A series of square-planar complexes [MLCl]ClO4 (M = Pd(II), Pt(II); L = bis(3-(diphenylphosphino) propyl) sulfide (psp), bis(3-(diphenylarsino) propyl) sulfide (asa)) have been prepared and characterized. The X-ray crystal structures of two of them have been determined: [Pd(psp)Cl]ClO4, P2(1)/c, a=12.519(2), b=15.766(2), c=16.501(2) Angstrom, beta=105.22(1)degrees, Z=4; and [Pt(asa)Cl]ClO4, P2(1)/c, a=12.583(5), b=16.007(6), c=16.549(6) Angstrom, beta=104.89(3)degrees, Z=4. In both structures, there is a conformational disorder between the chair and skew-boat orientation in one of the two six-membered chelate rings. The C-H ... O hydrogen bond between the hybrid ligand and the perchlorate counter ion that induces the conformational disorder is discussed.