Research Article

Synthesis, Structure, and Characterization of Keggin-Type Germanate

Table 3

Selected bond lengths (Å) and bond angles (°) for I.

Ge(1)–O(6)1.723(9)Ge(5)–O(10)1.724(8)
Ge(1)–O(7)1.731(9)Ge(5)–O(13)1.730(9)
Ge(1)–O(2)1.747(9)Ge(5)–O(2)1.738(9)
Ge(1)–O(8)1.759(7)Ge(5)–O(5)1.744(9)
Ge(2)–F(1)1.792(10)Ge(6)–F(3)1.778(12)
Ge(2)–O(10)ii1.881(9)Ge(6)–O(13)ii1.785(9)
Ge(2)–O(10)1.881(9)Ge(6)–O(13)1.785(9)
Ge(2)–O(1)ii1.883(10)Ge(6)–O(14)1.795(15)
Ge(2)–O(1)1.883(10)Ge(6)–O(11)2.034(13)
Ge(2)–O(11)1.891(12)Ge(7)–F(5)1.736(14)
Ge(3)–F(2)1.759(14)Ge(7)–O(14)1.771(16)
Ge(3)–O(6)iii1.880(10)Ge(7)–O(4)ii1.774(10)
Ge(3)–O(6)iv1.880(10)Ge(7)–O(4)1.774(10)
Ge(3)–O(6)i1.880(10)Ge(7)–O(11)2.168(13)
Ge(3)–O(6)1.880(10)Ge(8)–O(12)1.745(11)
Ge(3)–O(9)1.900(17)Ge(8)–O(7)iii1.761(9)
Ge(4)–O(1)1.703(9)Ge(8)–O(7)1.761(9)
Ge(4)–O(3)1.728(5)Ge(8)–F(4)1.797(15)
Ge(4)–O(4)1.742(9)Ge(8)–O(9)2.127(13)
Ge(4)–O(5)1.749(9)

O(6)–Ge(1)–O(7)115.5(5)F(3)–Ge(6)–O(13)ii92.5(4)
O(6)–Ge(1)–O(2)113.2(5)F(3)–Ge(6)–O(13)92.5(4)
O(7)–Ge(1)–O(2)100.1(4)O(13)ii–Ge(6)–O(13)116.0(7)
O(6)–Ge(1)–O(8)110.6(5)F(3)–Ge(6)–O(14)89.0(7)
O(7)–Ge(1)–O(8)110.3(5)O(13)ii–Ge(6)–O(14)121.9(3)
O(2)–Ge(1)–O(8)106.4(5)O(13)–Ge(6)–O(14)121.9(3)
F(1)–Ge(2)–O(10)ii88.9(4)F(3)–Ge(6)–O(11)171.1(6)
F(1)–Ge(2)–O(10)88.9(4)O(13)ii–Ge(6)–O(11)92.2(4)
O(10)ii–Ge(2)–O(10)88.6(6)O(13)–Ge(6)–O(11)92.2(4)
F(1)–Ge(2)–O(1)ii89.2(4)O(14)–Ge(6)–O(11)82.1(6)
O(10)ii–Ge(2)–O(1)ii90.8(4)F(5)–Ge(7)–O(14)93.5(8)
O(10)–Ge(2)–O(1)ii178.0(4)F(5)–Ge(7)–O(4)ii94.2(4)
F(1)–Ge(2)–O(1)89.2(4)O(14)–Ge(7)–O(4)ii120.5(4)
O(10)ii–Ge(2)–O(1)178.0(4)F(5)–Ge(7)–O(4)94.2(4)
O(10)–Ge(2)–O(1)90.8(4)O(14)–Ge(7)–O(4)120.5(4)
O(1)ii–Ge(2)–O(1)89.7(6)O(4)ii–Ge(7)–O(4)117.5(7)
F(1)–Ge(2)–O(11)179.7(6)F(5)–Ge(7)–O(11)172.3(7)
O(10)ii–Ge(2)–O(11)90.9(4)O(14)–Ge(7)–O(11)78.8(6)
O(10)–Ge(2)–O(11)90.9(4)O(4)ii–Ge(7)–O(11)89.8(4)
O(1)ii–Ge(2)–O(11)91.0(4)O(4)–Ge(7)–O(11)89.8(4)
O(1)–Ge(2)–O(11)91.0(4)O(12)–Ge(8)–O(7)iii122.5(3)
F(2)–Ge(3)–O(6)iii89.0(3)O(12)–Ge(8)–O(7)122.5(3)
F(2)–Ge(3)–O(6)iv89.0(3)O(7)iii–Ge(8)–O(7)113.5(7)
O(6)iii–Ge(3)–O(6)iv90.9(6)O(12)–Ge(8)–F(4)94.6(7)
F(2)–Ge(3)–O(6)i89.0(3)O(7)iii–Ge(8)–F(4)93.8(4)
O(6)iii–Ge(3)–O(6)i178.0(6)O(7)–Ge(8)–F(4)93.8(4)
O(6)iv–Ge(3)–O(6)i89.1(6)O(12)–Ge(8)–O(9)78.8(6)
F(2)–Ge(3)–O(6)89.0(3)O(7)iii–Ge(8)–O(9)89.8(3)
O(6)iii–Ge(3)–O(6)89.1(6)O(7)–Ge(8)–O(9)89.8(3)
O(6)iv–Ge(3)–O(6)178.0(6)F(4)–Ge(8)–O(9)173.5(6)
O(6)i–Ge(3)–O(6)90.9(6)Ge(4)–O(1)–Ge(2)118.1(5)
F(2)–Ge(3)–O(9)180.0(7)Ge(5)–O(2)–Ge(1)131.9(5)
O(6)iii–Ge(3)–O(9)91.0(3)Ge(4)i–O(3)–Ge(4)133.6(8)
O(6)iv–Ge(3)–O(9)91.0(3)Ge(4)–O(4)–Ge(7)123.5(6)
O(6)i–Ge(3)–O(9)91.0(3)Ge(5)–O(5)–Ge(4)120.5(5)
O(6)–Ge(3)–O(9)91.0(3)Ge(1)–O(6)–Ge(3)117.0(5)
O(1)–Ge(4)–O(3)110.8(6)Ge(1)–O(7)–Ge(8)123.5(5)
O(1)–Ge(4)–O(4)115.8(5)Ge(1)–O(8)–Ge(1)i119.5(8)
O(3)–Ge(4)–O(4)101.4(5)Ge(3)–O(9)–Ge(8)iv136.3(3)
O(1)–Ge(4)–O(5)109.8(5)Ge(3)–O(9)–Ge(8)136.3(3)
O(3)–Ge(4)–O(5)108.2(6)Ge(8)iv–O(9)–Ge(8)87.5(7)
O(4)–Ge(4)–O(5)110.3(5)Ge(5)–O(10)–Ge(2)117.0(5)
O(10)–Ge(5)–O(13)115.8(4)Ge(2)–O(11)–Ge(6)137.0(7)
O(10)–Ge(5)–O(2)110.9(4)Ge(2)–O(11)–Ge(7)134.5(7)
O(13)–Ge(5)–O(2)99.9(4)Ge(6)–O(11)–Ge(7)88.5(5)
O(10)–Ge(5)–O(5)110.3(4)Ge(8)–O(12)–Ge(8)iv114.9(11)
O(13)–Ge(5)–O(5)110.2(5)Ge(5)–O(13)–Ge(6)120.6(5)
O(2)–Ge(5)–O(5)109.1(5)Ge(7)–O(14)–Ge(6)110.6(7)

Symmetry transformations used to generate equivalent atoms: i ; ii ; iii ; iv .