| Identification code | 3160 |
| Empirical formula | C17H27FeNO2Si |
| Formula weight | 361.33 |
| Temperature/K | 173 |
| Crystal system | monoclinic |
| Space group | P21/c |
| a/Å | 12.2692(6) |
| b/Å | 16.7258(6) |
| c/Å | 18.2415(7) |
| α/° | 90 |
| β/° | 101.842(4) |
| γ/° | 90 |
| Volume/Å3 | 3663.7(3) |
| Z | 8 |
| ρcalcg/cm3 | 1.310 |
| μ/mm‑1 | 0.895 |
| F(000) | 1536.0 |
| Crystal size/mm3 | 0.095 × 0.082 × 0.04 |
| Radiation | MoKα (λ = 0.71073) |
| 2Θ range for data collection/° | 4.412 to 53.996 |
| Index ranges | -15 ≤ h ≤ 15, -21 ≤ k ≤ 21, -23 ≤ l ≤ 23 |
| Reflections collected | 74078 |
| Independent reflections | 7995 [Rint = 0.0712, Rsigma = 0.0434] |
| Data/restraints/parameters | 7995/4/423 |
| Goodness-of-fit on F2 | 1.037 |
| Final R indexes [I>=2σ (I)] | R1 = 0.0432, wR2 = 0.0861 |
| Final R indexes [all data] | R1 = 0.0671, wR2 = 0.0944 |
| Largest diff. peak/hole / e Å-3 | 0.43/-0.27 |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| Fe1 | 439.4(3) | 8174.3(2) | 3599.7(2) | 23.46(10) |
| Si1 | 1401.3(5) | 6179.6(4) | 3295.0(4) | 19.60(14) |
| O1 | 1170.2(13) | 5930.2(9) | 2404.6(9) | 21.5(4) |
| O2 | 2688.3(14) | 6466(1) | 3557.6(9) | 25.8(4) |
| N1 | -590.2(16) | 6640.9(13) | 1598.2(11) | 26.5(5) |
| C1 | 342.3(19) | 6957.7(13) | 3389.7(13) | 21.4(5) |
| C2 | -342.6(19) | 7402.4(14) | 2790.8(13) | 23.0(5) |
| C3 | -1136(2) | 7851.5(15) | 3085.5(14) | 27.6(6) |
| C4 | -962(2) | 7708.3(15) | 3865.5(14) | 28.7(6) |
| C5 | -66(2) | 7163.1(14) | 4053.7(14) | 25.0(5) |
| C6 | 1442(2) | 8905.1(15) | 3135.0(16) | 34.8(6) |
| C7 | 575(2) | 9353.4(15) | 3352.8(16) | 36.0(7) |
| C8 | 670(2) | 9254.0(15) | 4131.1(15) | 35.4(6) |
| C9 | 1585(2) | 8750.0(15) | 4405.0(16) | 34.9(6) |
| C10 | 2065(2) | 8535.8(16) | 3790.0(17) | 36.7(7) |
| C11 | -270(2) | 7414.2(15) | 1975.1(13) | 27.6(6) |
| C12 | -1707(2) | 6380.6(18) | 1667.8(16) | 40.1(7) |
| C13 | -512(2) | 6695.3(18) | 809.3(14) | 39.7(7) |
| C14 | 1267(2) | 5264.7(14) | 3875.1(14) | 26.9(6) |
| C15 | 49(2) | 5002.4(17) | 3759.2(16) | 39.8(7) |
| C16 | 1737(3) | 5407.1(16) | 4710.1(14) | 38.5(7) |
| C17 | 1958(2) | 4592.0(15) | 3612.7(16) | 37.1(7) |
| Fe2 | 4270.3(3) | 4867.1(2) | 1355.7(2) | 24.52(10) |
| Si2 | 3658.8(6) | 6911.3(4) | 1730.8(4) | 22.22(15) |
| O3 | 3940.7(14) | 7130.3(10) | 2626.9(9) | 25.7(4) |
| O4 | 2331.1(14) | 6724.7(10) | 1466.2(10) | 27.9(4) |
| N2 | 5605.3(17) | 6274.3(14) | 3380.6(12) | 31.8(5) |
| C18 | 4578.1(19) | 6062.0(14) | 1590.0(13) | 23.4(5) |
| C19 | 5232(2) | 5556.3(14) | 2157.9(14) | 25.6(5) |
| C20 | 5919(2) | 5056.4(16) | 1810.2(15) | 32.5(6) |
| C21 | 5696(2) | 5227.6(16) | 1030.9(15) | 32.1(6) |
| C22 | 4883(2) | 5838.6(15) | 897.3(14) | 28.4(6) |
| C23 | 2649(2) | 4633.8(16) | 1402.8(18) | 39.9(7) |
| C24 | 3365(2) | 4134.6(16) | 1893.2(17) | 36.9(7) |
