3

N-[(Pyridin-2-yl)meth­yl]thio­phene-2-carboxamide

In the title compound, C11H10N2OS, the dihedral angle between the thio­phene and pyridine rings is 77.79 (8)°. In the crystal, inversion dimers linked by pairs of N—H⋯N hydrogen bonds generate R22(10) loops. The dimers are reinforced by pairs of C—H⋯N inter­actions and C—H⋯O inter­actions link the dimers into [010] chains.




3

Bis(2-methyl­lactato)borate tetra­hydrate

The asymmetric unit of the title compound (systematic name: 3,3,8,8-tetra­methyl-1,4,6,9-tetra­oxa-λ4-bora­spiro­[4.4]nonane-2,7-dione tetra­hydrate), C8H12BO6·4H2O, consists of half a bis­(2-methyl­lactato)borate mol­ecule and two water mol­ecules of solvation. In the crystal, O—H⋯O hydrogen bonds link the components into a three-dimensional network.




3

(2S,3S,4R,4a'R,5R,5a'R,11a'R,12'S,12a'R)-5-(Acet­oxy­meth­yl)-2',2',10',10'-tetra­methyl­octa­hydro-3H,8'H-spiro­[furan-2,7'-[1,3]dioxino[4',5':5,6]pyrano[3,2-d][1,3,6]trioxocine]-3,4,12'-triyl tri­a

While the crystal structure analysis of the title compound, C26H38O15, a synthetic derivative of sucrose, was originally reported 40 years ago [Drew et al. (1979). Carbohydr. Res. 71, 35–42], the present work has allowed for the determination of its absolute configuration through the application of resonant scattering techniques.




3

1,2,4,5-Tetra­chloro-3,6-di­iodo­benzene benzene monosolvate

The title compound, C6Cl4I2·C6H6, crystallizes from benzene solution as cube-shaped crystals in the triclinic space group Poverline{1} with Z = 1. The asymmetric unit of the crystal structure contains one half of each mol­ecule. In the crystal, the benzene ring is almost orthogonal to the perhalo­benzene ring and the mol­ecules are linked by C—I⋯π inter­actions, with a close contact between the iodine atom and the benzene ring of 3.412 (1) Å.




3

catena-Poly[[di­aqua­cadmium(II)]-μ2-3-(4-carboxyl­atophen­yl)propionato]

In the title compound, [Cd(C10H8O4)(H2O)2)]n, the CdII cation is coordinated in a distorted trigonal–prismatic fashion. 3-(4-Carb­oxy­phen­yl)propionate (cpp) ligands connect the CdII cations into zigzag [Cd(cpp)(H2O)2)]n coordination polymer chains, which are oriented parallel to [101]. The chains aggregate into supra­molecular layers oriented parallel to (10overline{1}) by means of O—H⋯O hydrogen bonding between bound water mol­ecules and ligating cpp carboxyl­ate O atoms. The layers stack in an ABAB pattern along [100] via other O—H⋯O hydrogen-bonding mechanisms also involving the bound water mol­ecules. The crystal studied was an inversion twin.




3

Di-μ-acetato-bis­{[3-benzyl-1-(2,4,6-tri­methyl­phen­yl)imidazol-2-ylidene]silver(I)}

The title compound, [Ag2(C2H3O2)2(C19H20N2)2] (2), was readily synthesized by treatment of 3-benzyl-1-(2,4,6-tri­methyl­phen­yl)imidazolium chloride with silver acetate. The solution structure of the complex was analyzed by NMR spectroscopy, while the solid-state structure was confirmed by single-crystal X-ray diffraction studies. Compound 2 crystallizes in the triclinic space group Poverline{1}, with a silver-to-carbene bond length (Ag—CNHC) of 2.084 (3) Å. The mol­ecule resides on an inversion center, so that only half of the mol­ecule is crystallographically unique. The planes defined by the two imidazole rings are parallel to each other, but not coplanar [inter­planar distance is 0.662 (19) Å]. The dihedral angles between the imidazole ring and the benzyl and mesityl rings are 77.87 (12) and 72.86 (11)°, respectively. The crystal structure features π–π stacking inter­actions between the benzylic groups of inversion-related (−x + 1, −y + 1, −z + 1) mol­ecules and C—H⋯π inter­actions.




