A tale of hydrogen abstraction, initially detected via X-ray diffraction

X-ray diffraction led to the discovery of an unexpected tetra­zine ligand hydrogenation when the ligand is attached to a reducing V center. Density functional theory calculations were used to map out the relative stability of different H-atom locations and revealed the observed product to have an open-shell singlet electronic structure. [This paper is associated with the special issue on Special issue on Interplay of crystallography, spectroscopy and theoretical methods for solving chemical problems (Guest Editors: Larry Falvello and Alberto Albinati) published in December 2013.]

Disordered kalsilite KAlSiO₄

The directionality of (Al,Si)O₄ tetra­hedra within six-membered rings (S6R) could not be defined in disordered kalsilite, i.e. equal probability for U or D directionality [free apex pointing up (U) or down (D)] of (Al,Si)O₄ tetra­hedra is established. In ordered kalsilite, S6R of (Al,Si)O₄ tetra­hedra are characterized with the UDUDUD sequence of the directionality of the tetra­hedra.

In-house and synchrotron X-ray diffraction studies of 2-phenyl-1,10-phenanthroline, protonated salts, com­plexes with gold(III) and copper(II), and an orthometallation product with palladium(II)

The hexa­fluorido­phosphate, tri­fluoro­methane­sulfonate, tetra­chlorido­aurate and hydrated bromide salts of 2-phenyl-1,10-phenanthrolin-1-ium are reported, together with the gold(III) and copper(II) complexes of 2-phenyl-1,10-phenanthroline, and the 2-(phenanthrolin-2-yl)phenyl complex of palladium(II).

A new one-dimensional nickel metal–organic framework: catena-poly[[[di­aqua­bis­(4-{[(1-phenyl-1H-tetra­zol-5-yl)sulfan­yl]meth­yl}benzoato-κO)nickel(II)]-μ-4,4′-bi­pyridine-κ²N:N′] monohydrate]

A one-dimensional nickel coordination polymer incorporating 4-{[(1-phenyl-1H-tetra­zol-5-yl)sulfan­yl]meth­yl}benzoate and 4,4′-bi­pyridine ligands has an Ni⋯Ni separation of 11.361 (1) Å. The fishbone-like chains are linked by O—H⋯O, O—H⋯N and C—H⋯O hydrogen bonds and π–π stacking inter­actions to form a three-dimensional supra­molecular architecture.

Cobalt(II) chloride complexes with 1,1′-di­methyl-4,4′-bi­pyrazole featuring first- and second-sphere coordination of the ligand

The first cobalt(II) complexes involving N,N′-disubstituted 4,4′-bi­pyrazole tectons reveal the relatively poor coordination ability of the ligand, resulting in a Co–pyrazole coordination ratio of only 1:2.

A three-dimensional Zn^II coordination framework: poly[[μ₂-(E)-1,2-bis­(pyri­din-4-yl)ethene][μ₄-(E)-2,2′-(diazene-1,2-diyl)dibenzoato][μ₂-(E)-2,2′-(di­azene-1,2-di­yl)dibenzoato]dizinc(II)]

The title zinc(II) complex, prepared by the reaction of Zn(OAc)₂·2H₂O with 2,2′-(diazene-1,2-diyl)di­benzoic acid and 1,2-bis­(pyridin-4-yl)ethene in MeOH/H₂O at 393 K, possesses a three-dimensional framework with a 4⁶6⁴ topology. Powder X-ray diffraction and solid-state photoluminescent properties were also measured.

The cocrystal rac-1-[(N,4-di­methyl­benzene­sulfonamido)­methyl]-2-(di­phenyl­phosphoryl)­ferrocene–rac-1-[(N,4-di­methyl­benzene­sulfonamido)­methyl]-2-(di­phenyl­phosphanyl)­ferrocene (0.45/0.55)

Partial oxidation of a di­phenyl­phosphanyl group to a di­phenyl­phosphoryl group leads to a 0.55:0.45 cocrystal. The P=O distance [1.344 (4) Å] is the shortest observed for (di­phenyl­phosphoryl)­ferrocene compounds.

A coordination polymer consisting of two different one-dimensional copper(II) chains

Cu^II atoms exhibit different octa­hedral coordination geometries in two crystallographically independent one-dimensional chains. Extensive hydrogen bonding is observed among perchlorate anions, water mol­ecules and N-(4-methyl­pyrimidin-2-yl)pyrazin-2-amine ligands, and the one-dimensional chains are further linked to form a three-dimensional structure through inter­chain O—H⋯O and N—H⋯O hydrogen-bonding inter­actions.

The inorganic–organic hybrid zinc phosphite poly[(μ₃-hydrogen phosphito-κ³O:O′:O′′)(piperidin-1-ium-4-car­box­ylate-κO)zinc(II)]

A new inorganic–organic hybrid zinc phosphite features an unusual (3,4)-connected two-dimensional inorganic zinc–phosphite layer with organic piperidin-1-ium-4-carboxyl­ate ligands appended to the sheets and protruding into the inter­layer region.

