.5H2O}n or {[Cd(bct)(py)2(H2O)]·4.5H2O}n (I), consists of a Cd2+ cation coordinated to one bct2– carboxylate dianion, two molecules of pyridine and a water molecule as well as four and a half water molecules of crystallization. The metal ion in I possesses a pentagonal–bipyramidal environment with the four O atoms of the two bidentately coordinated carboxylate groups and the N atom of a pyridine molecule forming the O4N equatorial plane, while the N atom of another pyridine ligand and the O atom of the water molecule occupy the axial positions. The bct2– bridging ligand connects two metal ions via its carboxylic groups, resulting in the formation of a parallel linear polymeric chain running along the [1overline{1}1] direction. The coordinated water molecule of one chain forms a strong O—H⋯O hydrogen bond with the carboxylate O atom of a neighboring chain, leading to the formation of double chains with a closest distance of 5.425 (7) Å between the cadmium ions belonging to different chains. Aromatic π–π stacking interactions between the benzene fragments of the anions as well as between the coordinated pyridine molecules belonging to different chains results in the formation of sheets oriented parallel to the (overline{1}01) plane. As a result of hydrogen-bonding interactions involving the water molecules of crystallization, the sheets are joined together in a three-dimensional network. Full Article text
structure Crystal structure, Hirshfeld surface analysis and energy frameworks of 1-[(E)-2-(2-fluorophenyl)diazan-1-ylidene]naphthalen-2(1H)-one By journals.iucr.org Published On :: 2024-01-12 The title compound, C16H11N2OF, is a member of the azo dye family. The dihedral angle subtended by the benzene ring and the naphthalene ring system measures 18.75 (7)°, indicating that the compound is not perfectly planar. An intramolecular N—H⋯O hydrogen bond occurs between the imino and carbonyl groups. In the crystal, the molecules are linked into inversion dimers by C—H⋯O interactions. Aromatic π–π stacking between the naphthalene ring systems lead to the formation of chains along [001]. A Hirshfeld surface analysis was undertaken to investigate and quantify the intermolecular interactions. In addition, energy frameworks were used to examine the cooperative effect of these intermolecular interactions across the crystal, showing dispersion energy to be the most influential factor in the crystal organization of the compound. Full Article text
structure Synthesis and crystal structure of N1,N2-dimethylethanedihydrazide By journals.iucr.org Published On :: 2024-01-12 The title compound, N1,N2-dimethylethanedihydrazide, C4H10N4O2, was obtained by the methylation of oxalyl dihydrazide protected with phthalimide. The molecule is essentially non-planar with a dihedral angle between the two planar hydrazide fragments of 86.5 (2)°. This geometry contributes to the formation of a multi-contact three-dimensional supramolecular network via C—H⋯O, N—H⋯O and N—H⋯N hydrogen bonds. Full Article text
structure Synthesis, crystal structure and thermal properties of dibromidobis(2-methylpyridine N-oxide-κO)cobalt(II) By journals.iucr.org Published On :: 2024-01-12 Reaction of CoBr2 with 2-methylpyridine N-oxide in n-butanol leads to the formation of the title compound, [CoBr2(C6H7NO)2] or [CoBr2(2-methylpyridine N-oxide)2]. Its asymmetric unit consists of one CoII cation as well as two bromide anions and two 2-methylpyridine N-oxide coligands in general positions. The CoII cations are tetrahedrally coordinated by two bromide anions and two 2-methylpyridine N-oxides, forming discrete complexes. In the crystal structure, these complexes are linked predominantly by weak C–H⋯Br hydrogen bonding into chains that propagate along the crystallographic a-axis. Powder X-ray diffraction (PXRD) measurements indicate that a pure phase was obtained. Thermoanalytical investigations prove that the title compound melts before decomposition; before melting, a further endothermic signal of unknown origin was observed that does not correspond to a phase transition. Full Article text
structure Synthesis and crystal structures of boryl ortho-silylaryl trifluoromethanesulfonates By journals.iucr.org Published On :: 2024-01-12 We report the synthesis and structural characterization of three crystalline borylated ortho-silylaryl trifluoromethanesulfonates: 5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-2-(trimethylsilyl)phenyl trifluoromethanesulfonate, C16H24BF3O5SSi (1a), 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-2-(trimethylsilyl)phenyl trifluoromethanesulfonate, C16H24BF3O5SSi (1b), and 2-methyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-6-(trimethylsilyl)phenyl trifluoromethanesulfonate, C17H26BF3O5SSi (2), which are versatile aryne precursors. For all three compounds, the heteroatom substituents are almost coplanar with the central aromatic moiety. C—heteroatom bonding metrics are unexceptional and fall withing the typical range of C—B, C—Si, and C—O single bonds. Despite numerous electronegative sites, only weak intermolecular interactions are observed in the solid state. Full Article text
structure Synthesis and crystal structure of [1,3-bis(2,6-diisopropylphenyl)imidazol-2-ylidene](isocyanato-κN)gold(I) By journals.iucr.org Published On :: 2024-01-19 The title complex, [Au(NCO)(C27H36N2)], was synthesized by ligand metathesis from [1,3-bis(2,6-diisopropylphenyl)imidazol-2-ylidene]gold(I) chloride and sodium cyanate in anhydrous tetrahydrofuran and crystallized from toluene at 233 K in the orthorhombic space group P212121, as a neutral complex with the central Au atom di-coordinated by an N-heterocyclic carbene [Au—C = 1.963 (2) Å] and an isocyanate [Au—N 1.999 (2) Å] ligands, with a linear CAuNCO moiety. The crystal packing is consolidated by C—H⋯O hydrogen bonds. Full Article text
