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Methyl 1-(4-fluoro­benz­yl)-1H-indazole-3-carboxyl­ate

The title compound, C16H13FN2O2, was synthesized by nucleophilic substitution of the indazole N—H hydrogen atom of methyl 1H-indazole-3-carboxyl­ate with 1-(bromo­meth­yl)-4-fluoro­benzene. In the crystal, some hydrogen-bond-like inter­actions are observed.




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2-{1-[(6R,S)-3,5,5,6,8,8-Hexamethyl-5,6,7,8-tetra­hydro­naphthalen-2-yl]ethyl­idene}-N-methyl­hydrazinecarbo­thioamide

The reaction between a racemic mixture of (R,S)-fixolide and 4-methyl­thio­semicarbazide in ethanol with a 1:1 stoichiometric ratio and catalysed with HCl, yielded the title compound, C20H31N3S [common name: (R,S)-fixolide 4-methyl­thio­semicarbazone]. There is one crystallographically independent mol­ecule in the asymmetric unit, which is disordered over the aliphatic ring [site-occupancy ratio = 0.667 (13):0.333 (13)]. The disorder includes the chiral C atom, the neighbouring methyl­ene group and the methyl H atoms of the methyl group bonded to the chiral C atom. The maximum deviations from the mean plane through the disordered aliphatic ring amount to 0.328 (6) and −0.334 (6) Å [r.m.s.d. = 0.2061 Å], and −0.3677 (12) and 0.3380 (12) Å [r.m.s.d. = 0.2198 Å] for the two different sites. Both fragments show a half-chair conformation. Additionally, the N—N—C(=S)—N entity is approximately planar, with the maximum deviation from the mean plane through the selected atoms being 0.0135 (18) Å [r.m.s.d. = 0.0100 Å]. The mol­ecule is not planar due to the dihedral angle between the thio­semicarbazone entity and the aromatic ring, which amounts to 51.8 (1)°, and due to the sp3-hybridized carbon atoms of the fixolide fragment. In the crystal, the mol­ecules are connected by H⋯S inter­actions with graph-set motif C(4), forming a mono-periodic hydrogen-bonded ribbon along [100]. The Hirshfeld surface analysis suggests that the major contributions for the crystal cohesion are [(R,S)-isomers considered separately] H⋯H (75.7%), H⋯S/S⋯H (11.6%), H⋯C/C⋯H (8.3% and H⋯N/N⋯H (4.4% for both of them).




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5,6-Di­methyl­benzo[d][1,3]oxatellurole

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.




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meso-α,α-5,15-Bis(o-nicotinamido­phen­yl)-10,20-diphen­ylporphyrin n-hexane monosolvate

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.




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rac-Hy­droxy­isovaleric acid

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.




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Di­chlorido­(4,7-dimeth­oxy-1,10-phenanthroline-κ2N,N')zinc(II)

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).




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2-Amino­benzoxazole–oxalic acid (2/1)

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.




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Bis(2-hy­droxy-2,3-di­hydro-1H-inden-1-aminium) tetra­chlorido­palladate(II) hemihydrate

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.




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(2,2'-Bi­pyridine-κ2N,N')(4,4'-dimeth­oxy-2,2'-bipyridine-κ2N,N')palladium(II) bis­(tri­fluoro­meth­anesulfonate)

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.




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Bis[μ-bis­(pyridin-2-yl)methanone oxime-κ3N:,N',N'']bis­[di­acetato-κ2O,O';κO-zinc(II)]

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.




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Prop-2-ynyl 3-meth­oxy-4-(prop-2-yn­yloxy)benzoate

The title compound, C14H12O4, comprises of two crystallographically independent mol­ecules in the asymmetric unit, linked via C—H⋯O inter­actions to form dimeric entities. The allylic groups are twisted out of the phenyl planes with dihedral angles varying between 7.92 (13) and 25.42 (8)°. In the crystal, the packing follows a zigzag pattern along the c-axis direction. The absolute configuration of the sample could not be determined reliably.




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cis,cis,cis-Di­chlorido­bis­(N4,N4-di­methyl­pyridin-4-amine-κN1)bis­(dimethyl sulfoxide-κS)ruthenium(II)

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.




