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. 2018 Jan 17;644(3):149–154. doi: 10.1002/zaac.201700424

Table 1.

Crystallographic data and structure refinement for L and 1a1f

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 6.6655(6) 9.5823(9) 9.6779(7) 8.7345(5) 8.6833(7) 12.8952(5) 6.6921(6)
b 8.1466(6) 23.451(2) 23.5561(9) 10.0870(6) 21.923(2) 12.8952(5) 8.3224(8)
c 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