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. 2021 Mar 5;77(Pt 4):335–340. doi: 10.1107/S2056989021002310

Table 2. Experimental details.

  (Ia) (Ib) (II) (III)
Crystal data
Chemical formula C25H23N5OS2 2C24H19Cl2N5OS2·H2O C31H27N5O4S2 C32H22BrCl2N5OS2
M r 473.60 1074.94 597.69 707.47
Crystal system, space group Triclinic, P\overline{1} Monoclinic, P2/c Triclinic, P\overline{1} Triclinic, P\overline{1}
Temperature (K) 296 296 296 296
a, b, c (Å) 8.6269 (7), 9.8418 (9), 14.900 (1) 15.037 (1), 8.4266 (6), 19.471 (1) 10.783 (2), 11.683 (3), 13.577 (3) 12.3200 (9), 12.5700 (9), 12.7742 (9)
α, β, γ (°) 90.588 (7), 106.162 (8), 101.441 (7) 90, 96.246 (6), 90 93.54 (2), 105.17 (2), 113.20 (2) 117.202 (8), 102.879 (7), 105.727 (7)
V (Å3) 1188.05 (17) 2452.5 (3) 1490.9 (6) 1548.4 (2)
Z 2 2 2 2
Radiation type Mo Kα Mo Kα Mo Kα Mo Kα
μ (mm−1) 0.25 0.47 0.22 1.67
Crystal size (mm) 0.36 × 0.12 × 0.04 0.36 × 0.12 × 0.12 0.48 × 0.12 × 0.06 0.40 × 0.40 × 0.08
 
Data collection
Diffractometer Oxford Diffraction Xcalibur with Sapphire CCD detector Oxford Diffraction Xcalibur with Sapphire CCD detector Oxford Diffraction Xcalibur with Sapphire CCD detector Oxford Diffraction Xcalibur 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 ▸) Multi-scan (CrysAlis RED; Oxford Diffraction, 2009 ▸)
T min, T max 0.949, 0.990 0.922, 0.946 0.849, 0.987 0.779, 0.875
No. of measured, independent and observed [I > 2σ(I)] reflections 8241, 4898, 2524 10494, 5290, 3075 10433, 5561, 1730 10549, 5773, 3158
R int 0.030 0.033 0.138 0.022
(sin θ/λ)max (Å−1) 0.629 0.651 0.607 0.607
 
Refinement
R[F 2 > 2σ(F 2)], wR(F 2), S 0.056, 0.112, 1.03 0.046, 0.097, 0.98 0.079, 0.143, 0.88 0.039, 0.095, 0.93
No. of reflections 4898 5290 5561 5773
No. of parameters 319 335 395 402
No. of restraints 10 10 10 10
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-atom parameters constrained H-atom parameters constrained
Δρmax, Δρmin (e Å−3) 0.18, −0.18 0.26, −0.30 0.26, −0.24 0.47, −0.34

Computer programs: CrysAlis CCD and CrysAlis RED (Oxford Diffraction, 2009 ▸), SHELXT (Sheldrick, 2015a ▸), SHELXL2014 (Sheldrick, 2015b ▸) and PLATON (Spek, 2020 ▸).