| Identification code | mo_B0093_0m |
| Empirical formula | C21H27FeNO2Si |
| Formula weight | 409.37 |
| Temperature/K | 100.01 |
| Crystal system | orthorhombic |
| Space group | P212121 |
| a/Å | 7.6971(9) |
| b/Å | 10.4780(9) |
| c/Å | 24.508(3) |
| α/° | 90 |
| β/° | 90 |
| γ/° | 90 |
| Volume/Å3 | 1976.6(4) |
| Z | 4 |
| ρcalcg/cm3 | 1.376 |
| μ/mm‑1 | 0.838 |
| F(000) | 864.0 |
| Crystal size/mm3 | 0.3 × 0.2 × 0.02 |
| Radiation | MoKα (λ = 0.71073) |
| 2Θ range for data collection/° | 5.548 to 57.99 |
| Index ranges | -10 ≤ h ≤ 8, -10 ≤ k ≤ 14, -27 ≤ l ≤ 33 |
| Reflections collected | 15827 |
| Independent reflections | 5236 [Rint = 0.0171, Rsigma = 0.0185] |
| Data/restraints/parameters | 5236/0/239 |
| Goodness-of-fit on F2 | 1.105 |
| Final R indexes [I>=2σ (I)] | R1 = 0.0201, wR2 = 0.0523 |
| Final R indexes [all data] | R1 = 0.0207, wR2 = 0.0525 |
| Largest diff. peak/hole / e Å-3 | 0.29/-0.44 |
| Flack parameter | -0.001(3) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| Fe1 | 2658.6(3) | 4014.3(2) | 7365.3(2) | 9.42(6) |
| Si1 | 5195.2(6) | 4475.7(4) | 6174.9(2) | 10.84(9) |
| O1 | 6299.4(17) | 3573.1(13) | 5755.3(5) | 16.9(3) |
| O2 | 6412.1(16) | 5617.0(13) | 6428.4(5) | 15.8(2) |
| N1 | 2989.3(19) | 1177.2(13) | 6021.8(6) | 12.4(3) |
| C1 | 4508(2) | 3577.9(15) | 6785.7(6) | 9.8(3) |
| C2 | 3242(2) | 2564.9(15) | 6836.5(7) | 10.1(3) |
| C3 | 3267(2) | 2117.7(15) | 7388.1(7) | 12.1(3) |
| C4 | 4520(2) | 2836.6(15) | 7684.0(7) | 12.4(3) |
| C5 | 5287(2) | 3732.2(15) | 7318.8(7) | 11.0(3) |
| C6 | 1518(3) | 5731.2(18) | 7186.5(8) | 21.9(4) |
| C7 | 278(3) | 4729(2) | 7158.6(10) | 30.6(5) |
| C8 | 207(2) | 4133.7(18) | 7678.7(10) | 29.2(5) |
| C9 | 1394(3) | 4766.1(17) | 8024.9(8) | 20.8(4) |
| C10 | 2201(2) | 5752.4(15) | 7722.5(7) | 16.2(3) |
| C11 | 2084(2) | 2054.2(15) | 6395.3(7) | 12.1(3) |
| C12 | 3615(2) | 51.8(17) | 6309.4(7) | 16.1(3) |
| C13 | 1802(3) | 797.1(18) | 5583.8(7) | 18.7(4) |
| C14 | 7627(3) | 2738(2) | 5937.6(8) | 32.0(5) |
| C15 | 7554(3) | 6364(2) | 6102.4(8) | 26.2(4) |
| C16 | 3471(2) | 5162.3(17) | 5731.9(7) | 13.3(3) |
| C17 | 2949(2) | 6434.9(17) | 5788.3(7) | 16.6(3) |
| C18 | 1663(3) | 6955.5(19) | 5456.9(8) | 19.6(4) |