structure Crystal structure and Hirshfeld surface analysis of (2E)-1-phenyl-3-(1H-pyrrol-2-yl)propen-1-one By journals.iucr.org Published On :: 2024-01-26 The title compound, C13H11NO, adopts an E configuration about the C=C double bond. The pyrrole ring is inclined to the phenyl ring at an angle of 44.94 (8)°. In the crystal, molecules are linked by N—H⋯O hydrogen bonds, forming ribbons parallel to (020) in zigzag C(7) chains along the a axis. These ribbons are connected via C—H⋯π interactions, forming a three-dimensional network. No significant π–π interactions are observed. Full Article text
structure Synthesis and crystal structure of diisothiocyanatotetrakis(4-methylpyridine N-oxide)cobalt(II) and diisothiocyanatotris(4-methylpyridine N-oxide)cobalt(II) showing two different metal coor By journals.iucr.org Published On :: 2024-01-26 The reaction of Co(NCS)2 with 4-methylpyridine N-oxide (C6H7NO) leads to the formation of two compounds, namely, tetrakis(4-methylpyridine N-oxide-κO)bis(thiocyanato-κN)cobalt(II), [Co(NCS)2(C6H7NO)4] (1), and tris(4-methylpyridine N-oxide-κO)bis(thiocyanato-κN)cobalt(II), [Co(NCS)2(C6H7NO)3] (2). The asymmetric unit of 1 consists of one CoII cation located on a centre of inversion, as well as one thiocyanate anion and two 4-methylpyridine N-oxide coligands in general positions. The CoII cations are octahedrally coordinated by two terminal N-bonding thiocyanate anions in trans positions and four 4-methylpyridine N-oxide ligands. In the extended structure, these complexes are linked by C—H⋯O and C—H⋯S interactions. In compound 2, two crystallographically independent complexes are present, which occupy general positions. In each of these complexes, the CoII cations are coordinated in a trigonal–bipyramidal manner by two terminal N-bonding thiocyanate anions in axial positions and by three 4-methylpyridine N-oxide ligands in equatorial positions. In the crystal, these complex molecules are linked by C—H⋯S interactions. For compound 2, a nonmerohedral twin refinement was performed. Powder X-ray diffraction (PXRD) reveals that 2 was nearly obtained as a pure phase, which is not possible for compound 1. Differential thermoanalysis and thermogravimetry data (DTA–TG) show that compound 2 start to decompose at about 518 K. Full Article text
structure Crystal structures of the alkali aluminoboracites A4B4Al3O12Cl (A = Li, Na) By journals.iucr.org Published On :: 2024-01-26 Single crystals of alkali aluminoboracites, A4B4Al3O12Cl (A = Li, Na), were grown using the self-flux method, and their isotypic cubic crystal structures were determined by single-crystal X-ray diffraction. Na4B4Al3O12Cl is the first reported sodium boracite, and its lattice parameter [13.5904 (1) Å] is the largest among the boracites consisting of a cation–oxygen framework reported so far. For both crystals, structure models refined in the cubic space group Foverline{4}3c, which assume that all cubic octant subcells in the unit cell are equivalent, converged with R1 factors of ∼0.03. However, the presence of weak hhl reflections with odd h and l values indicates that refinements in the space group F23, which presume a checkerboard-like ordering of two types of subcells with slightly different atomic positions, are more appropriate. Full Article text
structure Synthesis, crystal structure and Hirshfeld surface analysis of sodium bis(malonato)borate monohydrate By journals.iucr.org Published On :: 2024-01-26 In the title salt, poly[aqua[μ4-bis(malonato)borato]sodium], {[Na(C6H4BO8)]·H2O}n or Na+·[B(C3H2O4)2]−·H2O, the sodium cation exhibits fivefold coordination by four carbonyl O atoms of the bis(malonato)borate anions and a water O atom. The tetrahedral B atom at the centre of the anion leads to the formation of a polymeric three-dimensional framework, which is consolidated by C—H⋯O and O—H⋯O hydrogen bonds. A Hirshfeld surface analysis indicates that the most significant contacts in the crystal packing are H⋯O/O⋯H (49.7%), Na⋯O/O⋯Na (16.1%), O⋯O (12.6%), H⋯H (10.7%) and C⋯O/O⋯C (7.3%). Full Article text
structure (E)-N,N-Diethyl-4-{[(4-methoxyphenyl)imino]methyl}aniline: crystal structure, Hirshfeld surface analysis and energy framework By journals.iucr.org Published On :: 2024-01-26 In the title benzylideneaniline Schiff base, C18H22N2O, the aromatic rings are inclined to each other by 46.01 (6)°, while the Car—N= C—Car torsion angle is 176.9 (1)°. In the crystal, the only identifiable directional interaction is a weak C—H⋯π hydrogen bond, which generates inversion dimers that stack along the a-axis direction. Full Article text
structure Crystal structures and Hirshfeld surface analyses of methyl 4-{2,2-dichloro-1-[(E)-phenyldiazenyl]ethenyl}benzoate, methyl 4-{2,2-dichloro-1-[(E)-(4-methylphenyl)diazenyl]ethenyl}benzoate and methyl 4- By journals.iucr.org Published On :: 2024-01-26 The crystal structures and Hirshfeld surface analyses of three similar azo compounds are reported. Methyl 4-{2,2-dichloro-1-[(E)-phenyldiazenyl]ethenyl}benzoate, C16H12Cl2N2O2, (I), and methyl 4-{2,2-dichloro-1-[(E)-(4-methylphenyl)diazenyl]ethenyl}benzoate, C17H14Cl2N2O2, (II), crystallize in the space group P21/c with Z = 4, and methyl 4-{2,2-dichloro-1-[(E)-(3,4-dimethylphenyl)diazenyl]ethenyl}benzoate, C18H16Cl2N2O2, (III), in the space group Poverline{1} with Z = 2. In the crystal of (I), molecules are linked by C—H⋯N hydrogen bonds, forming chains with C(6) motifs parallel to the b axis. Short intermolecular Cl⋯O contacts of 2.8421 (16) Å and weak van der Waals interactions between these chains stabilize the crystal structure. In (II), molecules are linked by C—H⋯O hydrogen bonds and C—Cl⋯π interactions, forming layers parallel to (010). Weak van der Waals interactions between these layers consolidate the molecular packing. In (III), molecules are linked by C—H⋯π and C—Cl⋯π interactions forming chains parallel to [011]. Furthermore, these chains are connected by C—Cl⋯π interactions parallel to the a axis, forming (0overline{1}1) layers. The stability of the molecular packing is ensured by van der Waals forces between these layers. Full Article text
