Synthesis, Structure, and Characterization of Keggin-Type Germanate

Table 1

The crystallographic data and structural refinement for I.

Empirical formula	H158 F36 Ge84 N36 O175
Formula weight	10245.60
Temperature/K	293(2) K
Wavelength/nm	0.71073 Å
Crystal system, space group	Tetragonal, I4/mmm
Unit cell dimensions	𝑎 = 28.280(4) Å
	𝑐 = 24.881(5) Å
𝑉/nm^3	19899(6) Å^3
𝑍, Dc/(Mg⋅m^−3)	2, 1.632 Mg/m^3
μ/mm^−1	6.309
𝐹(000)	9324
Crystal size	0.17 mm × 0.18 mm × 0.20 mm
Range of 𝜃	3.06° to 25.00°
Limiting indices	−33 ≤ℎ≤ 33, −33 ≤𝑘≤ 33, −29 ≤𝑙≤ 27
Reflections collected/unique	72989/4806 [𝑅(int) = 0.2021]
Completeness to 𝜃 = 25.00°	99.3%
Absorption correction	Semiempirical from equivalents
Max. and min. transmission	0.41 and 0.38
Refinement method	Full-matrix least-squares on 𝐹^2
Data/restraints/parameters	4806/0/224
Goodness-of-fit on 𝐹^2	1.319
Final 𝑅 indices [I>2𝜎(I)]	𝑅1 = 0.0946, 𝑤𝑅2 = 0.2277
𝑅 indices (all data)	𝑅1 = 0.1638, 𝑤𝑅2 = 0.2514
Largest diff. peak and hole	1.970 and −1.090 e/Å^3

𝑅₁=∑||𝐹_𝑜|−|𝐹_𝑐||/∑|𝐹_𝑜|; 𝑤𝑅₂={∑[𝑤(𝐹²_𝑜−𝐹²_𝑐)²]/∑[𝑤(𝐹²_𝑜)²]}^1/2.