3

trans-Bis(dimethyl sulfoxide-κO)bis­(3-nitro­benzo­hydroxamato-κ2O,O')zinc(II)

Single crystals of the title complex, [Zn(C7H5N2O4)2(C2H6OS)2] or [Zn(NBZH)2(DMSO)2], were isolated from a dimethyl sulfoxide (DMSO) solution containing [Zn(NBZH)2]·2H2O (NBZH = 3-nitro­benzo­hydroxamate anion). The asymmetric unit comprises of one O,O'-chelating NBZH anion, one O-bound DMSO ligand and one zinc(II) cation localized on an inversion centre. The three-dimensional crystal packing includes N—H⋯O and C—H⋯O hydrogen bonding, as well as O⋯H and H⋯H contacts identified by Hirshfeld isosurface analysis.




3

(2,2-Bi­pyridine-κ2N,N')chlorido­[η6-1-methyl-4-(propan-2-yl)benzene]­ruthenium(II) tetra­phenyl­borate

The title complex, [RuCl(C10H14)(C10H8N2)](C24H20B), has monoclinic (P21) symmetry at 100 K. It was prepared by the reaction of the di­chlor­ido[1-methyl-4-(propan-2-yl)benzene]­ruthenium(II) dimer with 2,2'-bi­pyridine, followed by the addition of ammonium tetra­phenyl­borate. The 1-methyl-4-(propan-2-yl)benzene group, the 2,2'-bi­pyridine unit and a chloride ion coordinate the ruthenium(II) atom, with the 1-methyl-4-(propan-2-yl)benzene ring and bi­pyridine moieties trans to each other. In the crystal, the complex cations are linked by C—H⋯Cl hydrogen bonds, forming chains parallel to [010]. These chains are linked by a number of C—H⋯π inter­actions, involving the phenyl rings of the tetra­phenyl­borate anion and a pyridine ring of the bpy ligand, resulting in the formation of layers parallel to (10overline{1}).




3

Poly[[μ4-4-(carb­oxylato­meth­yl)benzoato]zinc(II)]

In the title compound, [Zn(C9H6O4)]n, the ZnII cations are coordinated in a tetra­hedral fashion by carboxyl­ate O-atom donors belonging to four 4-(carb­oxy­meth­yl) benzoate (4-cmb) ligands. Each 4-cmb ligand binds to four ZnII cations in an exo­tetra­dentate fashion to create a non-inter­penetrated [Zn(4-cmb)]n three-dimensional coordination polymer network with a new non-diamondoid 66 topology. The crystal studied was refined as an inversion twin.




3

(1Z,2Z)-1,2-Bis{2-[3,5-bis­(tri­fluoro­meth­yl)phen­yl]hydrazinyl­idene}-1,2-bis­(4-meth­oxy­phen­yl)ethane including an unknown solvate

The complete mol­ecule of the title compound, C32H22F12N4O2, is generated by a crystallographic twofold axis aligned parallel to [010]. The F atoms of one of the CF3 groups are disordered over three orientations in a 0.6: 0.2: 0.2 ratio. In the crystal, mol­ecules are linked by N—H⋯O hydrogen bonds, forming zigzag chains propagating along the a-axis direction. In addition, weak C—H⋯O and C—H⋯F bonds are observed. The contribution of the disordered solvent to the scattering was removed using the SQUEEZE routine [Spek (2015). Acta Cryst. C71, 9–18] of PLATON. The solvent contribution is not included in the reported mol­ecular weight and density.




3

8,13-Diisopropyl-10,11-dimethyl-bis([1,3]dioxolo[4',5':6,7]naphtho)­[1,2-d;2,1-f][1,3]dioxepine

The title compound, C31H30O6, was obtained by protecting the six hy­droxy groups of apogossypol by acetalization with di­chloro­methane. The mol­ecule has a bridging dioxepine unit which hinders the rotation around the 2,2'-inter­naphthyl bond. The dihedral angle between the naphthyl units is 55.73 (3)°. In the crystal, very weak C—H⋯O inter­actions may help to consolidate the packing.




3

(S)-1-(Benzyl­selan­yl)-3-phenyl­propan-2-amine

In the title compound, C16H19NSe, the dihedral angle between the benzene rings is 66.49 (12) and a weak intra­molecular N—H⋯Se hydrogen bond generates an S(6) ring. In the crystal, weak N—H⋯N hydrogen bonds link the mol­ecules into [100] chains.




