The asymmetric unit of the title compound, (C12H16N3O)2[PdCl4]3, consists of a 4,4′-(1-azaniumyl-2-hydroxyethane-1,2-diyl)dipyridinium dication and one and a half tetrachloridopalladate(II) anions; the latter has inversion symmetry. In the cation, the pyridinium rings attached to the central 1-azaniumyl-2-hydroxyethane fragment show an anti conformation, as indicated by the central C—C—C—C torsion angle of −178.1 (4)°, and they are inclined to one another by 25.7 (2)°. In the crystal, the cations and anions are linked through N—H⋯Cl and O—H⋯Cl hydrogen bonds. There are also π–π contacts [centroid–centroid distance = 3.788 (3) Å] and a number of C—H⋯O and C—H⋯Cl interactions are present, consolidating the formation of a three-dimensional structure.
doi:10.1107/S1600536812050817
PMCID: PMC3588234
PMID: 23476356
The asymmetric unit of the title complex, [Ni(C12H8N2)3]S2O8·2C3H7NO·H2O, consists of a complex [Ni(phen)3]2+ cation and one isolated pds anion, with two DMF molecules and one water molecule as solvates (where phen is 1,10-phenanthroline, pds is the hexaoxido-μ-peroxoido-disulfate dianion and DMF is dimethylformamide). The [Ni(phen)3]2+ cation is regular, with an almost ideal NiII bond-valence sum of 2.07 v.u. The group, as well as the water solvent molecule, are well behaved in terms of crystallographic order, but the remaining three molecules in the structure display different kinds of disorder, viz. the two DMF molecules mimic a twofold splitting and the pds anion has both S atoms clamped at well-determined positions but with a not-too-well-defined central part. These peculiar behaviours are a consequence of the hydrogen-bonding interactions: the outermost SO3 parts of the pds anion are heavily connected to the complex cations via C—H⋯O hydrogen bonding, generating an [Ni(phen)3]pds network and providing for the stability of the terminal pds sites. Also, the water solvent molecule is strongly bound to the structure (being a donor of two strong bonds and an acceptor of one) and is accordingly perfectly ordered. The peroxide O atoms in the pds middle region, instead, appear as much less restrained into their sites, which may explain their tendency to disorder. The cation–anion network leaves large embedded holes, amounting to about 28% of the total crystal volume, which are occupied by the DMF molecules. The latter are weakly interacting with the rest of the structure, which renders them much more labile and, accordingly, prone to disorder.
doi:10.1107/S1600536812050775
PMCID: PMC3588241
PMID: 23476355
In the title salt {systematic name: 4-diphenylmethyl-1-[(E)-3-phenylprop-2-en-1-yl]piperazin-1-ium (2Z)-3-carboxyprop-2-enoate}, C26H29N2
+·C4H3O4
−, the piperazine ring in the cation adopts a distorted chair conformation and contains a positively charged N atom with quaternary character. The dihedral angle between the mean planes of the phenyl rings of the diphenylmethyl group is 74.2 (7)° and those between these rings and the phenyl ring of the 3-phenylprop-2-en-1-yl group are 12.7 (9) and 80.6 (8)°. In the crystal, N—H⋯O and O—H⋯O hydrogen bonds form chains along [001]. Weak C—H⋯O interactions connect parallel chains along [010], forming layers perpendicular to the a-axis direction.
doi:10.1107/S1600536812051239
PMCID: PMC3588249
PMID: 23476398
In the title compound, C15H14N2O, the fused five- and six-membered ring system is essentially planar, the maximum deviation from the mean plane being 0.009 (1) Å. The benzimidazol-2(3H)-one residue is nearly perpendicular to the benzyl ring, forming a dihedral angle of 77.41 (6)°. In the crystal, inversion dimers are formed by pairs of N—H⋯O hydrogen bonds; these dimers are linked by weak C—H⋯O interactions into a two-dimensional array in the (102) plane.
