i 5,6-Dimethylbenzo[d][1,3]oxatellurole By journals.iucr.org Published On :: 2024-01-05 The structure of the title compound, C9H10OTe, at 100 K has orthorhombic (P21212) symmetry with two independent molecules in the asymmetric unit (Z' = 2). The molecules are folded along their Te⋯O axes, with their Te–C–O planes angled at an average of 25.1° with respect to the remaining non-H atoms, which are almost coplanar (average deviation from planarity = 0.04 Å). A Hirshfeld plot shows weak intermolecular interactions between the two Te atoms located in each asymmetric molecule, with a Te⋯Te distance of 3.7191 (4) Å. The structure is strongly pseudosymmetric to the space group Pccn with Z' = 1. The crystal chosen for data collection was found to be was an inversion twin. Full Article text
i Bis[1,3-bis(2,4,6-trimethylphenyl)imidazolium] bis(μ-cis-1,2-diphenylethene-1,2-dithiolato-κ2S,S':κS)bis[(cis-1,2-diphenylethene-1,2-dithiolato-κ2S,S')iron(III)] dimethyl& By journals.iucr.org Published On :: 2023-12-26 The molecular structure of the solvated title salt, (C21H25N2)2[Fe2(C14H10S2)4]·2C3H7NO reveals that the anion is situated on a crystallographic inversion center in the triclinic space group Poverline{1}. The title compound crystallizes utilizing a network of weak π-stacking interactions of phenyl rings pertaining to the dithiolene unit. Moreover, the acidic imidazolium H atoms [N—C(H)—N] display non-classical hydrogen-bonding interactions of the C—H⋯O type to the oxygen atoms of the N,N-dimethyl formamide solvent, and hydrogen atoms on the backbone of imidazolium rings display weak C—H⋯S interactions with the dithiolene sulfur atoms. Full Article text
i meso-α,α-5,15-Bis(o-nicotinamidophenyl)-10,20-diphenylporphyrin n-hexane monosolvate By journals.iucr.org Published On :: 2023-12-22 The structure of the title solvated porphyrin, C56H38N8O2·C6H14, is reported. Two porphyrin molecules, one ordered and one disordered n-hexane solvate molecules are present in its asymmetric unit. The porphyrin macrocycle shows a characteristic saddle-shaped distortion, and the maximum deviation from the mean plane for non-hydrogen atoms is 0.48 Å. N—H⋯N, N—H⋯O, and C—H⋯O hydrogen bonds, as well as π–π interactions, are observed in the crystal structure. Full Article text
i rac-Hydroxyisovaleric acid By journals.iucr.org Published On :: 2024-01-05 The title compound (systematic name: rac-2-hydroxy-3-methylbutanoic acid), C5H10O3, is the constitutional isomer of α-hydroxybutanoic acid. In the crystal, hydrogen bonds involving the alcoholic hydroxyl group give rise to centrosymmetric dimers that are extended to sheets perpendicular to the crystallographic c axis. Full Article text
i 2-{3-Methyl-2-[(2Z)-pent-2-en-1-yl]cyclopent-2-en-1-ylidene}-N-phenylhydrazinecarbothioamide. Corrigendum By journals.iucr.org Published On :: 2024-01-31 In the paper by Oliveira et al. [IUCrData (2023), 8, x230971], there was an error in the name of the first author. Full Article text
i N-Methyl-2-{3-methyl-2-[(2Z)-pent-2-en-1-yl]cyclopent-2-en-1-ylidene}hydrazinecarbothioamide By journals.iucr.org Published On :: 2024-01-09 The equimolar and hydrochloric acid-catalysed reaction between cis-jasmone and 4-methylthiosemicarbazide in ethanolic solution yields the title compound, C13H21N3S (common name: cis-jasmone 4-methylthiosemicarbazone). Two molecules with all atoms in general positions are present in the asymmetric unit. In one of them, the carbon chain is disordered [site occupancy ratio = 0.821 (3):0.179 (3)]. The thiosemicarbazone entities [N—N—C(=S)—N] are approximately planar, with the maximum deviation from the mean plane through the selected atoms being −0.0115 (16) Å (r.m.s.d. = 0.0078 Å) for the non-disordered molecule and 0.0052 (14) Å (r.m.s.d. = 0.0031 Å) for the disordered one. The molecules are not planar, since the jasmone groups have a chain with sp3-hybridized carbon atoms and, in addition, the thiosemicarbazone fragments are attached to the respective carbon five-membered rings and the dihedral angles between them for each molecule amount to 8.9 (1) and 6.3 (1)°. In the crystal, the molecules are connected through pairs of N—H⋯S and C—H⋯S interactions into crystallographically independent centrosymmetric dimers, in which rings of graph-set motifs R22(8) and R21(7) are observed. A Hirshfeld surface analysis indicates that the major contributions for the crystal cohesion are from H⋯H (70.6%), H⋯S/S⋯H (16.7%), H⋯C/C⋯H (7.5%) and H⋯N/N⋯H (4.9%) interactions [considering the two crystallographically independent molecules and only the disordered atoms with the highest s.o.f. for the evaluation]. Full Article text