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Methyl N-{(1R)-2-[(meth­oxy­carbon­yl)­oxy]-1-phenyleth­yl}carbamate

The title mol­ecule, C12H15NO5, is a methyl carbamate derivative obtained by reacting (R)-2-phenyl­glycinol and methyl chloro­formate, with calcium hydroxide as heterogeneous catalyst. Supra­molecular chains are formed in the [100] direction, based on N—H⋯O hydrogen bonds between the amide and carboxyl­ate groups. These chains weakly inter­act in the crystal, and the phenyl rings do not display significant π–π inter­actions.




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{N-[1-(2-Oxidophen­yl)ethyl­idene]-dl-alaninato}(pentane-1,5-di­yl)silicon(IV)

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.




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4-Fluoro­benzyl (Z)-2-(2-oxoindolin-3-yl­idene)hydrazine-1-carbodi­thio­ate

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.




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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)]

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.




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Bis[2,6-bis­(1H-benzimidazol-2-yl)pyridine]ruthenium(II) bis(hexa­fluorido­phosphate) diethyl ether tris­olvate

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.




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13-Nitro­benzo[a][1,4]benzo­thia­zino[3,2-c]phenoxazine

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.




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mer-Bis(quinoline-2-carboxaldehyde 4-ethyl­thio­semicarbazonato)nickel(II) methanol 0.33-solvate 0.67-hydrate

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.




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Redetermination of germacrone type II based on single-crystal X-ray data

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.




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Methyl 2-hy­droxy-4-iodo­benzoate

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.




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(5-Fluoro-2,6-dioxo-1,2,3,6-tetra­hydro­pyrimidin-1-ido-κN1)(1,4,8,11-tetra­aza­cyclo­tetra­decane-κ4N)zinc(II) perchlorate

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.




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Chlorido­(2-{(2-hy­droxy­eth­yl)[tris­(hy­droxy­meth­yl)meth­yl]amino}­ethano­lato-κ5N,O,O',O'',O''')copper(II)

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.




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(S)-2-Carb­oxy­ethyl l-cysteinyl sulfone

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.




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Poly[[{μ2-5-[(di­methyl­amino)(thioxo)meth­oxy]benzene-1,3-di­carboxyl­ato-κ4O1,O1':O3,O3'}(μ2-4,4'-di­pyridyl­amine-κ2N4:N4')cobalt(II)] di­methyl­formamide hemisolvate monohydrate]

In the crystal structure of the title compound, {[Co(C11H9NSO5)(C10H9N3)]0.5C3H7NO·H2O}n or {[Co(dmtb)(dpa)]·0.5DMF·H2O}n (dmtb2– = 5-[(di­meth­yl­amino)­thioxometh­oxy]-1,3-benzene­dicarboxyl­ate and dpa = 4,4'-di­pyridyl­amine), an assembly of periodic [Co(C11H9NSO5)(C10H9N3)]n layers extending parallel to the bc plane is present. Each layer is constituted by distorted [CoO4N2] octa­hedra, which are connected through the μ2-coordination modes of both dmtb2– and dpa ligands. Occupationally disordered water and di­meth­yl­formamide (DMF) solvent mol­ecules are located in the voids of the network to which they are connected through hydrogen-bonding inter­actions.




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2-Oxo-2H-chromen-4-yl 3,3-di­methyl­butano­ate

In the crystal of the title compound, C15H16O4, the mol­ecules are connected through C—H⋯O hydrogen bonds, generating [100] chains, which are crosslinked by weak π–π stacking inter­actions.




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Chlorido­[5,10,15,20-tetra­kis­(quinoline-7-carboxamido)­porphinato]iron(III)

The title compound, [Fe(C84H52N12O4)Cl], crystallizes in space group C2/c. The central FeIII cation (site symmetry 2) is coordinated in a fivefold manner, with four pyrrole N atoms of the porphyrin core in the basal sites and one Cl atom (site symmetry 2) in the apical position, which completes a slightly distorted square-pyramidal environment. The porphyrin macrocycle shows a characteristic ruffled-shape distortion and the iron atom is displaced out of the porphyrin plane by 0.42 Å with the average Fe—N distance being 2.054 (4) Å; the Fe—Cl bond length is 2.2042 (7) Å. Inter­molecular C—H⋯N and C—H⋯O hydrogen bonds occur in the crystal structure.




