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Organophosphate-chloride complexes [{(2,6-<i>ⁱ</i>Pr₂C₆H₃-O)₂POO}₂LnCl(CH₃OH)₄]·2CH₃OH, Ln = Nd (<b>1</b>), Eu (<b>2</b>), Gd (<b>3</b>), and Tb (<b>4</b>) have been obtained and structurally characterized. Their reaction with 2,2′:6′,2″-terpyridine leads to the formation of 1:1 adducts ([{(2,6-<i>ⁱ</i>Pr₂C₆H₃-O)₂POO}₂LnCl(terpy)(H₂O)₂(CH₃OH)], Ln = Eu (<b>5</b>), Gd (<b>6</b>), Tb (<b>7</b>) with exception of Nd, where tris-diisopropylphenylphosphate complex [{(2,6-<i>ⁱ</i>Pr₂C₆H₃-O)₂POO}₃Nd) (terpy)(H₂O)(CH₃OH)] (<b>8</b>) was obtained due to the ligand metathesis. A bright luminescence observed for the Eu and Tb organophosphate complexes is the first example of an application of organophosphate ligands for 4f-ions luminescence sensitization. Photophysical properties of all complexes were analyzed by optical spectroscopy and an energy transfer scheme was discussed. A combination of two types of ligands into the coordination sphere (phosphate and phenanthroline) allows designing the Eu surrounding with very high intrinsic quantum yield <inline-formula><math display="inline"><semantics><mrow><msubsup><mi>Q</mi><mrow><mi>E</mi><mi>u</mi></mrow><mrow><mi>E</mi><mi>u</mi></mrow></msubsup></mrow></semantics></math></inline-formula> (0.92) and highly luminescent Ln complexes for both visible and near-infrared (NIR) regions.