i trans-Dichloridobis[(S)-(−)-1-(4-methylphenyl)ethylamine-κN]palladium(II) By journals.iucr.org Published On :: 2024-01-12 The title complex, [PdCl2(C9H13N)2], comprises a single molecule in the asymmetric unit. The PdII atom is tetracoordinated by two N atoms from two trans-aligned organic ligands and two Cl ligands, forming a square-planar metal coordination environment. The distances from the ortho-H atoms on the phenyl ring to the central PdII atom fall within the range 4.70–5.30 Å, precluding any significant intramolecular Pd⋯H interactions. Full Article text
i Dichlorido(4,7-dimethoxy-1,10-phenanthroline-κ2N,N')zinc(II) By journals.iucr.org Published On :: 2024-01-12 In the title complex, [ZnCl2(C14H12N2O2)], the ZnII atom is located on a twofold rotation axis and is fourfold coordinated by two chlorido ligands and a bidentate 4,7-methoxy-1,10-phenanthroline ligand in a distorted tetrahedral environment. Weak π–π stacking interactions between adjacent 4,7-dimethoxy-1,10-phenanthroline rings [centroid-to-centroid distances = 3.5969 (11) and 3.7738 (11) Å] contribute to the alignment of the complexes in layers parallel to (overline{2}01). Full Article text
i 2-Aminobenzoxazole–oxalic acid (2/1) By journals.iucr.org Published On :: 2024-01-26 In the title compound, 2C7H7N2O+·C2O42−, proton transfer from oxalic acid to the N atom of the heterocycle has occurred to form a 2:1 molecular salt. In the extended structure, N—H⋯O hydrogen bonds link the components into [100] chains, which feature R22(8) and R44(14) loops. Full Article text
i Synthesis and structure of trans-bis(4-amino-3-nitrobenzoato-κO)bis(4-amino-3-nitrobenzoic acid-κO)diaquamanganese(II) dihydrate By journals.iucr.org Published On :: 2024-01-19 The manganese title complex, [Mn(C7H5N2O4)2(C7H6N2O4)2(H2O)2]·2H2O, is one of the first 4-amino 3-nitrobenzoic acid (4 A3NBA) monoligand metal complexes to be synthesized. It crystallizes in the centrosymmetric monoclinic space group P21/n with the complex molecules located on inversion centers. Four 4 A3NBA ligand molecules are monodentately coordinated by the Mn2+ ion through the carboxylic oxygen atoms while the other two positions of the inner coordination sphere are occupied by water molecules, giving rise to a distorted octahedron, and two water molecules are in the outer coordination sphere. There are two intramolecular hydrogen bonds in the complex molecule. The first is of the common N—H⋯O=N type, while the second is a rarely occurring very strong hydrogen bond in which a common proton is shared by two uncoordinated oxygen atoms of neighboring carboxylate groups. In the crystal, an intricate system of intermolecular hydrogen bonds links the complex molecules into a three-dimensional-network. Full Article text
i Crystal structure of Ti4Ni2C By journals.iucr.org Published On :: 2024-01-19 Single crystals of the intermetallic phase with composition Ti4Ni2C were serendipitously obtained by high-pressure sintering of a mixture with initial chemical composition Ti2Ni. The Ti4Ni2C phase crystallizes in the Fdoverline{3}m space group and can be considered as a partially filled Ti2Ni structure with the C atom occupying an octahedral void. Ti4Ni2C is isotypic with Ti4Ni2O, Nb4Ni2C and Ta4Ni2C, all of which were studied previously by means of powder diffraction. Full Article text
i Bis(2-hydroxy-2,3-dihydro-1H-inden-1-aminium) tetrachloridopalladate(II) hemihydrate By journals.iucr.org Published On :: 2024-01-26 A new square-planar palladium complex salt hydrate, (C9H12NO)2[PdCl4]·0.5H2O, has been characterized. The asymmetric unit of the complex salt comprises two [PdCl4]2− dianions, four 2-hydroxy-2,3-dihydro-1H-inden-1-aminium cations, each derived from (1R,2S)-(+)-1-aminoindan-2-ol, and one water molecule of crystallization. In the crystal, a two-dimensional layer parallel to (001) features a number of O—H⋯O, N—H⋯O, O—H⋯Cl and N—H⋯Cl hydrogen bonds. Full Article text