| C25 | 3990(2) | 3675.5(15) | 1470.9(16) | 35.2(7) |
| C26 | 3654(2) | 3902.1(16) | 713.1(16) | 36.5(7) |
| C27 | 2822(2) | 4501.4(16) | 669.4(17) | 40.4(7) |
| C28 | 5194(2) | 5535.1(16) | 2979.4(14) | 31.9(6) |
| C29 | 5526(2) | 6208(2) | 4165.7(15) | 46.8(8) |
| C30 | 6747(2) | 6462(2) | 3315.0(18) | 54.4(9) |
| C31 | 3936(2) | 7814.4(15) | 1187.9(14) | 31.9(6) |
| C32 | 3290(3) | 8514.3(17) | 1454.0(17) | 54.0(9) |
| C33 | 3517(3) | 7730.4(16) | 341.9(14) | 37.6(7) |
| C34 | 5195(3) | 7989(2) | 1348.9(18) | 57.8(10) |
| Atom | U11 | U22 | U33 | U23 | U13 | U12 |
|---|---|---|---|---|---|---|
| Fe1 | 23.86(19) | 20.52(18) | 25.3(2) | -3.21(14) | 3.47(15) | 1.66(14) |
| Si1 | 20.1(3) | 21.3(3) | 18.7(3) | -0.3(3) | 6.9(3) | 0.4(3) |
| O1 | 21.8(9) | 25.4(9) | 18.3(9) | -2.8(7) | 6.7(7) | 1.5(7) |
| O2 | 21.3(9) | 32.5(10) | 23.9(9) | 1.4(8) | 5.2(7) | -2.5(7) |
| N1 | 21.6(11) | 37.2(12) | 20.4(11) | -7.3(9) | 4.2(9) | 1.5(9) |
| C1 | 21.7(12) | 21.1(12) | 23.5(13) | -5.6(10) | 9.5(10) | -3.5(9) |
| C2 | 22.0(13) | 24.0(12) | 23.5(13) | -4.8(10) | 6.2(10) | 0.1(10) |
| C3 | 23.3(13) | 28.4(13) | 31.1(14) | -5.3(11) | 5.6(11) | 3.1(10) |
| C4 | 23.7(13) | 32.5(14) | 32.9(15) | -11.2(11) | 13.3(11) | 0.1(11) |
| C5 | 30.3(14) | 23.1(12) | 22.8(13) | -1.7(10) | 8.6(11) | -3.1(10) |
| C6 | 36.7(16) | 28.0(14) | 40.6(17) | 0.6(12) | 9.9(13) | -9.0(12) |
| C7 | 40.2(17) | 21.2(13) | 43.5(17) | 2.9(12) | 1.5(13) | -0.4(12) |
| C8 | 44.0(17) | 22.7(13) | 37.6(16) | -7.4(12) | 3.9(13) | -0.6(12) |
| C9 | 40.6(17) | 24.9(14) | 33.8(15) | -3.7(11) | -5.1(13) | -5.1(12) |
| C10 | 24.5(14) | 25.6(14) | 56.7(19) | -0.9(13) | 0.8(13) | -4.9(11) |
| C11 | 29.6(14) | 28.2(14) | 25.2(13) | 2.3(10) | 6.2(11) | 3.9(11) |
| C12 | 25.0(15) | 53.4(19) | 41.2(17) | -15.6(14) | 5.4(13) | -3.4(13) |
| C13 | 41.6(17) | 55.4(19) | 20.4(14) | -3.1(13) | 2.3(12) | 7.9(14) |
| C14 | 34.1(15) | 25.0(13) | 24.5(13) | 0(1) | 12.6(11) | -2.4(11) |
| C15 | 45.2(18) | 38.9(17) | 39.1(17) | 5.1(13) | 17.9(14) | -9.9(13) |
| C16 | 52.6(19) | 37.2(16) | 25.7(15) | 7.6(12) | 8.0(13) | 2.1(13) |
| C17 | 48.3(18) | 25.6(14) | 40.3(17) | 5.3(12) | 16.0(14) | 5.6(12) |
| Fe2 | 23.9(2) | 22.78(19) | 29.1(2) | -1.18(15) | 10.75(15) | -1.96(14) |
| Si2 | 24.4(4) | 22.5(3) | 20.7(3) | 1.5(3) | 6.9(3) | -2.7(3) |
| O3 | 29.4(10) | 27.4(9) | 21.4(9) | 0.1(7) | 7.9(8) | 0.1(8) |
| O4 | 22.8(9) | 31.7(10) | 28.7(10) | 2.4(8) | 4.5(8) | -1.2(7) |
| N2 | 21.0(11) | 50.0(14) | 24.2(12) | -3.6(10) | 3.9(9) | 0.1(10) |
| C18 | 22.4(13) | 23.9(13) | 25.9(13) | -2.3(10) | 9.3(10) | -7.4(10) |
| C19 | 21.2(13) | 28.5(13) | 28.2(14) | -2.3(11) | 7.7(11) | -2.1(10) |
| C20 | 21.5(13) | 35.9(15) | 40.9(16) | -2.4(12) | 8.6(12) | 2.5(11) |
| C21 | 28.6(14) | 36.4(15) | 36.4(16) | -8.4(12) | 18.8(12) | -5.2(12) |