structure Crystal structure, Hirshfeld surface analysis, crystal voids, interaction energy calculations and energy frameworks and DFT calculations of ethyl 2-cyano-3-(3-hydroxy-5-methyl-1H-pyrazol-4-yl)-3-phenylpropanoate By journals.iucr.org Published On :: 2024-01-31 The title compound, C16H17N3O3, is racemic as it crystallizes in a centrosymmetric space group (Poverline{1}), although the trans disposition of substituents about the central C—C bond is established. The five- and six-membered rings are oriented at a dihedral angle of 75.88 (8)°. In the crystal, N—H⋯N hydrogen bonds form chains of molecules extending along the c-axis direction that are connected by inversion-related pairs of O—H⋯N into ribbons. The ribbons are linked by C—H⋯π(ring) interactions, forming layers parallel to the ab plane. A Hirshfeld surface analysis indicates that the most important contributions for the crystal packing are from H⋯H (45.9%), H⋯N/N⋯H (23.3%), H⋯C/C⋯H (16.2%) and H⋯O/O⋯H (12.3%) interactions. Hydrogen bonding and van der Waals interactions are the dominant interactions in the crystal packing. The volume of the crystal voids and the percentage of free space were calculated to be 100.94 Å3 and 13.20%, showing that there is no large cavity in the crystal packing. Evaluation of the electrostatic, dispersion and total energy frameworks indicates that the stabilization is dominated by the electrostatic energy contributions in the title compound. Moreover, the DFT-optimized structure at the B3LYP/6–311 G(d,p) level is compared with the experimentally determined molecular structure in the solid state. The HOMO–LUMO behaviour was elucidated to determine the energy gap. Full Article text
structure Crystal structure, Hirshfeld surface analysis, crystal voids, interaction energy calculations and energy frameworks, and DFT calculations of 1-(4-methylbenzyl)indoline-2,3-dione By journals.iucr.org Published On :: 2024-01-31 The indoline portion of the title molecule, C16H13NO2, is planar. In the crystal, a layer structure is generated by C—H⋯O hydrogen bonds and C—H⋯π(ring), π-stacking and C=O⋯π(ring) interactions. The Hirshfeld surface analysis of the crystal structure indicates that the most important contributions for the crystal packing are from H⋯H (43.0%), H⋯C/C⋯H (25.0%) and H⋯O/O⋯H (22.8%) interactions. Hydrogen bonding and van der Waals interactions are the dominant interactions in the crystal packing. The volume of the crystal voids and the percentage of free space were calculated to be 120.52 Å3 and 9.64%, respectively, showing that there is no large cavity in the crystal packing. Evaluation of the electrostatic, dispersion and total energy frameworks indicate that the stabilization is dominated by the dispersion energy contributions in the title compound. Moreover, the DFT-optimized structure at the B3LYP/6-311G(d,p) level is compared with the experimentally determined molecular structure in the solid state. Full Article text
structure Cadmium phosphates Cd2(PO4)OH and Cd5(PO4)2(OH)4 crystallizing in mineral structures By journals.iucr.org Published On :: 2024-01-26 Single crystals of two basic cadmium phosphates, dicadmium orthophosphate hydroxide, Cd2(PO4)OH, and pentacadmium bis(orthophosphate) tetrakis(hydroxide), Cd5(PO4)2(OH)4, were obtained under hydrothermal conditions. Cd2(PO4)OH adopts the triplite [(Mn,Fe)2(PO4)F] structure type. Its asymmetric unit comprises two Cd, one P and five O sites, all situated at the general Wyckoff position 8 f of space group I2/a; two of the O atoms are positionally disordered over two sites, and the H atom could not be localized. Disregarding the disorder, distorted [CdO6] polyhedra form a tri-periodic network by edge-sharing with neighbouring [CdO6] units and by vertex-sharing with [PO4] units. The site associated with the OH group is coordinated by four Cd atoms in a distorted tetrahedral manner forming 1∞[(OH)Cd4/2] chains parallel to [001]. The oxygen environment around the OH site suggests multiple acceptor atoms for possible O—H⋯O hydrogen-bonding interactions and is the putative reason for the disorder. Cd5(PO4)2(OH)4 adopts the arsenoclasite [Mn5(AsO4)2(OH)4] structure type. Its asymmetric unit comprises five Cd, two P, and twelve O sites all located at the general Wyckoff position 4 a of space group P212121; the H atoms could not be localized. The crystal structure of Cd5(PO4)2(OH)4 can be subdivided into two main sub-units. One consists of three edge-sharing [CdO6] octahedra, and the other of two edge- and vertex-sharing [CdO6] octahedra. Each sub-unit forms corrugated ribbons extending parallel to [100]. The two types of ribbons are linked into the tri-periodic arrangement through vertex-sharing and through common [PO4] tetrahedra. Quantitative structure comparisons are made with isotypic M5(XO4)2(OH)4 crystal structures (M = Cd, Mn, Co; X = P, As, V). Full Article text
structure Synthesis, crystal structure and Hirshfeld surface analysis of 2-({5-[(naphthalen-1-yl)methyl]-4-phenyl-4H-1,2,4-triazol-3-yl}sulfanyl)-1-(4-nitrophenyl)ethanone By journals.iucr.org Published On :: 2024-01-26 The title compound, C27H20N4O3S, crystallizes in the monoclinic system, space group P21/n, with Z = 4. The global shape of the molecule is determined by the orientation of the substituents on the central 4H-1,2,4-triazole ring. The nitrophenyl ring, phenyl ring, and naphthalene ring system are oriented at dihedral angles of 82.95 (17), 77.14 (18) and 89.46 (15)°, respectively, with respect to the triazole ring. The crystal packing features chain formation in the b-axis direction by S⋯O interactions. A Hirshfeld surface analysis indicates that the highest contributions to surface contacts arise from contacts in which H atoms are involved. Full Article text