i (4-Butyl-1-ethyl-1,2,4-triazol-5-ylidene)[(1,2,5,6-η)-cycloocta-1,5-diene](triphenylphosphane)rhodium(I) tetrafluoridoborate By journals.iucr.org Published On :: 2024-01-26 In the title triazole-based N-heterocyclic carbene rhodium(I) cationic complex with a tetrafluoridoborate counter-anion, [Rh(C8H12)(C8H15N3)(C18H15P)]BF4, which crystallizes with two cations and two anions in the asymmetric unit, the Rh center has a distorted square-planar coordination geometry with expected bond distances. Several nonclassical C—H⋯F hydrogen-bonding interactions help to consolidate the packing. Two of the F atoms of one of the anions are disordered over adjacent sites in a 0.814 (4):0.186 (4) ratio. Full Article text
i Bis[2,6-bis(benzimidazol-2-yl)pyridine-κ3N,N',N'']nickel(II) bis(trifluoromethanesulfonate) diethyl ether monosolvate By journals.iucr.org Published On :: 2024-01-31 In the title complex, [Ni(C19H13N5)2](CF3SO3)2·(CH3CH2)2O, the central NiII atom is sixfold coordinated by three nitrogen atoms of each 2,6-bis(2-benzimidazolyl)pyridine ligand in a distorted octahedral geometry with two trifluoromethanesulfonate ions and a molecule of diethyl ether completing the outer coordination sphere of the complex. Hydrogen bonding contributes to the organization of the asymmetric units in columns along the a axis generating a porous supramolecular structure. The structure was refined as a two-component twin with a refined BASF value of 0.4104 (13). Full Article text
i (2,2'-Bipyridine-κ2N,N')(4,4'-dimethoxy-2,2'-bipyridine-κ2N,N')palladium(II) bis(trifluoromethanesulfonate) By journals.iucr.org Published On :: 2024-02-08 In the title complex salt, [Pd(C10H8N2)(C12H12N2O2)](CF3SO3)2, the palladium(II) atom is fourfold coordinated by two chelating ligands, 2,2'-bipyridine and 4,4'-dimethoxy-2,2'-bipyridine, in a distorted square-planar environment. In the crystal, weak π–π stacking interactions between the 2,2'-bipyridine rings [centroid-to-centroid distances = 3.8984 (19) Å] and between the 4,4'-dimethoxy-2,2'-bipyridine rings [centroid-to-centroid distances = 3.747 (18) Å] contribute to the alignment of the complex cations in columns parallel to the b-axis direction. Full Article text
i Aquabis(2,2'-bipyridine-κ2N,N')(isonicotinamide-κN)ruthenium(II) bis(trifluoromethanesulfonate) By journals.iucr.org Published On :: 2024-02-08 In the title complex, [Ru(C10H8N2)2(C6H6N2O)(H2O)](CF3SO3)2, the central RuII atom is sixfold coordinated by two bidentate 2,2'-bipyridine, an isonicotinamide ligand, and a water molecule in a distorted octahedral environment with trifluoromethanesulfonate ions completing the outer coordination sphere of the complex. Hydrogen bonding involving the water molecule and weak π–π stacking interactions between the pyridyl rings in adjacent molecules contribute to the alignment of the complexes in columns parallel to the c axis. Full Article text
i Bis[μ-bis(pyridin-2-yl)methanone oxime-κ3N:,N',N'']bis[diacetato-κ2O,O';κO-zinc(II)] By journals.iucr.org Published On :: 2024-02-16 The structure of the title complex, [Zn2(C2H3O2)4(C11H9N3O)2], is triclinic containing half of the molecule in the asymmetric unit. Each zinc atom is coordinated to a pyridyl and oxime nitrogen from one di-2-pyridyl ketone oxime (dpko) ligand and a third nitrogen from the other dpko pyridyl ring. Additionally, each zinc is coordinated to two acetato anions, one of which is bidentate and the other monodentate. The uncoordinated oxygen of the monodentate acetato group is involved in a hydrogen bond with the oxime hydrogen. The packing in the crystal is assisted by weak C—H⋯O interactions between acetato groups and neighboring pyridyl rings. Full Article text
i 1-Ethyl-3,3-dimethylspiro[indoline-2,8'-phenaleno[1,9-fg]chromene] By journals.iucr.org Published On :: 2024-02-13 The title pyrene-fused spiropyran derivative, C30H25NO, crystallizes with two molecules in the asymmetric unit with dihedral angles between their fused-ring sub units of 76.20 (8) and 89.38 (9)°. In the crystal, weak C—H⋯π interactions link the molecules into a three-dimensional network. Full Article text
i Crystal structure of defect scheelite-type Nd2/3[WO4] By journals.iucr.org Published On :: 2024-03-06 Neodymium(III) ortho-oxidotungstate(VI) was synthesized as a side-product in an unsuccessful synthesis attempt at fluoride derivatives of neodymium tungstate in fused silica ampoules, using neodymium(III) oxide, neodymium(III) fluoride and tungsten trioxide. Violet, platelet-shaped single crystals of the title compound emerged of the bulk, which crystallize in the defect scheelite type with a trigonal dodecahedral coordination of oxide anions around the Nd3+ cations and the hexavalent tungsten cations situated in the centers of oxide tetrahedra. Full Article text
