Table 1.
L | 1a | 1b | 1c | 1d | 1e | 1f | |
---|---|---|---|---|---|---|---|
Empirical formula | C18H24O6P2 | C36H48LaN3O21P4 | C36H48CeN3O21P4 | C27H36N3O18P3Sm | C27H36EuN3O18P3 | C36H48CaN2O18P4 | C18H24N2O14P2U |
Formula weight | 398.31 | 1121.56 | 1122.77 | 933.85 | 935.46 | 960.72 | 792.36 |
Crystal description | colorless plate | colorless plate | colorless block | colorless plate | colorless plate | colorless block | colorless block |
Crystal size /mm | 0.220 × 0.160 × 0.040 | 0.160 × 0.060 × 0.020 | 0.230 × 0.127 × 0.070 | 0.140 × 0.060 × 0.020 | 0.110 × 0.060 × 0.010 | 0.250 × 0.200 × 0.200 | 0.160 × 0.120 × 0.060 |
Crystal system | triclinic | monoclinic | monoclinic | triclinic | triclinic | tetragonal | triclinic |
Space group | P 1 | P21 | P21 | P 1 | P 1 | I 42d | P 1 |
Radiation and λ /Å | Mo‐K α 0.71073 | Mo‐K α 0.71073 | Mo‐K α 0.71073 | Mo‐K α 0.71073 | Mo‐K α 0.71073 | Mo‐K α 0.71073 | Mo‐K α 0.71073 |
Monochromator | Graded multilayer mirror | plane graphite | plane graphite | plane graphite | plane graphite | plane graphite | plane graphite |
Temperature /K | 100(2) | 100(2) | 100(2) | 100(2) | 100(2) | 100(2) | 100(2) |
Unit cell dimensions | |||||||
a /Å | 6.6655(6) | 9.5823(9) | 9.6779(7) | 8.7345(5) | 8.6833(7) | 12.8952(5) | 6.6921(6) |
b /Å | 8.1466(6) | 23.451(2) | 23.5561(9) | 10.0870(6) | 21.923(2) | 12.8952(5) | 8.3224(8) |
c /Å | 9.4308(8) | 9.9136(9) | 10.0275(6) | 21.8040(14) | 10.0974(9) | 25.7346(11) | 11.9449(10) |
α /° | 74.575(6) | 90 | 90 | 89.380(5) | 89.783(8) | 90 | 81.331(7) |
β /° | 74.846(7) | 91.913(7) | 92.229(6) | 89.143(5) | 114.055(6) | 90 | 85.401(7) |
γ /° | 74.344(6) | 90 | 90 | 66.245(4) | 90.593(7) | 90 | 85.992(8) |
Volume /ų | 465.32(7) | 2226.5(4) | 2284.3(2) | 1758.06(19) | 1755.2(3) | 4279.3(4) | 654.42(10) |
Z | 1 | 2 | 2 | 2 | 2 | 4 | 1 |
Calculated density | 1.421 | 1.673 | 1.632 | 1.764 | 1.770 | 1.491 | 2.011 |
F(000) | 210 | 1140 | 1142 | 940 | 942 | 2008 | 380 |
Linear absorption coefficient μ /mm–1 | 0.266 | 1.188 | 1.219 | 1.889 | 2.006 | 0.374 | 6.393 |
Absorption correction | integration | integration | integration | integration | integration | integration | integration |
Unit cell determination | STOE X‐area | STOE X‐area | STOE X‐area | STOE X‐area | STOE X‐area | STOE X‐area | STOE X‐area |
Diffractometer | StadiVari | STOE IPDS 2 | STOE IPDS 2 | STOE IPDS 2 | STOE IPDS 2 | STOE IPDS 2 | STOE IPDS 2 |
Radiation source | Mo Genix | Genix Mo HF′ | Genix Mo HF | Genix Mo HF | Genix Mo HF | Genix Mo HF | Genix Mo HF |
Scan type | Omega scan | Omega scan | Omega scan | Omega scan | Omega scan | Omega scan | Omega scan |
Θ range for data collection | 2.29–31.67 | 1.74–26.44 | 1.73–26.28 | 1.87–26.25 | 1.86–25.14 | 1.59–26.19 | 1.73–26.28 |
Index ranges | –9 ≤ h ≤ 9 | –11 ≤ h ≤ 11 | –11 ≤ h ≤ 11 | –10 ≤ h ≤ 10 | –10 ≤ h ≤ 10 | –14 ≤ h ≤ 4 | –6 ≤ h ≤ 8 |
–11 ≤ k ≤ 11 | –28 ≤ k ≤ 28 | –28 ≤ k ≤ 28 | –10 ≤ k ≤ 12 | –26 ≤ k ≤ 26 | –15 ≤ k ≤ 15 | –10 ≤ k ≤ 10 | |
–13 ≤ l ≤ 13 | –12 ≤ l ≤ 12 | –12 ≤ l ≤ 12 | –26 ≤ l ≤ 26 | –12 ≤ l ≤ 12 | –31 ≤ l ≤ 27 | –14 ≤ l ≤ 14 | |
Refl. collected / unique | 6402 / 2617 | 15655 / 8357 | 16684 / 8577 | 13146 / 6603 | 13153 / 6614 | 5414 / 1934 | 4705 / 2448 |
Significant unique refl. | 2056 | 7103 | 7095 | 5530 | 3844 | 1782 | 2430 |
R(int), R(sigma) | 0.0370, 0.0470 | 0.0941, 0.0703 | 0.0477, 0.0505 | 0.0339, 0.0409 | 0.1150, 0.1390 | 0.0495, 0.0339 | 0.0307, 0.0277 |
Completeness to Θ = 26.0° | 0.839 | 0.968 | 0.995 | 0.990 | 0.984 | 0.996 | 0.992 |
Refinement method | SHELXL‐2014/7 | SHELXL‐2014/7 | SHELXL‐2014/7 | SHELXL‐2014/7 | SHELXL‐2014/7 | SHELXL‐2014/7 | SHELXL‐2014/7 |
Data/parameters/restraints | 2617 / 120 / 0 | 8357 / 516 / 1 | 8577 / 516 / 1 | 6603 / 533 / 0 | 6614 / 494 / 0 | 1934 / 111 / 0 | 2448 / 171 / 0 |
Goodness‐of‐fit on F 2 | 1.092 | 1.097 | 1.060 | 1.064 | 1.024 | 1.078 | 1.145 |
Final R indices [I > 2σ(I)] | 0.0453 | 0.0962 | 0.0610 | 0.0369 | 0.0878 | 0.1111 | 0.0259 |
R indices (all data) | 0.0633 | 0.1138 | 0.0744 | 0.0480 | 0.1470 | 0.1160 | 0.0267 |
Largest difference peak/hole /e·Å–3 | 0.763 / –0.330 | 2.581 / –2.899 | 1.590 / –1.188 | 1.512 / –1.495 | 1.369 / –2.378 | 1.282 / –0.827 | 0.922 / –1.253 |