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.

In the paper by Oliveira et al. [IUCrData (2023), 8, x230971], there was an error in the name of the first author.

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].

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.

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.

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.

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.

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).

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

The structure of pinaverium bromide (systematic name: 4-[(2-bromo-4,5-di­meth­oxy­phen­yl)meth­yl]-4-{2-[2-(6,6-dimethyl-2-bi­cyclo­[3.1.1]hepta­nyl)eth­oxy]eth­yl}morpholin-4-ium bromide; C26H41Br2NO4), was determined at 110 K. It has monoclinic (P21) symmetry. It is of inter­est with respect to its anti-inflammatory properties. The asymmetric unit contains two independent mol­ecules, one of which exhibits disorder of the bi­cyclo terminal group (occupancy factors: 0.78 and 0.22).

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.

The title compound, C15H15NO2, crystallizes with two mol­ecules in the asymmetric unit. In the crystal, the two mol­ecules associate to form an acid–acid dimer by pairwise O—H⋯O hydrogen bonds.

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].

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.

The title coordination polymer, [Co(N3)2(C9H8N2)]n, was synthesized solvothermally. The CoII atom exhibits a distorted octa­hedral [CoN6] coordination geometry with a bidentate 8-amino­quinoline ligand and four azide ligands. Bridging azide ligands result in chains extending along [100]. N—H⋯N hydrogen bonds join the chains to give an extended structure with sheets parallel to (002).

The title compound, [Ag2(C19H20N2)4]Cl·0.5C2H4Cl2, can be readily generated by treatment of (1-benzyl-3-(2,4,6-tri­methyl­phen­yl)imidazolium chloride with sodium bis­(tri­methyl­sil­yl)amide followed by silver chloride. The mol­ecular structure of the compound was confirmed using NMR spectroscopy and single-crystal X-ray diffraction analysis. The crystal structure of the title compound at 110 K has monoclinic (P21/c) symmetry. The represented silver compound is of inter­est with respect to anti­bacterial properties and the structure displays a series of weak inter­molecular hydrogen-bonding inter­actions with the chloride counter-anion.

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.

The title compound, C2H4BrNO, crystallizes in the monoclinic space group P21/c with one mol­ecule in the asymmetric unit. The almost planar mol­ecules are organized via N—H⋯O hydrogen bonds into a ladder-type network, which can be characterized by the graph sets R22(8) and R24(8). In addition, the mol­ecules are connected by C—H⋯O and C—H⋯Br contacts.

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.

The title compound, [Zn2(C6H8O4)2(C10H9N3)2]·3H2O or {Zn2[(C5H4N)2NH]2[μ-(CH2)4(COO)2]2}·3H2O, was separ­ated from the solvothermal reaction of zinc(II) sulfate hepta­hydrate, 2,2'-di­pyridyl­amine and sodium adipate. The dinuclear metal complex has a centrosymmetric structure, with the ZnII atom adopting a highly distorted octa­hedral coordination sphere composed of four oxygen atoms from bridging adipato ligands and two pyridine nitro­gen atoms. In the crystal, the title compound aggregates into a tri-periodic supra­molecular structure through inter­molecular hydrogen-bonding networks of the form O—H⋯O and N—H⋯O.

A new triazole-based N-heterocyclic carbene IrI cationic complex with a tetra­fluorido­borate counter-anion and hemi-solvating di­chloro­methane, [Ir(C8H12)(C8H15N3)(C18H15P)]BF4·0.5CH2Cl2, has been synthesized and structurally characterized. There are two independent ion pairs in the asymmetric unit and one di­chloro­methane solvent mol­ecule per two ion pairs. The cationic complex exhibits a distorted square-planar conformation around the IrI atom, formed by a bidentate cyclo­octa-1,5,diene (COD) ligand, a tri­phenyl­phosphane ligand, and an N-heterocyclic carbene (NHC). There are several close non-standard H⋯F hydrogen-bonding inter­actions that orient the tetra­fluorido­borate anions with respect to the IrI complex mol­ecules. The complex shows promising catalytic activity in transfer hydrogenation reactions. The structure was refined as a non-merohedral twin, and one of the COD mol­ecules is statistically disordered.

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.

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.

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.