i Bis[S-octyl 3-(2-methylpropylidene)dithiocarbazato-κ2N3,S]nickel(II) By journals.iucr.org Published On :: 2024-03-06 The central NiII atom in the title complex, [Ni(C13H25N2S2)2], is located on an inversion center and adopts a roughly square-planar coordination environment defined by two chelating N,S donor sets of two symmetry-related ligands in a trans configuration. The Ni—N and Ni—S bond lenghts are 1.9193 (14) and 2.1788 (5) Å, respectively, with a chelating N—Ni—S bond angle of 86.05 (4)°. These data are compared with those measured for similar dithiocarbazato ligands that bear n-octyl or n-hexyl alkyl chains. Slight differences are observed with respect to the phenylethylidene derivative where the ligands are bound cis relative to one another. Full Article text
i cis,cis,cis-Dichloridobis(N4,N4-dimethylpyridin-4-amine-κN1)bis(dimethyl sulfoxide-κS)ruthenium(II) By journals.iucr.org Published On :: 2024-03-06 The structure of the title compound, [RuCl2(C7H10N2)2(C2H6OS)2], has monoclinic (P21/n) symmetry. The Ru—N distances of the coordination compound are influenced by the trans chloride or dimethylsulfoxide-κS ligands. The molecular structure exhibits disorder for two of the terminal methyl groups of a dimethyl sulfoxide ligand. Full Article text
i 4-Fluoro-2-(phenylamino)benzoic acid By journals.iucr.org Published On :: 2024-03-06 The title compound, C13H10FNO2, was obtained by the reaction of 2-bromo-4-fluorobenzoic acid with aniline. There are two independent molecules, A and B, in the asymmetric unit, with slight conformational differences: the dihedral angles between the aromatic rings are 55.63 (5) and 52.65 (5)°. Both molecules feature an intramolecular N—H⋯O hydrogen bond. In the crystal, the molecules are linked by pairwise O—H⋯O hydrogen bonds to form A–B acid–acid dimers and weak C—H⋯F interactions further connect the dimers. Full Article text
i 5-Bromo-2-(phenylamino)benzoic acid By journals.iucr.org Published On :: 2024-03-06 The title compound, C13H10BrNO2, was obtained by the reaction of 2,5-dibromobenzoic acid and aniline. The molecule is twisted with a dihedral angle between the aromatic rings of 45.74 (11)° and an intramolecular N—H⋯O hydrogen bond is seen. In the crystal, pairwise O—H⋯O hydrogen bonds generate carboxylic acid inversion dimers. Full Article text
i 10-Bromo-N,N-diphenylanthracen-9-amine By journals.iucr.org Published On :: 2024-03-12 In the title compound, C26H18BrN, the dihedral angles between the anthracene ring system and the phenyl rings are 89.51 (14) and 74.03 (15)°. In the extended structure, a weak C—H⋯Br interaction occurs, which generates [100] chains, but no significant π–π or C—H⋯π interactions are observed. Full Article text
i {N-[1-(2-Oxidophenyl)ethylidene]-dl-alaninato}(pentane-1,5-diyl)silicon(IV) By journals.iucr.org Published On :: 2024-03-19 The title SiIV complex, C16H21NO3Si, is built up by a tridentate dinegative Schiff base ligand bound to a silacyclohexane unit. The coordination geometry of the pentacoordinated SiIV atom is a distorted trigonal bipyramid. The presence of the silacyclohexane ring in the complex leads to an unusual coordination geometry of the SiIV atom with the N atom from the Schiff base ligand and an alkyl-C atom in apical positions of the trigonal bipyramid. There is a disorder of the methyl group at the imine bond with two orientations resolved for the H atoms [major orientation = 0.55 (3)]. In the crystal, C—H⋯O interactions are found within corrugated layers of molecules parallel to the ab plane. Full Article text
i 2-Ferrocenyl-2-[(2-ferrocenylethenyl)(morpholin-4-yl)methyl]-1,3-dithiolane By journals.iucr.org Published On :: 2024-03-21 The molecular structure of 2-ferrocenyl-2-[(2-ferrocenylethenyl)(morpholin-4-yl)methyl]-1,3-dithiolane, [Fe2(C5H5)2(C19H21NOS2)] or C29H31Fe2NOS2, has the ferrocenyl fragments in a trans disposition with respect to the vinyl group. One of the methylene groups is disordered over two sites with occupancies of 0.782 (13):0.218 (13). In the crystal, cyclopentadienyl-C—H⋯O(morpholinyl) interactions feature within helical chains parallel to the c-axis direction. The chains are connected by methylene- and cyclopentadienyl-C—H⋯O(cyclopentadienyl) interactions. Full Article text