A one-dimensional silver(I) coordination polymer based on an asymmetric flexible N-donor carboxyl­ate ligand: catena-poly[(μ₃-4-{[(1-phenyl-1H-tetra­zol-5-yl)sulfanyl]­methyl}­benzo­ato-κ³O:O′:N⁴)silver(I)]

A one-dimensional silver(I) coordination polymer based on an asymmetric μ₃-bridging flexible carboxyl­ate ligand is reported. The structure displays intrachain π–π contacts and in addition forms a three-dimensional supramolecular framework. Thermogravimetric analysis and fluorescence spectroscopy reveal good thermal stability and a strong green luminescence at room temperature.

Hydrogen-bonded chains in three cis-di­chloridoplatinum(II) complexes bearing piperidine and amine ligands

The influence of nonpiperidine ligands on the mol­ecular structure and crystal packing of three cis-di­chlorido­platinum(II) complexes bearing piperidine and amine ligands has been investigated by X-ray diffraction.

A novel two-dimensional cobalt(II) complex composed of one-dimensional twisted pair-like chains: poly[[tetra­aqua­bis­(μ₃-pyridine-2,5-di­carboxyl­ato-κ⁴N,O²:O⁵:O^5′)dicobalt(II)] dihydrate]

A novel two-dimensional cobalt(II) complex, composed of one-dimensional twisted pair-like {[Co(2,5-PDC)₂]²⁻}_n chains interlinked by cationic [Co(H₂O)₄]⁺ units, is extended into a three-dimensional supra­molecular structure by hydrogen bonding involving uncoordinated water mol­ecules.

The bimolecular structure of aqua­hexa-μ-chlorido-μ₄-oxido-tris­(tetra­hydro­furan-κO)tetra­copper(II)–hexa-μ-chlorido-μ₄-oxido-tetra­kis(tetra­hydro­furan-κO)tetra­copper(II)–tetra­hydro­furan (2/1/4)

A bimolecular copper(II) structure contains nine symmetry-independent mol­ecules expressed in simplest mol­ecular form as 6[Cu₄Cl₆O(C₄H₈O)₃(H₂O)·2(C₄H₈O)]:3Cu₄Cl₆O(C₄H₈O)₄. The compound exhibits a supercell (smaller than the unit cell based on weak reflections) structure due to pseudotranslational symmetry.

Masking of Lewis acidity trends in the solid-state structures of tri­chlorido- and tri­bromido­(2,2′:6′,2′′-terpyridine-κ³N,N′,N′′)gallium(III)

The monoclinic P2₁/n crystal structure of complexes of GaCl₃ and GaBr₃ with 2,2′:6′,2′′-terpyridine (terpy) were determined using single-crystal X-ray diffraction. It is shown that the Ga—N distances in GaCl₃(terpy) and GaBr₃(terpy) are similar within experimental error.

Hydrogen-bonded two- and three-dimensional polymeric structures in the ammonium salts of 3,5-di­nitro­benzoic acid, 4-nitro­benzoic acid and 2,4-di­chloro­benzoic acid

The hydrogen-bonded two- and three-dimensional polymeric structures in the ammonium salts of 3,5-di­nitro­benzoic acid, 4-nitro­benzoic acid and 2,4-di­chloro­benzoic acid involve cation–anion N—H⋯O hydrogen-bonded cyclic associations. The presence or absence of the ring-stacking and ring-laddering models for ammonium carboxyl­ate structures is also tested particularly with respect to the hydrated examples.

3-[(Di­phenyl­phosphino­thio­yl)­oxy]-N-methyl­propan-1-aminium di­phenyl­phosphanyl­thio­ate

In the asymmetric unit of an ammonium phosphanyl­thio­ate salt, a cation–anion heterodimer is formed through an inter­molecular N—H⋯O hydrogen bond. Packing through N—H⋯O and N—H⋯S hydrogen bonds is responsible for the high melting point.

The structural properties of a noncentrosymmetric polymorph of 4-amino­benzoic acid

The first noncentrosymmetric polymorph of 4-amino­benzoic acid (PABA) is described. The two crystallographically independent PABA mol­ecules form pseudocentrosymmetric O—H⋯O hydrogen-bonded dimers that are further linked by N—H⋯O hydrogen bonds into a three-dimensional network.

The self-assembling zwitterionic form of L-phenyl­alanine at neutral pH

The zwitterion of L-phenyl­alanine was characterized using synchrotron X-rays. It crystallized in the monoclinic space group P2₁ with four mol­ecules in the asymmetric unit. The 0.62 Å resolution structure was obtained in the same configuration as that assumed to be adopted in the self-assembly of nanotubes.

Three closely related dibenzazepine carb­oxy­lic acids: hydrogen-bonded aggregation in one, two and three dimensions

In three 5-acetyl-11-ethyl-6,11-di­hydro-5H-dibenzo[b,e]azepine-6-carb­oxy­lic acids, which differ only in the presence of zero, one or two methyl substituents in one of the aryl rings, the hydrogen-bonded supra­molecular aggregation is, respectively, two-, one- and three-dimensional.

1,1′-Di­ethyl-4,4′-bi­pyridine-1,1′-di­ium bis­(1,1,3,3-tetra­cyano-2-eth­oxy­pro­penide): multiple C—H⋯N hydrogen bonds form a complex sheet structure

A bipyridinediium propenide salt forms complex hydrogen-bonded sheets in which each cation acts as a sixfold donor of C—H⋯N hydrogen bonds and each anion acts as a threefold acceptor.