2,7-Dichloro-3-O-methylnorlichexanthone

We report the hydro-thermal syntheses and crystal structures of aqua-bis-(2,2'-bi-pyridine-κ2 N,N')copper(II) hexa-fluorido-silicate tetra-hydrate, [Cu(bpy)2(H2O)][SiF6]·4H2O (bpy is 2,2'-bi-pyridine, C10H8N2), (I), bis-(2,2'-bi-pyridine-3κ2 N,N')-di-μ-fluorido-1:3κ2 F:F;2:3κ2 F:F-deca-fluorido-1κ5 F,2κ5 F-ditantalum(V)copper(II), [Cu(bpy)2(TaF6)2], (II), tris-(2,2'-bi-pyridine-κ2 N,N')copper(II) bis[hexa-fluorido-tantalate(V)], [Cu(bpy)3][TaF6]2, (III), and catena-poly[[di-aqua-(2,2'-bi-pyridine-κ2 N,N')copper(II)]-μ-fluorido-tetra-fluorido-tin-μ-fluorido], [Cu(bpy)(H2O)2SnF6] n , (IV). Compounds (I), (II) and (III) contain locally chiral copper coordination complexes with C 2, D 2, and D 3 symmetry, respectively. The extended structures of (I) and (IV) are consolidated by O-H⋯F and O-H⋯O hydrogen bonds. The structure of (III) was found to be a merohedral (racemic) twin.

The asymmetric unit of the title compound, C(9)H(4)S(7), contains two independent mol-ecules, in one of which the central five-membered ring is disordered over two orientations in a 0.924 (3):0.076 (3) ratio. The mol-ecular skeleton is almost planar: the average distance of the atoms from their mean plane is 0.128 (7) Å in the ordered mol-ecule, and 0.088 (5) and 0.123 (2) Å in the major and minor disorder components, respectively. The ordered and disordered mol-ecules form separate columns by stacking along the b axis. Adjacent columns inter-act via short S⋯S [3.33 (2), 3.434 (3), 3.444 (2), 3.503 (2), 3.519 (3) and 3.53 (4) Å] and S⋯H [2.814 (2), 2.87 (7), 2.92 (2), 2.9269 (18), 2.93 (2), 2.94 (2), 2.939 (2), 2.967 (2) and 2.974 (1) Å] contacts.

In the title compound, C19H17Cl2N3O2, there are three mol-ecules (A, B and C) in the asymmetric unit and each differs in the conformation adopted. As a result of steric repulsion, the amide group is rotated with respect to both the dichloro-phenyl and 2,3-dihydro-1H-pyrazol-4-yl rings, making dihedral angles of 44.5 (2) and 56.2 (2)°, respectively in A, 51.1 (2) and 54.1 (2)° in B, and 53.8 (2) and 54.6 (2)° in C. The dihedral angles between the dichloro-phenyl and 2,3-dihydro-1H-pyrazol-4-yl rings are 54.8 (2), 76.2 (2) and 77.5 (2)° in mol-ecules A, B and C, respectively, while the 2,3-dihydro-1H-pyrazol-4-yl and phenyl rings make dihedral angles of 45.3 (2), 51.2 (2) and 42.8 (2)°, respectively. In the crystal, two of the mol-ecules are linked through N-H⋯O hydrogen bonding to an adjoining mol-ecule, forming dimers of the R2(2)(10) type, while the third mol-ecule forms such dimers with itself. C-H⋯O inter-actions link the dimers.