3

1-(2-Amino-5-chloro­phen­yl)-2,2,2-tri­fluoro­ethan-1-one

In the title compound, C8H5ClF3NO, the F—C—C=O grouping shows a syn conformation [torsion angle = 1.1 (3)°] and an intra­molecular N—H⋯O hydrogen bond generates an S(6) ring. In the crystal, N—H⋯F and N—H⋯O hydrogen bonds link the mol­ecules into [010] chains.




3

(1,4,8,11-Tetra­aza­cyclo­tetra­deca­ne)palladium(II) diiodide monohydrate

In the title compound, [Pd(C10H24N4)]I2·H2O, the PdII ion is four-coordinated in a slightly distorted square-planar coordination environment defined by four N atoms from a 1,4,8,11-tetra­aza­cyclo­tetra­decane ligand. The cationic complex, two I− anions and the solvent water mol­ecule are linked through inter­molecular hydrogen bonds into a three-dimensional network structure.




3

(Pyridine-2,6-di­carboxyl­ato-κ3O,N,O')(2,2':6',2''- terpyridine-κ3N,N',N'')nickel(II) di­methyl­formamide monosolvate monohydrate

In the title complex, [Ni(C7H3NO4)(C15H11N3)]·C3H7NO·H2O, the NiII ion is six-coordinated within an octa­hedral geometry defined by three N atoms of the 2,2':6',2''-terpyridine ligand, and two O atoms and the N atom of the pyridine-2,6-di­carboxyl­ate di-anion. In the crystal, the complex mol­ecules are stacked in columns parallel to the a axis being connected by π–π stacking [closest inter-centroid separation between pyridyl rings = 3.669 (3) Å]. The connections between columns and solvent mol­ecules to sustain a three-dimensional architecture are of the type water-O—H⋯O(carbon­yl) and pyridyl-, methyl-C—H⋯O(carbon­yl).




3

S-Di­ethyl­amino-S-(3-methyl­benzoyl­imino)-S,S-di­phenyl­sulfonium tetra­fluoro­borate

The title salt, C24H27N2OS+·BF4−, was prepared by an alkyl­ation at the amino N atom attached to the sulfur atom of the corresponding sulfodi­imide. The configuration around the sulfur atom is a slightly distorted tetra­hedral geometry with two S—N bonds and two S—C bonds. The lengths of the S—N(di­ethyl­amine) and S=N(m-methyl­benzoyl­imine) bonds are 1.619 (2) and 1.551 (2) Å, respectively. The two N—S—N—C(eth­yl) and the N—S—N—C(m-methyl­benzoyl­imine) torsion angles are −85.43 (3), 58.94 (17) and 62.03 (16)°, respectively. The dihedral angle between the two phenyl rings is 84.03 (14)°. In the crystal, C—H⋯F hydrogen bonds link the cation and anion, forming a three-dimensional network.




3

3-(2,5-Di­chloro­thio­phen-3-yl)-5-(2,4-di­meth­oxy­phen­yl)-1-methyl-4,5-di­hydro-1H-pyrazole

In the title compound, C16H16Cl2N2O2S, the pyrazole ring has an envelope conformation with the C atom bearing the phenyl ring being the flap. The dihedral angles between the central pyrazole ring (all atoms) and pendant thio­phene and phenyl rings are 2.00 (14) and 81.49 (12)°, respectively. In the crystal, weak C—H⋯O, Cl⋯π and π–π stacking inter­actions link the mol­ecules into a three-dimensional network.




3

Bis(μ2-4-nitro­phenolato)bis­(4-nitro­phenolato)di-μ3-oxido-octaphenyltetra­tin chloro­form sesquisolvate [+ solvate]: a tetra­nuclear stannoxane

The title tetra­nuclear stannoxane, [Sn4(C6H5)8(C6H4NO3)4O2]·1.5CHCl3·solvent, crystallized with two independent complex mol­ecules, A and B, in the asymmetric unit together with 1.5 mol­ecules of chloro­form. There is also a region of disordered electron density, which was corrected for using the SQUEEZE routine [Spek (2015). Acta Cryst. C71, 9–18]. The oxo-tin core of each complex is in a planar `ladder' arrangement and each Sn atom is fivefold SnO3C2 coordinated, with one tin centre having an almost perfect square-pyramidal coordination geometry, while the other three Sn centres have distorted shapes. In the crystal, the complex mol­ecules are arranged in layers, composed of A or B complexes, lying parallel to the bc plane. The complex mol­ecules are linked by a number of C—H⋯O hydrogen bonds within the layers and between the layers, forming a supra­molecular three-dimensional structure.




