*3.5. Structure Determination*

Crystal data for **11af**: C15H9NO3, *<sup>M</sup>* <sup>=</sup> 251.23 g·mol−<sup>1</sup> , light yellow plate, 0.10 <sup>×</sup> 0.32 <sup>×</sup> 0.55 mm<sup>3</sup> , triclinic, space group *p* − 1 (no. 2), *a* = 6.8003(6) Å, *b* = 7.1934(7) Å, *c* = 13.471(1) Å; α = 75.075(4)◦ , β = 79.161(3)◦ , γ = 69.530(3)◦ , *V* = 593.0(1) Å<sup>3</sup> , *<sup>Z</sup>* <sup>=</sup> 2, *<sup>D</sup>*calc <sup>=</sup> 1.407 g·mL−<sup>1</sup> .

Full-set diffraction data were collected with an Apex 2 (Bruker, Billerica, MA, USA) diffractometer equipped with a Cryostream Cooler (Oxford Cryosystems, Oxford, UK) at 150(2) K using graphite-monochromated Mo Kα radiation (λ = 0.71073 Å). The data were corrected for absorption (µ = 0.10 mm−<sup>1</sup> ) using a multi-scan routine incorporated in the diffractometer software. A total of 5295 diffractions was recorded (θmax = 26◦ , data completeness = 99.3%), of which 2309 were unique (*R*int = 2.50%) and 1652 were observed according to the *I* > 2σ(*I*) criterion.

The structure was solved using direct methods (SHELXS-97 [43]) and refined by a full-matrix least-squares routine based on *F* 2 (SHELXL-2017 [44]). The non-hydrogen atoms were refined with anisotropic displacement parameters. All hydrogen atoms were included in their theoretical positions and refined as riding atoms with *U*iso(H) assigned to 1.2*U*eq(C). The refinement converged (∆/σ = 0.000, 172 parameters) to *R* = 5.77% for the observed, and *R* = 8.42%, *wR* = 15.8% for all diffractions. The final

difference map revealed no peaks of chemical significance (∆ρmax <sup>=</sup> 0.22, <sup>∆</sup>ρmin <sup>=</sup> <sup>−</sup>0.23 e Å−<sup>3</sup> ). CCDC deposition no. 2015269.
