Table 1.
Crystal data and structure refinement for [HIPTN3N]V(THF) and [HIPTN3N]V(NH3).
| [HIPTN3N]V(THF) | [HIPTN3N]V(NH3) | |
|---|---|---|
| Empirical formula | C132H199N4OV | C121H178N5V |
| Formula weight | 1908.89 | 1753.62 |
| Temperature | 100(2) K | 193(2) K |
| Crystal system | Triclinic | Monoclinic |
| Space group | P1̄ | Cc |
| Unit cell dimensions | a = 17.7727(6) Å | a = 16.1153(4) Å |
| b = 18.3700(7) Å | b = 39.7548(11) Å | |
| c = 21.2032(9) Å | c = 18.0197(5) Å | |
| a= 113.9930(10)° | a = 90° | |
| b= 99.8920(10)° | b = 93.0540(10)° | |
| g = 96.5660(10)° | g = 90° | |
| Volume | 6098.5(4) Å3 | 11528.1(5) Å3 |
| Z | 2 | 4 |
| Density (calculated) | 1.040 Mg/m3 | 1.010 Mg/m3 |
| Absorption coefficient | 0.130 mm−1 | 0.132 mm−1 |
| F(000) | 2100 | 3848 |
| Crystal size | 0.20 × 0.20 × 0.08 mm3 | 0.20 × 0.17 × 0.10 mm3 |
| Theta range for data collection | 1.40 to 28.28° | 1.99 to 25.03° |
| Index ranges | −23<=h<=23 | −18<=h<=19 |
| −24<=k<=24 | −47<=k<=41 | |
| −28<=l<=27 | −21<=l<=13 | |
| Reflections collected | 127420 | 29563 |
| Independent reflections | 30238 [R(int) = 0.0638] | 15469 [R(int) = 0.0305] |
| Completeness to theta = (x°) | 99.9 % (28.28) | 99.9 % (25.03) |
| Max. and min. transmission | 0.9897 and 0.9745 | 0.9869 and 0.9741 |
| Data/restraints/parameters | 30238/397/1243 | 15469/3023/1536 |
| Goodness-of-fit on F2 | 1.043 | 1.015 |
| Final R indices [I>2sigma(I)] | R1 = 0.0696, wR2 = 0.1764 | R1 = 0.0584, wR2 = 0.1452 |
| R indices (all data) | R1 = 0.1069, wR2 = 0.2005 | R1 = 0.0766, wR2 = 0.1585 |
| Largest diff. peak and hole | 0.896 and −0.562 e.Å−3 | 0.317 and −0.268 e.Å−3 |
a
In all cases the wavelength was 0.71073 Å, the absorption correction was semi-empirical from equivalents, and the refinement method was full-matrix least-squares on F2.