i trans-Dibromidotetrakis(5-methyl-1H-pyrazole-κN2)manganese(II) By journals.iucr.org Published On :: 2024-03-19 The title compound, trans-dibromidotetrakis(5-methyl-1H-pyrazole-κN2)manganese(II), [MnBr2(C4H6N2)4] or [Mn(3-MePzH)4Br2] (1) crystallizes in the triclinic Poverline{1} space group with the cell parameters a = 7.6288 (3), b = 8.7530 (4), c = 9.3794 (4) Å and α = 90.707 (4), β = 106.138 (4), γ = 114.285 (5)°, V = 542.62 (5) Å3, T = 120 K. The asymmetric unit contains only half the molecule with the manganese atom is situated on a crystallographic inversion center. The 3-MePzH ligands are present in an AABB type manner with two methyl groups pointing up and the other two down. The supramolecular architecture is characterized by several intermolecular C—H⋯N, N—H⋯Br, and C—H⋯π interactions. Earlier, a polymorphic structure of [Mn(3-MePzH)4Br2] (2) with a similar geometry and also an AABB arrangement for the pyrazole ligands was described [Reedijk et al. (1971). Inorg. Chem. 10, 2594–2599; a = 8.802 (6), b = 9.695 (5), c = 7.613 (8) Å and α = 105.12 (4), β = 114.98 (4), γ = 92.90 (3)°, V = 558.826 (5) Å3, T = 295 K]. A varying supramolecular pattern was reported, with the structure of 1 featuring a herringbone type pattern while that of structure 2 shows a pillared network type of arrangement along the a axis. A nickel complex [Ni(3-MePzH)4Br2] isomorphic to 1 and the analogous chloro derivatives of FeII, CoII and CuII are also known. Full Article text
i 4-Fluorobenzyl (Z)-2-(2-oxoindolin-3-ylidene)hydrazine-1-carbodithioate By journals.iucr.org Published On :: 2024-03-19 The title compound, C16H12FN3OS, a fluorinated dithiocarbazate imine derivative, was synthesized by the one-pot, multi-component condensation reaction of hydrazine hydrate, carbon disulfide, 4-fluorobenzyl chloride and isatin. The compound demonstrates near-planarity across much of the molecule in the solid state and a Z configuration for the azomethine C=N bond. The Z form is further stabilized by the presence of an intramolecular N—H⋯O hydrogen bond. In the extended structure, molecules are linked into dimers by N—H⋯O hydrogen bonds and further connected into chains along either [2overline{1}0] or [100] by weak C—H⋯S and C—H⋯F hydrogen bonds, which further link into corrugated sheets and in combination form the overall three-dimensional network. Full Article text
i Poly[(μ-2,3-diethyl-7,8-dimethylquinoxaline-κ2N:N)(2,3-diethyl-7,8-dimethylquinoxaline-κN)-μ-nitrato-κ2O:O'-nitrato-κ2O,O'-disilver(I)] By journals.iucr.org Published On :: 2024-03-21 The structure of the title compound, [C14H18N2)2Ag2](NO3)2, contains subtle differences in ligand, metal, and counter-anion coordination. One quinoxaline ligand uses one of its quinoxaline N atoms to bond to one silver cation. That silver cation is bound to a second quinoxaline which, in turn, is bound to a second silver atom; thereby using both of its quinoxaline N atoms. A nitrate group bonds with one of its O atoms to the first silver and uses the same oxygen to bond to a silver atom (related by symmetry to the second), thereby forming an extended network. The second nitrate group on the other silver bonds via two nitrate O atoms; one silver cation therefore has a coordination number of three whereas the second has a coordination number of four. One of the quinoxaline ligands has a disordered ethyl group. Full Article text
i Bis[2,6-bis(1H-benzimidazol-2-yl)pyridine]ruthenium(II) bis(hexafluoridophosphate) diethyl ether trisolvate By journals.iucr.org Published On :: 2024-03-28 The title compound, [Ru(C19H13N5)2](PF6)2·3C4H10O, was obtained from the reaction of Ru(bimpy)Cl3 [bimpy is 2,6-bis(1H-benzimidazol-2-yl)pyridine] and bimpy in refluxing ethanol followed by recrystallization from diethyl ether/acetonitrile. At 125 K the complex has orthorhombic (Pca21) symmetry. It is remarkable that the structure is almost centrosymmetric. However, refinement in space group Pbcn leads to disorder and definitely worse results. It is of interest with respect to potential catalytic reduction of CO2. The structure displays N—H⋯O, N—H⋯F hydrogen bonding and significant π–π stacking and C—H⋯π stacking interactions. Full Article text
