Syntheses,Crystal Structures and Optoelectronic Properties of Two New Inorganic Thioantimonates

Two new thioantimonates,(NH4)2Sb10S16(1)and K1.4(NH4)0.6Sb10S16(2),have been synthesized by solvothermal method with the yields of 80%and 85%,respectively.Single-crystal X-ray diffraction(SCXRD)study reveals that 1 crystallizes in the monoclinic space group of Pn with a=8.1284(4),b=19.4587(9),c=9.1030(4)A,β=91.736(5)°,V=1439.14(12)A^(3),Z=2,Dc=4.077 g·cm^(-3),F(000)=1576,μ=10.389 mm^(-1),R=0.0343 and w R=0.0624(I>2σ(I));2 also crystallizes in the monoclinic space group of Pn with a=8.0989(6),b=19.3730(17),c=9.0411(6)A,β=91.879(6)°,V=1417.79(19)A^(3),Z=2,Dc=4.207 g·cm^(-3),F(000)=1598,μ=10.748 mm-1,R=0.0323 and w R=0.0664(I>2σ(I)).The anionic frameworks of two compounds both feature two-dimensional(2D)[Sb10S16]n2n-layers.The stabilities and optoelectronic properties of 1 and 2 have been characterized.In particular,they are stable under acidic or alkaline conditions(pH=0 or 12.5),showing excellent acid-based resistance.

Solvothermal Synthesis and Crystal Structure of a Layered Thioantimonate(Ⅲ) [C_4H_9NH_3]_2Sb_4S_7

An inorganic-organic hybrid thioantimonate（Ⅲ） [CH3（CH2）3NH3]2Sb4S7 1 with layered structure was synthesized by solvothermal method. 1 crystallizes in the triclinic system, space group P1 with a = 7.0124（11）, b = 11.919（2）, c =14.879（3）A, α = 108.791（3）, β= 102.441（3）, γ = 92.846（2）°, V= 1140.1（3）A3, Mr = 859.71, Z= 2, Do = 2.504 g/cm^3 ,μ = 5.324 mm^-1, F（000） = 804, S = 1.013, the Final R = 0.0297 and wR = 0.0618 for 3534 observed reflections with Ⅰ 〉 2 σ（Ⅰ）. 1 consists of [C4HgNH3]＋ cations and two-dimensional [Sb4ST]n^2n- anion which is composed of three SbS3 trigonal pyranaids and one SbS4 unit joined by sharing common comers. The anionic layers are stacked perpendicularly to the c axis of the unit cell forming two-dimensional channels between the layers. The [C4H9NH3]^＋ cations interdigitate in a bilayer and reside in the 2D channels leading to a sandwich-like arrangement of the anion and cations.

A New One-dimensional Lanthanum Thioantimonate(Ⅴ) with Bidentate Ethylenediamine and Tetradentate Triethylenetetramine Mixed Ligands: La(teta)(en)(μ-η~1,η~2-SbS_4)

A new inorganic-organic hybrid lanthannm thioantimonate（V） with bidentate and tetradentate mixed amino ligands, namely La（teta）（en）（μ-η1,η2-SbS4） （1, teta = triethylenetetramine, en = ethylenediamine）, has been solvothermally synthesized and structurally, thermally and optically characterized. In 1, the en ligand is in situ produced by re-aggregation of teta which plays multiple roles in the reaction as ligand, reactive solvent and precursor. Single-crystal X-ray analysis reveals that 1 belongs to the orthorhombic space group P212121. Its structure features a one-dimensional organic-inorganic hybrid chain of [La（teta）（en）（μ-η1,η2-SbS4）],, constructed by alternating arrangement of μ-η1,η2-sbvs4 tetrahedron and La（teta）（en） complex. Keywords： thioantimonate, lanthanum, amino ligand, crystal structure, optical property