| C22 | 31.9(15) | 30.5(14) | 25.6(14) | -3.3(11) | 12.5(11) | -10.7(11) |
| C23 | 24.8(15) | 26.5(14) | 72(2) | -8.5(14) | 19.6(15) | -7.7(11) |
| C24 | 43.7(17) | 29.9(15) | 42.3(17) | -2.7(12) | 21.0(14) | -11.8(13) |
| C25 | 38.9(16) | 20.0(13) | 49.7(18) | 2.1(12) | 16.4(14) | -1.1(11) |
| C26 | 44.3(17) | 31.0(15) | 38.7(17) | -9.9(12) | 19.0(14) | -13.3(13) |
| C27 | 34.8(16) | 34.3(16) | 48.0(19) | 3.9(13) | -1.0(14) | -12.7(13) |
| C28 | 30.8(15) | 37.6(15) | 28.2(14) | 6.7(12) | 8.1(12) | 8.3(12) |
| C29 | 36.5(17) | 77(2) | 25.0(15) | -1.7(15) | 1.7(13) | 12.2(16) |
| C30 | 28.4(17) | 86(3) | 48(2) | -22.2(18) | 8.0(14) | -9.3(16) |
| C31 | 45.5(17) | 27.2(14) | 22.7(14) | 1.6(11) | 6.6(12) | -11.8(12) |
| C32 | 100(3) | 25.3(15) | 36.2(18) | 2.0(13) | 12.8(18) | 1.5(16) |
| C33 | 54.1(19) | 31.9(15) | 26.3(15) | 5.2(12) | 7.0(13) | -3.4(13) |
| C34 | 59(2) | 64(2) | 45.5(19) | 15.1(16) | -0.6(16) | -37.9(18) |
| Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
|---|---|---|---|---|---|---|
| Fe1 | C1 | 2.069(2) | Fe2 | C18 | 2.062(2) | |
| Fe1 | C2 | 2.045(2) | Fe2 | C19 | 2.038(2) | |
| Fe1 | C3 | 2.040(3) | Fe2 | C20 | 2.047(3) | |
| Fe1 | C4 | 2.035(2) | Fe2 | C21 | 2.049(2) | |
| Fe1 | C5 | 2.035(2) | Fe2 | C22 | 2.040(2) | |
| Fe1 | C6 | 2.038(3) | Fe2 | C23 | 2.046(3) | |
| Fe1 | C7 | 2.037(3) | Fe2 | C24 | 2.035(3) | |
| Fe1 | C8 | 2.042(3) | Fe2 | C25 | 2.041(2) | |
| Fe1 | C9 | 2.053(3) | Fe2 | C26 | 2.046(3) | |
| Fe1 | C10 | 2.045(3) | Fe2 | C27 | 2.046(3) | |
| Si1 | O1 | 1.6442(16) | Si2 | O3 | 1.6414(17) | |
| Si1 | O2 | 1.6253(17) | Si2 | O4 | 1.6313(18) | |
| Si1 | C1 | 1.872(2) | Si2 | C18 | 1.864(2) | |
| Si1 | C14 | 1.887(2) | Si2 | C31 | 1.875(2) | |
| N1 | C11 | 1.479(3) | N2 | C28 | 1.472(3) | |
| N1 | C12 | 1.468(3) | N2 | C29 | 1.460(3) | |
| N1 | C13 | 1.464(3) | N2 | C30 | 1.464(3) | |
| C1 | C2 | 1.441(3) | C18 | C19 | 1.446(3) | |
| C1 | C5 | 1.444(3) | C18 | C22 | 1.439(3) | |
| C2 | C3 | 1.420(3) | C19 | C20 | 1.426(3) | |
| C2 | C11 | 1.509(3) | C19 | C28 | 1.509(3) | |
| C3 | C4 | 1.415(4) | C20 | C21 | 1.421(4) | |
| C4 | C5 | 1.416(3) | C21 | C22 | 1.414(4) | |
| C6 | C7 | 1.423(4) | C23 | C24 | 1.395(4) | |
| C6 | C10 | 1.421(4) | C23 | C27 | 1.415(4) | |
| C7 | C8 | 1.410(4) | C24 | C25 | 1.419(4) | |
| C8 | C9 | 1.411(4) | C25 | C26 | 1.411(4) | |
| C9 | C10 | 1.416(4) | C26 | C27 | 1.421(4) | |
| C14 | C15 | 1.530(4) | C31 | C32 | 1.547(4) | |
| C14 | C16 | 1.533(4) | C31 | C33 | 1.530(4) | |
| C14 | C17 | 1.543(3) | C31 | C34 | 1.540(4) |
| Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|
| C2 | Fe1 | C1 | 40.99(9) | C19 | Fe2 | C18 | 41.29(9) | |
| C2 | Fe1 | C9 | 164.44(10) | C19 | Fe2 | C20 | 40.85(10) | |
| C3 | Fe1 | C1 | 69.00(10) | C19 | Fe2 | C21 | 68.82(10) | |
| C3 | Fe1 | C2 | 40.66(9) | C19 | Fe2 | C22 | 68.67(10) | |
