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Propane-1,3-diaminium squarate dihydrate, C 3 H 12 N 2 2+ ·C 4 O 4 2- ·2H 2 O, results from the proton-transfer reaction of propane-1,3-di-amine with squaric acid and subsequent crystallization from aqueous medium. The title compound crystallizes in the tetra-gonal crystal system (space group P 4 bm ) with Z = 2. The squarate dianion belongs to the point group D 4 h and contains a crystallographic fourfold axis. The propane-1,3-diaminium dication exhibits a C 2 v -symmetric all- anti conformation and resides on a special position with mm 2 site symmetry. The orientation of the propane-1,3-diaminium ions makes the crystal structure polar in the c- axis direction. The solid-state supra-molecular structure features a triperiodic network of strong hydrogen bonds of the N-H⋯O and O-H⋯O types., (© Seidel and Kolev 2024.)

The crystal structure of 1,2,3,4-tetra-hydro-isoquinolin-2-ium (2 S ,3 S )-3-carb-oxy-2,3-di-hydroxy-propano-ate monohydrate, C 9 H 12 N + ·C 4 H 5 O 6 - ·H 2 O, at 115 K shows ortho-rhom-bic symmetry (space group P 2 1 2 1 2 1 ). The hydrogen tartrate anions and solvent water mol-ecules form an intricate diperiodic O-H⋯O hydrogen-bond network parallel to (001). The tetra-hydro-isoquinolinium cations are tethered to the anionic hydrogen-bonded layers through N-H⋯O hydrogen bonds. The crystal packing in the third direction is achieved through van der Waals contacts between the hydro-carbon tails of the tetra-hydro-isoquinolinium cations, resulting in hydro-phobic and hydro-philic regions in the crystal structure., (© Seidel and Kolev 2024.)

The title compound, C 15 H 15 F 3 N 2 O 3 S, crystallizes in the monoclinic system, space group I 2/ a , with Z = 8. As expected, the nine-membered heterobicyclic system is virtually planar and the cyclo-hexyl group adopts a chair conformation. There is structural evidence for intra-molecular N-S⋯O chalcogen bonding between the benziso-thia-zolinone S atom and one O atom of the nitro group, approximately aligned along the extension of the covalent N-S bond [N-S⋯O = 162.7 (1)°]. In the crystal, the mol-ecules form centrosymmetric dimers through C-H⋯O weak hydrogen bonding between a C-H group of the electron-deficient benzene ring and the benzo-thia-zolinone carbonyl O atom with an R 2 2 (10) motif. In contrast to the previously described N -acyl 7-nitro-5-(tri-fluoro-meth-yl)benzo[ d ]iso-thia-zol-3(2 H )-ones, the title N -cyclo-hexyl-methyl analogue does not inhibit growth of Mycobacterium aurum and Mycobacterium smegmatis in vitro ., (© Richter et al. 2023.)

8-Nitro-1,3-benzo-thia-zin-4-ones are a promising class of new anti-tubercular agents, two candidates of which, namely BTZ043 and PBTZ169 (INN: macozinone), have reached clinical trials. The crystal and mol-ecular structures of two synthetic precursors, 2-chloro-3-nitro-5-(tri-fluoro-meth-yl)benzoic acid, C 8 H 3 ClF 3 NO 4 ( 1 ), and 2-chloro-3-nitro-5-(tri-fluoro-meth-yl)benzamide, C 8 H 4 ClF 3 N 2 O 3 ( 2 ), are reported. In 1 and 2 , the respective carb-oxy, carboxamide and the nitro groups are significantly twisted out of the plane of the benzene ring. In 1 , the nitro group is oriented almost perpendicular to the benzene ring plane. In the crystal, 1 and 2 form O-H⋯O and N-H⋯O hydrogen-bonded dimers, respectively, which in 2 extend into primary amide tapes along the [101] direction. The tri-fluoro-methyl group in 2 exhibits rotational disorder with an occupancy ratio of 0.876 (3):0.124 (3)., (© Richter et al. 2021.)

