A novel series of anionic mononuclear terdentate dicyclometalated complexes (NBu4)[Pt(CwedgeNwedgeC)X] (HCwedgeNwedgeCH=2,6-diphenylpyridine) containing acetylide (X=C[triple bond]CR, R=tBu, 1; Ph, 2; Tol, 3; (4-OMe)C6H4, 4) or another anionic ligand (X=CN, 5; S-2Py, 6; CH2COCH3, 7) have been synthesized and fully characterized. The solid-state structures of complexes 1 and 4-6 have also been determined by X-ray diffraction studies, showing, in all the cases, the presence of several types of weak hydrogen interactions, leading to the generation of supramolecular 2D (1) or 3D (4-6) architectures. All the complexes (1-7) are intensely luminescent at low temperature (solid and glassy CH2Cl2), exhibiting concentration dependence in the emissions of the glassy CH2Cl2 matrix.