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. 2021 Jul 7;12(33):11225–11235. doi: 10.1039/d1sc02948g

Fig. 3. Molecular structures of [K(dme)4][rac-1] (top left), rac-2 (top centre), [K(18-c-6)(dme)][rac-6] (top right), [K(dme)4][rac-7] (bottom left), [K(18-c-6)(dme)2][meso-8] (bottom centre) and [K(dme)][K(dme)2][rac-9] (bottom right) with ellipsoids at the 50% probability level. Only the anions are shown; the counterions are omitted for clarity. For all compounds, hydrogen atoms, except those interacting with Co1 in [rac-7] and with Ni1 in 2, are omitted for clarity. Additionally, the tert-butyl groups in 7 are drawn as wireframes for clarity. For [rac-9]2−, only one of two crystallographically independent anions in the asymmetric unit is shown; structural parameters of the second molecule are given in the ESI. Symmetry-generated atoms are marked with a prime symbol (′). Selected bond lengths [Å] and angles [°] of [K(dme)4][rac-1]: C1–C1′ 1.657(5), Co1–P1 2.1857(8), Co1–C2 2.041(7), Co1–C3 2.073(6), C2–C3 1.343(9), P1–Co1–P1′ 88.84(2), ∑P1 339.8(3) (sum of bond angles around P1); rac-2: C1–C1′ 1.650(2), Ni1–P1 2.1264(4), Ni1–C2 2.041(7), Co1–C3 1.962(2), Ni1–H1 2.56, Ni1–H2 2.88, P1–Ni1–P1′ 91.35(1), ∑P1 323.2(2). [K(18-c-6)(dme)][rac-6]: C1–C2 1.669(2), Co1–P1 2.1874(6), Co1–P2 2.1570(6), Co1–C3 1.784(2), Co1–C4 1.784(2), C3–N1 1.183(2), C4–N2 1.174(3), P1–Co1–P2 91.47(2), C3–N1–C5 153.6(2), C4–N2–C6 153.3(2), ∑P1 328.5(2), ∑P2 337.8(2); [K(dme)4][rac-7]: C1–C2 1.672(2), Co1–P1 2.2371(4), Co1–P2 2.0871(5), Co1–C2 2.049(2), Co1–C3 2.099(1), Co1–P3 2.2750(5), Co1–P4 2.2454(5), Co1–H1 2.64, C2–P3 1.800(1), C2–P4 1.805(2), P1–Co1–P2 92.29(2), ∑P1 325.3(2), ∑P2 351.1(2); [K(18-c-6)(dme)2][meso-8]: C1–C2 1.65(1), Co1–P1 2.136(2), Co1–P2 2.382(2), Co1–P3 2.141(2), Co1–P4 2.283(4), Co1–P5 2.276(2), Co1–P6 2.267(2), P1–P2 2.175(3), P4–P5 2.142(3), P5–P6 2.164(3), P1–P2–P3 78.0(1); [K(dme)x]2[rac-9]: C1–C2 1.685(9), Co1–P1 2.246(2), Co1–P2 2.170(2), Co1–P3 2.293(2), Co1–P4 2.333(2), Co1–P5 2.340(2), Co1–P6 2.183(2), Co1–Co1′ 2.651(1), P3–P4 2.095(3), P4–P5 2.336(3), P5–P6 2.112(3), P1–Co1–P2 92.63(7), ∑P1 323.5(8), ∑P2 340.7(7).

Fig. 3