3

6-Nitro-1,3-benzoxazole-2(3H)-thione

In the title compound, C7H4N2O3S, the dihedral angle between the fused ring system (r.m.s. deviation = 0.008 Å) and the nitro group at the 6-position is 7.3 (2)°. In the crystal, bifurcated N—H⋯(O,O) hydrogen bonds link the mol­ecules into [010] chains. The chains are cross-linked by π–π stacking inter­actions to form (001) sheets.




3

Crystal structure of a salt with a protonated sugar cation and a cobalt(II) complex anion: (GlcN–H, K)[Co(NCS)4]·2H2O

The title compound, d-(+)-glucosa­mmonium potassium tetra­thio­cyanato­cobaltate(II) dihydrate, K(C6H14NO5)[Co(NCS)4]·2H2O or (GlcNH)(K)[Co(NCS)4]·2H2O, has been obtained as a side product of an incomplete salt metathesis reaction of d-(+)-glucosa­mine hydro­chloride (GlcN·HCl) and K2[Co(NCS)4]. The asymmetric unit contains a d-(+)-glucos­ammonium cation, a potassium cation, a tetra­iso­thio­cyanato­cobalt(II) complex anion and two water mol­ecules. The water mol­ecules coordinate to the potassium cation, which is further coordinated via three short K+⋯SCN− contacts involving three [Co(NCS)4]2− complex anions and via three O atoms of two d-(+)-glucosa­mmonium cations, leading to an overall eightfold coordination around the potassium cation. Hydrogen-bonding inter­actions between the building blocks consolidate the three-dimensional arrangement.




3

1-(Cyclo­heptyl­idene)thio­semicarbazide

The asymmetric unit of the title compound, C8H15N3S, contains two independent mol­ecules. In both mol­ecules, the seven-membered cyclo­heptane ring adopts a chair conformation. An intra­molecular N—H⋯N hydrogen bond is observed in both mol­ecules, forming S(5) graph-set motifs. In the crystal, the two independent mol­ecules are connected through N—H⋯S hydrogen bonds, forming dimers which are in turn further connected by N—H⋯S hydrogen bonds into chains along [010].




3

N-[3-(Prop-1-yn-1-yl)phen­yl]benzene­sulfonamide

In the title sulfanilamide derivative, C15H13NO2S, which shows significant activity against Staphylococcus aureus and Escherichia coli, the dihedral angle between the planes of the aromatic rings is 62.15 (19)° and the four-coordinate S atom adopts an almost ideal tetra­hedral geometry. In the crystal, N—H⋯O and C—H⋯O hydrogen bonds link the mol­ecules into a three-dimensional network.




3

5,10-Di­hydro­indeno­[2,1-a]indene

The title compound, C16H12, crystallizes with four half mol­ecules in the asymmetric unit, each of which is located on a crystallographic centre of inversion. The mol­ecules are essentially planar. The crystal studied was a non-merohedral twin.




3

Bis(μ2-benzoato-κ2O,O')bis­(benzoato-κO)bis(ethanol-κO)bis­(μ3-hydroxido)hexa­kis­(μ-pyrazol­ato-κ2N,N')hexa­copper(II) ethanol disolvate

Trinuclear copper–pyrazolate entities are present in various Cu-based enzymes and nanojar supra­molecular arrangements. The reaction of copper(II) chloride with pyrazole (pzH) and sodium benzoate (benzNa) assisted by microwave radiation afforded a neutral centrosymmetric hexa­nuclear copper(II) complex, [Cu6(C7H5O2)4(OH)2(C3H3N2)6(C2H5OH)2]·2C2H5OH. Half a mol­ecule is present in the asymmetric unit that comprises a [Cu3(μ3-OH)(pz)3]2+ core with the copper(II) atoms arranged in an irregular triangle. The three copper(II) atoms are bridged by an O atom of the central hydroxyl group and by three bridging pyrazolate ligands on each of the sides. The carboxyl­ate groups show a chelating mode to one and a bridging syn,syn mode to the other two CuII atoms. The coordination environment of one CuII atom is square-planar while it is distorted square-pyramidal for the other two. Two ethanol mol­ecules are present in the asymmetric unit, one binding to one of the CuII atoms, one as a solvent mol­ecule. In the crystal, stabilization arises from inter­molecular O—H⋯O hydrogen-bonding inter­actions.




