Crystal structure of the 1:2 co-crystal of 1,3,6,8-tetra-aza-tri-cyclo-[126.96.36.199,8]undecane (TATU) and 4-chloro-phenol (1/2).
ABSTRACT: In the title compound, C7H14N4·2C6H5ClO, which crystallized with two crystallographically independent 4-chloro-phenol mol-ecules and one 1,3,6,8-tetra-aza-tri-cyclo-[188.8.131.52,8]undecane (TATU) mol-ecule in the asymmetric unit, the independent components are linked by two O-H?N hydrogen bonds. The hydrogen-bond acceptor sites are two non-equivalent N atoms from the aminal cage structure, and the tricyclic system distorts by changing the C-N bond lengths. In the crystal, these hydrogen-bonded aggregates are linked into chains along the c axis by C-H?N hydrogen bonds. The crystal structure also features C-H?? contacts.
Project description:The title compound C(14)H(29)N(4) (+)·I(-) salt, was obtained by the reaction of cage adamanzane-type aminal 1,3,6,8-tetra-aza-tricyclo-[184.108.40.206(3,8)]undecane with heptyl iodide. In the cation, the bond lengths and angles are within normal ranges, except for one N-C(ring) bond distance of 1.542?(3)?Å, which is unexpectedly long compared with related compounds. In the crystal, ions are linked through C-H?I hydrogen bonds. The crystal studied was a non-merohedral twin with a minor twin domain of 6.56?(5)%.
Project description:Solvent-free treatment of 1,3,6,8-tetra-aza-tri-cyclo-[220.127.116.11,8]undecano (TATU) with 4-chloro-3,5-di-methyl-phenol led to the formation of the title co-crystal, C7H14N4·2C8H9ClO. The asymmetric unit contains one aminal cage mol-ecule and two phenol mol-ecules linked via two O-H?N hydrogen bonds. In the aminal cage, the N-CH2-CH2-N unit is slightly distorted from a syn periplanar geometry. Aromatic ?-? stacking between the benzene rings from two different neighbouring phenol mol-ecules [centroid-centroid distance = 4.0570?(11)?Å] consolidates the crystal packing.
Project description:The asymmetric unit of the title co-crystalline adduct, 1,3,6,8-tetra-aza-tri-cyclo[18.104.22.168,8]dodecane (TATD)-4-iodo-phenol (1/2), C8H16N4·2C6H5IO, comprises a half mol-ecule of the aminal cage polyamine plus a 4-iodo-phenol mol-ecule. A twofold rotation axis generates the other half of the adduct. The components are linked by two inter-molecular O-H?N hydrogen bonds. The adducts are further linked into a three-dimensional framework structure by a combination of N?I halogen bonds and weak non-conventional C-H?O and C-H?I hydrogen bonds.
Project description:The structure of the 1:2 co-crystalline adduct C8H16N4·2C6H5BrO, (I), from the solid-state reaction of 1,3,6,8-tetra-aza-tri-cyclo-[22.214.171.124(3,8)]dodecane (TATD) and 4-bromo-phenol, has been determined. The asymmetric unit of the title co-crystalline adduct comprises a half mol-ecule of aminal cage polyamine plus a 4-bromo-phenol mol-ecule. A twofold rotation axis generates the other half of the adduct. The primary inter-species association in the title compound is through two inter-molecular O-H?N hydrogen bonds. In the crystal, the adducts are linked by weak non-conventional C-H?O and C-H?Br hydrogen bonds, giving a two-dimensional supra-molecular structure parallel to the bc plane.
Project description:The structure of the title compound, C(13)H(14)O(2), a penta-cyclo-undecane cage derivative, exhibits unusual Csp(3)-Csp(3) single-bond lengths ranging from 1.505?(3) to 1.607?(2)?Å and strained bond angles as small as 88.7?(1)° and as large as 121.0?(2)°. In this meso compound, an inter-nal non-crystallographic mirror plane exists, bis-ecting the mol-ecule. In the crystal, weak C-H?O hydrogen bonds link the mol-ecules into an infinite spiral about a twofold screw axis along the  direction.