| C3 | Fe1 | C8 | 118.57(11) | C19 | Fe2 | C23 | 120.13(11) | |
| C3 | Fe1 | C9 | 153.91(10) | C19 | Fe2 | C25 | 124.29(11) | |
| C3 | Fe1 | C10 | 162.83(11) | C19 | Fe2 | C26 | 161.60(11) | |
| C4 | Fe1 | C1 | 69.40(9) | C19 | Fe2 | C27 | 155.57(11) | |
| C4 | Fe1 | C2 | 68.65(9) | C20 | Fe2 | C18 | 69.05(10) | |
| C4 | Fe1 | C3 | 40.64(10) | C20 | Fe2 | C21 | 40.58(11) | |
| C4 | Fe1 | C6 | 160.12(11) | C21 | Fe2 | C18 | 69.14(10) | |
| C4 | Fe1 | C7 | 122.33(11) | C22 | Fe2 | C18 | 41.06(9) | |
| C4 | Fe1 | C8 | 105.50(11) | C22 | Fe2 | C20 | 68.05(11) | |
| C4 | Fe1 | C9 | 119.81(11) | C22 | Fe2 | C21 | 40.45(10) | |
| C4 | Fe1 | C10 | 156.26(11) | C22 | Fe2 | C23 | 127.75(11) | |
| C5 | Fe1 | C1 | 41.18(9) | C22 | Fe2 | C25 | 154.71(10) | |
| C5 | Fe1 | C2 | 68.41(10) | C22 | Fe2 | C26 | 121.15(10) | |
| C5 | Fe1 | C3 | 68.18(10) | C22 | Fe2 | C27 | 109.52(11) | |
| C5 | Fe1 | C4 | 40.71(10) | C23 | Fe2 | C18 | 108.32(10) | |
| C5 | Fe1 | C6 | 158.11(10) | C23 | Fe2 | C20 | 154.26(12) | |
| C5 | Fe1 | C7 | 160.06(11) | C23 | Fe2 | C21 | 164.39(12) | |
| C5 | Fe1 | C8 | 124.48(10) | C24 | Fe2 | C18 | 125.33(10) | |
| C5 | Fe1 | C9 | 108.64(11) | C24 | Fe2 | C19 | 106.69(11) | |
| C5 | Fe1 | C10 | 123.00(11) | C24 | Fe2 | C20 | 119.31(12) | |
| C6 | Fe1 | C1 | 121.97(10) | C24 | Fe2 | C21 | 154.01(12) | |
| C6 | Fe1 | C2 | 108.20(10) | C24 | Fe2 | C22 | 163.78(11) | |
| C6 | Fe1 | C3 | 124.28(11) | C24 | Fe2 | C23 | 39.98(11) | |
| C6 | Fe1 | C8 | 68.30(11) | C24 | Fe2 | C25 | 40.74(10) | |
| C6 | Fe1 | C9 | 68.48(11) | C24 | Fe2 | C26 | 68.11(11) | |
| C6 | Fe1 | C10 | 40.73(11) | C24 | Fe2 | C27 | 67.89(12) | |
| C7 | Fe1 | C1 | 156.22(10) | C25 | Fe2 | C18 | 162.30(11) | |
| C7 | Fe1 | C2 | 119.94(11) | C25 | Fe2 | C20 | 106.43(11) | |
| C7 | Fe1 | C3 | 105.50(11) | C25 | Fe2 | C21 | 119.28(11) | |
| C7 | Fe1 | C6 | 40.87(11) | C25 | Fe2 | C23 | 67.89(11) | |
| C7 | Fe1 | C8 | 40.45(11) | C25 | Fe2 | C26 | 40.39(11) | |
| C7 | Fe1 | C9 | 68.23(11) | C25 | Fe2 | C27 | 68.13(12) | |
| C7 | Fe1 | C10 | 68.29(11) | C26 | Fe2 | C18 | 156.00(11) | |
| C8 | Fe1 | C1 | 162.69(10) | C26 | Fe2 | C20 | 124.90(11) | |
| C8 | Fe1 | C2 | 154.11(10) | C26 | Fe2 | C21 | 107.66(11) | |
| C8 | Fe1 | C9 | 40.31(10) | C26 | Fe2 | C23 | 68.02(11) | |
| C8 | Fe1 | C10 | 67.82(11) | C27 | Fe2 | C18 | 121.04(11) | |
| C9 | Fe1 | C1 | 126.78(10) | C27 | Fe2 | C20 | 162.93(11) | |
| C10 | Fe1 | C1 | 109.83(10) | C27 | Fe2 | C21 | 126.64(12) | |
| C10 | Fe1 | C2 | 127.30(11) | C27 | Fe2 | C23 | 40.44(12) | |
| C10 | Fe1 | C9 | 40.44(11) | C27 | Fe2 | C26 | 40.65(11) | |
| O1 | Si1 | C1 | 106.58(10) | O3 | Si2 | C18 | 107.31(10) | |
| O1 | Si1 | C14 | 109.34(10) | O3 | Si2 | C31 | 108.80(10) | |
| O2 | Si1 | O1 | 109.04(9) | O4 | Si2 | O3 | 109.32(9) | |
| O2 | Si1 | C1 | 114.74(10) | O4 | Si2 | C18 | 114.15(10) | |