i 13-Nitrobenzo[a][1,4]benzothiazino[3,2-c]phenoxazine By journals.iucr.org Published On :: 2024-04-26 In the title compound, C22H11N3O3S, dihedral angle between the phenyl rings on the periphery of the molecule is 8.05 (18)°. In the crystal, aromatic π–π stacking distance and short C—H⋯O contacts are observed. The maximum absorption occurs at 688 nm. Full Article text
i Ethidium benzoate methanol monosolvate By journals.iucr.org Published On :: 2024-04-18 In the title salt solvate (systematic name: 8-amino-5-ethyl-6-phenylphenanthridin-5-ium benzoate methanol monosolvate), C21H20N3+·C6H5CO2−·CH3OH, two ethidium cations, C21H20N3+, dimerize about a twofold axis through π–π interactions [inter-centroid separation = 3.6137 (4) Å]. The benzoate anions are connected through hydrogen bonding with the –NH2 groups of the ethidium cations and the –OH group of the MeOH molecule. The MeOH molecule also accepts a hydrogen bond from the –NH2 group of the ethidium cation. The result is a one-dimensional hydrogen-bonded chain along the b-axis direction. Full Article text
i Bis[2,3-bis(thiophen-2-yl)pyrido[3,4-b]pyrazine]silver(I) perchlorate methanol disolvate By journals.iucr.org Published On :: 2024-04-26 The title compound, [Ag(C15H9N3S2)2]ClO4·2CH3OH, is monoclinic. The AgI atom is coordinated by pyrido N atoms and is two-coordinate; however, the AgI atom has nearby O atoms that can be assumed to be weakly bonded – one from the perchlorate anion and one from the methanol solvate molecule. One of the thienyl groups on a 2,3-bis(thiophen-2-yl)pyrido[3,4-b]pyrazine is flipped disordered and was refined to occupancies of 68.4 (6) and 31.6 (6)%. Full Article text
i mer-Bis(quinoline-2-carboxaldehyde 4-ethylthiosemicarbazonato)nickel(II) methanol 0.33-solvate 0.67-hydrate By journals.iucr.org Published On :: 2024-04-26 In the title compound, [Ni(C13H13N4S)2]·0.33CH3OH·0.67H2O, the NiII atom is coordinated by two tridentate quinoline-2-carboxaldehyde 4-ethylthiosemicarbazonate ligands in a distorted octahedral shape. At 100 K, the crystal symmetry is monoclinic (space group P21/n). A mixture of water and methanol crystallizes with the title complex, and one of the ethyl groups in the coordinating ligands is disordered over two positions, with an occupancy ratio of 58:42. There is intermolecular hydrogen bonding between the solvent molecules and the amine and thiolate groups in the ligands. No other significant interactions are present in the crystal packing. Full Article text
i Redetermination of germacrone type II based on single-crystal X-ray data By journals.iucr.org Published On :: 2024-04-26 The extraction and purification procedures, crystallization and crystal structure refinement (single-crystal X-ray data) of germacrone type II, C15H22O, are presented. The structural results are compared with a previous powder X-ray synchrotron study [Kaduk et al. (2022). Powder Diffr. 37, 98–104], revealing significant improvements in terms of accuracy and precision. Hirshfeld atom refinement (HAR), as well as Hirshfeld surface analysis, give insight into the intermolecular interactions of germacrone type II. Full Article text
i Poly[3-methylpyridinium [(μ2-dihydrogen phosphito)bis(μ3-hydrogen phosphito)dizinc]] By journals.iucr.org Published On :: 2024-04-26 In the title compound, {(C6H8N)[Zn2(HPO3)2(H2PO3)]}n, the constituent ZnO4, HPO3 and H2PO3 polyhedra of the inorganic component are linked into (010) sheets by Zn—O—P bonds (mean angle = 134.4°) and the layers are reinforced by O—H⋯O hydrogen bonds. The protonated templates are anchored to the inorganic sheets via bifurcated N—H⋯(O,O) hydrogen bonds. Full Article text
i Benzo[a][1,4]benzothiazino[3,2-c]phenothiazine By journals.iucr.org Published On :: 2024-04-30 The title compound, C22H12N2S2, crystallizes in space group P21/c with four molecules in the asymmetric unit. The heterocyclic molecule is quasi-planar with a dihedral angle between the phenyl rings on the periphery of the molecule of 1.73 (19)°. Short H⋯S (2.92 Å) and C—H⋯π [2.836 (3) Å] contacts are observed in the crystal with shorted π–π stacking distances of 3.438 (3) Å along the b axis. Surprisingly, and unlike a closely related material, this molecule readily forms large crystals by sublimation and by slow evaporation from dichloromethane. The maximum absorbance in the UV-Vis spectrum is at 533 nm. Emission was measured upon excitation at 533 nm with a fluorescence λmax of 658 nm and cutoff of 900 nm. Full Article text