In the crystal of the title compound, C12H17N3, the mol­ecules are linked by N—H⋯N hydrogen bonds, generating a C(4) chain extending along the c-axis direction. One of the ethyl groups is disordered over two sets of sites with a refined occupancy ratio of 0.582 (15):0.418 (15).

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].

The title compound, C14H20NO5+·Cl−, was prepared as a racemate of R,R- and S,S-enanti­omers by reduction of the corresponding hy­droxy­imino­ketone. In the crystal, layers are formed via hydrogen bridges of four ammonium groups to chloride ions; these lamellae are connected via inter­digitated benzoic ester groups.

The crystal structure of the title compound, C14H12N2O2S, reveals two symmetrically independent mol­ecules within the asymmetric unit. Each mol­ecule contains a chromenone core attached to a 2-thio­phene ring, cyano, and amino groups. The 2-thio­phene ring of one of the two mol­ecules in the asymmetric unit was found to be disordered over two positions, with the major component having a site occupancy factor of 0.837 (2). The 2-thio­phene ring is nearly orthogonal to the fused 4H-pyran ring, with dihedral angles between the two sets of planes being 89.5 (5) and 89.63 (8)°. Inter­molecular hydrogen bonding, involving N—H⋯N and N—H⋯O inter­actions, creates two distinct motifs leading to the formation of a two-dimensional supra­molecular network along the crystallographic ac plane.

The crystal structure of a new 1:1 cocrystal of carbamazepine and S-naproxen (C15H12N2O·C14H14O3) was solved from powder X-ray diffraction (PXRD). The PXRD pattern was measured at the high-resolution beamline CRISTAL at synchrotron SOLEIL (France). The structure was solved using Monte Carlo simulated annealing, then refined with Rietveld refinement. The positions of the H atoms were obtained from density functional theory (DFT) ground-state calculations. The symmetry is ortho­rhom­bic with the space group P212121 (No. 19) and the following lattice parameters: a = 33.5486 (9), b = 26.4223 (6), c = 5.3651 (10) Å and V = 4755.83 (19) Å3.

Beauveriolides, including the main beauveriolide I {systematic name: (3R,6S,9S,13S)-9-benzyl-13-[(2S)-hexan-2-yl]-6-methyl-3-(2-methyl­prop­yl)-1-oxa-4,7,10-tri­aza­cyclo­tridecane-2,5,8,11-tetrone, C27H41N3O5}, are a series of cyclo­depsipeptides that have shown promising results in the treatment of Alzheimer's disease and in the prevention of foam cell formation in atherosclerosis. Their crystal structure studies have been difficult due to their tiny crystal size and fibre-like morphology, until now. Recent developments in 3D electron diffraction methodology have made it possible to accurately study the crystal structures of submicron crystals by overcoming the problems of beam sensitivity and dynamical scattering. In this study, the absolute structure of beauveriolide I was determined by 3D electron diffraction. The cyclo­dep­si­peptide crystallizes in the space group I2 with lattice parameters a = 40.2744 (4), b = 5.0976 (5), c = 27.698 (4) Å and β = 105.729 (6)°. After dynamical refinement, its absolute structure was determined by comparing the R factors and calculating the z-scores of the two possible enanti­omorphs of beauveriolide I.