doi:10.1107/S1600536812050726
PMCID: PMC3588251
PMID: 23476384
In the dinuclear title compound, [Cu2I2(C3H8N2S)(C25H22P2)2]·1.5CH3CN, each CuI atom exhibits a distorted tetrahedral coordination with two P atoms from two bis(diphenylphosphanyl)methane (dppm) ligands, one metal-bridging S atom from the 1-ethylthiourea (ettu) ligand and one iodide ion. The dppm ligand and the bridging S atom of the ettu ligand force the two copper atoms into close proximity, leading to the formation of a close intramolecular Cu⋯Cu contact [3.3747 (17) Å]. The conformation of the dimeric complex is such that the two dppm ligands are located on one side of the dinuclear metal complex, while the two iodine atoms are pointed towards the other side of the complex, a conformation that is stabilized by two intramolecular N—H⋯I hydrogen bonds between the ettu NH2 and NHEt moieties and the I atoms. Another pair of symmetry-equivalent N—H⋯I hydrogen bonds is established between neighboring molecules across an inversion center, linking molecules into dimers. The dimers are connected with each other and with the interstitial acetonitrile solvent molecules via a range of weaker C—H⋯I and C—H⋯S interactions and through weak C—H⋯π interactions, leading to the formation of a three-dimensional network. One of the acetonitrile solvent molecules is disordered in a 1:1 ratio across a crystallographic inversion center.
doi:10.1107/S1600536812050970
PMCID: PMC3588258
PMID: 23476358
The structure of the title molecule, C16H19N5O7, is mainly determined by the steric effect of a bulky 2,4,6-trinitrophenyl group attached to the N atom of a pyrrolidine ring. Both pyrrolidine rings adopt an envelope conformation, with one of the methylene C atoms as the flap in each case, and the N—C—C—N torsion angle along the bond connecting the two pyrrolidine rings is −174.9 (2)°. The benzene ring of the 2,3,5-trinitrophenyl substituent is deformed and the r.m.s. deviation of its six atoms from the best plane is 0.026 Å. The N atoms of the two nitro groups in the ortho positions deviate from the best plane of the benzene ring by −0.033 (5) and 0.385 (5) Å. These groups, as well as the pyrrolidine ring, are twisted relative to the aromatic ring in the same direction, their best planes forming dihedral angles of 30.2 (2), 64.8 (1) and 46.6 (2)°, respectively, with the ring. An intramolecular C—H⋯O hydrogen bond occurs. In the crystal, there is a short [O⋯C = 3.019 (4) Å] contact between a nitro O atom and a C atom of the benzene ring bearing the nitro group and a C—H⋯O interaction between a methyl H atom and another nitro O atom.
doi:10.1107/S1600536812051161
PMCID: PMC3588260
PMID: 23476399
The asymmetric unit of the title compound, C11H12N2O·C25H28N4O2, contains two different molecules. The smaller is known as antipyrine [systematic name: 1,5-dimethyl-2-phenyl-1H-pyrazol-3(2H)-one] and the larger is built up from two antypirine molecules which are connected through a C atom of the pyrazolone ring to a central propanyl part [systematic name: 4,4′-(propane-2,2-diyl)bis[1,5-dimethyl-2-phenyl-1H-pyrazol-3(2H)-one]. Intramolecular C—H⋯O hydrogen bonds occur in the latter molecule. In the crystal, C—H⋯O hydrogen bonds link the molecules into a two-dimensional network parallel to (001).
doi:10.1107/S160053681205091X
PMCID: PMC3588274
PMID: 23476388
In the title compound, [Cd(NO3)2(C8H7N3)2(H2O)2], the CdII cation is situated on an inversion center and is coordinated by the O atoms of two nitrate anions, by the N atoms of two 4-(imidazol-2-yl)pyridine ligands and by two water O atoms in a slightly distorted N2O4 octahedral geometry. The dihedral angle between the imidazole and pyridine rings is 1.6 (2)°. In the crystal, molecules are linked by N—H⋯O, O—H⋯N and O—H⋯O hydrogen bonds, forming a three-dimensional network.
