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Crystal structure of 3,14-dimethyl-2,13-di-aza-6,17-diazo-niatri-cyclo-[16.4.0.0^7,12]docosane bis-(per-chlorate) from synchrotron X-ray data.

ABSTRACT: The crystal structure of the title salt, C₂₀H₄₂N₄ ²⁺·2ClO₄ ^-, has been determined using synchrotron radiation at 220 (2) K. The structure determination reveals that protonation has occurred at diagonally opposite amine N atoms. The asymmetric unit comprises one half of the organic dication, which lies about a center of inversion, and one perchlorate anion. The macrocyclic dication adopts the most stable endodentate trans-III conformation. The crystal structure is stabilized by intra-molecular N-H⋯N, and inter-molecular N-H⋯O and C-H⋯O hydrogen bonds involving the macrocycle N-H and C-H groups as donors and the O atoms of perchlorate anions as acceptors, giving rise to a three-dimensional network.

SUBMITTER: Moon D

PROVIDER: S-EPMC8100260 | biostudies-literature | 2021 May

REPOSITORIES: biostudies-literature

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Crystal structure of 3,14-dimethyl-2,13-di-aza-6,17-diazo-niatri-cyclo-[16.4.0.07,12]docosane bis-(per-chlorate) from synchrotron X-ray data.

Moon Dohyun D Jeon Sunghwan S Choi Jong-Ha JH

Acta crystallographica. Section E, Crystallographic communications 20210423 Pt 5

The crystal structure of the title salt, C20H42N4 2+·2ClO4 -, has been determined using synchrotron radiation at 220 (2) K. The structure determination reveals that protonation has occurred at diagonally opposite amine N atoms. The asymmetric unit comprises one half of the organic dication, which lies about a center of inversion, and one perchlorate anion. The macrocyclic dication adopts the most stable endodentate trans-II ...[more]

PMID: 34026263

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Crystal structure of 3,14-diethyl-2,13-di-aza-6,17-diazo-niatri-cyclo-[16.4.0.07,12]docosane dinitrate dihydrate from synchrotron X-ray data.

Project description:The crystal structure of title salt, C22H46N4 2+·2NO3 -·2H2O, has been determined using synchrotron radiation at 220 K. The structure determination reveals that protonation has occurred at diagonally opposite amine N atoms. The asymmetric unit contains half a centrosymmetric dication, one nitrate anion and one water mol-ecule. The mol-ecular dication, C22H46N4 2+, together with the nitrate anion and hydrate water mol-ecule are involved in an extensive range of hydrogen bonds. The mol-ecule is stabilized, as is the conformation of the dication, by forming inter-molecular N-H⋯O, O-H⋯O, together with intra-molecular N-H⋯N hydrogen bonds.

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3,14-Diethyl-2,13-di-aza-6,17-diazonia-tri-cyclo-[16.4.0.0(7,12)]docosane dichloride tetra-hydrate from synchrotron radiation.

Project description:The asymmetric unit of title hydrated salt, C22H46N4 (2+)·2Cl(-)·4H2O, comprises half a centrosymmetric dication, one Cl(-) anion and two water mol-ecules of crystallization. The structure determination reveals that protonation has occurred at diagonally opposite amine N atoms, and that the dication features intra-molecular N-H⋯N hydrogen bonds. In the crystal, a three-dimensional artchitecture is formed by O-H⋯Cl/N and N-H⋯Cl/O hydrogen bonds.

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Project description:In the title co-crystal, C(20)H(40)N(4)·2C(11)H(10)O, the macrocycle is generated by a crystallographic inversion centre. The N atoms show a pyramidal coordination, and the cyclo-hexane ring that is fused to the 14-membered C(10)N(4) ring exists in a chair conformation, whereas the methyl substituent occupies an axial site. The (naphthalen-1-yl)methanol mol-ecule forms an O-H?N hydrogen bond to a cyclam N atom. The mean-square-plane passing through the 14-membered ring is approximately coplanar with the naphthalene fused-ring [dihedral angle = 6.6?(1)°].

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Crystal structure of di-aqua-(3,14-diethyl-2,6,13,17-tetra-aza-tri-cyclo-[16.4.0.07,12]docosa-ne)copper(II) (3,14-diethyl-2,6,13,17-tetra-aza-tri-cyclo[16.4.0.07,12]docosa-ne)copper(II) tetra-bromide dihydrate, [Cu(C22H44N4)(H2O)2][Cu(C22H44N4)]Br4·2H2O.

Project description:The crystal structure of the new double CuII complex salt, [Cu(L)(H2O)2][Cu(L)]Br4·2H2O (L = 3,14-diethyl-2,6,13,17-tetra-aza-tri-cyclo-[16.4.0.07,12]docosane, C22H44N4) has been determined using synchrotron radiation. The asymmetric unit contains one half of a [Cu(L)(H2O)2]2+ cation, one half of a [Cu(L)]2+ cation (both completed by crystallographic inversion symmetry), two bromide anions and one water solvent mol-ecule. The CuII atom in the first complex exists in a tetra-gonally distorted octa-hedral environment with the four N atoms of the macrocyclic ligand in equatorial and two aqua ligands in axial positions, whereas the CuII atom in the second complex exists in a square-planar environment defined by the four nitro-gen atoms of the macrocyclic ligand. The two macrocyclic rings adopt the most stable trans-III configuration with normal Cu-N bond lengths from 2.016 (3) to 2.055 (3) Å and an axial Cu-O bond length of 2.658 (4) Å. The crystal structure is stabilized by inter-molecular hydrogen bonds involving the macrocycle N-H or C-H groups and the O-H groups of water mol-ecules as donor groups, and the O atoms of water mol-ecules and bromide anions as acceptor groups, giving rise to a one-dimensional network extending parallel to [100].

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Crystal structure of 3,14-dimethyl-2,6,13,17-tetra-azoniatri-cyclo-[16.4.0.07,12]docosane tetra-chloride tetra-hydrate from synchrotron X-ray data.

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