Table 2.

Control experiments under reported conditions for Ni/Ir-catalyzed C(sp³)–H acylation^a

Entry	Substrate	Conditions	Yield (3a)	Yield (2a-dimer)
1	2a	Standard conditions	74% (99% ee)	0%
2	2a	Ni(COD)2 (4 mol %), dtbbpy (5.2 mol %), [Ir(dFCF3ppy)2(dtbbpy)]PF6 (0.5 mol %) K3PO4 (2 equiv), Na2WO4• 2H2O (1 equiv), PhH [0.1 M], r.t., 48 h, blue LED	25% (93% ee)	26% (1:1 d.r.)
3	2a	NiCl2 • glyme (5 mol %), dtbbpy (10 mol %), [Ir(dFCF3ppy)2(dtbbpy)]PF6 (1 mol %) K2CO3 (2 equiv), PhH [0.1 M], r.t., 16 h, blue LED	28% (91% ee)	10% (1:1 d.r.)
4	35a	NiCl2 • glyme (5 mol %), dtbbpy (10 mol %), [Ir(dFCF3ppy)2(dtbbpy)]PF6 (1 mol %) K2CO3 (2 equiv), PhH [0.1 M], r.t., 16 h, blue LED	N.D.	N.D.

^aAll yields are isolated yields. Diastereomeric ratios were determined by ¹H NMR spectroscopy. N.D. = not detected.