Sadabs program

Crystals suitable for X-ray crystallography were obtained by allowing diffusion of ether vapor onto a CH₂Cl₂ solution of 10 mM AZP-TRZ. Single crystals were picked from the solution by using a nylon loop (Hampton Research Co.) at room temperature. Data collection for a single crystal was conducted on a Bruker, SMART CCD diffractometer equipped with a graphite-monochromated Mo Kα (λ = 0.71073 Å) radiation source under a nitrogen cold stream (223 K). Data collection and integration were performed with a Bruker, SAINT program. Semi-empirical absorption corrections based on equivalent reflections were applied with the Bruker SADABS program. Structures were obtained by using direct methods and refined using a full-matrix least-squares method on F2 by using SHELXL97. All non-hydrogen atoms were refined anisotropically. Hydrogen atoms were added to their geometrically ideal positions. Crystal data for AZP-TRZ: C₃₅H₂₆N₄, monoclinic, P2₁/c, Z = 8, a = 19.8371(6), b = 9.7227(3), c = 26.6431(9) Å, α = 90°, β = 91.6354(12)°, γ = 90°, V = 5136.6(3) ų, μ = 0.077 mm⁻¹, ρ_calcd = 1.300 g cm⁻³, R₁ = 0.0481, wR₂ = 0.0889 for 196332 unique reflections, 703 variables. The crystallographic data for AZP-TRZ are summarized in Supplementary Table 4. Supplementary Tables 5 and 6 list selected bond distances and angles, respectively.

Diffraction data were collected using a single-crystal X-ray diffractometer (D8 VENTURE, Bruker) equipped with a complementary metal oxide semiconductor detector and Mo Kα X-ray source (50 kV, 1 mA). A single crystal with a diameter of ∼50 µm was mounted on a borosilicate glass needle using an adhesive. Lattice constants were determined using the SAINT program (Bruker, 2015 ▸ ) and multi-scan absorption correction was carried out using the SADABS program (Bruker, 2015 ▸ ). The initial structure model was calculated using the SUPERFLIP program based on the charge-flipping algorithm (Palatinus & Chapuis, 2007 ▸ ). Crystal structure analysis was carried out using the JANA2006 program package (Petricek et al., 2014 ▸ ) and the analysed crystal structure was visualized using the VESTA program (Momma & Izumi, 2011 ▸ ).