Mixed methyl- and propyl-thiolate self-assembled monolayers (SAMs) are prepared on a Au(111) surface by exposing the gold substrate to methyl-propyl-disulfide vapor at room temperature. Scanning tunneling microscopy imaging of such SAMs reveals a (3 × 4) phase consisting of CH3-S-Au-S-CH3, CH3-S-Au-S-(CH2)2CH3, and CH3-(CH2)2-S-Au-S-(CH2)2CH3. Partial desorption of methyl-thiolate occurs when samples are thermally annealed to 373 K, leading to the formation of a striped phase consisting of primarily CH3-(CH2)2-S-Au-S-(CH2)2CH3.