Crystal structure oftrans-(1,8-dibutyl-1,3,6,8,10,13-hexaazacyclotetradecane-κ4N3,N6,N10,N13)bis(isonicotinato-κO)nickel(II) determined from synchrotron data

The new compounds [Ni(L1)][Ni(L1)Sn2S6]n·2H2O (I) and [Ni(L2)]2[Sn2S6]·4H2O (II) containing the macrocyclic ligands L1 (L1 = 1,8‐dimethyl‐1,3,6,8,10,13‐hexaazacyclotetradecane) and L2 (L2 = 1,8‐diethyl‐1,3,6,8,10,13‐hexaazacyclotetradecane) were prepared at room temperature by overlaying an aqueous solution of Na4SnS4·14H2O with the [Ni(L1)](ClO4)2 complex dissolved in CH3CN (I) or by overlaying a solution of the [Ni(L2)](ClO4)2 complex dissolved in DMSO with an aqueous solution of Na4SnS4·14H2O (II). The slow interdiffusion of the two solvents guarantees supersaturation in the interface region of the solvents so that crystallization of the compounds occurs. In the structure of I one Ni2+ cation has bonds to S2– anions of the thiostannate anion thus generating chains along [100]. This cation is in an octahedral environment of four N atoms of L1 and two S atoms of the [Sn2S6]4– anion. The second [Ni(L1)]2+ complex exhibits a square‐planar coordination geometry. These [Ni(L1)]2+ complexes and water molecules are located between the chains. In the structure of II isolated [Sn2S6]4– anions and [Ni(L2)]2+ cations are observed. The Ni2+ cations are fourfold coordinated by N atoms of the L2 ligand and feature also a square planar environment.

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Room Temperature Synthesis of New Thiostannates by Slow Interdiffusion of Different Solvents

Benkada

Näther

Bensch

2020

Zeitschrift anorg allge chemie

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Crystal structure oftrans-(1,8-dibutyl-1,3,6,8,10,13-hexaazacyclotetradecane-κ⁴N³,N⁶,N¹⁰,N¹³)bis(isonicotinato-κO)nickel(II) determined from synchrotron data

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References 18 publications

Room Temperature Synthesis of New Thiostannates by Slow Interdiffusion of Different Solvents

Room Temperature Synthesis of New Thiostannates by Slow Interdiffusion of Different Solvents

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