Dication in Two New Salts: Perchlorate and Peroxodisulfate

Zeitschrift für Kristallographie - New Crystal Structures, 2000

C3iH 3 6ClMnN 5 0 9 , triclinic, P1 (No. 2), a = 9.5173(9) A, b = 12.059(1) A, c = 15.752(2) A, a = 79.322(9)°, p = 79.550(8)°, y = 79.152(6)°, V= 1724.6 A 3 ,Z = 2, Rgt(F) = 0.072, wRKf(F 2 ) = 0.201, T= 293 K. To a stirred tintless solution of 5,5'-Me2-2,2'-dipyridine (1 mmol, 0.184 g) and />-aminobenzoic acid (0.5 mmol, 0.069 g) in 10 ml absolute ethanol was added manganese(II) acetate tetrahydrate (0.5 mmol, 0.123 g), and the solution turned pale yellow. Then sodium perchlorate hydrate (0.5 mmol, 0.071 g) was added and the resulting homogeneous solution was kept at ambient temperature for several hours. Suitable yellow crystals were obtained by slow vapour diffusion of diethyl ether. The structure proposed is consistent with elemental analysisxalculated C 56. 45, H 4.55, N 10.62; found C 56.27, H 4.47, N 10.41.

Structural Chemistry

This paper describes the X-ray crystal structure of a complex of acridino-18-crown-6 ether (S,S)-2 and sodium perchlorate. The structure shows a π-π bonded homodimer in the crystal. The average distance of the two tricyclic units (3.49±0.1 Å) indicates a strong π-π interaction. Fluorescence titration was performed in order to determine the stoichiometry and stability constant (K s) of the sodium ion-(S,S)-2 complex. Based on the global fitting of the fluorescence spectra we suggest the formation of a complex with 1:1 ligand to metal ion ratio and the logK value determined by nonlinear regression analysis was 5.23.

Acta Crystallographica Section C Crystal Structure Communications

Acta Crystallographica Section E Crystallographic Communications, 2016

The asymmetric unit of the title hydrated molecular salt, C6H16N22+·2ClO4−·2H2O, contains a half dication (completed by inversion symmetry), a perchlorate anion and a water molecule. The extended structure consists of infinite chains of formula [(ClO4)H2O]nn−ions extending along thebaxis linked by Ow—H...O (w = water) hydrogen bonds. These chains are cross-linked by the dicationsviaN—H...Owand weak C—H...O hydrogen bonds, thus forming a three-dimensional supramolecular network. Three-dimensional Hirshfeld surface analysis and two-dimensional fingerprint maps reveal that the structure is dominated by H...O/O...H and H...H contacts.

Acta Crystallographica Section E Crystallographic Communications, 2017

The title compound, [Cu2(ClO4)(C14H13N2O)2(H2O)]ClO4, crystallizes as an unsymmetrical dinuclear cation bridged by the phenoxy O atoms with one CuIIatom coordinated by a water molecule and the other by a perchlorate anion, thus making both CuIIatoms five-coordinate, and with a further perchlorate anion present for charge balance. A long interaction [2.9893 (5) Å] between one of the two CuIIatoms and an O atom of the perchlorate counter-ion links the cations and anions into linear chains along thea-axis direction. In addition, the water H atoms link with the perchlorate counter-ion. These interactions, along with numerous C—H...O interactions between the tetrahedral perchlorate anions, link the ions into a complex three-dimensional array. One of the perchlorate anions is disordered over two conformations with occupancies of 0.586 (4) and 0.414 (4).