1,3-Benzo-thia-zin-4-ones (BTZs) are a promising new class of anti-tuberculosis drug candidates, some of which have reached clinical trials. The title compound, the benzamide derivative [2-chloro-3-nitro-5-(tri-fluoro-meth-yl)phen-yl](piper-id-in-1-yl)methanone, C 13 H 12 ClF 3 N 2 O 3 , occurs as a side product as a result of competitive reaction pathways in the nucleophilic attack during the synthesis of the BTZ 8-nitro-2-(piperidin-1-yl)-6-(tri-fluoro-meth-yl)-1,3-benzo-thia-zin-4-one, following the original synthetic route, whereby the corresponding benzoyl iso-thio-cyanate is reacted with piperidine as secondary amine. In the title compound, the nitro group and the nearly planar amide group are significantly twisted out of the plane of the benzene ring. The piperidine ring adopts a chair conformation. The tri-fluoro-methyl group exhibits slight rotational disorder with a refined ratio of occupancies of 0.972 (2):0.028 (2). There is structural evidence for inter-molecular weak C-H⋯O hydrogen bonds., (© Eckhardt et al. 2020.)

The synthesis of ethyl 2-[(4-methyl-pyridin-2-yl)amino)-4-(pyridin-2-yl)thia-zole- 5-carboxyl-ate via the Hantzsch reaction and partial in situ transesterification during recrystallization from methanol- d 4 to the d 3 -methyl ester, resulting in the title solid solution, ethyl 2-[(4-methyl-pyridin-2-yl)amino)-4-(pyridin-2-yl)thia-zole-5-carboxyl-ate- d 3 -methyl 2-[(4-methyl-pyridin-2-yl)amino)-4-(pyridin-2-yl)thia-zole-5-carboxyl-ate (0.88/0.12), 0.88C 17 H 16 N 4 O 2 S·0.12C 16 D 3 H 11 N 4 O 2 S, is reported. The refined ratio of ethyl to d 3 -methyl ester in the crystal is 0.880 (6):0.120 (6). The pyridine ring is significantly twisted out of the plane of the approximately planar picoline thia-zole ester moiety. N-H⋯N hydrogen bonds between the secondary amino group and the pyridine nitro-gen atom of an adjacent symmetry-related mol-ecule link the mol-ecules into polymeric hydrogen-bonded zigzag tapes extending by glide symmetry in the [001] direction. There is structural evidence for intra-molecular N⋯S chalcogen bonding and inter-molecular weak C-H⋯O hydrogen bonds between adjacent zigzag tapes., (© Beuchel et al. 2020.)

The title compound, [HgI 2 (C 10 H 8 N 2 O 2 S 2 )] n , a one-dimensional coordination polymer with HgI 2 units and 2,2'-di-thio-bis-(pyridine N -oxide) spacer ligands in an alternating fashion, forms helical chains running along the b axis in the crystal. Within a single coordination polymer strand, the axially chiral 2,2'-di-thio-bis-(pyridine N -oxide) ligands are homochiral, but the enanti-omeric conformation is present in adjacent strands. Within a coordination polymer strand, the iodido ligands point towards the centroids of the aromatic rings of the pyridine N -oxide moieties in the coordination sphere of Hg II . Moreover, intra-strand C-H⋯O and C-H⋯I inter-actions, and inter-strand short S⋯I and S⋯O contacts are observed.

The title compound, [Cu(C20H23N3O4)], crystallizes in the space group Cc with two independent mol-ecules in the asymmetric unit. The Cu(II) atoms are each coordinated by the penta-dentate Schiff base ligand in a distorted trigonal bipyramidal N3O2 geometry. The equatorial plane is formed by the two phenolic O atoms and the amine N atom, while the axial positions are occupied by the two imine N atoms. In the crystal, the two independent mol-ecules are each connected into a column along the b axis through inter-molecular O-H⋯O hydrogen bonds. The two independent columns are further linked through an N-H⋯O hydrogen bond, forming a double-column structure.

In the crystal structure of the title mononuclear Cu(II) complex, [Cu(C11H16N3O2)(NO3)]·0.25C2H5OH, the complex molecules are linked by N-H⋯O and O-H⋯O hydrogen bonds, forming a dimer with an approximate non-crystallographic twofold rotation axis of symmetry. In the monomeric unit, the Cu(2+) ion exhibits a distorted square-pyramidal configuration, whereby the anionic [HL](-) Schiff base ligand binds in a tetradentate fashion via the O and the three N atoms which all are approximately coplanar. The O atom of a nitrate anion occupies the fifth coordination site, causing the Cu(II) atom to move slightly out of the approximate basal plane toward the bound nitrate group. The structure exhibits disorder of the ethanol solvent mol-ecule.