This report presents a comprehensive investigation into the synthesis and characterization of Schiff base com­pounds derived from benzene­sul­fon­amide. The synthesis process, involved the reaction between N-cyclo­amino-2-sulf­anil­amide and various substituted o-salicyl­aldehydes, resulted in a set of com­pounds that were subjected to rigorous characterization using advanced spectral techniques, including 1H NMR, 13C NMR and FT–IR spectroscopy, and single-crystal X-ray diffraction. Furthermore, an in-depth assessment of the synthesized com­pounds was conducted through Absorption, Distribution, Metabolism, Excretion and Toxicity (ADMET) analysis, in conjunction with docking studies, to elucidate their pharmacokinetic profiles and potential. Impressively, the ADMET analysis showcased encouraging drug-likeness properties of the newly synthesized Schiff bases. These computational findings were substanti­ated by mol­ecular properties derived from density functional theory (DFT) calculations using the B3LYP/6-31G* method within the Jaguar Module of Schrödinger 2023-2 from Maestro (Schrodinger LLC, New York, USA). The ex­plor­ation of frontier mol­ecular orbitals (HOMO and LUMO) enabled the computation of global reactivity descriptors (GRDs), encompassing charge separation (Egap) and global softness (S). Notably, within this analysis, one Schiff base, namely, 4-bromo-2-{N-[2-(pyr­rol­idine-1-sul­fonyl)phenyl]car­box­imid­oyl}phenol, 20, em­erged with the smallest charge separation (ΔEgap = 3.5780 eV), signifying heightened potential for biological properties. Conversely, 4-bromo-2-{N-[2-(piper­idine-1-sul­fonyl)phenyl]car­box­imid­oyl}phenol, 17, exhibited the largest charge separation (ΔEgap = 4.9242 eV), implying a relatively lower propensity for biological activity. Moreover, the synthesized Schiff bases displayed re­marke­able inhibition of tankyrase poly(ADP-ribose) polymerase enzymes, integral in colon cancer, surpassing the efficacy of a standard drug used for the same purpose. Additionally, their bioavailability scores aligned closely with established medications such as trifluridine and 5-fluoro­uracil. The ex­plor­ation of mol­ecular electrostatic potential through colour mapping delved into the electronic behaviour and reactivity tendencies intrinsic to this diverse range of mol­ecules.

X-ray and electron diffraction methods independently identify the S-enanti­omer of Berkecoumarin [systematic name: (S)-8-hy­droxy-3-(2-hy­droxy­prop­yl)-6-meth­oxy-2H-chromen-2-one]. Isolated from Berkeley Pit Lake Penicillium sp., Berkecoumarin is a natural product with a light-atom com­position (C13H14O5) that challenges in-house absolute structure determination by anomalous scattering. This study further demonstrates the utility of dynamical refinement of electron-diffraction data for absolute structure determination.

The crystal structures of three mixed-valence copper cyanide alkanolamine polymers are presented, together with thermogravimetric analysis (TGA) and electron spin resonance (ESR) data. In all three structures, a CuII moiety on a crystallographic center of symmetry is coordinated by two alkanolamines and links two CuICN chains via cyanide bridging groups to form diperiodic sheets. The sheets are linked together by cuprophilic CuI–CuI inter­actions to form a three-dimensional network. In poly[bis­(μ-3-amino­propano­lato)tetra-μ-cyan­ido-dicopper(I)dicopper(II)], [Cu4(CN)4(C3H8NO)2]n, 1, propano­lamine bases have lost their hydroxyl H atoms and coordinate as chelates to two CuII atoms to form a dimeric CuII moiety bridged by the O atoms of the bases with CuII atoms in square-planar coordination. The ESR spectrum is very broad, indicating exchange between the two CuII centers. In poly[bis­(2-amino­pro­pan­ol)tetra-μ-cyanido-dicopper(I)copper(II)], [Cu3(CN)4(C3H9NO)2]n, 2, and poly[bis­(2-amino­ethanol)tetra-μ-cyanido-dicopper(I)copper(II)], [Cu3(CN)4(CH7NO)2]n, 3, a single CuII atom links the CuICN chains together via CN bridges. The chelating alkanolamines are not ionized, and the OH groups form rather long bonds in the axial positions of the octa­hedrally coordinated CuII atoms. The coordination geometries of CuII in 2 and 3 are almost identical, except that the Cu—O distances are longer in 2 than in 3, which may explain their somewhat different ESR spectra. Thermal decom­position in 2 and 3, but not in 1, begins with the loss of HCN(g), and this can be correlated with the presence of OH protons on the ligands in 2 and 3, which are not present in 1.

We report on the latest advancements in Microcrystal Electron Diffraction (3D ED/MicroED), as discussed during a symposium at the National Center for CryoEM Access and Training housed at the New York Structural Biology Center. This snapshot describes cutting-edge developments in various facets of the field and identifies potential avenues for continued progress. Key sections discuss instrumentation access, research applications for small mol­ecules and biomacromolecules, data collection hardware and software, data reduction software, and finally reporting and validation. 3D ED/MicroED is still early in its wide adoption by the structural science community with ample opportunities for expansion, growth, and innovation.