The syntheses and single-crystal structures of Mo(CO) 3(phen)(dipy) ( 1), Mo(CO) 3(biquin)(dipy) ( 2) and Mo(CO) 3(dpme)(dipy) ( 3), (phen = 1,10-phenanthroline, C 12H 8N 2; dipy = 2,2'-dipyridylamine, C 10H 9N 3; biquin = 2,2'-biquinoline, C 18H 12N 2; dpme = 2,2'-dipyridylmethane, C 11H 10N 2) are described. In each case, distorted fac-MoC 3N 3 octahedral coordination geometries arise for the metal atoms. Short intramolecular N–H…C interactions from the dipy N–H group to a carbonyl carbon atom occur in each structure. Crystal data: 1 (C 25H 17MoN 5O 3), M r = 531.38, monoclinic, P2 1/ n (No. 14), Z = 4, a = 11.0965 (5) ？, b = 13.0586 (6) ？, c = 16.6138 (8) ？, b = 108.324 (1)°, V = 2285.31 (18) ？ 3, R( F) = 0.035, wR( F 2) = 0.070. 2 (C 31H 21MoN 5O 3), M r = 607.47, monoclinic, P2 1/ n (No. 14), Z = 4, a = 11.4788 (6) ？, b = 19.073 (1) ？, c = 11.9881 (6) ？, b = 95.179 (1)°, V = 2613.9 (2) ？ 3, R( F) = 0.030, wR( F 2) = 0.076. 3 (C 24H 19MoN 5O 3), M r = 521.38, monoclinic, P2 1/ n (No. 14), Z = 4, a = 8.4222 (3) ？, b = 21.5966 (9) ？, c = 12.5011 (5) ？, b = 94.065 (1)°, V = 2268.12 (15) ？ 3, R( F) = 0.025, wR( F 2) = 0.065.
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