BBaCoHO 9 P 2 ,triclinic, P1 (no. 2), a =5.3147(3) Å, b =7.9926(8) Å, c =8.2936(8) Å, a =88.63(1)°, b =79.46(1)°, g =87.14(1)°, V =345.9 Å 3 , Z =2, R gt(F) =0.029, wRref(F 2 ) =0.068, T =293 K.
Source of materialThe preparation was carried out hydrothermally by treating a mixture of 0.6332 gB a(OH) 2 ·8H2O( Merck, 98 %), 1.0000 g Co(C 2H3O2)2 ·4 H 2 O( Alfa Aesar, 99.9 %), 0.5590 gB 2 O 3 (Chempur, 99.99 %) and 2.7771 gH 3 PO 4 (Merck, 85 %) in the molar ratio Ba :Co:B:P=0.5 :1:2:6.10mlofdeionized water were added and the solution was stirred at 373 K. Meanwhile, 1.0 ml HCl (37 %) were added to adjust the pH value to 1. The mixture was filled into a20mlTeflon-lined autoclave (filling degree 40 %) and heated at 443 Ku nder autogenous pressure for two weeks. The reaction product was filtered, washed with deionized water/acetone and finally dried in air at 333 K. The reaction product contained pink platelets with dimensions ranging from 0.1 mm to 0.2 mm. The chemical composition of (Ba :Co:B:P)was confirmed by EDXS analyses. The IR spectrum and the loss of water during TG confirms the presence of P-OH groups. 4-,which is formed by alternating hydrogenborate and phosphate tetrahedra sharing common vertices with two additionally branching phosphate tetrahedra. The condensation of the borophosphate anions with CoO 5(OH) octahedra via common corners results in an overall three-dimensional framework containing channels running along [100]. The cross section of the channels is defined by eightmembered rings consisting of two Co coordination octahedra, four phosphate tetrahedra and two hydrogenborate-groups. Barium ions reside within the channels. Barium was found to be tenfold coordinated by oxygen and the Ba-O contacts vary from 2.742(3) Å to 2.998(3) Å.T he Co-O and Co-OH bond distances range from 2.046(3) Å to 2.224(3) Å.Bond lengths d(P-O) and d(B-O) as well as bond angles within the complex anion correspond to respective values similar to related borophosphates [6][7][8][9][10][11][12].
Experimental details