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The orientation nature of multilayer organosilicon compounds has been investigated by measuring the dependence of the Si K-shell near-edge x-ray absorption fine structures (NEXAFS) on the polarization angle. Two approaches helped to elucidate the orientation mechanism: the substitution effect and the deposition-rate dependence. The orientation angles (α) of Si–X bond axes were obtained for trimethylsilyl halides, (CH3)3Si–X (X = F,Cl,Br,I,NCO), condensed on Cu(111) at a low (∼82 K) temperature: the angles are 60°, 73°, 61°, 55°, and 55° with respect to the surface normal, for X = F, Cl, Br, I, and NCO, respectively. Chloride (X = Cl) produces the most parallel tilt angle. The specific orientation nature of chloride is attributed to its strong dipole moment as well as the regular tetrahedron shape of the molecule. The molecular volumes calculated verify this view. Furthermore, deposition rates are found to greatly influence the growth manner: namely, high deposition rates led to a slightly perpendicular orientation of Si–X bond axis.