i (2E,2'E)-1,1'-([1,1'-Biphenyl]-4,4'-diyl)bis[3-(dimethylamino)prop-2-en-1-one] By journals.iucr.org Published On :: 2024-04-26 The title compound, C22H24N2O2, crystallizes in space group P21/n. The molecular structure is almost planar except for a tilt of the phenyl rings. The allyl groups on both ends exhibit the trans-form and the connected N atoms show sp2 character. The molecules are stacked and assembled along the c-axis direction by C—H⋯π interactions. Full Article text
i (SC,RS)-Bromido(N-{4-methyl-1-[(4-methylphenyl)sulfanyl]pentan-2-yl}-N'-(pyridin-2-yl)imidazol-2-ylidene)palladium(II) bromide By journals.iucr.org Published On :: 2024-04-26 The molecule of the title NCNHCS pincer N-heterocyclic carbene palladium(II) complex, [PdBr(C21H25N3S)]Br, exhibits a slightly distorted square-planar coordination at the palladium(II) atom, with the five-membered chelate ring nearly planar. The six-membered chelate ring adopts an envelope conformation. Upon chelation, the sulfur atom becomes a stereogenic centre with an RS configuration induced by the chiral carbon of the precursor imidazolium salt. There are intramolecular C—H⋯Br—Pd hydrogen bonds in the structure. The two interstitial Br atoms, as the counter-anion of the structure, are both located on crystallographic twofold axes and are connected to the complex cations via C—H⋯·Br hydrogen bonds. Full Article text
i 4-(1H-2,3-Dihydronaphtho[1,8-de][1,3,2]diazaborinin-2-yl)-1-ethylpyridin-1-ium iodide By journals.iucr.org Published On :: 2024-04-26 The title compound, C17H17BN3I, is a type of diazaborinane featuring substitution at the 1, 2, and 3 positions of the nitrogen–boron six-membered heterocycle. The organic molecule has a planar structure, the dihedral angle between the pyridyl ring and the fused ring system being 3.46 (4)°. In the crystal, molecules are stacked in a head-to-tail manner. The iodide ion makes close contacts with three organic molecules and supports the alternating stack. Full Article text
i 4-(1H-2,3-Dihydronaphtho[1,8-de][1,3,2]diazaborinin-2-yl)-1-ethylpyridin-1-ium iodide monohydrate By journals.iucr.org Published On :: 2024-04-26 The cation of the title hydrated salt, C17H17BN3+·I−·H2O, is a diazaborinane featuring substitution at the 1, 2, and 3 positions in the nitrogen–boron six-membered heterocycle. The cation is approximately planar with a dihedral angle between the pyridyl ring and the diazaborinane ring system of 5.40 (5)°. In the crystal, the cations stack along [100] in an alternating head-to-tail manner, while the iodide ion and water molecule form one-dimensional hydrogen-bonded chains beside the cation stack. The cation stacks and I−–water chains are crosslinked by N—H⋯I and N—H⋯O hydrogen bonds. Full Article text
i trans-Dichloridobis(secnidazole-κN3)copper(II) By journals.iucr.org Published On :: 2024-05-03 The use of acetic acid (HOAc) in a reaction between CuCl2·2H2O and secnidazole, an active pharmaceutical ingredient useful in the treatment against a variety of anaerobic Gram-positive and Gram-negative bacteria, affords the title complex, [CuCl2(C7H11N3O3)2]. This compound was previously synthesized using ethanol as solvent, although its crystal structure was not reported [Betanzos-Lara et al. (2013). Inorg. Chim. Acta, 397, 94–100]. In the molecular complex, the Cu2+ cation is situated at an inversion centre and displays a square-planar coordination environment. There is a hydrogen-bonded framework based on intermolecular O—H⋯Cl interactions, characterized by H⋯Cl separations of 2.28 (4) Å and O—H⋯Cl angles of 175 (3)°. The resulting supramolecular network is based on R22(18) ring motifs, forming chains in the [010] direction. Full Article text
i Methyl 2-hydroxy-4-iodobenzoate By journals.iucr.org Published On :: 2024-05-17 The structure of the title compound, C8H7IO3, at 90 K has monoclinic (P21/c) symmetry. The extended structure is layered and displays intermolecular and intramolecular hydrogen bonding arising from the same OH group. Full Article text
