Sulfuration of hypervalent complexes of silicon and tin was attempted with several electrophilic sulfur reagents for making carbonsulfur bonds under almost neutral conditions. We provided a qualitative scale of reactivity between various hypervalent salts. Simple and practical methodologies involving non-odorous elemental sulfur were developed. It avoided the use of H 2S or standardized organolithium and Grignard solutions with sulfur, under highly basic conditions.