| C19 | 867(2) | 6208.3(19) | 5061.7(8) | 20.9(4) |
| C20 | 1360(3) | 4938(2) | 4995.8(8) | 21.0(4) |
| C21 | 2667(2) | 4430.7(17) | 5324.3(6) | 17.1(3) |
| Atom | U11 | U22 | U33 | U23 | U13 | U12 |
|---|---|---|---|---|---|---|
| Fe1 | 8.37(10) | 8.79(10) | 11.11(10) | -1.31(8) | 1.27(8) | 0.92(8) |
| Si1 | 9.6(2) | 14.07(19) | 8.80(18) | 0.91(16) | 0.66(15) | -0.61(16) |
| O1 | 14.6(6) | 23.7(6) | 12.5(6) | -1.5(5) | 1.9(5) | 3.5(5) |
| O2 | 15.3(6) | 18.8(6) | 13.3(5) | 1.2(5) | 1.0(5) | -6.9(5) |
| N1 | 14.2(7) | 12.6(6) | 10.4(6) | -2.2(5) | -0.4(5) | 0.1(5) |
| C1 | 8.8(7) | 11.3(6) | 9.3(7) | -0.8(5) | 0.5(5) | 0.8(6) |
| C2 | 9.9(7) | 9.2(6) | 11.2(7) | -1.9(5) | 1.1(5) | 1.3(5) |
| C3 | 13.7(7) | 10.1(6) | 12.5(7) | 0.6(6) | 2.8(6) | 2.2(5) |
| C4 | 13.8(7) | 12.7(6) | 10.8(7) | 1.1(6) | -0.1(6) | 3.6(6) |
| C5 | 9.0(6) | 13.0(6) | 10.9(7) | -1.1(5) | -0.1(6) | 1.8(5) |
| C6 | 26.7(10) | 18.7(9) | 20.5(8) | 0.4(7) | 3.6(7) | 13.6(7) |
| C7 | 16.4(9) | 32.6(11) | 42.9(12) | -21.9(9) | -11.4(8) | 15.4(8) |
| C8 | 12.9(8) | 16.3(8) | 58.4(14) | -9.9(9) | 16.8(9) | -1.3(7) |
| C9 | 25.1(10) | 16.9(8) | 20.5(8) | -0.1(7) | 12.3(7) | 7.5(7) |
| C10 | 14.8(7) | 11.9(7) | 22.0(8) | -5.6(6) | 4.0(6) | 1.7(6) |
| C11 | 10.9(7) | 11.8(7) | 13.7(7) | -1.1(6) | -0.2(6) | 0.1(6) |
| C12 | 19.5(8) | 13.1(8) | 15.7(8) | -1.5(6) | 1.1(6) | 2.3(7) |
| C13 | 22.2(9) | 19.4(8) | 14.3(7) | -3.7(6) | -4.2(6) | -1.1(7) |
| C14 | 28.9(11) | 42.2(12) | 24.8(9) | -11.3(9) | -6.1(9) | 19.5(10) |
| C15 | 24.6(10) | 29.8(9) | 24.2(9) | 5.2(7) | 3.5(8) | -14.2(9) |
| C16 | 11.9(7) | 17.7(8) | 10.4(7) | 3.4(6) | 0.6(6) | -1.2(6) |
| C17 | 16.6(9) | 15.2(7) | 17.8(8) | 3.0(6) | -0.5(6) | -3.7(6) |
| C18 | 17.9(9) | 17.8(8) | 23.2(9) | 7.3(7) | 1.1(7) | 1.3(7) |
| C19 | 16.6(8) | 28.3(10) | 17.9(8) | 7.0(7) | -1.6(7) | 4.4(7) |
| C20 | 20.3(9) | 29.0(9) | 13.7(7) | -1.7(7) | -5.0(7) | 1.7(7) |
| C21 | 18.5(8) | 19.3(7) | 13.5(7) | -0.6(6) | -1.3(7) | 1.5(7) |
| Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
|---|---|---|---|---|---|---|
| Fe1 | C1 | 2.0624(16) | N1 | C13 | 1.465(2) | |
| Fe1 | C2 | 2.0465(16) | C1 | C2 | 1.447(2) | |
| Fe1 | C3 | 2.0424(16) | C1 | C5 | 1.447(2) | |
