3.2. Crystallography Experiment

The XRD analyses were carried out using equipment of the Center for Joint Use “Spectroscopy and Analysis of Organic Compounds” at the Postovsky Institute of Organic Synthesis of the Russian Academy of Sciences (Ural Branch). The experiment was carried out on a standard procedure (MoK_α-irradiation, graphite monochromator, ω-scans with 1⁰ step at T = 295(2) K) on an automated X-ray diffractometer Xcalibur 3 with a CCD detector. Empirical absorption correction was applied. The solution and refinement of the structures were accomplished using the Olex program package [65]. The structures were solved by the method of the intrinsic phases in the ShelXT program and refined by the ShelXL by full-matrix least-squares method for non-hydrogen atoms [66]. The H atoms were placed in the calculated positions and refined in isotropic approximation.

Crystal Data for C₅₁H₃₀Cl₂N₈ (M = 825.73 g/mol): triclinic, space group P-1, a = 8.5135(4) Å, b = 10.4646(5) Å, c = 22.9053(12) Å, α = 88.784(4)°, β = 85.741(4)°, γ = 82.301(4)°, V = 2016.53(17) ų, Z = 2, T = 295(2) K, μ(MoK_α) = 0.210 mm⁻¹, Dcalc = 1.360 g/cm³, 20,634 reflections measured (7.384° ≤ 2Θ ≤ 60.982°), 10,876 unique (R_int = 0.0577, R_sigma = 0.0845), which were used in all calculations. The final R₁ = 0.0767, wR₂ = 0.1916 (I > 2σ(I)) and R₁ = 0.1463, wR₂ = 0.2616 (all data). Largest peak/hole difference is 0.34/−0.35.

The XRD data were deposited in the Cambridge Structural Database with the number CCDC 2215090. This data can be requested free of charge via www.ccdc.cam.ac.uk (accessed on 17 November 2022).