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(2,5-Di­methyl­imidazole){N,N',N'',N'''-[porphyrin-5,10,15,20-tetra­yltetra­(2,1-phenyl­ene)]tetra­kis(pyridine-3-carboxamide)}manganese(II) chloro­benzene disolvate

In the title compound, [Mn(C68H44N12O4)(C5H8N2)]·2C6H5Cl, the central MnII ion is coordinated by four pyrrole N atoms of the porphyrin core in the basal sites and one N atom of the 2,5-di­methyl­imidazole ligand in the apical site. Two chloro­benzene solvent mol­ecules are also present in the asymmetric unit. Due to the apical imidazole ligand, the Mn atom is displaced out of the 24-atom porphyrin mean plane by 0.66 Å. The average Mn—Np (p = porphyrin) bond length is 2.143 (8) Å, and the axial Mn—NIm (Im = 2,5-di­methyl­imidazole) bond length is 2.171 (8) Å. The structure displays inter­molecular and intra­molecular N—H⋯O, N—H⋯N, C—H⋯O and C—H⋯N hydrogen bonding. The crystal studied was refined as a two-component inversion twin.




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Bis{(S)-(−)-N-[(2-biphen­yl)methyl­idene]-1-(4-meth­oxy­phen­yl)ethyl­amine-κN}di­chlorido­palladium(II)

The PdII complex bis­{(S)-(−)-N-[(biphenyl-2-yl)methyl­idene]1-(4-meth­oxy­phen­yl)ethanamine-κN}di­chlorido­palladium(II), [PdCl2(C22H21NO)2], crystallizes in the monoclinic Sohncke space group P21 with a single mol­ecule in the asymmetric unit. The coordination environment around the palladium is slightly distorted square planar. The N—Pd—Cl bond angles are 91.85 (19), 88.10 (17), 89.96 (18), and 90.0 (2)°, while the Pd—Cl and Pd—N bond lengths are 2.310 (2) and 2.315 (2) Å and 2.015 (2) and 2.022 (6) Å, respectively. The crystal structure features inter­molecular N—H⋯Cl and intramolecular C—H⋯Pd inter­actions, which lead to the formation of a supramolecular framework structure.




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Bis(8-hy­droxy­quinolinium) naphthalene-1,5-di­sulfonate tetra­hydrate

The inter­action between 8-hy­droxy­quinoline (8HQ, C9H7NO) and naphthalene-1,5-di­sulfonic acid (H2NDS, C10H8O6S2) in aqueous media results in the formation of the salt hydrate bis­(8-hy­droxy­quinolinium) naphthalene-1,5-di­sulfonate tetra­hydrate, 2C9H8NO+·C10H6O6S22−·4H2O. The asymmetric unit comprises one protonated 8HQ+ cation, half of an NDS2– dianion symmetrically disposed around a center of inversion, and two water mol­ecules. Within the crystal structure, these components are organized into chains along the [010] and [10overline{1}] directions through O—H⋯O and N—H⋯O hydrogen-bonding inter­actions, forming a di-periodic network parallel to (101). Additional stabilizing inter­actions such as C—H⋯O, C—H⋯π, and π–π inter­actions extend this arrangement into a tri-periodic network structure




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6-[4-(tert-Butyl­dimethyl­sil­yloxy)phen­yl]-1-oxa­spiro­[2.5]hepta­ne

The title compound, C19H30O2Si, has triclinic (Poverline{1}) symmetry at 100 K. The O atom of the epoxide group has a pseudoaxial orientation and the dihedral angle between the cyclo­hexyl and benzene rings is 85.80 (8)°. The C—O—Si—Ct (t = tert-but­yl) torsion angle is −177.40 (14)°. In the crystal, pairwise C—H⋯O links connect the mol­ecules into inversion dimers featuring R22(8) loops.




