1,4,8,11-Tetraazoniacyclotetradecane diaquatetrachloridomanganese(II) dichloride dihydrate

The title compound, (C10H28N4)[MnCl4(H2O)2]Cl2·2H2O, consists of isolated octahedral [MnCl4(H2O)2]2− anions, tetraprotonated 1,4,8,11-tetraazoniacyclotetradecane cations, chloride anions and water molecules connected by a network of hydrogen bonds. The MnII atom is situated on an inversion centre, and the 1,4,8,11-tetraazoniacyclotetradecane cation is located on a mirror plane.

The title compound, (C 10 2À anions, tetraprotonated 1,4,8,11-tetraazoniacyclotetradecane cations, chloride anions and water molecules connected by a network of hydrogen bonds. The Mn II atom is situated on an inversion centre, and the 1,4,8,11-tetraazoniacyclotetradecane cation is located on a mirror plane.

Related literature
For bond distances and angles in the cyclam molecule, see: Melson (1979).

Experimental
To an acidic solution of cyclam (1 mmol) was added MnCl 2 .4H 2 O (1 mmol) in 10 ml of distilled water. The mixture was then stirred at room temperature for 3 h after which it was left to evaporate in air. After three weeks, crystals appeared, which were filtered off and washed with 90% ethanol solution.

Refinement
All hydrogen atoms were discernible in difference Fourier maps and could be refined to reasonable geometry. Despite of it the hydrogen atoms bonded to carbon and nitrogen atoms were constrained to ideal positions. The O-H distances were restrained to 0.82 Å with sigma 0.01. The isotropic temperature parameters of hydrogen atoms were calculated as 1.2*U eq of the parent atom.) supplementary materials sup-2 Figures   Fig. 1. View of the cyclamH4 4+ cation, the [MnCl 4 (H 2 O) 2 ] 2anion, free water molecule and chloride anions, together with atom-labelling scheme. Displacement ellipsoids are shown at the 50% probability level.  Refinement. The refinement was carried out against all reflections. The conventional R-factor is always based on F. The goodness of fit as well as the weighted R-factor are based on F and F 2 for refinement carried out on F and F 2 , respectively. The threshold expression is used only for calculating R-factors etc. and it is not relevant to the choice of reflections for refinement.
All the H atoms were discrenible in difference Fourier maps and could be refined to reasonable geometry. Despite of it the H atoms bonded to catbon and nitrogen atoms were constrained to ideal positions. The O-H distances were restrained to 0.82 Å with σ 0.01.
The isotropic temperature parameters of hydrogen atoms were calculated as 1.2*U eq of the parent atom.
The program used for refinement, Jana2006, uses the weighting scheme based on the experimental expectations, see _refine_ls_weighting_details,