| Fe1 | C4 | 2.0458(16) | C2 | C3 | 1.431(2) | |
| Fe1 | C5 | 2.0482(16) | C2 | C11 | 1.500(2) | |
| Fe1 | C6 | 2.0492(18) | C3 | C4 | 1.422(2) | |
| Fe1 | C7 | 2.044(2) | C4 | C5 | 1.425(2) | |
| Fe1 | C8 | 2.0413(18) | C6 | C7 | 1.420(3) | |
| Fe1 | C9 | 2.0447(18) | C6 | C10 | 1.415(3) | |
| Fe1 | C10 | 2.0511(15) | C7 | C8 | 1.420(4) | |
| Si1 | O1 | 1.6352(13) | C8 | C9 | 1.412(3) | |
| Si1 | O2 | 1.6412(13) | C9 | C10 | 1.415(3) | |
| Si1 | C1 | 1.8454(17) | C16 | C17 | 1.400(2) | |
| Si1 | C16 | 1.8593(18) | C16 | C21 | 1.403(2) | |
| O1 | C14 | 1.418(2) | C17 | C18 | 1.392(3) | |
| O2 | C15 | 1.423(2) | C18 | C19 | 1.388(3) | |
| N1 | C11 | 1.472(2) | C19 | C20 | 1.393(3) | |
| N1 | C12 | 1.456(2) | C20 | C21 | 1.394(3) |
| Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|
| C2 | Fe1 | C1 | 41.22(6) | C14 | O1 | Si1 | 122.24(12) | |
| C2 | Fe1 | C5 | 68.96(6) | C15 | O2 | Si1 | 122.76(12) | |
| C2 | Fe1 | C6 | 127.59(7) | C12 | N1 | C11 | 111.16(13) | |
| C2 | Fe1 | C10 | 165.22(7) | C12 | N1 | C13 | 109.93(14) | |
| C3 | Fe1 | C1 | 69.20(6) | C13 | N1 | C11 | 109.26(13) | |
| C3 | Fe1 | C2 | 40.97(6) | Si1 | C1 | Fe1 | 130.06(9) | |
| C3 | Fe1 | C4 | 40.72(6) | C2 | C1 | Fe1 | 68.80(9) | |
| C3 | Fe1 | C5 | 68.57(6) | C2 | C1 | Si1 | 129.56(12) | |
| C3 | Fe1 | C6 | 163.38(8) | C2 | C1 | C5 | 106.49(14) | |
| C3 | Fe1 | C7 | 124.69(8) | C5 | C1 | Fe1 | 68.87(9) | |
| C3 | Fe1 | C9 | 117.54(7) | C5 | C1 | Si1 | 123.83(12) | |
| C3 | Fe1 | C10 | 153.08(7) | C1 | C2 | Fe1 | 69.98(9) | |
| C4 | Fe1 | C1 | 69.26(6) | C1 | C2 | C11 | 126.89(15) | |
| C4 | Fe1 | C2 | 68.93(7) | C3 | C2 | Fe1 | 69.36(9) | |
| C4 | Fe1 | C5 | 40.74(6) | C3 | C2 | C1 | 108.20(14) | |
| C4 | Fe1 | C6 | 155.68(8) | C3 | C2 | C11 | 124.91(15) | |
| C4 | Fe1 | C10 | 119.54(7) | C11 | C2 | Fe1 | 126.23(11) | |
| C5 | Fe1 | C1 | 41.21(6) | C2 | C3 | Fe1 | 69.67(9) | |
| C5 | Fe1 | C6 | 122.56(8) | C4 | C3 | Fe1 | 69.77(9) | |
| C5 | Fe1 | C10 | 108.77(7) | C4 | C3 | C2 | 108.52(14) | |
| C6 | Fe1 | C1 | 110.07(7) | C3 | C4 | Fe1 | 69.51(9) | |
| C6 | Fe1 | C10 | 40.37(7) | C3 | C4 | C5 | 108.03(14) | |
| C7 | Fe1 | C1 | 121.97(8) | C5 | C4 | Fe1 | 69.72(9) | |
| C7 | Fe1 | C2 | 108.17(7) | C1 | C5 | Fe1 | 69.92(9) | |
