Diaqua­(5,10,15,20-tetra­phenyl­porphyrinato-κ⁴N)magnesium–18-crown-6 (1/1)

In the title compound, [Mg(C₄₄H₂₈N₄)(H₂O)₂]·C₁₂H₂₄O₆, the Mg^II cation lies on an inversion center and is octa­hedrally coordinated by the four N atoms of the deprotonated tetra­phenyl­porphyrin (TPP) ligand and by two water mol­ecules. The asymmetric unit contains one half of the [Mg(TPP)(H₂O)₂] complex and one half of an 18-crown-6 mol­ecule. The average equatorial magnesium–pyrrole N atom distance (Mg—N_p) is 2.071 (1) Å and the axial Mg—O(H₂O) bond length is 2.213 (1) Å. The crystal packing is stabilized by two O—H...O hydrogen bonds between coordinating water mol­ecules and adjacent 18-crown-6 mol­ecules, and exhibits a one-dimensional supramolecular structure along the a axis. The supramolecular architecture is futher stabilized by weak C—H...π inter­actions. The 18-crown-6 mol­ecule is disordered over two sets of sites with an occupancy ratio of 0.8:0.2.

Bis(cinnamato-κO)(1,10-phenanthroline-κ²N,N′)copper(II)

The title mononuclear Cu^II complex, [Cu(C₉H₇O₂)₂(C₁₂H₈N₂)], is comprised of a Cu^II cation, two cinnamate (L⁻) ligands and a 1,10-phenanthroline (phen) ligand. The Cu^II atom and phen ligand lie on a twofold rotation axis. The Cu^II atom is coordinated by two O atoms from two carboxyl­ate groups of two (L⁻) ligands and two N atoms from one phen ligand, exhibiting a distorted square-planar geometry. In the crystal, mol­ecules are assembled into supra­molecular chains parallel to the c axis through weak C—H...O hydrogen bonds involving the phen and cinnamate ligands.

Aqua­(5,10,15,20-tetra­phenyl­porphyrin­ato-κ⁴N)cadmium(II)–18-crown-6 (1/1)

The title compound, [Cd(C₄₄H₂₈N₄)(H₂O)]·(C₁₂H₂₄O₆), was made by the reaction of the [Cd(TPP)] with an excess of 18-crown-6 in chloro­benzene (where TPP is tetra­phenyl­porphyrinate). The Cd^II cation is chelated by a TPP anion and coordinated by a water mol­ecule in a distorted N₄O square-pyramidal geometry, the Cd^II cation being displaced by 0.7533 (9) Å from the mean plane of four N atoms of TPP anion. The porphyrin core presents a significant distortion, the maximum atomic deviation from the 24-atom mean plane is 0.1517 (2) Å. The 18-crown-6 mol­ecule is linked with the Cd^II complex via classical O—H...O hydrogen bonds. In the crystal, weak C—H...π inter­actions link the complex and 18-crown-6 mol­ecules into a three-dimensional supra­molecular architecture.

catena-Poly[bis­(μ₃-2-phenyl­acetato-κ³O,O′:O)bis­(μ₂-2-phenyl­acetato-κ²O:O′)dicopper(II)(Cu—Cu)]

The title polymeric compound, [Cu₂(C₈H₇O₂)₄]_n, was synthesized by the reaction of copper acetate with aqueous phenyl­acetic acid. The unique Cu^II atom is coordinated by five O atoms from the carboxyl­ate groups of phenyl­acetate ligands, and the strongly distorted octa­hedral coordination environment is completed by a Cu—Cu bond of 2.581 (2) Å, at whose mid-point is located an inversion centre. The crystal structure consists of infinite polymeric linear chains of Cu²⁺ ions, running along [100], linked by bridging phenyl­acetate groups.

(5,10,15,20-Tetra­phenyl­porphyrinato-κ⁴N)zinc–18-crown-6 (1/1)

In the title compound, [Zn(C₄₄H₂₈N₄)]·C₁₂H₂₄O₆, the Zn^II ion lies on an inversion center and the asymmetric unit contains one half of a Zn(TPP) complex (TPP = 5,10,15,20-tetra­phenyl­porphyrin dianion) and one half of a centrosymmetric 18-crown-6 mol­ecule. The Zn(TPP) complex exhibits a nearly planar conformation of the porphyrin core [maximum deviation = 0.106 (2) Å] with an average Zn—N distance of 2.047 (2) Å. The title compound is considered as a one-dimensional polymer along [010], in which the Zn(TPP) moiety is linked to the closest O atoms of two symmetry-related 18-crown-6 mol­ecules with a Zn—O distance of 2.582 (1) Å, completing a distorted octahedral coordination environment of the metal ion. The chains are mainly sustained by weak C—H...π inter­actions. An ethyl­ene group of the 18-crown-6 mol­ecule is disordered over three sites with occupancies of 0.50, 0.25 and 0.25.

Di-μ-chlorido-bis­[(2-amino­benzamide-κ²N²,O)chlorido­copper(II)]

The title compound, [Cu₂Cl₄(C₇H₈N₂O)₂], crystallizes as discrete [CuLCl₂]₂ (L = 2-amino­benzamide) dimers with inversion symmetry. Each Cu^II ion is five-coordinated and is bound to two bridging chloride ligands, a terminal chloride ligand and a bidentate 2-amino­benzamide ligand. The crystal structure exhibits alternating layers parallel to (010) along the b-axis direction. In the crystal, the components are linked via N—H...Cl hydrogen bonds, forming a three-dimensional network. These inter­actions link the mol­ecules within the layers and also link the layers together and reinforce the cohesion of the structure.

