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. 2018 Nov 6;74(Pt 12):1710–1716. doi: 10.1107/S2056989018015207

Table 5. Experimental details.

  (I) (II) (III)
Crystal data
Chemical formula C13H10ClN3O4S C14H13N3O4S C14H13N3O4S·H2O
M r 339.75 319.33 337.35
Crystal system, space group Monoclinic, P21 Monoclinic, P21/c Monoclinic, P21/c
Temperature (K) 293 293 293
a, b, c (Å) 4.9498 (6), 22.340 (3), 7.0003 (9) 7.190 (1), 15.288 (2), 13.596 (2) 22.589 (2), 5.4424 (4), 12.7180 (9)
β (°) 104.40 (1) 97.68 (2) 92.146 (6)
V (Å3) 749.76 (17) 1481.1 (4) 1562.4 (2)
Z 2 4 4
Radiation type Mo Kα Mo Kα Mo Kα
μ (mm−1) 0.42 0.24 0.24
Crystal size (mm) 0.24 × 0.24 × 0.12 0.50 × 0.48 × 0.24 0.40 × 0.36 × 0.16
 
Data collection
Diffractometer Oxford Diffraction Xcalibur single crystal X-ray diffractometer with Sapphire CCD detector Oxford Diffraction Xcalibur single crystal X-ray diffractometer with Sapphire CCD detector Oxford Diffraction Xcalibur single crystal X-ray diffractometer with Sapphire CCD detector
Absorption correction Multi-scan (CrysAlis RED; Oxford Diffraction, 2009 ▸) Multi-scan (CrysAlis RED; Oxford Diffraction, 2009 ▸) Multi-scan (CrysAlis RED; Oxford Diffraction, 2009 ▸)
T min, T max 0.907, 0.952 0.889, 0.945 0.911, 0.963
No. of measured, independent and observed [I > 2σ(I)] reflections 4582, 2696, 2457 9810, 2719, 2271 9384, 2870, 2178
R int 0.015 0.020 0.021
(sin θ/λ)max (Å−1) 0.602 0.602 0.602
 
Refinement
R[F 2 > 2σ(F 2)], wR(F 2), S 0.030, 0.078, 1.01 0.038, 0.097, 1.05 0.034, 0.092, 1.02
No. of reflections 2696 2719 2870
No. of parameters 202 203 218
No. of restraints 2 2 6
H-atom treatment H atoms treated by a mixture of independent and constrained refinement H atoms treated by a mixture of independent and constrained refinement H atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å−3) 0.14, −0.20 0.28, −0.32 0.19, −0.28
Absolute structure Flack x determined using 1102 quotients [(I +)−(I −)]/[(I +)+(I −)] (Parsons et al., 2013 ▸) – –
Absolute structure parameter 0.05 (3) – –

Computer programs: CrysAlis CCD and CrysAlis RED (Oxford Diffraction, 2009 ▸), SHELXS2013 (Sheldrick, 2008 ▸), SHELXL2014 (Sheldrick, 2015 ▸) and PLATON (Spek, 2009 ▸).