| C7 | Fe1 | C4 | 160.69(9) | C4 | C5 | Fe1 | 69.54(9) | |
| C7 | Fe1 | C5 | 157.68(9) | C4 | C5 | C1 | 108.76(14) | |
| C7 | Fe1 | C6 | 40.61(9) | C7 | C6 | Fe1 | 69.49(11) | |
| C7 | Fe1 | C9 | 68.15(9) | C10 | C6 | Fe1 | 69.89(10) | |
| C7 | Fe1 | C10 | 68.04(7) | C10 | C6 | C7 | 107.82(18) | |
| C8 | Fe1 | C1 | 155.62(8) | C6 | C7 | Fe1 | 69.90(11) | |
| C8 | Fe1 | C2 | 119.11(8) | C8 | C7 | Fe1 | 69.56(11) | |
| C8 | Fe1 | C3 | 105.15(7) | C8 | C7 | C6 | 107.90(18) | |
| C8 | Fe1 | C4 | 122.73(8) | C7 | C8 | Fe1 | 69.75(12) | |
| C8 | Fe1 | C5 | 160.59(9) | C9 | C8 | Fe1 | 69.91(10) | |
| C8 | Fe1 | C6 | 68.31(8) | C9 | C8 | C7 | 107.95(17) | |
| C8 | Fe1 | C7 | 40.69(10) | C8 | C9 | Fe1 | 69.65(11) | |
| C8 | Fe1 | C9 | 40.44(9) | C8 | C9 | C10 | 108.17(17) | |
| C8 | Fe1 | C10 | 68.04(7) | C10 | C9 | Fe1 | 70.03(10) | |
| C9 | Fe1 | C1 | 163.43(8) | C6 | C10 | Fe1 | 69.74(10) | |
| C9 | Fe1 | C2 | 153.00(7) | C6 | C10 | C9 | 108.17(17) | |
| C9 | Fe1 | C4 | 105.30(8) | C9 | C10 | Fe1 | 69.54(10) | |
| C9 | Fe1 | C5 | 124.74(8) | N1 | C11 | C2 | 112.92(13) | |
| C9 | Fe1 | C6 | 68.09(8) | C17 | C16 | Si1 | 121.06(13) | |
| C9 | Fe1 | C10 | 40.43(7) | C17 | C16 | C21 | 117.65(16) | |
| C10 | Fe1 | C1 | 127.55(7) | C21 | C16 | Si1 | 121.29(13) | |
| O1 | Si1 | O2 | 111.28(7) | C18 | C17 | C16 | 121.34(17) | |
| O1 | Si1 | C1 | 111.36(7) | C19 | C18 | C17 | 119.99(18) | |
| O1 | Si1 | C16 | 103.15(7) | C18 | C19 | C20 | 119.99(17) | |
| O2 | Si1 | C1 | 103.17(7) | C19 | C20 | C21 | 119.61(18) | |
| O2 | Si1 | C16 | 110.27(8) | C20 | C21 | C16 | 121.41(17) | |
| C1 | Si1 | C16 | 117.80(8) |
| A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|---|---|
| Fe1 | C1 | C2 | C3 | -59.02(11) | C1 | C2 | C11 | N1 | 78.4(2) | |
| Fe1 | C1 | C2 | C11 | 120.86(16) | C2 | C1 | C5 | Fe1 | -58.75(11) | |
| Fe1 | C1 | C5 | C4 | 58.85(11) | C2 | C1 | C5 | C4 | 0.10(18) | |
| Fe1 | C2 | C3 | C4 | -59.13(11) | C2 | C3 | C4 | Fe1 | 59.07(11) | |
| Fe1 | C2 | C11 | N1 | 169.49(11) | C2 | C3 | C4 | C5 | -0.21(17) | |
| Fe1 | C3 | C4 | C5 | -59.28(11) | C3 | C2 | C11 | N1 | -101.74(18) | |
| Fe1 | C4 | C5 | C1 | -59.09(11) | C3 | C4 | C5 | Fe1 | 59.15(11) | |
