Saturn 724 ccd diffractometer

Crystallographic data and details of structure refinement parameters are summarized in Table 4 and Table 5. The single crystals 1–4 were grown from a hot acetonitrile solution. The single crystals of 5 were obtained using the slow diffusion method (acetonitrile/ether). Diffraction intensity data were collected with a Rigaku AFC11 with Saturn 724+ CCD diffractometer, and a semiempirical multi-scan absorption correction [41 ] was performed. The structures were solved using SIR97 [42 (link)] by subsequent difference Fourier syntheses and refined by full-matrix least-squares procedures on F². All non-hydrogen atoms were refined with anisotropic displacement coefficients. Hydrogen atoms were treated as idealized contributions and refined in rigid group model. All software and sources of scattering factors are contained in the SHELXL-97 [43 ] and the SHELXL-2018/3 [44 ] program package. The Cambridge Crystallographic Data Centre (CCDC) deposition numbers of 1–5 and Et₄N[Tp*W(CO)₃] are included in Table 4 and Table 5.

Single crystal X-ray diffraction analysis of Co3 and Co4 was carried out on a Saturn 724+ CCD diffractometer (Rigaku, Tokyo, Japan) with the graphite-monochromated Mo-Kα radiation (λ = 0.71073 Å) at 173(2) K and cell parameters were obtained by global refinement of the positions of all collected reflections. Intensities were corrected for Lorentz and polarization effects, and an empirical absorption. The structures were solved by direct methods and refined by full-matrix least-squares on F². All hydrogen atoms were placed in calculated positions. Structural solution of each complex and refinement were performed by SHELXT [67 (link),68 (link)]. In the structural solution of each crystal, two identical structures were found. The solvent molecules which have no effect on the geometry of the main compound were also processed by using SHELXT [67 (link),68 (link)]. All hydrogen atoms and one identical molecule of the complex have been omitted in the ORTEP diagrams for clarity. Crystal data and processing parameters for Co3 and Co4 are summarized in Table 7.

Single crystals of compound 1, 1c, and 3 were prepared by a slow vapor diffusion of methanol into a concentrated solution of 1 or 1c in chloroform and a slow evaporation of toluene solution of 3 at room temperature. X-ray crystallographic analyses for 1c and 3 was performed on a Rigaku Saturn724+ CCD diffractometer with a graphite-monochromated Mo Kα radiation (λ = 0.71075 Å). The data collection and cell refinement were performed using CrystalClear-SM Expert 2.1 b46 software (Rigaku, 2016). X-ray crystallographic analysis for 1 was performed on a Bruker Single Crystal CCD X-ray Diffractometer (SMART APEX II) with Mo Kα radiation (λ = 0.71073 Å). The data collection and cell refinement were performed using APEX3 software (v2016.9-0, Bruker AXS, 2016). The structure of 1 observed based on the diffraction data was refined as a two-component twin using Olex2 software. The all structures were solved by direct methods (SHELXT) and refined by a full-matrix least-squares techniques against F² (SHELXL). The all non-hydrogen atoms were refined anisotropically. Hydrogen atoms were placed using AFIX instructions.

To increase the structural diversity and discover more potent inhibitors of transketolase, it is important to design new compounds based on the structures of candidate compounds that have good activities. All reagents and solvents for the syntheses and analyses were of analytical grade and used without further treatment unless otherwise stated. Column chromatography purification was carried out by using silica gel (200~300 mesh). The melting points were measured on an XT-4A apparatus, and are uncorrected. NMR spectra were obtained on an AV-400 spectrometer (Bruker, Rheinstetten, Germany) operating at 400 MHz for ¹H NMR and 100 MHz for ¹³C NMR using CDCl₃ or DMSO-d₆ as solvents and TMS as the internal standard. The high-resolution mass spectra were recorded on a 6520-QTOF LC/MS (Agilent, Santa Clara, CA, USA) with an ESI source in the positive ion mode. The single-crystal structure was determined on a Saturn 724 CCD diffractometer (Rigaku, Woodlands, TX, USA).