Project description:In the crystal of the title co-crystalline adduct, C8H16N4·C8H9ClO, (I), prepared by solid-state reaction, the mol-ecules are linked by inter-molecular O-H?N hydrogen bonds, forming a D motif. The aza-adamantane structure in (I) is slightly distorted, with N-CH2-CH2-N torsion angles of 10.4?(3) and -9.0?(3)°. These values differ slightly from the corresponding torsion angles in the free aminal cage (0.0°) and in related co-crystalline adducts, which are not far from a planar geometry and consistent with a D 2d mol-ecular symmetry in the tetra-aza-tri-cyclo structure. The structures also differ in that there is a slight elongation of the N-C bond lengths about the N atom that accepts the hydrogen bond in (I) compared with the other N-C bond lengths. In the crystal, the two mol-ecules are not only linked by a classical O-H?N hydrogen bond but are further connected by weak C-H?? inter-actions, forming a two-dimensional supra-molecular network parallel to the bc plane.
Project description:In the title mol-ecule, C(17)H(18)O(5), which was prepared by the reaction of (R)-1,5-dioxaspiro-[5.5]undecane-2,4-dione and 4-meth-oxy-benzaldehyde with ethanol, the 1,3-dioxane ring is in a distorted envelope conformation with the spiro C atom forming the flap. The crystal structure is stabilized by weak inter-molecular C-H?O hydrogen bonds.
Project description:In the title ternary co-crystalline adduct, C7H14N4·2C6H5NO3, mol-ecules are linked by two inter-molecular O-H?N hydrogen bonds, forming a tricomponent aggregates in the asymmetric unit. The hydrogen-bond formation to one of the N atoms is enough to induce structural stereoelectronic effects in the normal donor?acceptor direction. In the title adduct, the two independent nitro-phenol mol-ecules are essentially planar, with maximum deviations of 0.0157?(13) and 0.0039?(13)?Å. The dihedral angles between the planes of the nitro group and the attached benzene rings are 4.04?(17) and 5.79?(17)°. In the crystal, aggregates are connected by C-H?O hydrogen bonds, forming a supra-molecular dimer enclosing an R 6 (6)(32) ring motif. Additional C-H?O inter-molecular hydrogen-bonding inter-actions form a second supra-molecular inversion dimer with an R 2 (2)(10) motif. These units are linked via C-H?O and C-H?N hydrogen bonds, forming a three-dimensional network.
Project description:The structure of the title compound, C(26)H(29)NO(7), at 173?K has an inter-molecular N-H?O hydrogen bond. This is one of the few examples where a mono-ketone penta-cyclo-undecane (PCU) mol-ecule exibits hydrogen bonding in the solid state. The dihedral angles of the amide and ester groups are normal and unaffected by the cage structure. A longer than normal C-C bond [1.571?(4)?Å] was found within the cage structure.
Project description:The structure of the title complex, [CrCl2(2,3,2-tet)]ClO4 (2,3,2-tet is 1,4,8,11-tetra-aza-undecane, C7H20N4), has been determined from synchrotron data. The Cr(III) ion is coordinated by the four N atoms of the 1,4,8,11-tetra-aza-undecane ligand in the equatorial plane and two chloride ions in an axial arrangement, displaying a slightly distorted octa-hedral coordination environment. The two H atoms of the secondary amines are grouped on the same side of the equatorial N4 plane (meso-RS conformation). The Cr-N bond lengths range from 2.069?(2) to 2.084?(2)?Å, while the mean Cr-Cl bond length is 2.325?(2)?Å. The crystal structure is stabilized by inter-molecular hydrogen-bonding inter-actions between the primary and secondary amine groups of the 2,3,2-tet ligands, the Cl ligands and the O atoms of the perchlorate counter-anion, forming corrugated layers parallel to (010).