3

3-(3,5-Di­chloro­phen­yl)benzene-1,2-diol

The title structure, C12H8Cl2O2, is a putative metabolite of 3,5-di­chloro­biphenyl (PCB 14). The dihedral angle between the two benzene rings of the title compounds is 58.86 (4)°. In the crystal, it displays intra- and inter­molecular O—H⋯O hydrogen bonding and inter­molecular O—H⋯Cl hydrogen⋯chlorine inter­actions. The inter­molecular inter­actions form a two-dimensional network parallel to (010).




3

[SP-4-2]-(Aceto­nitrile-κN)chlorido­[2-(4,6-di­phenyl­pyridin-2-yl)phenyl-κ2C1,N]platinum(II)

The synthesis and crystal structure of the title PtII complex, [Pt(C23H16N)Cl(CH3CN)], based on the C,N-chelating 2,4,6-tri­phenyl­pyridine as the primary ligand, is described. The central PtII atom is in a distorted square-planar coordination environment. In the crystal, mol­ecules are arranged via a metallophilic inter­action between platinum atoms with a Pt⋯Pt contact of 7.052 (2) Å. In addition, a π–π inter­action occurs.




3

1:1 Co-crystal of 3-ethyl-4-methyl-3-pyrrolin-2-one and 3-ethyl-4-methyl-3-pyrroline-2,5-dione

Crystallization from a 20-year-old commercial source of 3-ethyl-4-methyl-3-pyrrolin-2-one afforded 1:1 co-crystals of this compound (C7H11NO) with its oxidized derivative, 3-ethyl-4-methyl-3-pyrroline-2,5-dione (C7H9NO2). The compound crystallizes in the space group Poverline{1}, with two mol­ecules of each species in the asymmetric unit. These four mol­ecules form a hydrogen-bonded tetra­mer with a dimer of 3-ethyl-4-methyl-3-pyrrolin-2-one as the core flanked by one mol­ecule of the dione on each side.




3

7-{3-Eth­oxy-4-[2-(2-meth­oxy­eth­oxy)eth­oxy]phen­yl}-5,6,8,9-tetra­hydro­dibenzo[c,h]acridine

In the title compound, C34H35NO4, the dihedral angle between the pyridine ring and attached benzene ring is 79.17 (8)°. The meth­oxy­eth­oxy–eth­oxy side chain is disordered over two orientations in a 0.732 (7):0.268 (7) ratio. In the crystal, very weak C—H⋯N and C—H⋯O inter­actions link the mol­ecules.




3

N,N,N-Trimethyl-1-[4-(pyridin-2-yl)phen­yl]meth­anaminium hexa­fluorido­phosphate

In the cation of the title mol­ecular salt, C15H19N2+·PF6−, the dihedral angle between the benzene and pyridine rings is 38.21 (10)°. In the crystal, weak C—H⋯F inter­actions arising from methyl and methyl­ene groups adjacent to the quaternary N atom generate (001) sheets.




3

3,4',5,5'-Tetra­meth­oxy-2'-methyl­biphen­yl-4-ol

The asymmetric unit of the title compound, C17H20O5, contains two independent mol­ecules, A and B, with similar geometries [dihedral angles between the phenyl rings = 56.19 (8) and 54.98 (7)°, respectively]. Intra­molecular O—H⋯O hydrogen bonds occur in both mol­ecules. In the crystal, the A mol­ecules form [1overline{1}0] chains linked by O—H⋯O hydrogen bonds from the hydroxyl group to one of the meth­oxy O atoms. The B mol­ecules form O—H⋯O hydrogen bonds to the hydroxyl O atoms of the A mol­ecules and thus act as fixed spacers between the chains of mol­ecule A. Some weak C—H⋯O contacts are also present.