| O2 | Si1 | C14 | 105.37(11) | O4 | Si2 | C31 | 106.03(11) | |
| C1 | Si1 | C14 | 111.72(11) | C18 | Si2 | C31 | 111.14(12) | |
| C12 | N1 | C11 | 112.48(19) | C29 | N2 | C28 | 109.8(2) | |
| C13 | N1 | C11 | 109.7(2) | C29 | N2 | C30 | 110.8(2) | |
| C13 | N1 | C12 | 110.7(2) | C30 | N2 | C28 | 112.0(2) | |
| Si1 | C1 | Fe1 | 133.32(12) | Si2 | C18 | Fe2 | 132.59(12) | |
| C2 | C1 | Fe1 | 68.61(13) | C19 | C18 | Fe2 | 68.44(13) | |
| C2 | C1 | Si1 | 126.64(17) | C19 | C18 | Si2 | 127.54(18) | |
| C2 | C1 | C5 | 105.3(2) | C22 | C18 | Fe2 | 68.65(13) | |
| C5 | C1 | Fe1 | 68.13(13) | C22 | C18 | Si2 | 126.35(19) | |
| C5 | C1 | Si1 | 127.55(18) | C22 | C18 | C19 | 105.7(2) | |
| C1 | C2 | Fe1 | 70.40(13) | C18 | C19 | Fe2 | 70.26(13) | |
| C1 | C2 | C11 | 127.7(2) | C18 | C19 | C28 | 126.9(2) | |
| C3 | C2 | Fe1 | 69.48(14) | C20 | C19 | Fe2 | 69.93(14) | |
| C3 | C2 | C1 | 108.9(2) | C20 | C19 | C18 | 108.4(2) | |
| C3 | C2 | C11 | 123.4(2) | C20 | C19 | C28 | 124.7(2) | |
| C11 | C2 | Fe1 | 126.11(17) | C28 | C19 | Fe2 | 124.67(17) | |
| C2 | C3 | Fe1 | 69.86(14) | C19 | C20 | Fe2 | 69.22(14) | |
| C4 | C3 | Fe1 | 69.48(14) | C21 | C20 | Fe2 | 69.78(15) | |
| C4 | C3 | C2 | 108.5(2) | C21 | C20 | C19 | 108.5(2) | |
| C3 | C4 | Fe1 | 69.88(14) | C20 | C21 | Fe2 | 69.64(14) | |
| C3 | C4 | C5 | 107.6(2) | C22 | C21 | Fe2 | 69.43(14) | |
| C5 | C4 | Fe1 | 69.64(14) | C22 | C21 | C20 | 107.6(2) | |
| C1 | C5 | Fe1 | 70.69(13) | C18 | C22 | Fe2 | 70.30(13) | |
| C4 | C5 | Fe1 | 69.65(14) | C21 | C22 | Fe2 | 70.12(14) | |
| C4 | C5 | C1 | 109.6(2) | C21 | C22 | C18 | 109.7(2) | |
| C7 | C6 | Fe1 | 69.54(15) | C24 | C23 | Fe2 | 69.59(15) | |
| C10 | C6 | Fe1 | 69.90(15) | C24 | C23 | C27 | 108.4(2) | |
| C10 | C6 | C7 | 107.4(3) | C27 | C23 | Fe2 | 69.76(15) | |
| C6 | C7 | Fe1 | 69.59(15) | C23 | C24 | Fe2 | 70.43(15) | |
| C8 | C7 | Fe1 | 69.94(15) | C23 | C24 | C25 | 108.4(3) | |
| C8 | C7 | C6 | 107.9(2) | C25 | C24 | Fe2 | 69.83(14) | |
| C7 | C8 | Fe1 | 69.61(15) | C24 | C25 | Fe2 | 69.43(14) | |
| C7 | C8 | C9 | 108.8(3) | C26 | C25 | Fe2 | 70.01(15) | |
| C9 | C8 | Fe1 | 70.26(14) | C26 | C25 | C24 | 107.7(3) | |
| C8 | C9 | Fe1 | 69.43(15) | C25 | C26 | Fe2 | 69.60(15) | |
| C8 | C9 | C10 | 107.5(2) | C25 | C26 | C27 | 107.8(2) | |
| C10 | C9 | Fe1 | 69.49(15) | C27 | C26 | Fe2 | 69.67(15) | |
| C6 | C10 | Fe1 | 69.37(15) | C23 | C27 | Fe2 | 69.79(16) | |
| C9 | C10 | Fe1 | 70.07(15) | C23 | C27 | C26 | 107.6(3) | |
| C9 | C10 | C6 | 108.5(2) | C26 | C27 | Fe2 | 69.68(16) | |
| N1 | C11 | C2 | 112.5(2) | N2 | C28 | C19 | 113.4(2) | |
| C15 | C14 | Si1 | 110.50(18) | C32 | C31 | Si2 | 106.50(18) | |
| C15 | C14 | C16 | 109.8(2) | C33 | C31 | Si2 | 113.51(18) | |
| C15 | C14 | C17 | 109.4(2) | C33 | C31 | C32 | 107.4(2) | |
| C16 | C14 | Si1 | 111.91(17) | C33 | C31 | C34 | 109.0(2) | |
