Table 5. Crystal Data and Collection Parameters of [V(NR)Cl2(L)] [R = Ad (1), C6H5 (2), 2,6-Me2C6H3 (3); L = 2-(2′-Benzimidazolyl)-6-methylpyridyl]a.
| 1b | 2 | 3 | |
|---|---|---|---|
| formula | C24H27Cl4N4V | C19H15Cl2N4V | C42H38Cl4N8V2 |
| formula weight | 564.26 | 421.20 | 898.51 |
| crystal color, habit | red, block | red, plate | red, block |
| crystal size (mm) | 0.120 × 0.110 × 0.060 | 0.100 × 0.080 × 0.060 | 0.100 × 0.060 × 0.020 |
| crystal system | monoclinic | triclinic | orthorhombic |
| space group | P21 (#4) | P1̅ (#2) | P212121 (#19) |
| a (Å) | 8.3276(11) | 7.4884(7) | 7.2388(3) |
| b (Å) | 11.0967(15) | 9.3222(9) | 15.3494(8) |
| c (Å) | 13.592(2) | 13.6821(15) | 36.6025(16) |
| α (deg) | 70.369(10) | ||
| β (deg) | 99.934(4) | 87.341(8) | |
| γ (deg) | 88.592(8) | ||
| V (Å3) | 1237.2(3) | 898.60(17) | 4066.9(3) |
| Z value | 2 | 2 | 4 |
| Dcalcd (g/cm3) | 1.515 | 1.557 | 1.467 |
| F000 | 580.00 | 428.00 | 1840.00 |
| temp (K) | 93(2) | 93(2) | 93(2) |
| μ (Mo Kα) (cm–1) | 8.533 | 8.590 | 7.642 |
| no. of reflections measured (Rint) | total: 10 045, unique: 4251 (0.0327) | total: 7640, unique: 3837 (0.0756) | total: 31 734, unique: 8255 (0.1129) |
| 2θmax (deg) | 55.0 | 55.0 | 55.0 |
| no. of observations [I > 2.00σ(I)] | 4251 | 3837 | 8255 |
| no. of variables | 298 | 235 | 505 |
| R1 [I > 2.00σ(I)] | 0.0214 | 0.0730 | 0.0657 |
| wR2 [I > 2.00σ(I)] | 0.0538 | 0.1938 | 0.1595 |
| goodness of fit | 1.019 | 0.999 | 1.007 |
a
Structure reports and xyz files for complexes 1–3 are shown in the Supporting Information. CCDC reference numbers for 1–3 are 1544623–1544625, respectively.
b
Structure for 1 contains CH2Cl2.