3

Poly[(μ4-phenyl­phospho­nato)zinc(II)]

The title two-dimensional coordination polymer, [Zn(C6H5PO3)]n, was synthesized serendipitously by reacting a tetra­phospho­nate cavitand Tiiii[C3H7, CH3, C6H5] and Zn(CH3COO)2·2H2O in a DMF/H2O mixture. The basic conditions of the reaction cleaved the phospho­nate bridges at the upper rim of the cavitand, making them available for reaction with the zinc ions. The coordination polymer can be described as an inorganic layer in which zinc coordinates the oxygen atoms of the phospho­nate groups in a distorted tetra­hedral environment, while the phenyl groups, which are statistically disordered over two orientations, point up and down with respect to the layer. The layers inter­act through van der Waals inter­actions. The crystal studied was refined as a two-component twin.




3

Bis(quinolinium) tetra­bromido­manganate(II)

The title compound, (C9H8N)2[MnBr4], consists of two quinolinium cations and a [MnBr4]2− anion. The manganese(II) atom, which lies on a twofold rotation axis, is coordinated by four bromide ligands and exhibits a tetra­hedral coordination geometry. The [MnBr4]2− anion and the quinolinium cations are linked by N—H⋯Br hydrogen bonds. π–π stacking inter­actions are observed between the quinolinium cations.




3

Poly[di(μ2-2-hy­droxy­propano­ato)cadmium]

The asymmetric unit of the title inorganic–organic salt, poly[di(μ2-2-hy­droxy­propano­ato)cadmium], [Cd(C3H5O3)2]n or [Cd(Hlac)2]n (H2lac = 2-hy­droxy­propanoic acid), comprises of a cadmium cation and two 2-hy­droxy­propano­ate anions. The cadmium cation exhibits a distorted penta­gonal–bipyramidal coordination environment defined by the hy­droxy and carbonyl O atoms of the 2-hy­droxy­propano­ate anions. The coordination mode leads to the formation of layers extending parallel to (010). O—H⋯O hydrogen bonding between the hy­droxy and carbonyl groups stabilizes the structure packing.




3

1,1',3,3'-Tetra­mesitylquinobis(imidazole)-2,2'-di­thione

The solid-state structural analysis of the title compound [systematic name: 5,11-disulfanylidene-4,6,10,12-tetrakis(2,4,6-trimethylphenyl)-4,6,10,12-tetraazatricyclo[7.3.0.03,7]dodeca-1(9),3(7)-diene-2,8-dione], C44H44N4O2S2 [+solvent], reveals that the mol­ecule crystallizes in a highly symmetric cubic space group so that one quarter of the mol­ecule is crystallographically unique, the mol­ecule lying on special positions (two mirror planes, two twofold axes and a center of inversion). The crystal structure exhibits large cavities of 193 Å3 accounting for 7.3% of the total unit-cell volume. These cavities contain residual density peaks but it was not possible to unambiguously identify the solvent therein. The contribution of the disordered solvent mol­ecules to the scattering was removed using a solvent mask and is not included in the reported mol­ecular weight. No classical hydrogen bonds are observed between the main mol­ecules.




3

(E)-1-(2-Hy­droxy-6-meth­oxy­phen­yl)-3-(2-meth­oxy­naphthalen-1-yl)prop-2-en-1-one

In the title compound, C21H18O4, the dihedral angle between the naphthelene ring system (r.m.s. deviation = 0.014 Å) and the benzene ring is 9.68 (1)°. The C atom of the meth­oxy group of the naphthalene ring system is almost coplanar with the ring [C—O—C—C = −2.0 (3)°], whereas the C atom of the meth­oxy group of the phenol ring is slightly twisted [C—O—C—C = 6.2 (3)°]. An intra­molecular O—H⋯O hydrogen bond generates an S(6) ring motif.




3

3-Bromo­pyridine-2-carbo­nitrile

The title compound, C6H3BrN2, also known as 3-bromo­picolino­nitrile, was synthesized by cyanation of 2,3-di­bromo­pyridine. In the solid state, short inter­molecular Br⋯N contacts are observed. Additionally, the crystal packing is consolidated by π–π stacking inter­actions with centroid–centroid distances of 3.7893 (9) Å.




3

3,3'-[(1E,1'E)-Hydrazine-1,2-diylidenebis(ethan-1-yl-1-yl­idene)]bis­(4-hy­droxy-6-methyl-2H-pyran-2-one)

The title compound, C16H16N2O6, lies about an inversion centre at the mid-point of the N—N bond. The mol­ecule features two intra­molecular O—H⋯N and two C—H⋯O hydrogen bonds, each of which forms an S(6) ring motif. In the crystal, mol­ecules are linked by C—H⋯O hydrogen bonds into infinite zigzag chains propagating along the c-axis direction. π–π stacking inter­actions between the pyrone rings [centroid–centroid distances = 3.975 (2) Å] stack the mol­ecules along b.




