The title compound, C26H18, consists of a benzene ring with meta-substituted 1-naphthalene substituents, which are essentially planar (r.m.s. deviation = 0.039 and 0.027 Å). The conformation is mixed syn/anti, with equivalent torsion angles about the benzene–naphthalene bonds of 121.46 (11) and 51.58 (14)°.
The title compound, C26H18, consists of a benzene ring with meta-substituted 2-naphthalene substituents, which are essentially planar [r.m.s. deviations = 0.022 (1) and 0.003 (1) Å]. The conformation is syn, with equivalent torsion angles about the benzene–naphthalene bonds of −36.04 (13) and +34.14 (13)°. The molecule has quasi-C
s molecular symmetry.
The title compound, C32H40N2O4, is a 1,10-diaza-18-crown-6 cryptand with an o-terphenyl bridge. In the polyether ring, two adjacent –CH2– groups are disordered with very nearly equal populations of two conformers. The ordered bond lengths are normal, with average C—C = 1.511 (3) Å, C—O = 1.421 (3) Å, and C—N = 1.466 (4) Å. The r.m.s. deviations of the three rings of the terphenyl bridge vary from 0.007 to 0.009 Å and the two rings ortho to one another are twisted by 50.75 (5) and 47.76 (4)° with respect to the third ring. The N⋯N distance is 5.408 (1) Å.
The dirhodium complex, [Rh2(C18H15P)4(CO)2]·2(CH3)2CO, has crystallographic twofold symmetry and the Rh—Rh distance is 2.6266 (8) Å. The four atoms proximate to each Rh atom [Rh—P = 2.3222 (7) and 2.3283 (8) Å, and Rh—C = 1.961 (3) and 2.045 (3) Å] form a distorted tetrahedron with large deviations from the putative tetrahedral angles [r.m.s. deviation = 23 (1)°]. The six angles more closely approximate those of a trigonal bipyramid [r.m.s. deviation = 14 (1)°] with one missing equatorial ligand. The two bridging carbonyl ligands are much more linearly coordinated to one Rh [Rh—C O = 151.0 (2)°] than to the other [127.0 (2)°], and the two Rh2CO planes form a dihedral angle of 45.43 (5)°. The two acetone solvent molecules are disordered, and their estimated scattering contribution was subtracted from the observed diffraction data using the SQUEEZE routine in PLATON [Spek (2009 ▶). Acta Cryst.
The title compound, C34H30N4O2, lies on an inversion center and consists of two 3-substituted-1H-indole units linked by a 1,2-dimethylenehydrazine bridge. It is one of numerous examples in which two aromatic ring systems are joined by this 4-atom bridge. The geometry of the centrosymmetric bridge is: C(arom)—C = 1.444 (3), C=N = 1.284 (3), N—N = 1.414 (4) Å, C(arom)—C=N = 122.6 (2) and C=N—N = 111.9 (2)°. The nine non-H atoms of the indole unit lie in a plane (δr.m.s. = 0.0089 Å) which is twisted 6.0 (2)° with respect to the hydrazine bridge plane. The benzyloxymethyl substituents do not lie in the plane of the rest of the molecule and are in a folded rather than an extended conformation. This is described by the three torsion angles in the middle of the C=N—C—O—CBz group, viz. 98.5 (3), −62.1 (3), and −66.3 (2)°.
The title compound, C12H14O3, is a natural product derived from the medium-sized hawthorn Crataegus persimilis (’prunifolia’). The mean plane of the butene moiety is twisted by 13.27 (7)° with respect to the that of the dioxobenzaldehyde moiety. There is an intramolecular hydrogen bond between the hydroxyl group and the carbonyl O atom.
In the title complex, [Cu(C15H19N2)2] or [Cu(L
2)] (HL is 3,3′,4,4′,5,5′-hexamethylpyrromethene), the CuII atom is coordinated by four N atoms [Cu—N 1.939 (2)–1.976 (2) Å] from two L ligands in a distorted tetrahedral geometry. The mean planes of the CuN2C3 metallocyclic rings form a dihedral angle of 72.73 (6)°. In the L ligands, the pyrrole rings are inclined to each other at dihedral angles of 3.03 (7) and 9.83 (7)°. The crystal packing exhibits weak intermolecular C—H⋯π interactions, which form chains in .