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Bis(ethyl­enedi­ammonium) μ-ethyl­enedi­aminetetra­acetato-1κ3O,N,O':2κ3O'',N',O'''-bis­[tri­oxidomolybdate(VI)] tetra­hydrate

The title compound, (C2H10N2)2[(C10H12N2O8)(MoO3)2]·4H2O, which crystallizes in the monoclinic C2/c space group, was obtained by mixing molybdenum oxide, ethyl­enedi­amine and ethyl­enedi­amine­tetra­acetic acid (H4edta) in a 2:4:1 ratio. The complex anion contains two MoO3 units bridged by an edta4− anion. The midpoint of the central C—C bond of the edta4− anion is located on a crystallographic inversion centre. The independent Mo atom is tridentately coordin­ated by a nitro­gen atom and two carboxyl­ate groups of the edta4− ligand, together with the three oxo ligands, producing a distorted octa­hedral coordination environment. In the three-dimensional supra­molecular crystal structure, the dinuclear anions, the organo­ammonium counter-ions and the solvent water mol­ecules are linked by N—H⋯Ow, N—H⋯Oedta and O—H⋯O hydrogen bonds.




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(η6-Benzene)­chlorido­[(S)-2-(4-isopropyl-4,5-di­hydro­oxazol-2-yl)phenolato]ruthenium(II)

The title compound, [Ru(C12H14NO2)Cl(η6-C6H6)], exhibits a half-sandwich tripod stand structure and crystallizes in the ortho­rhom­bic space group P212121. The arene group is η6 π-coordinated to the Ru atom with a centroid-to-metal distance of 1.6590 (5) Å, with the (S)-2-(4-isopropyl-4,5-di­hydro­oxazol-2-yl)phenolate chelate ligand forming a bite angle of 86.88 (19)° through its N and phenolate O atoms. The pseudo-octa­hedral geometry assumed by the complex is completed by a chloride ligand. The coordination of the optically pure bidentate ligand induces metal centered chirality onto the complex with a Flack parameter of −0.056.




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Redetermined structure of 4-(benz­yloxy)benzoic acid

In the title compound, C14H14O3, the dihedral angle between the aromatic rings is 39.76 (9)°. In the crystal, the mol­ecules associate to form centrosymmetric acid–acid dimers linked by pairwise O—H⋯O hydrogen bonds. The precision of the geometric parameters in the present single-crystal study is about an order of magnitude better than the previous powder diffraction study [Chattopadhyay et al. (2013). CrystEngComm, 15, 1077–1085].




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Di­chloridotetra­kis­(3-meth­oxy­aniline)nickel(II)

The reaction of nickel(II) chloride with 3-meth­oxy­aniline yielded di­chlorido­tetra­kis­(3-meth­oxy­aniline)nickel(II), [NiCl2(C7H9NO)4], as yellow crystals. The NiII ion is pseudo-octa­hedral with the chloride ions trans to each other. The four 3-meth­oxy­aniline ligands differ primarily due to different conformations about the Ni—N bond, which also affect the hydrogen bonding. Inter­molecular N—H⋯ Cl hydrogen bonds and short Cl⋯Cl contacts between mol­ecules link them into chains parallel to the b axis.




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Methyl 2-[(Z)-5-bromo-2-oxoindolin-3-yl­idene]­hydrazinecarbodi­thio­ate

The title compound, C10H8BrN3OS2, a brominated di­thio­carbazate imine deriv­ative, was obtained from the condensation reaction of S-methyl­dithio­carbazate (SMDTC) and 5-bromo­isatin. The essentially planar mol­ecule exhibits a Z configuration, with the di­thio­carbazate and 5-bromo­isatin fragments located on the same sides of the C=N azomethine bond, which allows for the formation of an intra­molecular N—H⋯Ob (b = bromo­isatin) hydrogen bond generating an S(6) ring motif. In the crystal, adjacent mol­ecules are linked by pairs of N—H⋯O hydrogen bonds, forming dimers characterized by an R22(8) loop motif. In the extended structure, mol­ecules are linked into a three-dimensional network by C—H⋯S and C—H⋯Br hydrogen bonds, C—Br⋯S halogen bonds and aromatic π–π stacking.




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Norfloxacinium nitrate

In the title salt [systematic name: 4-(3-carb­oxy-1-ethyl-6-fluoro-4-oxo-1,4-di­hydro­quin­olin-7-yl)piperazin-1-ium nitrate], C16H19FN3O3+·NO3−, proton transfer from nitric acid to the N atom of the piperazine ring of norfloxacin has occurred to form a mol­ecular salt. In the extended structure, N—H⋯O hydrogen bonds link alternating cations and anions into [100] chains, which are reinforced by aromatic π–π stacking inter­actions between the quinoline moieties of the norfloxacinium cations.