3

4-Amino-5-{[cyclo­hex­yl(meth­yl)amino]­meth­yl}iso­phthalo­nitrile

The title compound, C16H20N4, was synthesized by cyanation of brom­hexine. The compound crystallizes with two unique mol­ecules in the asymmetric unit. The substituted aniline and cyclo­hexane rings are inclined to one another by 37.26 (6)° in one mol­ecule and by 22.84 (7)° in the other. In the crystal packing, intra- and inter­molecular N—H⋯N hydrogen bonds and an inter­molecular C—H⋯N contact were observed.




3

Decacarbon­yl(μ-ethyl­idenimino-1κN:2κC)-μ-hydrido-triangulo-triosmium(3 Os–Os)

The title complex, [Os3(C2H4N)H(CO)10] or [Os3(CO)10(μ-H)(μ-HN=C—CH3-1κN:2κC)], was synthesized in 41.6% yield by reactions between Os3(CO)11(CH3CN) and 2,4,6-tri­methyl­hexa­hydro-1,3,5-triazine. The central osmium triangle has two OsI atoms bridged by a hydride ligand and a μ-HN= C—CH3-1κN:2κC triazine fragment. Three CO ligands complete the coordination sphere around each OsI atom, while the remaining Os0 atom has four CO ligands. Each Os atom exhibits a pseudo-octa­hedral coordination environment, discounting the bridging Os—Os bond.




3

5,13-Bis(4-meth­oxy­phen­yl)di­naphtho­[2,3-b:2',3'-d]thio­phene S,S-dioxide di­chloro­methane hemisolvate

The title com­pound, C34H24O4S·0.5CH2Cl2, crystallizes with two independent mol­ecules and one di­chloro­methane solvent mol­ecule in the asymmetric unit. The crystal packing is consolidated by C—H⋯O hydrogen bonds.




3

1-Isobutyl-8,9-dimeth­oxy-3-phenyl-5,6-dihidro­imidazo[5,1-a]isoquinolin-2-ium chloride

The molecular salt, C23H26N2O2+·Cl−, was obtained from 1-isobutyl-8,9-dimeth­oxy-3-phenyl-5,6-di­hydro­imidazo[5,1-a]iso­quinoline, which was synthesized by cyclo­condensation of α-benzoyl­amino-γ-methyl-N-[2-(3,4-di­meth­oxy­phen­yl)eth­yl]valeramide in the presence of phosphoryl chloride. The tetra­hydro­pyridine ring adopts a twist–boat conformation. In the crystal structure, centrosymmetric dimers are formed by N—H⋯Cl and C—H⋯Cl hydrogen bonds.




3

2,4-Di­chloro-6-[(2-hy­droxy-5-methyl­anilino)methyl­idene]cyclo­hexa-2,4-dienone

The title compound, C14H11Cl2NO2, has been prepared by the condensation of 3,5-di­chloro­salicyl­aldehyde and 2-amino-4-methyl­phenol. The asymmetric unit consists of two independent mol­ecules, both of which are almost planar; the dihedral angle between the two benzene rings is 10.61 (8)° for one mol­ecule and 2.46 (8)° for the other. There is an intra­molecular N—H⋯O hydrogen bond that generates S(6) ring motifs in each mol­ecule. In the crystal, the two independent mol­ecules are linked by O—H⋯O and C—H⋯Cl hydrogen bonds, forming a pseudo-inversion dimer. A π–π inter­action, with a centroid–centroid distance of 3.6065 (12) Å, is also observed.




3

9α-Hy­droxy-4,8-dimethyl-3'-phenyl-3,14-dioxatri­cyclo­[9.3.0.02,4]tetra­dec-7-en-13-one-12-spiro-5'-isoxazole monohydrate

In the title compound, C22H25NO5·H2O, the ten-membered ring displays an approximate chair–chair conformation, whereas the five-membered furan ring has an envelope conformation, with the C atom of the methine group adjacent to the spiro C atom as the flap. The isoxazole ring is almost planar and its plane is slightly inclined to the plane of the attached phenyl ring. The mean plane of the furan ring is nearly perpendicular to that of the isoxazole ring, as indicated by the dihedral angle between them of 89.39 (12)°. In the crystal, the organic mol­ecules are linked into [010] chains by O—H⋯O hydrogen bonds. The water mol­ecule forms O—H⋯O and O—H⋯N hydrogen bonds and a weak C—H⋯O inter­action is also observed. Together, these lead to a three-dimensional network.