In the title solvate, [Rh2(C22H18N2O2)(C8H12)2]·CH2Cl2, each organometallic molecule is composed of two RhI cations, the tetradentate dianion α,α′-bis(salicylaldiminato)-m-xylene and two 1,5-cyclooctadiene (COD) ligands. Each RhI atom is coordinated by one O atom [Rh—O = 2.044 (2) and 2.026 (2) Å], one N atom [Rh—N = 2.083 (2) and 2.090 (2) Å], and one COD ligand via two η2-bonds, each directed toward the mid-point of a C=C bond (Cg): Rh—Cg = 2.007 (2), 2.013 (2), 2.000 (2) and 2.021 (2) Å. Each RhI atom has a quasi-square-planar coordination geometry, with average r.m.s. deviations of 0.159 (1) and 0.204 (1) Å from the mean planes defined by Rh and the termini of its four coordinating bonds. The two COD ligands have quasi-C
2 symmetry, twisted from ideal C
2v symmetry by 30.0 (3) and −33.1 (3)°, and are quasi-enantiomers of one another. The intramolecular Rh⋯Rh distance of 5.9432 (3) Å suggests that there is no direct metal–metal interaction.
The title compound, C15H17NO2S, exhibits intramolecular hydrogen bonding between the amine H atom and a sulfonyl O atom. The conformation of the molecule is described by the four PhCH2—NH—CH2—CH2—SO2Ph torsion angles of 79.6 (2), −166.21 (14), −70.29 (17) and −58.93 (13)°.
The title compound, C24H26O2Si2, has C
2 crystallographic symmetry. The dihedral angle between the aromatic rings is 84.5 (2)°. The acetylene group is slightly non-linear, with angles at the acetylene C atoms of 175.7 (2) and 177.0 (2)°. In the crystal structure, only van de Waals interactions occur.
The title compound, C18H14O, is polymorphic at 123 K. The orthorhombic form reported herein has two independent molecules in the asymmetric unit, with molecular volume 313.5 Å3. The previously reported triclinic (P-1) form [Raston & Scott (2000 ▶). Green Chem., 2, 49–52] has molecular volume 309.6 Å3 at the same temperature. All three molecules deviate significantly and systematically from the putative Cs symmetry (δr.m.s. = 0.0265, 0.0256, 0.0497 Å). Comparison of the two molecules in the orthorhombic polymorph shows that 16 of the 19 equivalent pairs of framework atoms have a mirror-image pattern of deviations (above/below plane), suggesting that the two are quasi-enantiomorphs. The pattern of deviations in the triclinic form is nearly the same (13 of 19 atom pairs) as the orthorhombic form.
The title compound C20H20O4S, is polymorphic. In the tetragonal form, the molecule lies on a crystallographic twofold axis, while the monoclinic form has only approximate C
2 molecular symmetry. The greatest excursion from C
2 symmetry is in the orientation of the two phenyl rings; at 100 K, one of the rings is rotated −37.2 (3)° and the other by 46.9 (3)° from their symmetric (tetragonal) positions. There are only minor differences in the three-ring nucleus; the best molecular fit of the tetragonal and monoclinic forms, both at 100 K and excluding phenyl rings and H atoms, shows an r.m.s. deviation of 0.066 Å. Both forms have the same absolute configuration.
The title compound, C19H24O6, is a sesquiterpene lactone isolated from the Kenyan plant Warburgia ugandensis. Ring A adopts a chair conformation, ring B is in a C
2 twist conformation and the lactone ring is nearly planar with maximum deviation 0.007 (1) Å. The reported absolute configuration is based on that of the similar compound bromo-parasiticolide A and is supported by analysis of Bijvoet differences from light atoms in Mo Kα radiation.
The title molecule, C20H24O2, is a chalconoid derivative in which the keto–enone group is slightly distorted from planarity; the O=C—C=C torsion angle is 12.24 (13)°.