| Fe1 | C6 | C7 | C8 | 59.41(13) | C3 | C4 | C5 | C1 | 0.06(18) | |
| Fe1 | C6 | C10 | C9 | -59.12(12) | C5 | C1 | C2 | Fe1 | 58.79(11) | |
| Fe1 | C7 | C8 | C9 | 59.71(13) | C5 | C1 | C2 | C3 | -0.23(18) | |
| Fe1 | C8 | C9 | C10 | 59.67(12) | C5 | C1 | C2 | C11 | 179.65(14) | |
| Fe1 | C9 | C10 | C6 | 59.25(12) | C6 | C7 | C8 | Fe1 | -59.62(13) | |
| Si1 | C1 | C2 | Fe1 | -125.09(14) | C6 | C7 | C8 | C9 | 0.1(2) | |
| Si1 | C1 | C2 | C3 | 175.88(12) | C7 | C6 | C10 | Fe1 | 59.36(13) | |
| Si1 | C1 | C2 | C11 | -4.2(3) | C7 | C6 | C10 | C9 | 0.2(2) | |
| Si1 | C1 | C5 | Fe1 | 124.86(12) | C7 | C8 | C9 | Fe1 | -59.61(13) | |
| Si1 | C1 | C5 | C4 | -176.29(11) | C7 | C8 | C9 | C10 | 0.1(2) | |
| Si1 | C16 | C17 | C18 | 179.82(14) | C8 | C9 | C10 | Fe1 | -59.43(12) | |
| Si1 | C16 | C21 | C20 | 179.25(15) | C8 | C9 | C10 | C6 | -0.2(2) | |
| O1 | Si1 | O2 | C15 | 45.22(17) | C10 | C6 | C7 | Fe1 | -59.61(12) | |
| O1 | Si1 | C1 | Fe1 | -164.13(10) | C10 | C6 | C7 | C8 | -0.2(2) | |
| O1 | Si1 | C1 | C2 | -69.44(16) | C11 | C2 | C3 | Fe1 | -120.48(15) | |
| O1 | Si1 | C1 | C5 | 106.07(14) | C11 | C2 | C3 | C4 | -179.61(14) | |
| O1 | Si1 | C16 | C17 | -140.64(14) | C12 | N1 | C11 | C2 | 62.45(18) | |
| O1 | Si1 | C16 | C21 | 38.38(16) | C13 | N1 | C11 | C2 | -176.05(14) | |
| O2 | Si1 | O1 | C14 | 69.61(18) | C16 | Si1 | O1 | C14 | -172.18(16) | |
| O2 | Si1 | C1 | Fe1 | 76.42(12) | C16 | Si1 | O2 | C15 | -68.62(16) | |
| O2 | Si1 | C1 | C2 | 171.11(15) | C16 | Si1 | C1 | Fe1 | -45.29(14) | |
| O2 | Si1 | C1 | C5 | -13.38(15) | C16 | Si1 | C1 | C2 | 49.40(18) | |
| O2 | Si1 | C16 | C17 | -21.73(16) | C16 | Si1 | C1 | C5 | -135.09(13) | |
| O2 | Si1 | C16 | C21 | 157.30(13) | C16 | C17 | C18 | C19 | 0.1(3) | |
| C1 | Si1 | O1 | C14 | -44.90(18) | C17 | C16 | C21 | C20 | -1.7(3) | |
| C1 | Si1 | O2 | C15 | 164.73(15) | C17 | C18 | C19 | C20 | -0.1(3) | |
| C1 | Si1 | C16 | C17 | 96.26(15) | C18 | C19 | C20 | C21 | -0.8(3) | |
| C1 | Si1 | C16 | C21 | -84.72(16) | C19 | C20 | C21 | C16 | 1.7(3) | |
| C1 | C2 | C3 | Fe1 | 59.41(11) | C21 | C16 | C17 | C18 | 0.8(3) | |
| C1 | C2 | C3 | C4 | 0.27(18) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| H3 | 2565 | 1453 | 7532 | 15 |