(1S,3R,8R)-2,2-Di­chloro-3,7,7,10-tetra­methyl­tri­cyclo­[6.4.0.0^1,3]dodec-9-en-11-one

The title compound, C₁₆H₂₂Cl₂O, was synthesized from β-himachalene (3,5,5,9-tetra­methyl-2,4a,5,6,7,8-hexa­hydro-1H-benzo­cyclo­heptene), which was isolated from the essential oil of the Atlas cedar (Cedrus Atlantica). The mol­ecule is built up from fused six- and seven-membered rings and an additional three-membered ring arising from the reaction of himachalene with di­chloro­carbene. The six-membered ring has an envelope conformation, with the C atom belonging to the three-membered ring forming the flap, whereas the seven-membered ring displays a screw-boat conformation; the dihedral angle between the rings (all atoms) is 59.65 (14)°.

(3R*,6R*,4'S*,8'R*,3''R*,6''R*)-3,3''-Diisopropyl-6,6''-dimethyl-2',6'-di­phenyl­dispiro­[cyclo­hexane-1,4'-(3,7-dioxa-2,6-di­aza­bicyclo­[3.3.0]octa­ne)-8',1''-cyclo­hexa­ne]-2,2''-dione

The two oxazolidine rings (A and B) of the title compound, C₃₄H₄₄N₂O₄, display roughly half-chair conformations, which could be described as twisted on the C-O bond. Together, the fused oxazolidine rings have a butterfly shape, with the H atoms attached to the ring junction C atoms in a cis orientation. The cyclo­hexane rings of both p-menthone fragments display chair conformations. The absolute configuration could not be determined from the X-ray diffraction data, but the relative configuration of the stereocentres could be deduced.

Absolute configuration of (1R,3S,8R,11R)-3,7,7,10-tetra­methyl­tri­cyclo­[6.4.0.0^1,3]dodec-9-en-11-ol

The absolute configuration of the title compound, C₁₆H₂₆O, was determined as (1R,3S,8R,11R) based mainly on the synthetic pathway but is also implied by the X-ray analysis. The mol­ecule contains fused six- and seven-membered rings. Part of the seven-membered ring was refined as disordered over two sets of sites with the occupancy ratio fixed at 0.86:0.14. The disorder corresponds to a major chair conformation and a minor boat conforation. In the crysyal, O—H...O hydrogen bonds connect the mol­ecules into chains parallel to the a axis.

8-Hy­droxy­quinolin-1-ium hydrogen sulfate monohydrate

In the crystal structure of the title salt hydrate, C₉H₈NO⁺·HSO₄⁻·H₂O, the quinoline N—H atoms are hydrogen bonded to the bis­ulfate anions. The bis­ulfate anions and water mol­ecules are linked together by O—H...O hydrogen-bonding inter­actions. The cations and anions form separate layers alternating along the c axis, which are linked by N—H...O and O—H...O hydrogen bonds into a two-dimensional network parallel to (100). Further O—H...O contacts connect these layers, forming a three-dimensional network, in which two R₄⁴(12) rings and C₂²(13) infinite chains can be identified.

3-{[(E)-(2-Hydroxynaphthalen-1-yl)methylidene]amino}pyridinium per­chlorate

In the title Schiff base salt, C₁₆H₁₃N₂O⁺·ClO₄⁻, the pyridine ring and the naphthalene ring system are approximately co-planar [making a dihedral angle of 6.05 (12)°] and an intra­molecular O—H...N hydrogen bond occurs between the hydroxyl and imino groups. In the crystal, the cations and anions are linked by N—H...O and weak C—H...O hydrogen bonds, forming the supra­molecular layers parallel to (100). The crystal studied was an inversion twin refined with minor component = 0.43 (13).

Absolute configuration of (1S,3R,8R)-10-bromo­methyl-2,2-di­chloro-3,7,7-tri­methyl­tri­cyclo­[6.4.0.0^1,3]dodec-9-ene

The absolute configuration of the title compound, C₁₆H₂₃BrCl₂, has been deduced from the chemical pathway and fully confirmed by refinement of the Flack and Hooft parameters. The six-membered ring adopts a half-chair conformation, whereas the seven-membered ring is a twisted chair. The mol­ecular packing within the crystal is stabilized only by van der Waals inter­actions.

(1R,4R,6S,7S)-5,5-Di­chloro-1,4,8,8-tetra­methyl­tri­cyclo­[5.4.1^1,7.0^4,6]dodecan-12-one

The title compound, C₁₆H₂₄Cl₂O, was synthesized in three steps from β-himachalene (3,5,5,9-tetra­methyl-2,4a,5,6,7,8-hexa­hydro-1H-benzo­cyclo­heptene), which was isolated from essential oil of the Atlas cedar (cedrus atlantica). The asymmetric unit contains two independent mol­ecules with similar conformations. Each mol­ecule is built up from two fused seven-membered rings and an additional three-membered ring arising from the reaction of himachalene with di­chloro­carbene. The dihedral angles between the mean planes of the two seven-membered rings are 75.03 (9) and 75.02 (9)° in the two independent mol­ecules.

(1S,3R,8R,10R)-2,2-Di­bromo-3,7,7,10-tetra­methyl­tri­cyclo­[6.4.0.0^1,3]dodecan-9-one

The title compound, C₁₆H₂₄Br₂O was synthesized by three steps from β-himachalene (3,5,5,9-tetra­methyl-2,4a,5,6,7,8-hexa­hydro-1H-benzo­cyclo­heptene), which was isolated from essential oil of the Atlas cedar (Cedrus atlantica). The mol­ecule is built up from a seven-membered ring to which a six- and a three-membered ring are fused. The six-membered ring shows a chair conformation. One C atom in the seven-membered ring and two methyl groups attached to the ring are disordered over two sets of sites, with an occupancy ratio of 0.658 (7):0.342 (7).