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Phosphorylation of (S)-prolinol with P(NEt2)3was used to synthesize aminophosphite (2R,5S)- $${\text{HCH}}_{\text{2}} {\text{OPNEt}}_{\text{2}} $$ , which was reacted with the corresponding amino alcohols to afford (2S,5R)- $${\text{CH}}_{\text{2}} \left( {{\text{CH}}_{\text{2}} } \right)_2 {\text{NCHCH}}_{\text{2}} {\text{OPO}}\left( {{\text{CH}}_{\text{2}} } \right)_2 {\text{NMe}}_{\text{2}} $$ (Va) and (2S,5R)- $${\text{CH}}_{\text{2}} \left( {{\text{CH}}_{\text{2}} } \right)_2 {\text{NCHCH}}_{\text{2}} {\text{OPO}}\left( {{\text{CH}}_{\text{2}} } \right)_2 {\text{N}}\left( {{\text{CH}}_{\text{2}} } \right)_{\text{4}} {\text{CH}}_{\text{2}} $$ (Vb). Reaction of Vawith [Rh(CO)2Cl]2(P/Rh = 1) yields the mononuclear chelate [Rh(CO)(P^N)Cl] (VIIa), while the analogous reaction with Vbresults in a mixture of products with cis- and trans-orientation of the coordinated phosphorus and nitrogen atoms. Spectral characteristics of the products of coordination of ligands Vaand Vbwere compared with those for the binuclear reference complex [Rh(CO)(L)Cl]2(VIII), where L is P-monodentate ligand (2S,5R)- $${\text{CH}}_{\text{2}} \left( {{\text{CH}}_{\text{2}} } \right)_2 {\text{NCHCH}}_{\text{2}} {\text{OPOEt}}_{\text{2}} $$ (VI). The ligands and complexes were studied by IR, NMR, 31P and 13C spectroscopy, mass spectrometry, and elemental analysis methods. X-ray diffraction analysis of crystals VIIIwas performed.