*3.5. X-Ray Crystallographic Analysis*

Crystallographic data have been deposited in the Cambridge Crystallographic Data Centre [15]. Crystallographic data were collected on an Agilent Xcalibur Eos Gemini CCD plate diffractometer equipped with a graphite-monochromatic Cu-Kα radiation (λ = 1.54178) Å at 293 (2) K. The data were corrected for absorption by using the program SADABS [16]. The structures were solved by

direct methods with the SHELXTL software package [17]. All non-hydrogen atoms were refined anisotropically. The H atoms connected to C atoms were calculated theoretically, and those to O atoms were assigned by difference Fourier maps [18]. The absolute structure was determined by refinement of the Flack parameter [19], based on anomalous scattering. The structures were optimized by full-matrix least-squares techniques.

Crystal data of compound **1**: C20H26N2O6S2·H2O, F.W. = 472.56, orthorhombic space group *P*2(1)2(1)2(1), unit cell dimensions *a* = 8.5746 (5) Å, *b* = 10.9602 (8) Å, *c* = 24.3158 (16) Å, *V* = 2285.2 (3) Å3, <sup>α</sup> <sup>=</sup> <sup>β</sup> <sup>=</sup> <sup>γ</sup> <sup>=</sup> <sup>90</sup>◦, *<sup>Z</sup>* <sup>=</sup> 4, *<sup>d</sup>*calcd <sup>=</sup> 1.374 mg/m3, crystal dimensions 0.40 <sup>×</sup> 0.21<sup>×</sup> 0.13 mm, <sup>μ</sup> <sup>=</sup> 2.491 mm<sup>−</sup>1, *F*(000) = 1000. The 5006 measurements yielded 3321 independent reflections after equivalent data were averaged. The final refinement gave *R*<sup>1</sup> = 0.0525 and *wR*<sup>2</sup> = 0.1263 [*I* > 2σ(*I*)]. The absolute structure parameter was 0.01(3).

Crystal data of compound **2**: C21H28N2O8S2, F.W. = 500.57, monoclinic space group *P*2(1), unit cell dimensions *a* = 6.8423 (4) Å, *b* = 20.5136 (10) Å, *c* = 8.2231 (5) Å, *V* = 1130.48 (11) Å3, α = γ = 90◦, <sup>β</sup> <sup>=</sup> 101.635 (2)◦, *<sup>Z</sup>* <sup>=</sup> 2, *<sup>d</sup>*calcd <sup>=</sup> 1.471 mg/m3, crystal dimensions 0.20 <sup>×</sup> 0.17<sup>×</sup> 0.10 mm, <sup>μ</sup> <sup>=</sup> 2.587 mm<sup>−</sup>1, *F*(000) = 528. The 6832 measurements yielded 2789 independent reflections after equivalent data were averaged. The final refinement gave *R*<sup>1</sup> = 0.0514 and *wR*<sup>2</sup> = 0.1199 [*I* > 2σ(*I*)]. The absolute structure parameter was 0.02(4).

Crystal data of compound **3**: C20H20N2O7S2·CH3OH, F.W. = 496.54, orthorhombic space group *P*2(1)2(1)2(1), unit cell dimensions *a* = 10.1030 (6) Å, *b* = 10.8478 (5) Å, *c* = 19.6848 (10) Å, *V* = 2157.4 (2) <sup>Å</sup>3, <sup>α</sup> <sup>=</sup> <sup>β</sup> <sup>=</sup> <sup>γ</sup> <sup>=</sup> <sup>90</sup>◦, *<sup>Z</sup>* <sup>=</sup> 4, *<sup>d</sup>*calcd <sup>=</sup> 1.529 mg/m3, crystal dimensions 0.25 <sup>×</sup> 0.17<sup>×</sup> 0.13 mm, <sup>μ</sup> <sup>=</sup> 2.711 mm<sup>−</sup>1, *F*(000) = 1040. The 4782 measurements yielded 3033 independent reflections after equivalent data were averaged. The final refinement gave *R*<sup>1</sup> = 0.0510 and *wR*<sup>2</sup> = 0.1001 [*I* > 2σ(*I*)]. The absolute structure parameter was 0.02(3).