3

Bis[2-(di­methyl­amino-κN)-α,α-di­phenyl­benzene­methano­lato-κO](tetra­hydro­furan-κO)magnesium(II)

The title magnesium complex, [Mg(C21H20NO2)2(C4H8O)]n, exhibits two N,O-bidentate 2-(di­methyl­amino)-α,α-di­phenyl­benzene­methano­late ligands, form­ing two six-membered chelate rings. The distorted square-pyramidal coordination sphere of the MgII atom is completed by the O atom of a tetra­hydro­furan ligand, with its O atom in the apical position. The O and N atoms are in a mutual trans arrangement. Except for two C—H⋯π inter­actions, no significant inter­molecular inter­actions are observed in the crystal.




3

1,4-Bis(2-nitro­benz­yl)piperazine

The title compound, C18H20N4O4, was synthesized via the base-assisted reaction of piperazine and 2-nitro­benyl bromide in toluene: the complete mol­ecule is generated by a crystallographic inversion centre in the solid state.




3

Bis(4-hy­droxy-N,N-di-n-propyl­tryptammonium) fumarate tetra­hydrate

The title compound (systematic name: bis­{[2-(4-hy­droxy-1H-indol-3-yl)eth­yl]bis­(propan-2-yl)aza­nium} but-2-enedioate tetra­hydrate), 2C16H25N2O+·C4H2O42−·4H2O, has a singly protonated DPT cation, one half of a fumarate dianion (completed by a crystallographic centre of symmetry) and two water mol­ecules of crystallization in the asymmetric unit. A series of N—H⋯O and O—H⋯O hydrogen bonds form a three-dimensional network in the solid state.




3

N-(tert-But­yl)-2-(2-nitro­phen­yl)imidazo[1,2-a]pyridin-3-amine

In the title compound, C17H18N4O2, the dihedral angle between the pyridine and benzene rings is 55.68 (11)°. In the crystal, N—H⋯N hydrogen bonds link the mol­ecules into [010] chains.




3

(4-Carb­oxy­benz­yl)tri­phenyl­phospho­nium hexa­fluorido­phosphate tetra­hydro­furan monosolvate

The title compound, C26H22O2P+·PF6−·C4H7O, crystallizes as a cation-anion pair with a single solvent mol­ecule in the asymmetric unit. Hydrogen bonding occurs between the carb­oxy­lic acid group on the cation and the oxygen atom of the solvent mol­ecule. Longer hydrogen-bonding inter­actions are observed between fluorine atoms of the anion and H atoms on the phenyl rings of the cation.




3

2-[1-(1,3-Dioxo-1,3-di­hydro-2H-inden-2-yl­idene)eth­yl]hydrazinecarbo­thio­amide

The title compound, C12H11N3O2S, was synthesized by a condensation reaction of 2-acetyl­indan-1,3-dione and thio­semicarbazide in ethanol in the presence of glacial acetic acid. The mol­ecule adopts a thio­ketone form. The dihedral angle between the mean planes of 1H-inden-1,3(2H)-dione and hydrazinecarbo­thio­amide units is 86.32 (7)°. Weak intra­molecular N—H⋯O and C—H⋯O hydrogen bonds are observed. In the crystal, mol­ecules are linked via pairs of weak inter­molecular N—H⋯O hydrogen bonds, forming inversion dimers. The dimers are further linked into a three-dimensional network through N—H⋯S and N—H⋯O hydrogen bonds, and π–π inter­actions [centroid–centroid distances = 3.5619 (10)–3.9712 (9) Å].




3

2-[(1-Benzyl-1H-1,2,3-triazol-4-yl)meth­oxy]-1-naphthaldehyde

In the title compound, C21H17N3O2, the triazole ring system is inclined at dihedral angles of 4.14 (18) and 69.24 (11)° with the naphthalene ring system and phenyl ring, respectively. In the crystal, mol­ecules are linked by C—H⋯O hydrogen bonds into double columns propagating along the b-axis direction.