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Bis(2-carb­oxy­quinolinium) hexa­chlorido­stan­nate(IV) dihydrate

In the hydrated title salt, (C10H8NO2)2[SnCl6]·2H2O, the tin(IV) atom is located about a center of inversion. In the crystal structure, the organic cation, the octa­hedral inorganic anion and the water mol­ecule of crystallization inter­act through O—H⋯O, N—H⋯O and O—H⋯Cl hydrogen bonds, supplemented by weak π–π stacking between neighboring cations, and C—Cl⋯π inter­actions.




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Poly[tris­(2-amino­butan-1-ol)copper(II) [hexa­kis-μ2-cyanido-κ12C:N-tetra­copper(I)] bis­(2-amino­butan-1-olato)aqua­copper(II) monohydrate]

The title structure, {[Cu(C4H11NO)3][Cu4(CN)6]·[Cu(C4H10NO)2(H2O)]·H2O}n, is made up of diperiodic honeycomb CuICN networks built from [Cu4(CN)6]2− units, together with two independent CuII complexes: six-coord­inate [Cu(CH3CH2CH(NH2)CH2OH)3]2+ cations, and five-coordinate [Cu(CH3CH2CH(NH2)CH2O)2·H2O] neutral species. The two CuII complexes are not covalently bonded to the CuICN networks. Strong O—H⋯O hydrogen bonds link the CuII complexes into pairs and the pairs are hydrogen bonded into chains along the crystallographic b axis via the hydrate water mol­ecule. In addition, O—H⋯(CN) and N—H⋯(CN) hydrogen bonds link the cations to the CuCN network. In the honeycomb polymeric moiety, all bridging cyanido ligands are disordered over two orientations, head-to-tail and tail-to-head, with occupancies for C and N atoms varying for each CN group.




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Bis[2-(isoquinolin-1-yl)phenyl-κ2N,C1](2-phenyl-1H-imidazo[4,5-f][1,10]phenanthroline-κ2N,N')iridium(III) hexa­fluorido­phosphate methanol monosolvate

The title compound, [Ir(C15H10N)2(C19H12N4)]PF6·CH3OH, crystallizes in the C2/c space group with one monocationic iridium complex, one hexa­fluorido­phosphate anion, and one methanol solvent mol­ecule of crystallization in the asymmetric unit, all in general positions. The anion and solvent are linked to the iridium complex cation via hydrogen bonding. All bond lengths and angles fall into expected ranges compared to similar compounds.




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(E)-1-(3,4-Di­meth­oxy­phen­yl)-3-(1,3-diphenyl-1H-pyrazol-4-yl)prop-2-en-1-one

In the title compound, C26H22N2O3, the dihedral angle between the benzene and pyrazole rings of the chalcone unit is 88.3 (1)°. The pyrazole ring has two attached phenyl rings that form dihedral angles with the pyrazole ring of 22.6 (2) and 40.0 (1)°. In the crystal, pairwise C—H⋯O hydrogen bonds generate R22(20) inversion dimers.




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Redetermined structure of methyl 3-{4,4-di­fluoro-2-[2-(methoxy­car­bon­yl)­ethyl]-1,3,5,7-tetra­methyl-4-bora-3a,4a-di­aza-s-in­da­cen-6-yl}pro­pion­ate

In the title compound, C21H27BF2N2O4, a highly fluorescent boron–dipyrromethene dye, the methyl­propionate moieties have different conformations. In the crystal, weak C—H⋯F and C—H⋯O inter­actions link the mol­ecules. Some optical properties are presented.




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(1R,2S,4aR,6S,8R,8aS)-1-(3-Hy­droxy­propano­yl)-1,3,6,8-tetra­methyl-1,2,4a,5,6,7,8,8a-octa­hydronaphthalene-2-carb­oxy­lic acid

The mol­ecular structure of C18H28O4, (+)-diplodiatoxin, is described, whereby the absolute configuration of the structure of diplodiatoxin has been confirmed by single-crystal X-ray diffraction. Diplodiatoxin crystallizes in the chiral P43212 space group with one mol­ecule in the asymmetric unit.




