Langmuir-Blodgett (LB) multilayers from fatty acid salts can be charac
terized by finite sized scattering aggregates. High-resolution atomic
force microscopy maps reveal a substructure of molecular ordering. The
se blocks are to be considered as 3D domains. Furthermore, macroscopic
holes and scratches appear at the surface. These defect structures ha
ve to be taken into account when interpreting observed X-ray and neutr
on reflectivity curves. The density loss due to the holes can be detec
ted from the angular shift of the critical angle of total external ref
lection. Off-diagonal scans demonstrate a slight inclination of domain
s relative to each other. Neutron reflectivity patterns of sequentiall
y deuterated and hydrogenated carbon chains provide information about
the disorder of the organic chains. In the second part of the paper a
structure model of the molecular order within the domains is developed
using 16 in-plane Bragg peaks and their truncation rods measured by X
-ray grazing incidence diffraction. The refined 3D unit cell contains
at least four monolayers in a herringbone arrangement of the hydrocarb
on chains. Its stability is given by the inter-chain coupling between
two neighbouring monolayers.