Table 3.
Summary of X-ray Crystallographic Data Collection and Structure Refinement
| 1A • CH2Cl2 | 1B • 2CH2Cl2 a | 1C | 1D • [HNEt3]OTf | 1F | 2E•2Et2O | [2F(MeCN)]•2DCE b | |
|---|---|---|---|---|---|---|---|
| empirical formula | C60H47BCl2FeN8O2 | C55H45BCl4FeN6O3 | C53H41BFeN6O2 | C59H57BF3FeN7O6S | C68H55BFeN8O2 | C106H96B2Fe2N12O6 | C104H87B2Cl4Fe2N13O2 |
| formula weight | 1049.62 | 1046.46 | 860.58 | 1115.84 | 1082.86 | 1767.27 | 1826.02 |
| crystal system | Monoclinic | Orthorhombic | Monoclinic | Triclinic | Monoclinic | Triclinic | Monoclinic |
| space group | P21/c | P212121 | P21/n | P -1 | P21/c | P -1 | Pn |
| a, Å | 14.5859(5) | 11.2362(4) | 10.4129(2) | 9.6832(4) | 17.8034(7) | 9.6359(10) | 13.4895(3) |
| b, Å | 13.6416(4) | 17.7643(6) | 30.8300(5) | 9.8868(5) | 22.3235(10) | 13.4413(14) | 10.0544(3) |
| c, Å | 25.2090(8) | 25.2782(8) | 13.1758(2) | 28.3671(15) | 13.6123(6) | 18.205(2) | 32.9607(9) |
| α, deg | 90 | 90 | 90 | 85.740(4) | 90 | 95.633(9) | 90 |
| β, deg | 93.779(3) | 90 | 90.634(2) | 86.952(4) | 99.746(4) | 105.298(10) | 96.806(3) |
| γ, deg | 90 | 90 | 90 | 81.003(4) | 90 | 99.002(9) | 90 |
| V, Å3 | 5005.0(3) | 5045.6(3) | 4229.6(1) | 2672.5(2) | 5331.9(4) | 2222.1(4) | 4438.9(2) |
| Z | 4 | 4 | 4 | 2 | 4 | 1 | 2 |
| Dcalc, g/cm3 | 1.393 | 1.351 | 1.351 | 1.387 | 1.349 | 1.321 | 1.342 |
| λ, Å | 1.5418 | 1.5418 | 0.7107 | 1.5418 | 0.7107 | 1.5418 | 1.5418 |
| μ, mm−1 | 3.831 | 4.518 | 0.408 | 3.209 | 0.340 | 3.131 | 4.018 |
| θ-range, deg | 7 to 148 | 7 to 148 | 7 to 59 | 9 to 148 | 7 to 59 | 7 to 148 | 7 to 148 |
| reflections collected | 35336 | 19096 | 58359 | 15029 | 62124 | 15573 | 23318 |
| independent reflections | 9913 [Rint = 0.0382] | 8984 [Rint = 0.0435] | 10931 [Rint = 0.0402] | 15029 | 13600 [Rint = 0.0409] | 8687 [Rint = 0.0622] | 12059 [Rint = 0.0406] |
| data / restraints / parameters | 9913 / 0 / 672 | 8984/0/634 | 10931 /0 / 569 | 15029 / 0 / 709 | 13600 / 0 / 731 | 8687 / 24 / 569 | 12059 / 31 / 1132 |
| GOF (on F2) | 1.041 | 1.103 | 1.027 | 1.074 | 1.058 | 1.026 | 1.024 |
| R1/wR2 (I > 2σ(I)) c | 0.0354 / 0.0891 | 0.0814 / 0.2410 | 0.0375 / 0.0891 | 0.0864 / 0.2278 | 0.0414 / 0.1005 | 0.0718 / 0.1807 | 0.0638 / 0.1662 |
| R1/wR2 (all data) c | 0.0449 / 0.0954 | 0.0838 / 0.2437 | 0.0462 / 0.0953 | 0.1008 / 0.2402 | 0.0552 / 0.1083 | 0.1152 / 0.2227 | 0.0821 / 0.1826 |
a
One of the solvate molecules in 1B • 2CH2Cl2 is only partially (77%) populated.
b
One of the solvate molecules in [2F(MeCN)]• 2DCE is only partially (68%) populated.
c
R1 = Σ ||Fo| − |Fc|| / Σ|Fo|; wR2 = [Σw(Fo2 − Fc2)2 / Σw(Fo2)2]1/2