Influence of the Synthesis Parameters onto Nucleation and Crystallization of Five New Tin–Sulfur Containing Compounds

Abstract

The distinct control of the synthesis parameters achieved crystallization of five new inorganic-organic hybrid tin sulfides with 1,10-phenanthroline (phen) as the organic component: {[Mn(phen)2]2(μ2-Sn2S6)} (1, 3), {[Mn(phen)2]2(μ2-Sn2S6)}·phen (2), {[Mn(phen)2]2(μ2-Sn2S6)}·phen·H2O (4), and {[Mn(phen)2]2[μ-η(2)-η(2)-SnS4]2[Mn(phen)]2}·H2O (5). Compounds 1, 3, and 4 occur successively under static conditions by increasing the reaction time up to 8 weeks. Stirring the reaction mixtures and keeping the educt ratio constant allow preparation of distinct phase pure samples within very short reaction times. At higher autogenous pressure, crystallization and conversion of several compounds are suppressed, and only 1 crystallized. Compound 2 could only be obtained in glass tubes at low pH value of the reaction mixture or at low amine concentration. Adjusting the pH value of the solution, the concentration, and the volume of the solvent, compounds 1-4 crystallize sequentially and were successively converted into each other. Results of thermal stability experiments and solubility studies suggest that compounds 1 and 3 are polymorphs following the density rule. Compounds 2 and 4 may be viewed as pseudopolymorphs of 1 and 3.

High Nuclearity Antimonato‐Polyoxovanadate Cluster {V15Sb6O42} as a Synthon for the Solvothermal in situ Generation of α‐ and β‐{V14Sb8O42} Isomers

“…Between the [Ni(phen) 3 ] 2+ complexes in III , the arrangement of the phen ligands (Figure ) leads to two types of intermolecular distances Ø =3.613 Å for sandwich‐type arrangements (shortest: 3.486 Å) and of Ø =3.881 Å (shortest: 3.607 Å, T‐shaped arrangements). The often called π – π interactions are in the order of 10 kcal mol −1 , thus further stabilizing the structural arrangement …”

The [Sn2S6]4– Anion Acting as Tetradentate Linker: ­Solvothermal Synthesis and Selected Properties of {[TM(phen)2]2Sn2S6} and {[TM(phen)2]2Sn2S6}·phen·H2O (TM = Fe, Co)

“…In our previous study of the system Mn/Sn/S/1,10-phenanthroline five different compounds could be isolated. [41] These compounds were obtained whilst stirring conditions of the reaction slurry varying the time, temperature and amount of solvent. All attempts to synthesize the analogous Fe/Co compounds applying identical reaction conditions failed.…”

“…These angles scatter around 92.56-93.32°(S 3 -Sn-S 3a ), 86.68-87.47°(Sn-S 3 -Sn), and 99.57-119.62°(S 1 -Sn-S 2 , S 1 -Sn-S 3 ) (see Table 2), indicating a deviation from the ideal tetrahedral arrangement, but are comparable to literature data. [17,18,[38][39][40][41] The Fe 2+ /Co 2+ -S/N bonds are in the range reported for tin-sulfur compounds containing these cations. [17,18,40] The values of the dihedral angles between the phen ligands scatter around 90°by about Ϯ 10° (Table 3).…”

“…We were able to isolate and characterize four new compounds featuring the [Sn 2 S 6 ] 4anion acting as tetradentate ligand and one compound with the [SnS 4 ] 4anion exhibiting an unusual coordination mode. [41] To investigate the influence of the metal cation into more detail we now extended the synthetic experiments to Fe 2+ and Co 2+ . Within these investigations we prepared four new compounds of composition {[TM(C 12 H 8 N 2 ) 2 ] 2 Sn 2 S 6 } and {[TM(C 12 H 8 N 2 ) 2 ] 2 Sn 2 S 6 }·C 12 H 8 N 2 ·H 2 O (TM = Fe, Co. C 12 H 8 N 2 = phen).…”

Syntheses and Characterization of Three New Compounds Based on Terephthalate and 2‐(2‐Pyridin‐4‐yl‐vinyl)benzimidazole Ligands

“…[1][2][3][4][5][6][7] The final structure is greatly influenced by the coordination arrangement of the metal ions, the shape and density of the organic ligands, hydrogen bonding, counter anions, pH values of the solution, temperature, the ligand-to-metal ratio, etc. [8][9][10][11][12][13] Any subtle change of the factors may lead to complexes with different final supramolecular structures as well as their properties. Therefore, the exploration of synthetic strategies and routines is still a long-term challenge, and a great deal of work is required to extend the knowledge of relevant structural types and establish proper synthetic strategies in the aim of syntheses desirable supramolecular species.…”