structure Crystal structure and Hirshfeld surface analysis of 4-(2-chloroethyl)-5-methyl-1,2-dihydropyrazol-3-one By journals.iucr.org Published On :: 2024-01-31 In the crystal of the title compound, C6H9ClN2O, molecular pairs form dimers with an R22(8) motif through N—H⋯O hydrogen bonds. These dimers are connect into ribbons parallel to the (100) plane with R44(10) motifs by N—H⋯O hydrogen bonds along the c-axis direction. In addition, π–π [centroid-to-centroid distance = 3.4635 (9) Å] and C—Cl⋯π interactions between the ribbons form layers parallel to the (100) plane. The three-dimensional consolidation of the crystal structure is also ensured by Cl⋯H and Cl⋯Cl interactions between these layers. According to a Hirshfeld surface study, H⋯H (43.3%), Cl⋯H/H⋯Cl (22.1%) and O⋯H/H⋯O (18.7%) interactions are the most significant contributors to the crystal packing. Full Article text
structure Crystal structure and characterization of a new lanthanide coordination polymer, [Pr2(pydc)(phth)2(H2O)3]·H2O By journals.iucr.org Published On :: 2024-01-31 A new lanthanide coordination polymer, poly[[triaquabis(μ4-phthalato)(μ3-pyridine-2,5-dicarboxylato)dipraseodymium] monohydrate], {[Pr2(C7H3NO4)2(C8H4O4)(H2O)3]·H2O}n or {[Pr2(phth)2(pydc)(H2O)3]·H2O}n, (pydc2− = pyridine-2,5-dicarboxylate and phth2− = phthalate) was synthesized and characterized, revealing the structure to be an assembly of di-periodic {Pr2(pydc)(phth)2(H2O)3}n layers. Each layer is built up by edge-sharing {Pr2N2O14} and {Pr2O16} dimers, which are connected through a new coordination mode of pydc2− and phth2−. These layers are stabilized by internal hydrogen bonds and π–π interactions. In addition, a three-dimensional supramolecular framework is built by interlayer hydrogen-bonding interactions involving the non-coordinated water molecule. Thermogravimetric analysis shows that the title compound is thermally stable up to 400°C. Full Article text
structure Crystal structure, Hirshfeld surface analysis and DFT study of N-(2-nitrophenyl)maleimide By journals.iucr.org Published On :: 2024-02-02 The title compound [systematic name: 1-(2-nitrophenyl)pyrrole-2,5-dione], C10H6N2O4, crystallizes in the monoclinic system (space group P21/n) with two molecules in the asymmetric unit, which are linked by C—H⋯O hydrogen bonds. Hirshfeld surface analysis showed that the most significant contributions to the crystal packing are from H⋯O/O⋯H, H⋯C/C⋯H and H⋯H interactions, which contribute 54.7%, 15.2% and 15.6%, respectively. A DFT study was conducted using three different levels of theory [(B3LYP/6–311+G(d,p), wB97XD/Def2TZVPP and LC-wpbe/6–311(2 d,2p)] in order to determine the stability, structural and electronic properties of the title molecule with a view to its potential applications and photochemical and copolymer properties. Full Article text
structure Synthesis and crystal structure of the adduct between 2-pyridylselenyl chloride and isobutyronitrile By journals.iucr.org Published On :: 2024-02-06 The reaction between 2-pyridylselenenyl chloride and isobutyronitrile results in the formation of the corresponding cationic pyridinium-fused 1,2,4-selenodiazole, namely, 3-(propan-2-yl)-1,2,4-[1,2,4]selenadiazolo[4,5-a]pyridin-4-ylium chloride, C9H11N2Se+·Cl−, in high yield (89%). The structure of the compound, established by means of single-crystal X-ray analysis at 100 K, has monoclinic (P21/c) symmetry and revealed the presence of bifurcated chalcogen-hydrogen bonding Se⋯Cl−⋯H—Cl, and these non-covalent contacts were analysed by DFT calculations followed by a topological analysis of the electron-density distribution (ωB97XD/6-311++G** level of theory). Full Article text
structure [4-(2-Aminoethyl)morpholine-κ2N,N']dibromidocadmium(II): synthesis, crystal structure and Hirshfeld surface analysis By journals.iucr.org Published On :: 2024-02-08 The title compound, [CdBr2(C6H14N2O)], was synthesized upon complexation of 4-(2-aminoethyl)morpholine and cadmium(II) bromide tetrahydrate at 303 K. It crystallizes as a centrosymmetric dimer, with one cadmium atom, two bromine atoms and one N,N'-bidentate 4-(2-aminoethyl)morpholine ligand in the asymmetric unit. The metal atom is six-coordinated and has a distorted octahedral geometry. In the crystal, O⋯Cd interactions link the dimers into a polymeric double chain and intermolecular C—H⋯O hydrogen bonds form R22(6) ring motifs. Further C—H⋯Br and N—H⋯Br hydrogen bonds link the components into a three-dimensional network. As the N—H⋯Br hydrogen bonds are shorter than the C—H⋯Br interactions, they have a larger effect on the packing. A Hirshfeld surface analysis reveals that the largest contributions to the packing are from H⋯H (46.1%) and Br⋯H/H⋯Br (38.9%) interactions with smaller contributions from the O⋯H/H⋯O (4.7%), Br⋯Cd/Cd⋯Br (4.4%), O⋯Cd/Cd⋯O (3.5%), Br⋯Br (1.1%), Cd⋯H/H⋯Cd (0.9%), Br⋯O/O⋯Br (0.3%) and O⋯N/N⋯O (0.1%) contacts. Full Article text
structure Crystal structure and Hirshfeld surface analysis of (Z)-N-{chloro[(4-ferrocenylphenyl)imino]methyl}-4-ferrocenylaniline N,N-dimethylformamide monosolvate By journals.iucr.org Published On :: 2024-02-02 The title molecule, [Fe2(C5H5)2(C23H17ClN2)]·C3H7NO, is twisted end to end and the central N/C/N unit is disordered. In the crystal, several C—H⋯π(ring) interactions lead to the formation of layers, which are connected by further C—H⋯π(ring) interactions. A Hirshfeld surface analysis of the crystal structure indicates that the most important contributions for the crystal packing are from H⋯H (60.2%) and H⋯C/C⋯H (27.0%) interactions. Hydrogen bonding, C—H⋯π(ring) interactions and van der Waals interactions dominate the crystal packing. Full Article text