| C16 | C14 | C17 | 107.6(2) | C34 | C31 | Si2 | 109.6(2) | |
| C17 | C14 | Si1 | 107.50(16) | C34 | C31 | C32 | 110.8(2) |
| D | H | A | d(D-H)/Å | d(H-A)/Å | d(D-A)/Å | D-H-A/° |
|---|---|---|---|---|---|---|
| O1 | H1 | N1 | 0.931(17) | 1.716(18) | 2.634(3) | 168(3) |
| O2 | H2 | O3 | 0.927(17) | 1.845(18) | 2.747(2) | 164(3) |
| O3 | H3A | N2 | 0.944(17) | 1.697(18) | 2.638(3) | 174(3) |
| O4 | H4A | O1 | 0.958(18) | 1.826(19) | 2.779(2) | 173(3) |
| A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|---|---|
| Fe1 | C1 | C2 | C3 | -58.96(17) | Fe2 | C18 | C19 | C20 | 59.76(17) | |
| Fe1 | C1 | C2 | C11 | 121.0(2) | Fe2 | C18 | C19 | C28 | -119.1(3) | |
| Fe1 | C1 | C5 | C4 | 58.94(17) | Fe2 | C18 | C22 | C21 | -59.18(17) | |
| Fe1 | C2 | C3 | C4 | -58.90(17) | Fe2 | C19 | C20 | C21 | 58.90(18) | |
| Fe1 | C2 | C11 | N1 | 160.10(16) | Fe2 | C19 | C28 | N2 | -157.04(17) | |
| Fe1 | C3 | C4 | C5 | -59.68(17) | Fe2 | C20 | C21 | C22 | 59.27(17) | |
| Fe1 | C4 | C5 | C1 | -59.57(16) | Fe2 | C21 | C22 | C18 | 59.29(16) | |
| Fe1 | C6 | C7 | C8 | 59.70(18) | Fe2 | C23 | C24 | C25 | -59.75(18) | |
| Fe1 | C6 | C10 | C9 | -59.37(18) | Fe2 | C23 | C27 | C26 | 59.65(18) | |
| Fe1 | C7 | C8 | C9 | 59.52(18) | Fe2 | C24 | C25 | C26 | -59.76(18) | |
| Fe1 | C8 | C9 | C10 | 59.28(18) | Fe2 | C25 | C26 | C27 | -59.40(18) | |
| Fe1 | C9 | C10 | C6 | 58.94(18) | Fe2 | C26 | C27 | C23 | -59.72(18) | |
| Si1 | C1 | C2 | Fe1 | -128.82(18) | Si2 | C18 | C19 | Fe2 | 127.89(18) | |
| Si1 | C1 | C2 | C3 | 172.21(17) | Si2 | C18 | C19 | C20 | -172.35(18) | |
| Si1 | C1 | C2 | C11 | -7.8(4) | Si2 | C18 | C19 | C28 | 8.8(4) | |
| Si1 | C1 | C5 | Fe1 | 128.60(19) | Si2 | C18 | C22 | Fe2 | -127.92(18) | |
| Si1 | C1 | C5 | C4 | -172.46(17) | Si2 | C18 | C22 | C21 | 172.90(18) | |
| O1 | Si1 | C1 | Fe1 | -109.11(16) | O3 | Si2 | C18 | Fe2 | 107.68(17) | |
| O1 | Si1 | C1 | C2 | -14.7(2) | O3 | Si2 | C18 | C19 | 13.3(2) | |
| O1 | Si1 | C1 | C5 | 156.4(2) | O3 | Si2 | C18 | C22 | -158.7(2) | |
| O1 | Si1 | C14 | C15 | -70.79(19) | O3 | Si2 | C31 | C32 | -52.2(2) | |
| O1 | Si1 | C14 | C16 | 166.45(17) | O3 | Si2 | C31 | C33 | -170.12(19) | |
| O1 | Si1 | C14 | C17 | 48.5(2) | O3 | Si2 | C31 | C34 | 67.7(2) | |
| O2 | Si1 | C1 | Fe1 | 11.7(2) | O4 | Si2 | C18 | Fe2 | -13.6(2) | |
| O2 | Si1 | C1 | C2 | 106.1(2) | O4 | Si2 | C18 | C19 | -108.0(2) | |
| O2 | Si1 | C1 | C5 | -82.9(2) | O4 | Si2 | C18 | C22 | 80.0(2) | |
| O2 | Si1 | C14 | C15 | 172.15(17) | O4 | Si2 | C31 | C32 | 65.3(2) | |
| O2 | Si1 | C14 | C16 | 49.4(2) | O4 | Si2 | C31 | C33 | -52.6(2) | |
| O2 | Si1 | C14 | C17 | -68.59(19) | O4 | Si2 | C31 | C34 | -174.82(19) | |
| C1 | Si1 | C14 | C15 | 46.9(2) | C18 | Si2 | C31 | C32 | -170.15(19) | |
| C1 | Si1 | C14 | C16 | -75.8(2) | C18 | Si2 | C31 | C33 | 71.9(2) | |