doi:10.1107/S1600536812050908
PMCID: PMC3588280
PMID: 23476357
The molecule in the structure of the title compound, C34H60Si4, lies on a twofold rotation axis that passes through the two Si atoms, resulting in a planar cyclotetrasilane ring. The dihedral angle between the cyclotetrasilane ring and the phenyl ring is 68.20 (5)°. The Si—Si bonds [2.4404 (8) and 2.4576 (8) Å] are longer than a standard Si—Si bond (2.34 Å) and the C—Si—C bond angle [97.07 (14)°] of the phenyl-substituted Si atom is smaller than the tetrahedral bond angle (109.5°). These long bonds and small bond angle are favorable for reducing the steric hindrance among the bulky substituents.
doi:10.1107/S160053681205074X
PMCID: PMC3588281
PMID: 23476402
The benzimidazolone part of the title molecule, C10H8N2O, is almost planar [r.m.s. deviation = 0.014 (1) Å] and the NCH2C CH group forms a dihedral angle of 67.95 (6)° with its best plane. In the crystal, molecules form inversion dimers via pairs of N—H⋯O hydrogen bonds. C—H⋯O interactions connect the dimers, forming a two-dimensional polymeric network parallel to (100).
doi:10.1107/S160053681205088X
PMCID: PMC3588288
PMID: 23476381
In the asymmetric unit of the title compound, C19H16O2, there are two symmetry-independent molecules (A and B) that differ in the conformation of the ester ethoxy group. In the crystal, the molecules form inversion dimers via pairs of C—H⋯O interactions. Within the dimers, the anthracenyl units have interplanar distances of 0.528 (2) and 0.479 (2) Å for dimers of molecules A and B, respectively. Another short C—H⋯O contact between symmetry-independent dimers links them into columns parallel to [10-1]. These columns are arranged into (111) layers and there are π–π stacking interactions [centroid–centroid distances = 3.6446 (15) and 3.6531 (15) Å] between the anthracenyl units from the neighbouring columns. In addition, there are C—H⋯π interactions between the anthracenyl unit of dimers A and dimers B within the same column.
doi:10.1107/S1600536812051033
PMCID: PMC3588290
PMID: 23476390
The title compound, C17H19N3O2, crystallizes with two independent molecules (A and B) in the asymmetric unit. In both molecules, the pyran ring has a twisted conformation (5
S
4), with Q = 0.301 (3) Å, θ = 116.7 (6) and ϕ= 213.6 (7)° for molecule A, and Q = 0.364 (2) Å, θ = 113.7 (3) and ϕ = 213.0 (4)° for molecule B. In molecule B, the terminal ethyl group is disordered over two orientations with an occupancy ratio of 0.55 (1):0.45 (1). In the crystal, molecules A and B form very similar but separate R
1
2(7) motifs through N—H⋯O and C—H⋯O hydrogen bonds. The resulting chains along [001] are interlinked by weaker C—H⋯O and C—H⋯π interactions, forming layers parallel to the bc plane.
doi:10.1107/S1600536812051124
PMCID: PMC3588295
PMID: 23476394
In the title molecule, C10H8O2, all non-H atoms are essentailly coplanar (r.m.s. deviation = 0.0192 Å), indicating an effective conjugation of the carbonyl group, the benzene ring and the lone pair of the propynyloxy O atom. In the crystal, π–π stacking interactions [centroid–centroid distance = 3.5585 (15) Å] connect molecules into inversion dimers which are linked by Csp—H⋯O=C hydrogen bonds, forming a ladder-like structure.
doi:10.1107/S1600536812050866
PMCID: PMC3588297
PMID: 23476386
In the title molecule, C14H15NO3, the ring system is essentially planar, with an r.m.s. deviation of 0.003 Å. The atoms of the ethane-1,2-diol group were refined as disordered over two sets of sites in a ratio of 0.815 (3):0.185 (3). The molecular conformation is stabilized in part by an intramolecular N—H⋯O hydrogen bond, which forms an S(6) ring. In the crystal, molecules are connected by N—H⋯O and O—H⋯O hydrogen bonds, forming a two-dimensional network parallel to (100). The network also features weak C—H⋯O hydrogen bonds. Weak C—H⋯π interactions also observed.
