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The phosphide oxides La 3 Cu 4 P 4 O 2  and La 5 Cu 4  P 4 O 4 Cl 2  were synthesized from lanthanum, copper(I) oxide, red phosphorus, and lanthanum(III) chloride through a ceramic technique. Single crystals can be grown in a NaCl/KCl flux. Both structures were refined from single crystal X-ray diffractometer data:  I 4/ mmm ,  a  = 403.89(4),  c  = 2681.7(3) pm,  wR 2 = 0.0660, 269 F 2  values, 19 variables for La 3 Cu 4 P 4 O 2  and  a  = 407.52(5),  c  = 4056.8(7) pm,  wR 2 = 0.0905, 426 F 2  values, 27 variables for La 5 Cu 4 P 4 O 4 Cl 2 . Refinement of the occupancy parameters revealed full occupancy for the oxygen sites in both compounds. The structures are composed of cationic (La 2 O 2 ) 2+  layers and covalently bonded (Cu 4 P 4 ) 5–  polyanionic layers with metallic characteristics, and an additional La 3+  between two adjacent (Cu 4 P 4 ) 5–  layers. The structure of La 5 Cu 4 P 4 O 4 Cl 2  comprises two additional LaOCl slabs per unit cell. Temperature-dependent magnetic susceptibility studies revealed Pauli paramagnetism. The phosphide substructure of La 3 Cu 4 P 4 O 2  was studied by  31 P solid state NMR spectroscopy. By using a suitable dipolar re-coupling approach the two distinct resonances belonging to the P 2  4–  and the P 3–  units could be identified.

La 3 Cu 4 P 4 O 2 and La 5 Cu 4 P 4 O 4 Cl 2 : synthesis, structure and 31 P solid state NMR spectroscopy