Acta Crystallographica Section E-structure Reports Online, 2014

Acta Crystallographica Section E Structure Reports Online, 2011

Bis{tris[2-(2-oxidobenzylideneazaniumyl)ethyl]amine-3 O,O',O''}calcium bis(perchlorate) acetonitrile disolvate M. Kose and V. McKee Comment The crystal structures and coordination chemistry of transition metal complexes of H 3 saltren, tris(2hydroxybenzoylaminoethyl)amine (L), a tripodal ligand, have been described in detail (Steinhauser et al., 2004; Elerman et al., 1994); Elerman et al., 1995). Here, we report the first example of an earth alkaline metal (Ca +2) complex of H 3 saltren. The crystal structure of the title complex contains centrosymmetric (CaL 2) +2 cations, uncoordinated perchlorate anions and acetonitrile molecules (Fig. 1). Each calcium ion is six-coordinated, bonded to all phenoxy O atoms from two saltren molecules. There are strong intramolecular hydrogen bonds of the type N-H•••O between protonated imine and deprotonated phenol-oxygen atoms (Table 1). The cations are linked into chains via intermolecular C-H•••O and C-H••• N type weak hydrogen bonds and C-H•••π interactions (Tab. 1 and Fig. 2). There is evidence of π-π stacking in the crystal structure; C16 is stacked with C16 * and C15 * of an adjacent molecule (* = 2-x,-y, 1-z) with separation of 3.306 (3) and 3.415 (3) Å, respectively (Fig. 2). Protonated imine distances (C═N distances) (mean 1.300 (2) Å) are longer than the corresponding C═N distances reported in the neutral ligand (mean 1.267 Å) (Gündüz et al., 1985). The longer C═N distances were also determined by IR spectroscopy; while C═N stretch is observed at 1633 cm-1 in the neutral ligand, by protonation of imine, C═N stretch shifts to 1654 cm-1. Experimental H 3 Saltren (0.508 g, 1.11 mmol) was dissolved in methanol (50 ml) followed by addition of Ca(ClO 4) 2 .3H 2 O (0.185 g, 0.63 mmol) in methanol (20 ml). The reaction mixture was stirred at room temperature for two hours. Yellow precipitate was collected and washed with methanol (5 ml) and diethylether (20 ml) (yield 0.506 g, 0.44 mmol, 69.6%). X-ray quality crystals were obtained from acetonitrile solution of the title complex by slow evaporation. Refinement H atoms bonded to C were inserted at calculated positions with C-H distances of 0.95, 0.98 and 0.99 Å for aryl, methyl and methylene H atoms, respectively, and refined using a riding model with U iso (H) = 1.2 or 1.5U eq (C). The H-atoms bonded to N-atoms were taken from the difference Fourier maps and were refined isotropically.

Acta Crystallographica Section E Structure Reports Online, 2010

In the title compound, C 11 H 18 N 2 2+ Á2ClO 4 À ÁH 2 O, one perchlorate anion is disordered over two orientations in a 0.66 (3):0.34 (3) ratio. Intermolecular O-HÁ Á ÁO, N-HÁ Á ÁO and C-HÁ Á ÁO hydrogen bonds link the cations, anions and water molecules into ribbons extending along [100]. Related literature For general background to the properties of perchlorate salts containing organic cations, see:

Acta Crystallographica Section C Crystal Structure Communications, 1985

The crystal structure of di-n-butyltin pyridine-2-phosphonate-6-carboxylate, [C 14 H 24 NO 6 -PSn] 2 , features centrosymmetric dimers disposed about a central Sn 2 O 2 core. The phosphonate carboxylate dianion is µ 2 -tetradentate, coordinating one tin atom via one of the phosphonate oxygen atoms, the pyridine nitrogen atom, and one of the carboxylate oxygen atoms; the latter atom also coordinates the second tin atom of the dimer. The remaining positions in the seven-coordinate, distorted pentagonal bipyramidal geometry are occupied by a water molecule and two n-butyl groups that occupy axial positions. The lattice is stabilized by hydrogen-bonding contacts leading to an arrangement of parallel, orthogonally related chains of dimeric units. In methanol solution, the dimer is involved in a dissociation equilibrium that is fast on the NMR time scale. (1) (a) Gielen, M.; Joosen, E.; Mancilla, T.; Jurkschat, K.; Willem, R.; Roobol, C.; Bernheim, J.; Atassi, G.; Huber, F.; Hoffmann, E.; Preut, H.; Mahieu, B. Main Group Met. Chem. 1987, 10, 147. (b) Gielen, M.; Acheddad, M.; Bouâ lam, M.; Biesemans, M.; Willem, R. Bull. Soc. Chim. Belg. 1991, 100, 743. (c) Gielen, M.; Acheddad, M.; Mahieu, M.; Willem, R. Main Group Met. Chem. 1991, 14, 73. (d) Willem, R.; Biesemans, M.; Bouâ lam, M.; Delmotte, A.; El Khloufi, A.; Gielen, M. Appl. Organomet. Chem. 1993, 7, 311. (2) (a) Huber, F.; Preut, H.; Hoffmann, E.; Gielen, M. Acta Crystallogr. 1989, C45, 51. (b) Gielen, M.; Acheddad, M.; Tiekink, E. R. T.