Table 2. Crystal data and refinement quality indicators for the five determinations of the structure of (nBu4N)[Co(Or)2(bipy)]·3H2O, (2).
Molecular formula C36H54CoN7O11 or (C16H36N)[Co(C5H2N2O4)2(C10H8N2)2]·3H2O; M r = 819.79.
| Structure | (2a) | (2b) | (2c) | (2d) | (2e) |
|---|---|---|---|---|---|
| CCDC reference | 1560739 | 1560740 | 1560741 | 1560742 | 1560743 |
| Crystal | 1 | 1 | 2 | 2 | |
| Crystal history | as prepared | after one transition monoclinic to triclinic | following one full cycle monoclinic to triclinic to monoclinic | following 1.5 full cycles, monoclinic to triclinic to monoclinic to mixed monoclinic/triclinic | |
| T (K) | 277 (1) | 100 (1) | 220 (1) | 170 (1) | 170 (1) |
| Crystal condition | single | twin | single | multicrystal | |
| Crystal system | monoclinic | triclinic | monoclinic | monoclinic | triclinic |
| Space group | P2/n |
P
|
P2/n | P2/n |
P
|
| Z | 2 | 2 | 2 | 2 | 2 |
| Ha (H2O, N—H) located and refined | xyz and U iso refined | no | xyz and U iso refined | xyz refined and U iso constrained | xyz refined and U iso constrained |
| Resolutionb (Å) | 0.84 | 0.78 | 0.77 | 0.77 | 0.84 |
| No. data, total | 10924 | 15136 | 21720 | 22527 | 25546 |
| Independent data | 4564 | 15136 | 4673 | 4643 | 6796 |
| R int | 0.0664 | twinc | 0.0499 | 0.1647 | 0.1521 |
| Parameters | 264 | 501 | 264 | 282 | 524 |
| Restraints | 0 | 0 | 0 | 39 | 0 |
| R1 [F 2 > 2σ(F 2] | 0.0549 | 0.0949 | 0.0480 | 0.0664 | 0.0617 |
| wR2 (all data used) | 0.1100 | 0.2481 | 0.1294 | 0.1646 | 0.1608 |
| Quality-of-fit | 1.021 | 1.439 | 1.070 | 1.075 | 1.052 |
| a (Å) | 13.1679 (12) | 12.9054 (8) | 13.0259 (4) | 13.0080 (8) | 13.0155 (15) |
| b (Å) | 9.3413 (9) | 9.3791 (8) | 9.3504 (3) | 9.3320 (6) | 9.4028 (14) |
| c (Å) | 16.3388 (14) | 16.1290 (12) | 16.3308 (5) | 16.3753 (12) | 16.2640 (17) |
| α (°) | 90 | 88.724 (6) | 90 | 90 | 88.794 (11) |
| β (°) | 102.669 (9) | 102.898 (6) | 103.847 (3) | 104.364 (7) | 103.054 (9) |
| γ (°) | 90 | 88.528 (6) | 90 | 90 | 88.687 (11) |
| V, Å3 | 1960.8 (3) | 1901.6 (2) | 1931.24 (11) | 1925.7 (2) | 1937.8 (4) |
| Δρmax,Δρmin (e Å−3) | 0.478, −0.309 | 2.876, −0.771 | 1.044, −0.915 | 0.741, −0.731 | 1.630, −0.899 |
Notes: (a) H atoms bonded to O or N atoms. Whether or not these H atoms are located and refined is an indicator for the reliability of the structure analysis. (b) Resolution is estimated as the minimum Bragg spacing to which data are at least 95% complete, based on the Laue group. (c) Structure (2b) was refined using data from two domains in the same refinement. Traditional data merging was not performed. Computer programs: CrysAlis CCD (Oxford Diffraction, 2006 ▸), CrysAlis RED (Oxford Diffraction, 2006 ▸, 2009 ▸), CrysAlis PRO (Agilent, 2011 ▸), SIR92 (Altomare et al., 1994 ▸), SHELXL2014 (Sheldrick, 2015 ▸) and DIAMOND (Brandenburg & Putz, 2004 ▸).