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Δ-Bis[(S)-2-(4-isopropyl-4,5-di­hydro­oxazol-2-yl)phenolato-κ2N,O1](1,10-phenanthroline-κ2N,N')ruthenium(III) hexa­fluorido­phosphate

The title compound, [Ru(C12H14NO2)2(C12H8N2)]PF6 crystallizes in the tetra­gonal Sohnke space group P41212. The two bidentate chiral salicyloxazoline ligands and the phenanthroline co-ligand coordinate to the central RuIII atom through N,O and N,N atom pairs to form bite angles of 89.76 (15) and 79.0 (2)°, respectively. The octa­hedral coordination of the bidentate ligands leads to a propeller-like shape, which induces metal-centered chirality onto the complex, with a right-handed (Δ) absolute configuration [the Flack parameter value is −0.003 (14)]. Both the complex cation and the disordered PF6− counter-anion are located on twofold rotation axes. Apart from Coulombic forces, the crystal cohesion is ensured by non-classical C—H⋯O and C—H⋯F inter­actions.




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4-Bromo-N,N'-di­phenyl­benzimidamide N'-oxide

The title compound, C19H15BrN2O, crystallizes with two similar mol­ecules in the asymmetric unit. The extended structure features dimers linked by pairs of N—H⋯O and C—H⋯O hydrogen bonds. The HNCNO moiety of the title compound shows delocalization over the N—C—N part, as evidenced by the similar C—N bond distances.




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Methyl 2-[(Z)-5-methyl-2-oxoindolin-3-yl­idene]hydrazinecarbodi­thio­ate

The title di­thio­carbazate imine, C11H11N3OS2, was obtained from the condensation reaction of S-methyl­dithio­carbazate (SMDTC) and 5-methyl­isatin. It shows a Z configuration about the imine C=N bond, which is associated with an intra­molecular N—H⋯O hydrogen bond that closes an S(6) ring. In the crystal, inversion dimers linked by pairwise N—H⋯O hydrogen bonds generate R22(8) loops. The extended structure features C—H⋯S contacts as well as reciprocal carbon­yl–carbonyl (C=O⋯C=O) inter­actions.




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(Z)-N-(2,6-Diiso­propyl­phen­yl)-1-[(2-meth­oxyphen­yl)amino]­methanimine oxide

The mol­ecular structure of the title compound, C20H26N2O2 reveals non-co-planarity between the central formamidine backbone and each of the outer meth­oxy- and i-propyl- substituted benzene rings with dihedral angles of 7.88 (15) and 81.17 (15)°, respectively, indicating significant twists in the mol­ecule. In the crystal, inter­molecular C—H⋯O inter­actions, forming an R34(30) graph set, occur within a two-dimensional layer that extends along the ac plane.




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(Z)-N-(2,6-Di­methyl­phen­yl)-1-[(2-meth­oxy­phen­yl)amino]­methanimine oxide methanol monosolvate

In the title solvate, C16H18N2O2·CH4O, the dihedral angles between the formamidine backbone and the pendant 2-meth­oxy­phenyl and 2,6-di­methyl­phenyl groups are 14.84 (11) and 81.61 (12)°, respectively. In the crystal, the components are linked by C—H⋯O, O—H⋯O and C—H⋯ π hydrogen bonds, generating a supra­molecular chain that extends along the crystallographic a-axis direction.




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2-Chloro-N-(4-hy­droxy­phen­yl)acetamide

The title compound, C8H8ClNO2, is significantly distorted from planarity, with a twist angle between the planes through the hy­droxy­benzene and acetamide groups being 23.5 (2)°. This conformation is supported by intra­molecular C—H⋯O and N—H⋯Cl contacts. In the crystal, N—H⋯O hydrogen-bonding contacts between acetamide groups and O—H⋯O contacts between hydroxyl groups form tapes propagating parallel to [103].




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3aH,4H,5H,8H,9H,9aH-Cyclo­octa­[d][1,3]dioxole-2-thione

The thio­nocarbonate of trans-cyclo­octenediol, C9H12O2S, crystallizes with a 9/1 disorder in the position of the R,R and S,S-enanti­omers. As a result of trans-annulation, both rings adopt a twist conformation.