Single crystal growth of the novel Mn2(OH)2SO3, Mn2F(OH)SO3, and Mn5(OH)4(H2O)2[SO3]2[SO4] compounds using a hydrothermal method

Abstract

The new compounds Mn2(OH)2SO3, Mn2F(OH)SO3, and Mn5(OH)4(H2O)2[SO3]2[SO4] were synthesized using a hydrothermal route and their crystal structures were determined using single crystal X-ray diffraction data. Mn2(OH)2SO3 and Mn2F(OH)SO3 crystallized with the space group Pnma, a = 7.3580(14), b = 10.3429(20), c = 5.7611(11) Å, Z = 4; and a = 7.413(4), b = 10.139(5), c = 5.717(3) Å, Z = 4, respectively, whereas Mn5(OH)4(H2O)2[SO3]2[SO4] crystallized with the space group P2(1)/m, a = 7.6117(7), b = 8.5326(7), c = 10.9273(9) Å, β = 101.6005(13)°, Z = 2. Mn2(OH)2SO3 and Mn2F(OH)SO3 consist of a 3D-framework of manganese octahedra sharing corners and edges and giving rise to 1D-tunnels along the a axis in which are located the sulfur atoms, whereas Mn5(OH)4(H2O)2[SO3]2[SO4] consists of a 3D-framework of MnO5, MnO6, SO3, and SO4 polyhedra. Mn5(OH)4(H2O)2[SO3]2[SO4] is the first transition metal mixed sulfate-sulfite inorganic compound. Bent and symmetrically bifurcated hydrogen bonds were observed in these materials.

Variable Dimensionality, Valence, and Magnetism in Fluoride-Rich Iron Phosphates BaxFex(PO4)Fy (1 ≤ x ≤ 3, 2 ≤ y ≤ 12)

“…EDX analyses of the isolated crystals were qualitatively carried out using a Hitachi S-3400N instrument. EDX analyses under the similar process are reported elsewhere. , BaFe­(PO 4 )­F 2 , Ba 2 Fe 2 (PO 4 )­F 6 , and Ba 3 Fe 3 (PO 4 )­F 12 exhibited approximate Ba/Fe/P/F ratios of 0.98:1.00:1.02:2.54, 2.37:2.00:1.04:6.27, and 3.14:3.00:1.35:11.5, respectively. Surplus P ratios in Ba 3 Fe 3 (PO 4 )­F 12 were found because of overlapped peaks of P and Au.…”

Lone-pair self-containment in pyritohedron-shaped closed cavities: optimized hydrothermal synthesis, structure, magnetism and lattice thermal conductivity of Co15F2(TeO3)14

“…27 Energy-dispersive analysis by Xray (EDAX) of the isolated blue crystals was carried out using a Hitachi S-3400N. EDX analyses under the similar process and reported elsewhere, 28,29 which indicated the peaks for Co and F in the EDX analysis were overlapped; however, (Co + F): Te ratio was identified as 16.4:14.6, in agreement with the expected one (Figure S2).…”