structure Crystal structures of sulfonamide protected bicyclic guanidines: (S)-8-{[(tert-butyldimethylsilyl)oxy]methyl}-1-[(2,2,4,6,7-pentamethyl-2,3-dihydrobenzofuran-5-yl)sulfonyl]-1,3,4,6,7,8-hexa By journals.iucr.org Published On :: 2024-02-20 Two compounds, (S)-8-{[(tert-butyldimethylsilyl)oxy]methyl}-1-[(2,2,4,6,7-pentamethyl-2,3-dihydrobenzofuran-5-yl)sulfonyl]-1,3,4,6,7,8-hexahydro-2H-pyrimido[1,2-a]pyrimidin-1-ium trifluoromethanesulfonate, C27H46N3O4SSi+·CF3O3S−, (1) and (S)-8-(iodomethyl)-1-tosyl-1,3,4,6,7,8-hexahydro-2H-pyrimido[1,2-a]pyrimidin-1-ium iodide, C15H21IN3O2S+·I−, (2), have been synthesized and characterized. They are bicyclic guanidinium salts and were synthesized from N-(tert-butoxycarbonyl)-l-methionine (Boc-l-Met-OH). The guanidine is protected by a 2,2,4,6,7-pentamethyldihydrobenzofuran-5-sulfonyl (Pbf, 1) or a tosyl (2) group. In the crystals of both compounds, the guanidinium group is almost planar and the N–H forms an intramolecular hydrogen bond in a six-membered ring to the oxygen atom of the sulfonamide protecting group. Full Article text
structure Crystal structure of diethylammonium dioxido{Z)-N-[(pyridin-2-yl)carbonylazanidyl]pyridine-2-carboximidato}vanadate(1−) monohydrate By journals.iucr.org Published On :: 2024-02-08 The title compound, (C4H12N)[V(C12H8N4O2)O2]·H2O, was synthesized via aerial oxidation on refluxing picolinohydrazide with ethyl picolinate followed by addition of VIVO(acac)2 and diethylamine in methanol. It crystallizes in the triclinic crystal system in space group Poverline{1}. In the complex anion, the dioxidovanadium(V) moiety exhibits a distorted square-pyramidal geometry. In the crystal, extensive hydrogen bonding links the water molecule to two complex anions and one diethylammonium ion. One of the CH2 groups in the diethylamine is disordered over two sets of sites in a 0.7:0.3 ratio. Full Article text
structure Syntheses, characterizations, crystal structures and Hirshfeld surface analyses of methyl 4-[4-(difluoromethoxy)phenyl]-2,7,7-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate, isopropyl 4-[4-(difluoro& By journals.iucr.org Published On :: 2024-02-08 The crystal structures and Hirshfeld surface analyses of three similar compounds are reported. Methyl 4-[4-(difluoromethoxy)phenyl]-2,7,7-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate, (C21H23F2NO4), (I), crystallizes in the monoclinic space group C2/c with Z = 8, while isopropyl 4-[4-(difluoromethoxy)phenyl]-2,6,6-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate, (C23H27F2NO4), (II) and tert-butyl 4-[4-(difluoromethoxy)phenyl]-2,6,6-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate, (C24H29F2NO4), (III) crystallize in the orthorhombic space group Pbca with Z = 8. In the crystal structure of (I), molecules are linked by N—H⋯O and C—H⋯O interactions, forming a tri-periodic network, while molecules of (II) and (III) are linked by N—H⋯O, C—H⋯F and C—H⋯π interactions, forming layers parallel to (002). The cohesion of the molecular packing is ensured by van der Waals forces between these layers. In (I), the atoms of the 4-difluoromethoxyphenyl group are disordered over two sets of sites in a 0.647 (3): 0.353 (3) ratio. In (III), the atoms of the dimethyl group attached to the cyclohexane ring, and the two carbon atoms of the cyclohexane ring are disordered over two sets of sites in a 0.646 (3):0.354 (3) ratio. Full Article text
structure Crystal structure of 4-(benzo[d]thiazol-2-yl)-1,2-dimethyl-1H-pyrazol-3(2H)-one By journals.iucr.org Published On :: 2024-02-16 In the title compound, C12H11N3OS, the interplanar angle between the pyrazole and benzothiazole rings is 3.31 (7)°. In the three-dimensional molecular packing, the carbonyl oxygen acts as acceptor to four C—H donors (with one H⋯O as short as 2.25 Å), while one methyl hydrogen is part of the three-centre system H⋯(S, O). A double layer structure parallel to (overline{1}01) can be recognized as a subsection of the packing. Full Article text
structure Crystal structure of the tetraethylammonium salt of the non-steroidal anti-inflammatory drug nimesulide (polymorph II) By journals.iucr.org Published On :: 2024-02-20 The crystal structure of the tetraethylammonium salt of the non-steroidal anti-inflammatory drug nimesulide (polymorph II) (systematic name: tetraethylammonium N-methanesulfonyl-4-nitro-2-phenoxyanilinide), C8H20N+·C13H11N2O5S−, was determined using single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic space group P21/c with one tetraethylammonium cation and one nimesulide anion in the asymmetric unit. In the crystal, the ions are linked by C—H⋯N and C—H⋯O hydrogen bonds and C—H⋯π interactions. There are differences in the geometry of both the nimesulide anion and the tetraethylammonium cation in polymorphs I [Rybczyńska & Sikorski (2023). Sci. Rep. 13, 17268] and II of the title compound. Full Article text
structure Crystal structure and characterization of a new one-dimensional copper(II) coordination polymer containing a 4-aminobenzoic acid ligand By journals.iucr.org Published On :: 2024-02-20 A CuII coordination polymer, catena-poly[[[aquacopper(II)]-bis(μ-4-aminobenzoato)-κ2N:O;κ2O:N] monohydrate], {[Cu(pABA)2(H2O)]·H2O}n (pABA = p-aminobenzoate, C7H4NO2−), was synthesized and characterized. It exhibits a one-dimensional chain structure extended into a three-dimensional supramolecular assembly through hydrogen bonds and π–π interactions. While the twinned crystal shows a metrically orthorhombic lattice and an apparent space group Pbcm, the true symmetry is monoclinic (space group P2/c), with disordered Cu atoms and mixed roles of water molecules (aqua ligand/crystallization water). The luminescence spectrum of the complex shows an emission at 345 nm, cf. 349 nm for pABAH. Full Article text
structure Crystal structure of the sodium salt of mesotrione: a triketone herbicide By journals.iucr.org Published On :: 2024-02-16 The crystal structure of the sodium salt of mesotrione, namely, catena-poly[[sodium-μ3-2-[(4-methanesulfonyl-2-nitrophenyl)carbonyl]-3-oxocyclohex-1-en-1-olato] ethanol monosolvate], {[Na(C14H12NO7S)]C2H5OH}n, is described. The X-ray structural analysis results reveal that the coordination sphere is established by two chelating O atoms, the O atom of the coordinated ethanol molecule, and an O atom from the methylsulfonyl group of a neighboring molecule. Simultaneously, an O atom of the cyclohexane fragment serves as a bridge to a neighboring sodium ion, forming a flat Na–O–Na–O quadrangle, thereby forming a mono-periodic polymer. The structure displays O—H⋯O hydrogen bonds and C—H⋯O short contacts. Thermogravimetric analysis (TGA) data indicate that the sodium salt of mesotrione decomposes in four stages. Full Article text