| H4 | 4796 | 2737 | 8059 | 15 |
| H5 | 6166 | 4332 | 7410 | 13 |
| H6 | 1833 | 6288 | 6897 | 26 |
| H7 | -387 | 4499 | 6847 | 37 |
| H8 | -512 | 3433 | 7776 | 35 |
| H9 | 1614 | 4564 | 8396 | 25 |
| H10 | 3053 | 6329 | 7856 | 19 |
| H11A | 1094 | 1600 | 6565 | 15 |
| H11B | 1609 | 2778 | 6183 | 15 |
| H12A | 2629 | -399 | 6474 | 24 |
| H12B | 4428 | 312 | 6596 | 24 |
| H12C | 4209 | -515 | 6052 | 24 |
| H13A | 2407 | 226 | 5331 | 28 |
| H13B | 1406 | 1558 | 5387 | 28 |
| H13C | 798 | 354 | 5741 | 28 |
| H14A | 8530 | 2672 | 5657 | 48 |
| H14B | 7133 | 1891 | 6007 | 48 |
| H14C | 8137 | 3073 | 6275 | 48 |
| H15A | 6894 | 6772 | 5808 | 39 |
| H15B | 8454 | 5814 | 5945 | 39 |
| H15C | 8099 | 7022 | 6329 | 39 |
| H17 | 3484 | 6954 | 6058 | 20 |
| H18 | 1329 | 7822 | 5501 | 24 |
| H19 | -13 | 6563 | 4836 | 25 |
| H20 | 808 | 4421 | 4729 | 25 |
| H21 | 3020 | 3571 | 5271 | 21 |
Experimental
Single crystals of C21H27FeNO2Si [mo_B0093_0m] were []. A suitable crystal was selected and [] on a 'Bruker APEX-II CCD' diffractometer. The crystal was kept at 100.01 K during data collection. Using Olex2 [1], the structure was solved with the XT [2] structure solution program using Direct Methods and refined with the XL [3] refinement package using Least Squares minimisation.
Crystal structure determination of [mo_B0093_0m]
Crystal Data for C21H27FeNO2Si (M =409.37 g/mol): orthorhombic, space group P212121 (no. 19), a = 7.6971(9) Å, b = 10.4780(9) Å, c = 24.508(3) Å, V = 1976.6(4) Å3, Z = 4, T = 100.01 K, μ(MoKα) = 0.838 mm-1, Dcalc = 1.376 g/cm3, 15827 reflections measured (5.548° ≤ 2Θ ≤ 57.99°), 5236 unique (Rint = 0.0171, Rsigma = 0.0185) which were used in all calculations. The final R1 was 0.0201 (I > 2σ(I)) and wR2 was 0.0525 (all data).
Refinement model description
Number of restraints - 0, number of constraints - unknown.
Details:
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
C11(H11A,H11B)
2.b Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C17(H17),
C18(H18), C19(H19), C20(H20), C21(H21)
2.c Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,
H15C)
This report has been created with Olex2, compiled on 2017.01.04 svn.r3372 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.