C 4 H 24 ClCoF 6 GaN 2 O 6 ,monoclinic, P2 1 /m (no. 11), a =5.757(2) Å, b =15.028(4) Å, c =9.697(3) Å, b =100.439(3)°, V =825.1 Å 3 , Z =2,R gt (F) =0.041, wR ref (F 2 ) =0.108, T =298 K.
Source of materialSingle crystals of the title compound were obtained by mild solvothermal reaction as follows: 0.041 gofH 3 BO 3 ,0.254 gof CoCl 2. · . 6H 2 Oand 0.696 goftrithylenedieamine were dissolved in amixture solution of 2mlofH 2 Oand 0.1 ml of hydrofluoric acid under constant stirring. After ten minutes, 0.097 gofGa 2O3 was added to this mixture and stirred for 6hatroom temperature. The resulting mixture with pH 4.0 was sealed in a20mlTeflon-lined stainless steel vessel, heated at 443 Kfor about 6days under autogenous pressure and then cooled to room temperature. The resulting pink prism-like crystals were separated by filtration, washed with deionized water, alcohol, and dried in adryer to a constant mass at room temperature. Elemental analysis -found: N, 5.56 %; C, 10.61 %; H, 4.78 %; calculated for C 4 H 24 ClCoF 6 GaN 2 O 6 :N,5.90 %; C, 10.12 %; H, 5.06 %. All the experimental results are consistent with the calculated values based on the formula given crystal structure determination. FT-IR and Raman data are available in the CIF. ,and two kinds of anions, an isolated [GaF 6 ] 3-and aCl -( figure, top). The organic piperazinium comes from the decomposition of trithylenediamine material under hydrothermal condition. The [Co(H 2O)6)] 2+ octahedron is quite regular with Co-Od istances from 2.065(7) Å to 2.086(5) . Å (mean 2.075 Å)a nd the O-Co-Oa ngles between 89.1(2)°and 178.7(3)°.The [GaF 6 ] 3-octahedron is almost regular with Ga-Fdistances from 1.873(4) Å to 1.901(3) .Å (mean 1.890 Å)and the F-Ga-Fangles between 89.0(2)°and 179.4(1)°, which are consistent with those observed in other gallium fluorides [4,5]. The cations and anions are held together through both electrostatic interactions and the N-H···F, O-H···Fand O-H···Cl hydrogen bonds. In this crystal, extensive hydrogen bondings play avery important role in stabilizing the structure (figure, bottom).
Discussion