structure Synthesis, characterization, and crystal structure of 2-(2-azidophenyl)-3-oxo-3H-indole 1-oxide By journals.iucr.org Published On :: 2024-02-20 An attempt to explore the reactivity of the nitro group in the presence of gold catalysis in comparison to the azide group yielded intriguing results. Surprisingly, only the nitro group exhibited reactivity, ultimately giving rise to the formation of the title isatogen, C14H8N4O2. In the crystal structure, weak C—H⋯O hydrogen bonds and π–π stacking interactions link the molecules. The structure exhibits disorder of the molecule. Full Article text
structure Crystal structure and Hirshfeld surface analysis of 3-phenyl-1-{3-[(3-phenylquinoxalin-2-yl)oxy]propyl}-1,2-dihydroquinoxalin-2-one By journals.iucr.org Published On :: 2024-02-20 In the title compound, C31H24N4O2, the quinoxaline units are distinctly non-planar and twisted end-to-end. In the crystal, C—H⋯O and C—H⋯N hydrogen bonds link the molecules into chains extending along the a-axis direction. The chains are linked through π-stacking interactions between inversion-related quinoxaline moieties. Full Article text
structure Synthesis and crystal structures of bis[1-oxopyridin-2-olato(1−)]bis(pentafluorophenyl)silicon(IV)–tetrahydrofuran–pentane (2/1/1), bis[1-oxopyridin-2-olato(1−)]bis(p-tolyl)silicon(IV), and dimes By journals.iucr.org Published On :: 2024-02-20 The neutral organosilicon(IV) complex, (C6F5)2Si(OPO)2 (OPO = 1-oxopyridin-2-one, C5H4NO2), was synthesized from (C6F5)2Si(OCH3)2 and 2 equiv. of 1-hydroxypyridin-2-one in tetrahydrofuran (THF). Single crystals grown from the diffusion of n-pentane into a THF solution were identified as a THF hemisolvate and an n-pentane hemisolvate, (C6F5)2Si(OPO)2·0.5THF·0.5C5H12 (1). p-Tolyl2Si(OPO)2 (2) and mesityl2Si(OPO)2 (3) crystallized directly from reaction mixtures of 2 equiv. of Me3Si(OPO) with p-tolyl2SiCl2 and mesityl2SiCl2, respectively, in acetonitrile. The oxygen-bonded carbon and nitrogen atoms of the OPO ligands in 1, 2, and 3 were modeled as disordered indicating co-crystallization of up to three possible diastereomers in each. Solution NMR studies support the presence of exclusively the all-cis isomer in 1 and multiple isomers in 2. Poor solubility of 3 limited its characterization in solution. Full Article text
structure Synthesis, crystal structure and Hirshfeld surface analysis of N-(6-acetyl-1-nitronaphthalen-2-yl)acetamide By journals.iucr.org Published On :: 2024-03-06 The title compound, C14H12N2O4, was obtained from 2-acetyl-6-aminonaphthalene through two-step reactions of acetylation and nitration. The molecule comprises the naphthalene ring system consisting of functional systems bearing a acetyl group (C-2), a nitro group (C-5), and an acetylamino group (C-6). In the crystal, the molecules are assembled into two-dimensional sheet-like structures by intermolecular N—H⋯O and C—H⋯O hydrogen-bonding interactions. Hirshfeld surface analysis illustrates that the most important contributions to the crystal packing are from O⋯H/H⋯O (43.7%), H⋯H (31.0%), and C⋯H/H⋯C (8.5%) contacts. Full Article text
structure Crystal structure and Hirshfeld surface analysis of 4-oxo-3-phenyl-2-sulfanylidene-5-(thiophen-2-yl)-3,4,7,8,9,10-hexahydro-2H-pyrido[1,6-a:2,3-d']dipyrimidine-6-carbonitrile By journals.iucr.org Published On :: 2024-02-20 In the title compound, C21H15N5OS2, molecular pairs are linked by N—H⋯N hydrogen bonds along the c-axis direction and C—H⋯S and C—H⋯O hydrogen bonds along the b-axis direction, with R22(12) and R22(16) motifs, respectively, thus forming layers parallel to the (10overline{4}) plane. In addition, C=S⋯π and C≡N⋯π interactions between the layers ensure crystal cohesion. The Hirshfeld surface analysis indicates that the major contributions to the crystal packing are H⋯H (43.0%), C⋯H/H⋯C (16.9%), N⋯H/H⋯N (11.3%) and S⋯H/H⋯S (10.9%) interactions. Full Article text
structure Crystal structure of tetrakis(μ-2-hydroxy-3,5-diisopropylbenzoato)bis[(dimethyl sulfoxide)copper(II)] By journals.iucr.org Published On :: 2024-02-27 Metal complexes of 3,5-diisopropylsalicylate are reported to have anti-inflammatory and anti-convulsant activities. The title binuclear copper complex, [Cu2(C13H17O3)4(C2H6OS)2] or [Cu(II)2(3,5-DIPS)4(DMSO)2], contains two five-coordinate copper atoms that are bridged by four 3,5-diisopropylsalicylate ligands and capped by two axial dimethyl sulfoxide (DMSO) moieties. Each copper atom is attached to four oxygen atoms in an almost square-planar fashion, with the addition of a DMSO ligand in an apical position leading to a square-pyramidal arrangement. The hydroxy group of the diisopropylsalicylate ligands participates in intramolecular O—H⋯O hydrogen-bonding interactions. Full Article text
structure Crystal structure of 1-{4-[bis(4-methylphenyl)amino]phenyl}ethene-1,2,2-tricarbonitrile By journals.iucr.org Published On :: 2024-02-29 The title compound, C25H18N4, crystallizes in the centrosymmetric orthorhombic space group Pbca, with eight molecules in the unit cell. The main feature noticeable in the structure is the impact of the tricyanovinyl (TCV) group in forcing partial planarity of the portion of the molecule carrying the TCV group and directing the molecular packing in the solid state, resulting in the formation of π-stacks of dimers within the unit cell. Short π–π stack closest atom-to-atom distances of 3.444 (15) Å are observed. Such motif patterns are favorable as they are thought to be conducive for better charge transport in organic semiconductors, which results in enhanced device performance. Intramolecular charge transfer is evident from the shortening in the observed experimental bond lengths. The nitrogen atoms (of the cyano groups) are involved in extensive short contacts, primarily through C—H⋯NC interactions with distances of 2.637 (17) Å. Full Article text
