1. In the drybox, 48.8 mg (0.20 mmol) of YbCl2and 57.5 mg (0.19 mmol) of K2[Pd(CN)4]·H2O were added to a 15 mL of dry2DMF. An orange solution was formed. The mixture was stirred 15 days at ambient temperature under an N2atmosphere, and then the mixture was filtered, leaving a white precipitate (KCl) on the frit and an orange filtrate. The color of the solution changed gradually from orange to light yellow upon the removal of the DMF from the filtrate, and a yellowish viscous oil was formed. After 24 h, light yellow and colorless crystals formed that were manually separated. The light yellow crystals were {[(DMF)16Yb6(μ6-O)(μ3-OH)8(μ-NC)Pd(μ-CN)(CN)2][Pd(CN)4]3·4DMF}∞(10 mg, 8.5% yield based on YbCl2). IR (KBr pellet, cm-1): νOH3656 (m), νCN2161 (s), 2139 (s), νO(DMF)-Yb684 (s), the rest of absorption bands belong to DMF molecules: 2993 (m), 2818 (w), 1666 (vs), 1496 (m), 1437 (s), 1420 (sh, m), 1385 (s), 1252 (m), 1116 (s), 1061 (w), 1019 (w), 866 (w). IR (DMF, cm-1): 2167 (m), 2142 (m), 2135 (s), 2126 (vs). The colorless crystals were {[(DMF)8(H2O)2Yb2[Pd(CN)4]3·0.26H2O}∞(50 mg, 31% yield based on YbCl2). IR (KBr pellet, cm-1): νwater3400 (br, m), ρr801 (m), νCN2179 (sh, s), 2170 (vs), 2147(sh, s), 2141 (vs), νO(DMF)-Yb682 (s), the rest of absorption bands belong to DMF molecules: 2961 (w), 2933 (m), 1662 (vs), 1506 (m), 1437 (s), 1420 (sh, m), 1379 (s), 1252 (m), 1109 (s), 1060 (m), 1016 (w), IR(DMF, cm-1): 2167 (m), 2142 (m), 2135 (s), 2126 (vs).
2. Cyanide-Bridged Lanthanide−Transition Metal One-Dimensional Arrays {(DMF)10Yb2[Ni(CN)4]3}∞ and {(DMF)10Yb2[Pt(CN)4]3}∞
3. Unusual One-Dimensional Ladder Structures Containing Divalent Europium and the Tetracyanometalates Ni(CN)42- and Pt(CN)42-
4. Nakamoto, K.Infrared and Raman Spectra of Inorganic and CoordinationCompounds, 4th ed.; John Wiley & Sons: New York, 1986; p 230.
5. Potential constants of the tetracyanide ions of nickel, palladium, and platinum