Using crystallography, topology and graph set analysis for the description of the hydrogen bond network of triamterene: a rational approach to solid form selection.

This study has demonstrated the use of crystallography, topology and graph set analysis in the description and classification of the complex hydrogen bonded network of triamterene. The aim is to give a brief overview of the methodology used to discuss the crystal structure of triamterene with a view to extending the study to include the solvates, cocrystals and salts of this compound. Graphical abstract One of the structurally significant dimers (supramolecular synthons) of triamterene identified by this study.

Hydrogen-bonding patterns in bis[2,4,6-triazaniumylcyclohexane-1,3,5-tris(olate)-κ(3)O,O',O'']germanium(IV) tetrachloride hexahydrate.

A first preliminary report on the crystal structure of a hydrated salt formulated as [Ge(taci)2]Cl4·13H2O (taci is 1,3,5-triamino-1,3,5-trideoxy-cis-inositol) appeared more than 20 years ago [Ghisletta (1994). PhD thesis, ETH Zürich. Switzerland]. At that time it was not possible to discriminate unambiguously between the positions of some of the chloride ions and water O atoms, and disorder was thus postulated. In a new determination, a conclusive scheme of hydrogen bonding proves to be a particularly appealing aspect of the structure. Single crystals of the title compound, C12H30GeN6O6(4+)·4Cl(-)·6H2O or [Ge(taci)2]2Cl8·12H2O, were grown from an aqueous solution by slow evaporation of the solvent. The two [Ge(taci)2](4+) cations exhibit a double-adamantane-type structure with exclusive O-atom coordination and approximate D3d symmetry. The taci ligands adopt a zwitterionic form with deprotonated hydroxy groups and protonated amino groups. Both cations are hydrogen bonded to six water molecules. The structure of the hydration shell of the two cations is, however, slightly different. The {[Ge(taci)2]·6H2O}(4+) aggregates are interlinked in all three dimensions by further hydrogen bonds of the types N-H...Cl...H-N, N-H...O(H)2...H-N, (Ge)O...H-O(H)...H-N, N-H...O(H)-H...Cl...H-N, (Ge)O...H-O-H...Cl...H-N, N-H...O(H)-H...Cl...H-(H)O...H-N, (Ge)O...H-O-H...Cl...H-(H)O...H-N and Ge(O)...H-O-H...Cl...H-O-H...O(Ge).

Crystal structure of [4-(2-meth-oxy-phen-yl)-3-methyl-1-phenyl-6-tri-fluoro-methyl-1H-pyrazolo-[3,4-b]pyridin-5-yl](thio-phen-2-yl)methanone.

The title compound, C26H18F3N3O2S, a 2-meth-oxy-substituted derivative, is closely related to its 4-methyl- and 4-chloro-substituted analogues and yet displays no structural relationships with them. The thio-phene ring is disorder free and the -CF3 group exhibits disorder, respectively, in contrast and similar to that observed in the 4-methyl- and 4-chloro-substituted derivatives. The torsion angle which defines the twist of the thio-phene ring is -69.6 (2)° (gauche) in the title compound, whereas it is anti-clinal in the 4-methyl- and 4-chloro-substituted derivatives, with respective values of 99.9 (2) and 99.3 (2)°. The absence of disorder in the thio-phene ring facilitates one of its ring C atoms to participate in the lone inter-molecular C-H⋯O hydrogen bond present in the crystal, leading to a characteristic C(5) chain graph-set motif linking mol-ecules related through glides along [010]. An intra-moleculr C-H⋯N hydrogen bond also occurs.

Disentangling steric and electronic factors in monomeric bis(2-bromo-4-chloro-6-{[(2-hydroxyethyl)imino]methyl}phenolato-κ(2)N,O)copper(II).

The title compound, [Cu(C9H8BrClNO2)2], is a square-planar complex. The potentially tridentate dibasic 2-bromo-4-chloro-6-{[(2-hydroxyethyl)imino]methyl}phenolate ligand coordinates in a trans-bis fashion to the Cu(II) centre via the imine N and phenolate O atoms. The Cu(II) atom lies on the centre of inversion of the molecule. The potentially coordinating hydroxyethyl group remains protonated and uncoordinated, taking part in intermolecular hydrogen bonds with vicinal groups, leading to the formation of a two-dimensional hydrogen-bond network with sheets parallel to the (101) plane. Substituent effects on the crystal packing and coordination modes of the ligand are discussed.

Formation of lithium, sodium and potassium complexes with 1,3,5-triamino-1,3,5-trideoxy-cis-inositol (taci).

Single crystals of (1,3-diamino-5-azaniumyl-1,3,5-trideoxy-cis-inositol-κ(3)O(2),O(4),O(6))(1,3,5-triamino-1,3,5-trideoxy-cis-inositol-κ(3)O(2),O(4),O(6))lithium(I) diiodide dihydrate, [Li(C6H16N3O3)(C6H15N3O3)]I2·2H2O or [Li(Htaci)(taci)]I2·2H2O (taci is 1,3,5-triamino-1,3,5-trideoxy-cis-inositol), (I), bis(1,3,5-triamino-1,3,5-trideoxy-cis-inositol-κ(3)O(2),O(4),O(6))sodium(I) iodide, [Na(C6H15N3O3)2]I or [Na(taci)2]I, (II), and bis(1,3,5-triamino-1,3,5-trideoxy-cis-inositol-κ(3)O(2),O(4),O(6))potassium(I) iodide, [K(C6H15N3O3)2]I or [K(taci)2]I, (III), were grown by diffusion of MeOH into aqueous solutions of the complexes. The structures of the Na and K complexes are isotypic. In all three complexes, the taci ligands adopt a chair conformation with axial hydroxy groups, and the metal cations exhibit exclusive O-atom coordination. The six O atoms of the resulting MO6 unit define a centrosymmetric trigonal antiprism with approximate D3d symmetry. The interligand O···O distances increase significantly in the order Li < Na < K. The structure of (I) exhibits a complex three-dimensional network of R-NH2-H···NH2-R, R-O-H···NH2-R and R-O-H···O(H)-H···NH2-R hydrogen bonds. The structures of the Na and K complexes consist of a stack of layers, in which each taci ligand is bonded to three neighbours via pairwise O-H···NH2 interactions between vicinal HO-CH-CH-NH2 groups.