Table 3. Crystallographic Details for [dmcc][I], [decc][I]-i, [decc][I]-ii, [decc][Cl], [decc][TS], [decc][NS], [decc][AS], [decc][CS], and [decc][PS].
| [dmcc][I] | [decc][I]-i | [decc][I]-ii | [decc][Cl] | |
|---|---|---|---|---|
| formula | C23H21N2I | C25H25N2I·0.5CH3CN | C25H25N2I·CH3OH | C25H25N2Cl·H2O |
| fw | 452.32 | 500.90 | 512.41 | 404.92 |
| crystal size, mm | 0.28 × 0.25 × 0.10 | 0.060 × 0.0005 × 0.0005 | 0.41 × 0.10 × 0.08 | 0.68 × 0.35 × 0.19 |
| crystal system | monoclinic | orthorhombic | monoclinic | monoclinic |
| space group | C2/c (no. 15) | Pbcm (no. 57) | P21/c (no. 14) | P21/n (no. 14) |
| a, Å | 17.8673(7) | 5.5329(2) | 7.7512(5) | 17.6674(2) |
| b, Å | 12.4033(4) | 23.3656(7) | 35.350(2) | 20.4329(3) |
| c, Å | 18.5217(7) | 33.5452(12) | 17.2582(14) | 24.7550(3) |
| α, deg | 90 | 90 | 90 | 90 |
| β, deg | 109.5131(9) | 90 | 101.3040(19) | 108.276(2) |
| γ, deg | 90 | 90 | 90 | 90 |
| V, Å3 | 3868.9(2) | 4336.7(3) | 4637.1(6) | 5422(2) |
| ρcalcd, g cm–3 | 1.553 | 1.302 | 1.422 | 1.268 |
| Z | 8 | 8 | 8 | 16 |
| T, K | 299(2) | 90(2) | 300(2) | 302(2) |
| μ, mm–1 | 1.664 (Mo Kα) | 1.907 (synchrotron) | 1.398 (Mo Kα) | 0.199 (Mo Kα) |
| no. of reflns | 18 488 | 21 871 | 66 690 | 128 521 |
| no. of unique reflns | 4397 | 3964 | 10 591 | 24 327 |
| variables | 237 | 276 | 569 | 1129 |
| λ, Å | 0.71075 (Mo Kα) | 0.78255 (synchrotron) | 0.71075 (Mo Kα) | 0.71075 (Mo Kα) |
| R1 [I > 2σ(I)] | 0.0291 | 0.0313 | 0.0663 | 0.0449 |
| wR2 [I > 2σ(I)] | 0.0693 | 0.0667 | 0.1320 | 0.1213 |
| GOF | 1.108 | 1.045 | 1.016 | 1.099 |
| [decc][TS] | [decc][NS] | [decc][AS] | [decc][CS] | |
|---|---|---|---|---|
| formula | C32H32N2O3S | C31H29N3O5S | C31H31N3O3S | C35H40N2O4S |
| fw | 524.65 | 555.63 | 525.65 | 584.75 |
| crystal size, mm | 0.080 × 0.010 × 0.010 | 0.200 × 0.020 × 0.010 | 0.030 × 0.010 × 0.010 | 0.100 × 0.080 × 0.070 |
| crystal system | monoclinic | triclinic | monoclinic | monoclinic |
| space group | P21/c (no. 14) | P1̅ (no. 2) | P21/c (no. 14) | P21 (no. 4) |
| a, Å | 12.5134(6) | 6.9225(4) | 8.4283(3) | 10.484(3) |
| b, Å | 20.2976(11) | 12.6080(7) | 12.7194(4) | 23.392(6) |
| c, Å | 20.5065(7) | 15.2450(7) | 24.0128(8) | 13.186(3) |
| α, deg | 90 | 77.178(4) | 90 | 90 |
| β, deg | 90.120(3) | 88.607(4) | 93.708(3) | 105.978(7) |
| γ, deg | 90 | 89.549(4) | 90 | 90 |
| V, Å3 | 5208.5(4) | 1297.00(12) | 2568.85(15) | 3109.0(13) |
| ρcalcd, g cm–3 | 1.338 | 1.423 | 1.359 | 1.249 |
| Z | 8 | 2 | 4 | 4 |
| T, K | 90(2) | 90(2) | 90(2) | 100(2) |
| μ, mm–1 | 0.162 (synchrotron) | 0.174 (synchrotron) | 0.166 (synchrotron) | 0.051 (synchrotron) |
| no. of reflns | 28 220 | 10 876 | 13 798 | 67 796 |
| no. of unique reflns | 9142 | 4637 | 4646 | 13 930 |
| variables | 691 | 363 | 345 | 781 |
| λ, Å | 0.78228 (synchrotron) | 0.78192 (synchrotron) | 0.78228 (synchrotron) | 0.4299 (synchrotron) |
| R1 [I > 2σ(I)] | 0.0631 | 0.0549 | 0.0488 | 0.0719 |
| wR2 [I > 2σ(I)] | 0.1503 | 0.1374 | 0.1086 | 0.2013 |
| GOF | 1.101 | 1.126 | 1.187 | 1.050 |
| [decc][PS] | |
|---|---|
| formula | C41H34N2O3S·CH3OH |
| fw | 666.80 |
| crystal size, mm | 0.30 × 0.22 × 0.10 |
| crystal system | monoclinic |
| space group | P21/n (no. 14) |
| a, Å | 14.4690(15) |
| b, Å | 14.4551(12) |
| c, Å | 18.1193(17) |
| α, deg | 90 |
| β, deg | 104.764(3) |
| γ, deg | 90 |
| V, Å3 | 3664.5(6) |
| ρcalcd, g cm–3 | 1.345 |
| Z | 4 |
| T, K | 287(2) |
| μ, mm–1 | 0.132 (Mo Kα) |
| no. of reflns | 35 126 |
| no. of unique reflns | 8334 |
| variables | 445 |
| λ, Å | 0.71075 (Mo Kα) |
| R1 [I > 2σ(I)] | 0.0971 |
| wR2 [I > 2σ(I)] | 0.2389 |
| GOF | 0.921 |