doi:10.1107/S1600536812051070
PMCID: PMC3588305
PMID: 23476393
The molecular structure of the title compound, C10H12O4, contains an intramolecular hydrogen bond between the phenol and acetyl substituents. In the crystal, C—H⋯π interactions act between the molecules in a cyclic manner to stabilize stacks of molecules along the b axis. Several C—H⋯O interactions are present between the stacks.
doi:10.1107/S1600536812051057
PMCID: PMC3588311
PMID: 23476395
The title compound, C18H18O4, is a triclinic polymorph of the previously reported monoclinic polymorph [Han & Zhen (2005 ▶). Acta Cryst. E61, o4358–o4359]. In the crystal of the triclinic polymorph, molecules are linked by two pairs of C—H⋯O hydrogen bonds, forming a two-dimensional network parallel to (102), and enclosing loops with graph set motifs of R
2
2(8) and R
2
2(6).
doi:10.1107/S1600536812050994
PMCID: PMC3588312
PMID: 23476387
In the title compound, C20H15ClIN3O3, the dihedral angle between the quinazolinone ring system [r.m.s. deviation = 0.047 (2) Å] and the pendant benzene ring is 82.63 (11)°. The molecular conformation is stabilized by intramolecular C—H⋯O interactions. In the crystal, the molecules are linked by N—H⋯O hydrogen bonds into chains along the a-axis direction. Another set of chains propagating along [101] is formed due to intermolecular I⋯Cl short contacts of 3.427 (1) Å, thus giving layers parallel to (010). The layers are connected by C—H⋯π and π–π interactions, the shortest distance between the centroids of aromatic rings being 3.8143 (16) Å.
doi:10.1107/S1600536812050787
PMCID: PMC3588318
PMID: 23476385
The 4-chlorobenzoate anion of the title salt, C6H9N2
+·C7H4ClO2
−, is nearly planar with a dihedral angle of 5.14 (16)° between the benzene ring and the carboxylate group. In the crystal, the protonated N atom and the 2-amino group of the cation are hydrogen bonded to the carboxylate O atoms of the anion via a pair of N—H⋯O hydrogen bonds with an R
2
2(8) ring motif. The ion pairs are further connected via N—H⋯O and weak C—H⋯O hydrogen bonds, forming a two-dimensional network parallel to the bc plane. The crystal structure also features a π–π stacking interaction between the pyridinium and benzene rings with a centroid–centroid distance of 3.7948 (9) Å.
doi:10.1107/S1600536812051021
PMCID: PMC3588320
PMID: 23476392
In the title salt, C23H21NOP+·Br−, the dihedral angles between the phenyl rings are 70.41 (18), 73.6 (2) and 80.85 (19)°. In the crystal, neighboring molecules are linked through an N—H⋯Br hydrogen bond and four weak C—H⋯Br contacts, forming a three-dimensional network.
doi:10.1107/S1600536812050805
PMCID: PMC3588329
PMID: 23476380
Rubidium ytterbium(III) tetrakis(polyphosphate), RbYb(PO3)4, was synthesized by solid-state reaction. It adopts structure type IV of the MRE(PO3)4 (M = alkali metal and RE = rare earth metal) family of compounds. The structure is composed of a three-dimensional framework made up from double spiral polyphosphate chains parallel to [10-1] and irregular [YbO8] polyhedra. There are eight PO4 tetrahedra in the repeat unit of the polyphosphate chains. The Rb+ cation is located in channels extending along [100] that are delimited by the three-dimensional framework. It is surrounded by 11 O atoms, defining an irregular polyhedron.
doi:10.1107/S1600536812050969
PMCID: PMC3588346
PMID: 23476312
21.