i (5-Fluoro-2,6-dioxo-1,2,3,6-tetrahydropyrimidin-1-ido-κN1)(1,4,8,11-tetraazacyclotetradecane-κ4N)zinc(II) perchlorate By journals.iucr.org Published On :: 2024-05-21 In the structure of the title complex, [Zn(C4H2FN2O2)(C10H24N4)]ClO4, the zinc(II) ion forms coordination bonds with the four nitrogen atoms of cyclam (1,4,8,11-tetraazacyclotetradecane or [14]aneN4) as well as with the nitrogen atom of a deprotonated 5-fluorouracil ion (FU−). Cyclam adopts a trans-I type conformation within this structure. The coordination structure of the zinc(II) ion is a square pyramid with a distorted base plane formed by the four nitrogen atoms of the cyclam. FU− engages in intermolecular hydrogen bonding with neighboring FU− molecules and with the cyclam molecule. Full Article text
i Chlorido(2-{(2-hydroxyethyl)[tris(hydroxymethyl)methyl]amino}ethanolato-κ5N,O,O',O'',O''')copper(II) By journals.iucr.org Published On :: 2024-05-24 The title complex, [Cu(C8H18NO5)Cl] or [Cu(H4bis-tris)Cl], was obtained starting from the previously reported [Cu(H5bis-tris)Cl]Cl compound. The deprotonation of the aminopolyol ligand H5bis-tris {[bis(2-hydroxyethyl)amino]tris(hydroxymethyl)methane, C8H19NO5} promotes the formation of a very strong O—H⋯O intermolecular hydrogen bond, characterized by an H⋯O separation of 1.553 (19) Å and an O—H⋯O angle of 178 (4)°. The remaining hydroxy groups are also engaged in hydrogen bonds, forming R22(8), R44(16), R44(20) and R44(22) ring motifs, which stabilize the triperiodic supramolecular network. Full Article text
i Octakis(dibutylammonium) decamolybdate(VI) By journals.iucr.org Published On :: 2024-05-31 In the title salt, (C8H20N)8[Mo10O34], the [Mo10O34]8− polyanion is located about an inversion centre and can be considered as a β-type octamolybdate anion to which two additional MoO4 tetrahedra are linked via common corners. The [Mo10O34]8− polyanions are packed in rows extending parallel to [001] and are connected to the dibutylammonium counter-cations through N—H⋯O hydrogen-bonding interactions. Full Article text
i 2-(10-Bromoanthracen-9-yl)-N-phenylaniline By journals.iucr.org Published On :: 2024-05-31 In the title compound, C26H18BrN, the central benzene ring makes dihedral angles with its adjacent anthracene ring system and pendant benzene ring of 87.49 (13) and 62.01 (17)°, respectively. The N—H moiety is sterically blocked from forming a hydrogen bond, but weak C—H⋯π interactions occur in the extended structure. Full Article text
i Tetrakis(2,4,6-trimethylanilido)tin(IV) By journals.iucr.org Published On :: 2024-05-31 Transamination of Sn(NMe2)4 with H2NMes (Mes is 2,4,6-trimethylphenyl, C9H11) led to the formation of the title compound, [Sn(C9H12N)4] or Sn(NHMes)4, which crystallizes in the tetragonal space group Poverline{4}21c, with four formula units per unit cell. The molecular structure consists of a central tin(IV) atom, which is surrounded by four NHMes groups. Sn(NHMes)4 possesses crystallographically imposed overline{4} symmetry. The SnN4 coordination polyhedron is best described as a compressed bisphenoid. Full Article text
i (S)-2-Carboxyethyl l-cysteinyl sulfone By journals.iucr.org Published On :: 2024-05-31 The title compound {systematic name: (2S)-2-azaniumyl-3-[(2-carboxyethane)sulfonyl]propanoate}, C6H11NO6S, forms enantiopure crystals in the monoclinic space group P21 and exists as a zwitterion, with a protonated α-amino group and a deprotonated α-carboxyl group. Both the carboxyl groups and the amino group are involved in an extensive multicentered intermolecular hydrogen-bonding scheme. In the crystal, the diperiodic network of hydrogen bonds propagates parallel to (101) and involves interconnected heterodromic R43(10) rings. Electrostatic forces are major contributors to the structure energy, which was estimated by DFT calculations as Etotal = −333.5 kJ mol−1. Full Article text
i Ilmenite-type Na2(Fe2/3Te4/3)O6 By journals.iucr.org Published On :: 2024-05-31 Na2(Fe2/3Te4/3)O6 (Z = 3) or Na3(FeTe2)O9 (Z = 2), trisodium iron(III) ditellurium(VI) nonaoxide, adopts the ilmenite (FeTiO3, Z = 6) structure type with the Ti site (site symmetry 3.) replaced by Na and the Fe site (site symmetry 3.) replaced by a mixed-occupied (FeIII,TeVI) site in a Fe:Te ratio of 1:2. Whereas the [(Fe,Te)O6] octahedron is only slightly distorted, the [NaO6] octahedron shows much stronger distortions, as revealed by a larger spread of the bond lengths and some distortion parameters. Full Article text