1,2,3,4,5,6,7,8,13,13,14,14-Dodecachloro-1,4,4a,4b,5,8,8a,12b-octahydro-1,4:5,8-dimethanotriphenylene at 90 K1
The previously reported room-temperature crystal structure [Jaud Baldy, Negrel, Poite & Chanon (1993 ▶). Z. Kristallogr.
204, 289–291] of the title compound, C20H8Cl12, is monoclinic with Z′ = 1, whereas the 90 K structure reported herein is triclinic with Z′ = 2 and shows a 2% volume contraction. The crystallographically independent unit chosen consists of both enantiomers (Λ and Δ) of this propeller-like molecule. Both enantiomers display quasi-twofold symmetry, with average bond-length/bond-angle deviations of 0.0018 (4) Å and 0.41 (2)° for Λ, and 0.0026 (4) Å and 0.50 (2)° for Δ.
In the title HBr salt of (S)-homoserine lactone, C4H8NO2
+·Br−, the five-membered ring has an envelope conformation, with the –CH2– C atom adjacent to the N-substituted C atom at the flap position. The four-atom mean plane (r.m.s. deviation = 0.005 Å) of the envelope forms a dihedral angle of 32.12 (9)° with the three-atom flap plane. The distorted square-pyramidal coordination about the anion involves five surrounding cations, with the square base defined by three N—H⋯Br hydrogen bonds [Br⋯N = 3.3046 (10), 3.3407 (12) and 3.3644 (13) Å] and near-contact with an H atom attached to C [Br⋯C = 3.739 (1) Å]. Another Br⋯C contact of 3.427 (1) Å defines the apex. There is also an N—H⋯O hydrogen bond present linking the cations.
In the title co-crystal, C22H16O10·C22H18O8, the independent tetramethyl 9,10-dihydro-9,10-dioxoanthracene-2,3,6,7-tetracarboxylate, (I), and tetramethyl anthracene-2,3,6,7-tetracarboxylate, (II), components occupy separate crystallographic inversion centers. In (II), the dihedral angles between the mean aromatic plane and the two independent carboxylate planes are 41.32 (10) and −38.35 (10)°. The methylcarboxylate groups of (I) are disordered, with each resolvable into two groups. In the least disordered carboxylate, the apparent angles between the mean aromatic plane and the two partial carboxylate planes [site occupations = 0.510 (3) and 0.490 (3)] are 16.8 (3) and 23.3 (3)°. In the highly disordered group, the apparent angles between the mean aromatic plane and the two partial carboxylate planes [site occupations = 0.510 (3) and 0.490 (3)] are 78.3 (3) and −74.1 (3)°. In addition, this extreme disorder leads to an artificially elongated C(aromatic)—C(carboxyl) bond.
The title compound, C30H18Cl6O3·0.82CH2Cl2, consists of a slightly cup-shaped seven-ring truxene nucleus with hydroxy and dichloromethyl substituents at stereocenters 5R/S, 10R/S and 15R/S. C—Cl distances are in the range 1.759 (4)–1.783 (3) Å. Solvent channels parallel to the b axis appear to be partially occupied by highly disordered dichloromethane solvent molecules, the contribution of which were removed from the refinement with the SQUEEZE procedure in PLATON [Spek (2009 ▶). Acta Cryst. D65, 148–155]. Only one of the OH groups forms a hydrogen bond, which is intermolecular to another OH group, forming centrosymmetric dimers in the crystal.
The title compound, C11H23NO5P+·I−, consists of an eight-membered cationic heterocyclic ring in a boat–chair conformation. The ring features a tetraalkylammonium N and a methylphosphonate P atom. A –CH2(CO)OC2H5 ester side chain at the C adjacent to oxygen produces two chiral centers at that substituted C atom and the P atom, both of which were determined to have absolute R,R configurations. A previously determined racemic bromide analog has exactly the same ring but with a –C15H31 side chain. In that structure, both chiral centers show the same relative R/S,R/S configurations, but the ring in the bromide analog is in a boat conformation.
