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Four open-framework transition-metal phosphates; (NH 4 ) 2 Co 3 (HPO 4 ) 2 F 4 ( 1 ), (NH 4 )Co 3 (HPO 4 ) 2 (H 2 PO 4 )F 2 ( 2 ), KCo 3 (HPO 4 ) 2 (H 2 PO 4 )F 2 ( 3 ), and KFe 3 (HPO 4 ) 2 (H 2 PO 4 )F 2 ( 4 ); are prepared by ionothermal synthesis using pyridinium hexafluorophosphate as the ionic liquid. Single-crystal X-ray diffraction analyses reveal that the four compounds contain cobalt/iron-oxygen/fluoride layers with Kagomé topology composed of interlinked face-sharing MO 3 F 3 /MO 4 F 2 octahedra. PO 3 OH pseudo-tetrahedral groups augment the [M 3 O 6 F 4 ] ( 1 )/[M 3 O 8 F 2 ] layers on both sides to give M 3 (HPO 4 ) 2 F 4 ( 1 ) and M 3 (HPO 4 ) 2 F 2 ( 2-4 ) layers. These layers are stacked along the a axis in a sequence AA…, resulting in the formation of a layer structure for (NH 4 ) 2 Co 3 (HPO 4 ) 2 F 4 ( 1 ). In NH 4 Co 3 (HPO 4 ) 2 (H 2 PO 4 )F 2 and KM 3 (HPO 4 ) 2 (H 2 PO 4 )F 2 , the M 3 (HPO 4 ) 2 F 2 layers are stacked along the a axis in a sequence AA  i  … and are connected by [PO 3 (OH)] tetrahedra, giving rise to a 3-D open framework structure with 10-ring channels along the [001] direction. The negative charges of the inorganic framework are balanced by K + /NH 4  + ions located within the channels. The magnetic transition metal cations themselves form layers with stair-case Kagomé topology. Magnetic susceptibility and magnetization measurements reveal that all four compounds exhibit a canted anti-ferromagnetic ground state ( T  c = 10 or 13 K for Co and T  c = 27 K for Fe) with different canting angles. The full orbital moment is observed for both Co 2+ and Fe 2+ .

Ionothermal synthesis of open-framework metal phosphates with a Kagomé lattice network exhibiting canted anti-ferromagnetism