structure Crystal structure of (S)-5-(3-acetyl-5-chloro-2-ethoxy-6-fluorophenyl)-2-oxazolidinone By journals.iucr.org Published On :: 2024-03-19 The structure of (S)-5-(3-acetyl-5-chloro-2-ethoxy-6-fluorophenyl)-2-oxazolidinone, C13H13ClFNO4, at 100 K has monoclinic (P21) symmetry. The compound has a polymeric structure propagated by a screw axis parallel to the b axis with N—H⋯O hydrogen bonding. It is of interest with respect to efforts in the synthesis of a candidate anticancer drug, parsaclisib. Full Article text
structure Crystal structures of ten phosphane chalcogenide complexes of gold(III) chloride and bromide By journals.iucr.org Published On :: 2024-03-12 The structures of ten phosphane chalcogenide complexes of gold(III) halides, with general formula R13–nR2nPEAuX3 (R1 = t-butyl; R2 = i-propyl; n = 0 to 3; E = S or Se; X = Cl or Br) are presented. The eight possible chlorido derivatives are: 9a, n = 3, E = S; 10a, n = 2, E = S; 11a, n = 1, E = S; 12a, n = 0, E = S; 13a, n = 3, E = Se; 14a, n = 2, E = Se; 15a, n = 1, E = Se; and 16a, n = 0, E = Se, and the corresponding bromido derivatives are 9b–16b in the same order. Structures were obtained for 9a, 10a (and a second polymorph 10aa), 11a (and its deuterochloroform monosolvate 11aa), 12a (as its dichloromethane monosolvate), 14a, 15a (as its deuterochloroform monosolvate 15aa, in which the solvent molecule is disordered over two positions), 9b, 11b, 13b and 15b. The structures of 11a, 15a, 11b and 15b form an isotypic set, and those of compounds 10aa and 14a form an isotypic pair. All structures have Z' = 1. The gold(III) centres show square-planar coordination geometry and the chalcogenide atoms show approximately tetrahedral angles (except for the very wide angle in 12a, probably associated with the bulky t-butyl groups). The bond lengths at the gold atoms are lengthened with respect to the known gold(I) derivatives, and demonstrate a considerable trans influence of S and Se donor atoms on a trans Au—Cl bond. Each compound with an isopropyl group shows a short intramolecular contact of the type C—Hmethine⋯Xcis; these may be regarded as intramolecular ‘weak’ hydrogen bonds, and they determine the orientation of the AuX3 groups. The molecular packing is analysed in terms of various short contacts such as weak hydrogen bonds C—H⋯X and contacts between the heavier atoms, such as X⋯X (9a, 10aa, 11aa, 15aa and 9b), S⋯S (10aa, 11a and 12a) and S⋯Cl (10a). The packing of the polymorphs 10a and 10aa is thus quite different. The solvent molecules take part in C—H⋯Cl hydrogen bonds; for 15aa, a disordered solvent region at z ≃ 0 is observed. Structure 13b involves unusual inversion-symmetric dimers with Se⋯Au and Se⋯Br contacts, further connected by Br⋯Br contacts. Full Article text
structure Crystal structure of tetraphenyl phosphate tetrakis[dimethyl (2,2,2-trichloroacetyl)phosphoramidato]lutetium(III), PPh4[LuL4] By journals.iucr.org Published On :: 2024-03-12 A lutetium(III) complex based on the anion of the ligand dimethyl (2,2,2-trichloroacetyl)phosphoramidate (HL) and tetraphenylphosphonium, of composition PPh4[LuL4] (L = CAPh = carbacylamidophosphate), or (C24H20)[Lu(C4H6Cl3NO4P)4], has been synthesized and structurally characterized. The X-ray diffraction study of the compound revealed that the lutetium ion is surrounded by four bis-chelating CAPh ligands, forming the complex anion [LuL4]− with a coordination number of 8[O] for LuIII, while PPh4+ serves as a counter-ion. The coordination geometry around the Lu3+ ion was determined to be a nearly perfect triangular dodecahedron. The complex crystallizes in the monoclinic crystal system, space group P21/c, with four molecules in the unit cell. Weak hydrogen bonds O⋯HC(Ph), Cl⋯HC(Ph) and N⋯HC(Ph) are formed between the cations and anions. For a comparative study, HL-based structures were retrieved from the Cambridge Structural Database (CSD) and their geometries and conformations are discussed. A Hirshfeld surface analysis was also performed. Full Article text
structure Crystal structure and Hirshfeld surface analysis of 8-benzyl-1-[(4-methylphenyl)sulfonyl]-2,7,8,9-tetrahydro-1H-3,6:10,13-diepoxy-1,8-benzodiazacyclopentadecine ethanol hemisolvate By journals.iucr.org Published On :: 2024-03-26 The asymmetric unit of the title compound, 2C31H28N2O4S·C2H6O, contains a parent molecule and a half molecule of ethanol solvent. The main compound stabilizes its molecular conformation by forming a ring with an R12(7) motif with the ethanol solvent molecule. In the crystal, molecules are connected by C—H⋯O and O—H⋯O hydrogen bonds, forming a three-dimensional network. In addition, C—H⋯π interactions also strengthen the molecular packing. Full Article text
structure Crystal structure and Hirshfeld surface analysis of 4,4'-dimethoxybiphenyl-3,3',5,5'-tetracarboxylic acid dihydrate By journals.iucr.org Published On :: 2024-03-26 In the crystal of the title compound, C18H14O10·2H2O, the arene rings of the biphenyl moiety are tilted at an angle of 24.3 (1)°, while the planes passing through the carboxyl groups are rotated at angles of 8.6 (1) and 7.7 (1)° out of the plane of the benzene ring to which they are attached. The crystal structure is essentially stabilized by O—H⋯O bonds. Here, the carboxyl groups of neighbouring host molecules are connected by cyclic R22(8) synthons, leading to the formation of a three-dimensional network. The water molecules in turn form helical supramolecular strands running in the direction of the crystallographic c-axis (chain-like water clusters). The second H atom of each water molecule provides a link to a methoxy O atom of the host molecule. A Hirshfeld surface analysis was performed to quantify the contributions of the different intermolecular interactions, indicating that the most important contributions to the crystal packing are from H⋯O/O⋯H (37.0%), H⋯H (26.3%), H⋯C/C⋯H (18.5%) and C⋯O/O⋯C (9.5%) interactions. Full Article text
