Skip to main content
. 2021 Mar 19;77(Pt 4):406–411. doi: 10.1107/S2056989021002735

Table 1. Experimental details.

  1 2 3 4
Crystal data
Chemical formula (NH4)2W3SeO12 Cs2W3SeO12 Rb2W3SeO12 K2W3SeO12
M r 858.59 1088.33 993.40 900.66
Crystal system, space group Hexagonal, P63 Hexagonal, P63 Hexagonal, P63 Monoclinic, P21/n
Temperature (K) 297 293 293 293
a, b, c (Å) 7.2303 (3), 7.2303 (3), 12.1491 (5) 7.2580 (3), 7.2580 (3), 12.5291 (5) 7.2380 (1), 7.2380 (1), 12.1115 (3) 7.2310 (2), 11.4863 (4), 12.6486 (4)
α, β, γ (°) 90, 90, 120 90, 90, 120 90, 90, 120 90, 90.096 (2), 90
V (Å3) 550.03 (5) 571.59 (5) 549.50 (2) 1050.56 (6)
Z 2 2 2 4
Radiation type Mo Kα Mo Kα Mo Kα Mo Kα
μ (mm−1) 34.67 39.63 43.49 37.09
Crystal size (mm) 0.10 × 0.10 × 0.05 0.10 × 0.08 × 0.05 0.10 × 0.05 × 0.05 0.08 × 0.05 × 0.02
 
Data collection
Diffractometer Bruker APEXII CCD Bruker APEXII CCD Bruker APEXII CCD Bruker APEXII CCD
Absorption correction Multi-scan (SADABS; Krause et al., 2015 ▸) Multi-scan (SADABS; Krause et al., 2015 ▸) Multi-scan (SADABS; Krause et al., 2015 ▸) Multi-scan (SADABS; Krause et al., 2015 ▸)
T min, T max 0.129, 0.276 0.110, 0.242 0.098, 0.220 0.155, 0.524
No. of measured, independent and observed [I > 2σ(I)] reflections 14419, 1079, 1069 2825, 831, 730 3497, 675, 654 26562, 4026, 3456
R int 0.049 0.058 0.033 0.073
(sin θ/λ)max (Å−1) 0.702 0.643 0.666 0.770
 
Refinement
R[F 2 > 2σ(F 2)], wR(F 2), S 0.023, 0.052, 1.27 0.029, 0.054, 1.02 0.018, 0.033, 1.06 0.032, 0.105, 1.15
No. of reflections 1079 831 675 4026
No. of parameters 57 56 57 165
No. of restraints 1 13 7 24
H-atom treatment H-atom parameters not defined – – –
Δρmax, Δρmin (e Å−3) 2.63, −2.37 1.90, −1.65 0.90, −1.14 3.94, −3.11
Absolute structure Flack x determined using 492 quotients [(I +)−(I −)]/[(I +)+(I −)] (Parsons et al., 2013 ▸) Flack x determined using 297 quotients [(I +)−(I −)]/[(I +)+(I −)] (Parsons et al., 2013 ▸) Flack x determined using 182 quotients [(I +)−(I −)]/[(I +)+(I −)] (Parsons et al., 2013 ▸)  
Absolute structure parameter 0.015 (13) 0.00 (3) −0.08 (3) –

Computer programs: APEX2 and SAINT (Bruker, 2004 ▸), SHELXT (Sheldrick, 2015a ▸), SHELXL2013 (Sheldrick, 2015b ▸), SHELXL (Sheldrick, 2015b ▸), ORTEP-3 for Windows (Farrugia, 2012 ▸), DIAMOND (Pennington, 1999 ▸) and SHELXL97 (Sheldrick, 2008 ▸).