| C1 | Si1 | C14 | C17 | 166.19(17) | C18 | Si2 | C31 | C34 | -50.2(2) | |
| C1 | C2 | C3 | Fe1 | 59.53(16) | C18 | C19 | C20 | Fe2 | -59.96(16) | |
| C1 | C2 | C3 | C4 | 0.6(3) | C18 | C19 | C20 | C21 | -1.1(3) | |
| C1 | C2 | C11 | N1 | 67.9(3) | C18 | C19 | C28 | N2 | -66.7(3) | |
| C2 | C1 | C5 | Fe1 | -58.82(15) | C19 | C18 | C22 | Fe2 | 58.66(16) | |
| C2 | C1 | C5 | C4 | 0.1(3) | C19 | C18 | C22 | C21 | -0.5(3) | |
| C2 | C3 | C4 | Fe1 | 59.13(17) | C19 | C20 | C21 | Fe2 | -58.55(17) | |
| C2 | C3 | C4 | C5 | -0.5(3) | C19 | C20 | C21 | C22 | 0.7(3) | |
| C3 | C2 | C11 | N1 | -112.1(3) | C20 | C19 | C28 | N2 | 114.6(3) | |
| C3 | C4 | C5 | Fe1 | 59.83(17) | C20 | C21 | C22 | Fe2 | -59.41(17) | |
| C3 | C4 | C5 | C1 | 0.3(3) | C20 | C21 | C22 | C18 | -0.1(3) | |
| C5 | C1 | C2 | Fe1 | 58.51(15) | C22 | C18 | C19 | Fe2 | -58.79(16) | |
| C5 | C1 | C2 | C3 | -0.5(3) | C22 | C18 | C19 | C20 | 1.0(3) | |
| C5 | C1 | C2 | C11 | 179.5(2) | C22 | C18 | C19 | C28 | -177.9(2) | |
| C6 | C7 | C8 | Fe1 | -59.48(18) | C23 | C24 | C25 | Fe2 | 60.13(18) | |
| C6 | C7 | C8 | C9 | 0.0(3) | C23 | C24 | C25 | C26 | 0.4(3) | |
| C7 | C6 | C10 | Fe1 | 59.70(18) | C24 | C23 | C27 | Fe2 | -59.05(18) | |
| C7 | C6 | C10 | C9 | 0.3(3) | C24 | C23 | C27 | C26 | 0.6(3) | |
| C7 | C8 | C9 | Fe1 | -59.12(19) | C24 | C25 | C26 | Fe2 | 59.40(18) | |
| C7 | C8 | C9 | C10 | 0.2(3) | C24 | C25 | C26 | C27 | 0.0(3) | |
| C8 | C9 | C10 | Fe1 | -59.24(18) | C25 | C26 | C27 | Fe2 | 59.35(18) | |
| C8 | C9 | C10 | C6 | -0.3(3) | C25 | C26 | C27 | C23 | -0.4(3) | |
| C10 | C6 | C7 | Fe1 | -59.93(17) | C27 | C23 | C24 | Fe2 | 59.16(18) | |
| C10 | C6 | C7 | C8 | -0.2(3) | C27 | C23 | C24 | C25 | -0.6(3) | |
| C11 | C2 | C3 | Fe1 | -120.5(2) | C28 | C19 | C20 | Fe2 | 118.9(2) | |
| C11 | C2 | C3 | C4 | -179.4(2) | C28 | C19 | C20 | C21 | 177.8(2) | |
| C12 | N1 | C11 | C2 | 55.7(3) | C29 | N2 | C28 | C19 | 179.2(2) | |
| C13 | N1 | C11 | C2 | 179.5(2) | C30 | N2 | C28 | C19 | -57.3(3) | |
| C14 | Si1 | C1 | Fe1 | 131.52(16) | C31 | Si2 | C18 | Fe2 | -133.48(17) | |
| C14 | Si1 | C1 | C2 | -134.1(2) | C31 | Si2 | C18 | C19 | 132.1(2) | |
| C14 | Si1 | C1 | C5 | 37.0(2) | C31 | Si2 | C18 | C22 | -39.9(2) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| H1 | 513(18) | 6112(18) | 2101(15) | 58(10) |
| H2 | 3010(20) | 6765(15) | 3229(14) | 46(9) |
| H3 | -1690 | 8191 | 2806 | 33 |
| H4 | -1373 | 7937 | 4202 | 34 |
| H5 | 223 | 6963 | 4542 | 30 |
| H6 | 1579 | 8861 | 2643 | 42 |
| H7 | 29 | 9664 | 3031 | 43 |
| H8 | 196 | 9488 | 4423 | 42 |
| H9 | 1834 | 8584 | 4910 | 42 |
| H10 | 2698 | 8202 | 3812 | 44 |
| H11A | -765 | 7839 | 1715 | 33 |
| H11B | 502 | 7546 | 1935 | 33 |
| H12A | -1724 | 6303 | 2198 | 60 |
| H12B | -1890 | 5876 | 1397 | 60 |
| H12C | -2254 | 6789 | 1455 | 60 |
| H13A | -691 | 6175 | 568 | 60 |