structure Crystal structure, Hirshfeld surface analysis, calculations of crystal voids, interaction energy and energy frameworks as well as density functional theory (DFT) calculations of 3-[2-(morpholin-4-yl)ethyl]-5,5-diphenylimidazolidine By journals.iucr.org Published On :: 2024-03-26 In the title molecule, C21H23N3O3, the imidazolidine ring slightly deviates from planarity and the morpholine ring exhibits the chair conformation. In the crystal, N—H⋯O and C—H⋯O hydrogen bonds form helical chains of molecules extending parallel to the c axis that are connected by C—H⋯π(ring) interactions. A Hirshfeld surface analysis reveals that the most important contributions for the crystal packing are from H⋯H (55.2%), H⋯C/C⋯H (22.6%) and H⋯O/O⋯H (20.5%) interactions. The volume of the crystal voids and the percentage of free space were calculated to be 236.78 Å3 and 12.71%, respectively. Evaluation of the electrostatic, dispersion and total energy frameworks indicates that the stabilization is dominated by the nearly equal electrostatic and dispersion energy contributions. The DFT-optimized molecular structure at the B3LYP/6-311 G(d,p) level is compared with the experimentally determined molecular structure in the solid state. Moreover, the HOMO–LUMO behaviour was elucidated to determine the energy gap. Full Article text
structure Crystal structure and Hirshfeld surface analysis of 6-imino-8-(4-methylphenyl)-1,3,4,6-tetrahydro-2H-pyrido[1,2-a]pyrimidine-7,9-dicarbonitrile By journals.iucr.org Published On :: 2024-03-21 In the ten-membered 1,3,4,6-tetrahydro-2H-pyrido[1,2-a]pyrimidine ring system of the title compound, C17H15N5, the 1,2-dihydropyridine ring is essentially planar (r.m.s. deviation = 0.001 Å), while the 1,3-diazinane ring has a distorted twist-boat conformation. In the crystal, molecules are linked by N—H⋯N and C—H⋯N hydrogen bonds, forming a three-dimensional network. In addition, C—H⋯π interactions form layers parallel to the (100) plane. Thus, crystal-structure cohesion is ensured. According to a Hirshfeld surface study, H⋯H (40.4%), N⋯H/H⋯N (28.6%) and C⋯H/H⋯C (24.1%) interactions are the most important contributors to the crystal packing. Full Article text
structure Synthesis and crystal structure of N-phenyl-2-(phenylsulfanyl)acetamide By journals.iucr.org Published On :: 2024-03-26 N-Phenyl-2-(phenylsulfanyl)acetamide, C14H13NOS, was synthesized and structurally characterized. In the crystal, N—H⋯O hydrogen bonding leads to the formation of chains of molecules along the [100] direction. The chains are linked by C—H⋯π interactions, forming a three-dimensional network. The crystal studied was twinned by a twofold rotation around [100]. Full Article text
structure Crystal structure of 2,4-diamino-5-(4-hydroxy-3-methoxyphenyl)-8,8-dimethyl-6-oxo-6,7,8,9-tetrahydro-5H-chromeno[2,3-b]pyridine-3-carbonitrile–dimethylformamide–water (1/1/1) By journals.iucr.org Published On :: 2024-03-26 In the structure of the title compound, C22H22N4O4·C3H7NO·H2O, the entire tricyclic system is approximately planar except for the carbon atom bearing the two methyl groups; the methoxyphenyl ring is approximately perpendicular to the tricycle. All seven potential hydrogen-bond donors take part in classical hydrogen bonds. The main molecule and the DMF combine to form broad ribbons parallel to the a axis and roughly parallel to the ab plane; the water molecules connect the residues in the third dimension. Full Article text
structure Synthesis, crystal structure and Hirshfeld surface analysis of 2-phenyl-3-(prop-2-yn-1-yloxy)quinoxaline By journals.iucr.org Published On :: 2024-03-21 In the title compound, C17H12N2O, the quinoxaline moiety shows deviations of 0.0288 (7) to −0.0370 (7) Å from the mean plane (r.m.s. deviation of fitted atoms = 0.0223 Å). In the crystal, corrugated layers two molecules thick are formed by C—H⋯N hydrogen bonds and π-stacking interactions. Full Article text
structure Crystal structure and Hirshfeld surface analysis of ethyl 2-(7-chloro-3-methyl-2-oxo-1,2-dihydroquinoxalin-1-yl)acetate By journals.iucr.org Published On :: 2024-03-26 The quinoxaline moiety in the title molecule, C13H13ClN2O3, is almost planar (r.m.s. deviation of the fitted atoms = 0.033 Å). In the crystal, C—H⋯O hydrogen bonds plus slipped π-stacking and C—H⋯π(ring) interactions generate chains of molecules extending along the b-axis direction. The chains are connected by additional C—H⋯O hydrogen bonds. Hirshfeld surface analysis indicates that the most important contributions to the crystal packing are from H⋯H (37.6%), H⋯O/O⋯H (22.7%) and H⋯Cl/Cl⋯H (13.1%) interactions. Full Article text
structure Synthesis, crystal structure and Hirshfeld surface analysis of bromidotetrakis[5-(prop-2-en-1-ylsulfanyl)-1,3,4-thiadiazol-2-amine-κN3]copper(II) bromide By journals.iucr.org Published On :: 2024-03-26 A novel cationic complex, bromidotetrakis[5-(prop-2-en-1-ylsulfanyl)-1,3,4-thiadiazol-2-amine-κN3]copper(II) bromide, [CuBr](C5H7N3S2)4Br, was synthesized. The complex crystallizes with fourfold molecular symmetry in the tetragonal space group P4/n. The CuII atom exhibits a square-pyramidal coordination geometry. The Cu atom is located centrally within the complex, being coordinated by four nitrogen atoms from four AAT molecules, while a bromine anion is located at the apex of the pyramid. The amino H atoms of AAT interact with bromine from the inner and outer spheres, forming a two-dimensional network in the [100] and [010] directions. Hirshfeld surface analysis reveals that 33.7% of the intermolecular interactions are from H⋯H contacts, 21.2% are from S⋯H/H⋯S contacts, 13.4% are from S⋯S contacts and 11.0% are from C⋯H/H⋯C, while other contributions are from Br⋯H/H⋯Br and N⋯H/H⋯N contacts. Full Article text