rac-5′′-(4-Fluorobenzylidene)-1′-(4-fluorophenyl)-1′′-methyl-1′,2′,3′,5′,6′,7′,8′,8a′-octahydrodispiro[acenaphthylene-1,3′-indolizine-2′,3′′-piperidine]-2,4′′(1H)-dione
In the title E isomer of the racemic compound, C37H32F2N2O2, the pyridinone ring adopts a twisted half-chair conformation with the N atom deviating by −0.355 (3) Å and with the methylene C atom next to octahydroindolizine moiety deviating by 0.415 (3) Å from the mean plane defined by other four atoms. In the octahydroindolizine system, the pyrrolidine ring exhibits an envelope conformation with the fused methyne C atom deviating by 0.6496 (1) Å from the mean plane defined by four other atoms, and the piperidine ring exhibits a distorted chair conformation as evident from the puckering parameters Q = 0.568 (2) Å, θ = 1.0 (2) and Φ = 256 (11)°. In the crystal, C—H⋯O interactions connect the molecules into chains along [101].
doi:10.1107/S1600536812051094
PMCID: PMC3588349
PMID: 23476397
In the title compound, C18H18N2O, the morpholine ring adopts a chair conformation with the exocyclic N—C bond in an equatorial orientation. The dihedral angles between the central benzene ring and the morpholine ring (all atoms) and the cyanobenzene ring are 87.87 (7) and 52.54 (7)°, respectively. No significant intermolecular interactions are observed in the crystal structure.
doi:10.1107/S1600536812050957
PMCID: PMC3588350
PMID: 23476389
In the title compound, C28H24O6·CHCl3, the two 4-methoxybenzoyl groups at the 1- and 8-positions of the naphthalene ring system are aligned almost antiparallel, the benzene rings making a dihedral angle of 25.76 (7)°. The naphthalene ring system makes dihedral angles of 72.51 (7) and 73.33 (7)° with the benzene rings. In the crystal, the naphthalene molecules are linked by C—H⋯O interactions, forming a helical chain along the b-axis direction. A C—H⋯Cl interaction is also observed between the aroylated naphthalene and chloroform molecules. The chloroform molecule is disordered over two positions with site occupancies of 0.478 (5) and 0.522 (5).
doi:10.1107/S1600536812050799
PMCID: PMC3588358
PMID: 23476400
In the 5-chlorosalicylate anion of the title salt, C6H9N2
+·C7H4ClO3
−, an intramolecular O—H⋯O hydrogen bond with an S(6) graph-set motif is observed and the dihedral angle between the benzene ring and the –CO2 group is 1.6 (6)°. In the crystal, the protonated N atom and the 2-amino group of the cation are hydrogen bonded to the carboxylate O atoms via a pair of N—H⋯O hydrogen bonds, forming an R
2
2(8) ring motif. The crystal structure also features N—H⋯O and weak C—H⋯O interactions, resulting in a layer parallel to (10-1).
doi:10.1107/S160053681205101X
PMCID: PMC3588363
PMID: 23476391
In the title compound, [Co(C8H5N5O3)(C12H8N2)(H2O)]·3H2O, a tridentate 2-amino-7-methyl-4-oxidopteridine-6-carboxylate ligand, a bidentate ancillary 1,10-phenanthroline (phen) ligand and a water molecule complete a distorted octahedral geometry around the CoII atom. The pterin ligand forms two chelate rings. The phen and pterin ring systems are nearly perpendicular [dihedral angle = 85.15 (8)°]. N—H⋯O, O—H⋯N and O—H⋯O hydrogen bonds link the complex molecules and lattice water molecules into a layer parallel to (001). π–π stacking contacts (involving phen–phen and pteridine–pteridine) are also observed [centroid–centroid distances = 3.670 (2), 3.547 (2), 3.698 (2) and 3.349 (2) Å].
doi:10.1107/S1600536812051185
PMCID: PMC3588366
PMID: 23476360