Synthesis, Structure Analysis, and Characterization of a New Thiostannate, (C₁₂H₂₅NH₃)₄[Sn₂S₆]·2H₂O

Abstract

A new thiostannate, (C(12)H(25)NH(3))(4)[Sn(2)S(6)].2H(2)O, was synthesized from SnCl(4), Na(2)S, and dodecylamine (DDA) in the ethanol-water two-solvent system at room temperature. First a suspension was obtained. With increasing crystallization time, single crystals up to several millimeters in size were found at the bottom of the vessel. The compound was characterized by single-crystal X-ray diffraction, solid state (119)Sn CPMAS NMR and (13)C CPMAS NMR, IR absorption spectroscopy, and thermal analysis. The crystal data are a = 7.533(2) Å, b = 10.162(2) Å, c = 21.688(4) Å, alpha = 101.22(3) degrees, beta = 90.76(3) degrees, gamma = 101.82(3) degrees, triclinic, space group = P&onemacr;, and Z = 1. The structure consists of one [Sn(2)S(6)](4)(-) anion, four n-dodecylammonium cations, and two water molecules per unit cell. The [Sn(2)S(6)](4)(-) dimers are formed by two edge-sharing [SnS(4)] tetrahedra. The hydrocarbon chains of the cations are straight with the chain direction running parallel to [001]. The chains are in van der Waals contact to each other with the nitrogen atoms pointing in opposite directions for neighboring chains. The positions of all hydrogen atoms were determined; in particular three positions were found which may suggest that the nitrogen atoms are protonated to form cationic groups. The nonorganic constituents of the structure, i.e., anions, water molecules, and ammonium groups, interact to form an infinite layer-like unit parallel to (001).

Mesolamellar Phases Containing [Re6Q8(CN)6]4– (Q = Te, Se, S) Cluster Anions

“…This type of formula was also observed in previously reported lamellar phases prepared from the clusters and the surfactants, and resulted from the cationic exchange reaction. [4][5][6][7][8][9][10][11] Figure 9. Thermogravimetric analysis of 2.…”

Inorganic–Organic Hybrid Surfactant Crystals: Structural Aspects and Functions

“…The formation of single crystals tends to require size matching between the inorganic anions and hydrophilic heads of surfactant cations, resulting in a specific combination of inorganic and surfactant constituents. Alkylammonium ( Figure 6c) [72,80,81,84,86,88] and alkyldiammonium ( Figure 6d) [73,89,90] often give single crystals, being different from the case of hybrid surfactant single crystals of coordinated compounds. The primary ammonium cations can form hydrogen bonds between inorganic anions by using N-H bonds to stabilize the crystal structures [87].…”

“…These inorganic monolayers The polymeric anions realize more integrated metal ions confined in the two-dimensional inorganic layer, and are expected to emerge specific electronic properties [10][11][12][13][14]16]. The metal halides tend to form a perovskite-type infinite two-dimensional layered structure [13], which consists of a polymeric metal halide layer such as [PbI 4 ] 2´( Figure 5) Figure 5), and are hybridized to form layered single crystals [81][82][83][84][85]. Such molecular cluster-surfactant hybrid single crystals are much more unconventional materials.…”

Preparation and structural evolution of SiO2–TiO2 pillared layered manganese oxide nanocomposite upon intercalating reaction

“…The bands around 515 and 463 cm −1 in BirMO(H) spectrum can be assigned to the Mn-O stretching vibrations [22]. Bands at 2853, 2926 cm −1 corresponding to the C-H asymmetric and C-H symmetric stretching frequencies of the intercalated dodecylamine molecules can be observed in sample C-12LMO [23]. The spectra of samples C-12STLMO, C-12STLMO(200), and C-12STLMO(300) are different from those of BirMO(H) and C-12LMO.…”