An inorganic-organic hybrid thioantimonate(III) [CH3(CH2)(3)NH3](2)Sb4S7 1 with layered structure was synthesized by solvothermal method. 1 crystallizes in the triclinic system, space group P-(1) over bar with a = 7.0124(11), b = 11.919(2), c = 14.879(3) angstrom, alpha = 108.791(3), beta = 102.441(3), gamma = 92.846(2)degrees, V= 1140.1(3) angstrom(3), M-r= 859.71, Z= 2, D-c = 2.504 g/cm(3), mu = 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 sigma(I). 1 consists Of [C4H9NH3](+) cations and two-dimensional [Sb4S7](n)(2n-) anion which is composed of three SbS3 trigonal pyramids and one SbS4 unit joined by sharing common corners. 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.