| H13B | 246 | 6850 | 775 | 60 |
| H13C | -1040 | 7098 | 558 | 60 |
| H15A | -383 | 5415 | 3954 | 60 |
| H15B | 2 | 4499 | 4026 | 60 |
| H15C | -252 | 4926 | 3223 | 60 |
| H16A | 2524 | 5558 | 4783 | 58 |
| H16B | 1668 | 4916 | 4991 | 58 |
| H16C | 1320 | 5838 | 4891 | 58 |
| H17A | 1656 | 4472 | 3084 | 56 |
| H17B | 1923 | 4112 | 3914 | 56 |
| H17C | 2735 | 4765 | 3673 | 56 |
| H3A | 4567(19) | 6850(16) | 2892(15) | 53(9) |
| H4A | 1980(30) | 6420(18) | 1797(17) | 78(12) |
| H20 | 6439 | 4674 | 2058 | 39 |
| H21 | 6032 | 4977 | 666 | 38 |
| H22 | 4583 | 6067 | 422 | 34 |
| H23 | 2133 | 5000 | 1539 | 48 |
| H24 | 3424 | 4107 | 2420 | 44 |
| H25 | 4537 | 3285 | 1664 | 42 |
| H26 | 3935 | 3692 | 305 | 44 |
| H27 | 2449 | 4765 | 227 | 48 |
| H28A | 4417 | 5442 | 3031 | 38 |
| H28B | 5649 | 5080 | 3217 | 38 |
| H29A | 5981 | 5757 | 4397 | 70 |
| H29B | 4748 | 6118 | 4198 | 70 |
| H29C | 5795 | 6703 | 4429 | 70 |
| H30A | 7240 | 6018 | 3517 | 82 |
| H30B | 6994 | 6950 | 3597 | 82 |
| H30C | 6772 | 6543 | 2787 | 82 |
| H32A | 2496 | 8381 | 1367 | 81 |
| H32B | 3393 | 8999 | 1174 | 81 |
| H32C | 3572 | 8606 | 1990 | 81 |
| H33A | 3899 | 7283 | 156 | 56 |
| H33B | 3671 | 8225 | 93 | 56 |
| H33C | 2713 | 7630 | 235 | 56 |
| H34A | 5474 | 8027 | 1891 | 87 |
| H34B | 5330 | 8495 | 1112 | 87 |
| H34C | 5583 | 7556 | 1146 | 87 |
Experimental
Single crystals of C17H27FeNO2Si [3160] were []. A suitable crystal was selected and [] on a Xcalibur, Sapphire3 diffractometer. The crystal was kept at 173 K during data collection. Using Olex2 [1], the structure was solved with the ShelXS [2] structure solution program using Direct Methods and refined with the XL [3] refinement package using Least Squares minimisation.
Crystal structure determination of [3160]
Crystal Data for C17H27FeNO2Si (M =361.33 g/mol): monoclinic, space group P21/c (no. 14), a = 12.2692(6) Å, b = 16.7258(6) Å, c = 18.2415(7) Å, β = 101.842(4)°, V = 3663.7(3) Å3, Z = 8, T = 173 K, μ(MoKα) = 0.895 mm-1, Dcalc = 1.310 g/cm3, 74078 reflections measured (4.412° ≤ 2Θ ≤ 53.996°), 7995 unique (Rint = 0.0712, Rsigma = 0.0434) which were used in all calculations. The final R1 was 0.0432 (I > 2σ(I)) and wR2 was 0.0944 (all data).
Refinement model description
Number of restraints - 4, 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. Restrained distances
O4-H4A = O3-H3A = O2-H2 = O1-H1
1 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
C11(H11A,H11B), C28(H28A,H28B)
3.b Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C20(H20),
C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27)
3.c Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
H16C), C17(H17A,H17B,H17C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,
H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
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.