In the title compound, C32H28, the central cyclooctatetraene ring has a boat conformation, and the molecule is saddle shaped. The seat is defined by the mean plane of the four-atom attachment points (r.m.s. deviation = 0.014 Å) of the two bicycloheptenyl substituents. These substituents comprise the pommel and cantle, with each mean plane defined by four atoms proximate to the seat (r.m.s. deviations = 0.002 and 0.004 Å). Relative to the seat, the pommel and cantle bend up 31.16 (4) and 29.40 (5)°, while the benzo units (flaps, r.m.s. deviations = 0.006 and 0.009 Å) bend down 36.75 (4) and 38.46 (4)°. The mean planes of the dimethylethylidene units are almost perpendicular to the saddle seat, making dihedral angles 86.89 (4) and 88.01 (4)°.
(E)-3,3′,4,4′,7,7′,8,8′-Octamethyl-2H,2′H-1,1′-bi(cyclopenta[fg]acenaphthylenylidene)-2,2′,5,5′,6,6′-hexaone dichloromethane monosolvate
The title compound, C36H24O6·CH2Cl2, is a dimer of two essentially planar (r.m.s., deviations of fitted plane of 14 pyracene C atoms = 0.0539 and 0.0543 Å) tetracyclic pyracene frameworks (each with four methyl groups and three carbonyl groups on the peripheral carbon atoms) twisted along a central C=C bond with an angle of 50.78 (3)° at 90 K. There are notably long Csp
2 bonds associated with the carbonyl groups, the longest being 1.601 (3) Å between two carbonyl C atoms. There are also intermolecular carbonyl⋯carbonyl interactions of both parallel and antiparallel types, with C⋯O distances in the range 3.041 (3) to 3.431 (2) Å. This compound is of interest with respect to the synthesis of fullerene fragments, such as corannulene and semibuckminsterfullerene derivatives (or ‘buckybowls’), and is a side product of the previously reported oxidation reaction. Structural details, such as planarity analysis of fused rings, out-of-plane deviation of substituents, intermolecular interactions, and longer than typical bond lengths, will be discussed as well as comparisons to structurally related compounds.
The title compound, C48H40, is a tetraisopropyl-substituted polyannulenoenyne. The unsubstituted polyannulenoenyne, C36H16 (CSD: RICVEE; CAS: 186494-87-1), has quasi-D
2 (222) symmetry, as determined by least-squares fit (excluding H atoms) to a model optimized in D
2 symmetry by molecular mechanics (r.m.s. deviation = 0.239 Å). The least-squares fits of 36 common C atoms of the title compound (at 90 K) to the parent (at 295 K) and to the optimized model show r.m.s. deviations of 0.419 and 0.426 Å, respectively.
The title molecule, C30H24, was prepared as a possible precursor to buckminsterfullerene cages. The two enantiomers adopt the anti configuration, with one S/R and two R/S methyl groups, one anti to the other two. The truxene framework is slightly non-planar: with respect to the central six-ring mean plane, the three methyl C atoms are 1.377 (3), −1.475 (3) and 1.515 (3) Å distant, whereas the respective proximate peripheral six-ring mean planes make dihedral angles of 6.27 (6), 3.45 (7) and −7.37 (7)°.
In the title compound, C26H24, the central cyclooctatetraene ring has a boat conformation, and the molecule is saddle shaped. The seat is defined by the mean plane of the four-atom attachment points (r.m.s. deviation = 0.014 Å) of the two bicycloheptane substituents. These substituents comprise the pommel and cantle, with each mean plane defined by four atoms proximate to the seat (r.m.s. deviations = 0.001 and 0.000 Å). Relative to the seat, the pommel and cantle bend up 33.36 (5) and 34.22 (4)°, while the benzo units (flaps, r.m.s. deviations = 0.008 and 0.013 Å) bend down 33.48 (4) and 36.58 (4)°.
The title compound, C24H42N2O7, is a chiral lactam-constrained amino acid with a six-membered ring backbone and isopropyl and tert-butyl ester side chains. The conformation of the six-membered ring can be described as a half chair, with two CH2 C atoms lying 0.443 (1) and −0.310 (1) Å out of the best plane of the other four atoms (mean deviation = 0.042 Å). Both N atoms are sp
2 hybridized, lying 0.0413 (9) and 0.067 (1) Å out of the planes defined by the three C atoms bonded to them. The absolute configuration was determined, based on resonant scattering of light atoms in Cu Kα radiation.