| Identification code | mo_B0129_0m |
| Empirical formula | C40H48Fe2N2O3Si2 |
| Formula weight | 772.68 |
| Temperature/K | 100.0 |
| Crystal system | monoclinic |
| Space group | P21/n |
| a/Å | 11.0354(10) |
| b/Å | 19.3902(15) |
| c/Å | 17.5694(12) |
| α/° | 90 |
| β/° | 101.549(3) |
| γ/° | 90 |
| Volume/Å3 | 3683.4(5) |
| Z | 4 |
| ρcalcg/cm3 | 1.393 |
| μ/mm‑1 | 0.893 |
| F(000) | 1624.0 |
| Crystal size/mm3 | 0.48 × 0.303 × 0.232 |
| Radiation | MoKα (λ = 0.71073) |
| 2Θ range for data collection/° | 4.732 to 57.996 |
| Index ranges | -14 ≤ h ≤ 15, -22 ≤ k ≤ 26, -23 ≤ l ≤ 23 |
| Reflections collected | 42889 |
| Independent reflections | 9768 [Rint = 0.0289, Rsigma = 0.0275] |
| Data/restraints/parameters | 9768/2/454 |
| Goodness-of-fit on F2 | 1.022 |
| Final R indexes [I>=2σ (I)] | R1 = 0.0297, wR2 = 0.0687 |
| Final R indexes [all data] | R1 = 0.0378, wR2 = 0.0718 |
| Largest diff. peak/hole / e Å-3 | 0.66/-0.67 |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| Fe1 | 1703.2(2) | 4297.2(2) | 4300.2(2) | 11.23(5) |
| Fe2 | 7463.0(2) | 3868.5(2) | 1211.0(2) | 13.45(5) |
| Si1 | 4412.6(4) | 3804.6(2) | 3710.0(2) | 12.08(8) |
| Si2 | 5919.2(4) | 4435.5(2) | 2589.8(2) | 13.43(8) |
| O2 | 3759.8(10) | 3222.2(5) | 3104.8(6) | 17.1(2) |
| O1 | 5548.8(10) | 4184.9(5) | 3403.6(6) | 15.8(2) |
| O3 | 4715.1(10) | 4511.2(6) | 1905.6(6) | 18.3(2) |
| N1 | 2339.1(12) | 4754.8(7) | 1932.8(7) | 17.1(2) |
| N2 | 4872.9(12) | 2485.1(6) | 2106.0(7) | 17.1(2) |
| C1 | 3250.1(13) | 4461.6(7) | 3837.8(8) | 13.0(3) |
| C2 | 2145.1(13) | 4677.5(7) | 3305.9(8) | 13.8(3) |
| C3 | 1543.0(14) | 5195.5(7) | 3675.2(9) | 16.0(3) |
| C4 | 2252.0(14) | 5307.2(7) | 4433.4(9) | 16.5(3) |
| C5 | 3293.2(14) | 4861.0(7) | 4536.1(8) | 14.4(3) |
| C6 | 1643.9(14) | 3262.7(7) | 4518.5(9) | 18.3(3) |
| C7 | 548.8(14) | 3473.2(7) | 3996.3(9) | 17.5(3) |
| C8 | -44.3(14) | 3985.2(8) | 4374.1(9) | 17.8(3) |
| C9 | 687.1(15) | 4091.2(8) | 5131.1(9) | 19.5(3) |
| C10 | 1730.0(15) | 3646.5(8) | 5220.5(9) | 19.5(3) |
| C11 | 1699.2(14) | 4418.2(7) | 2495.8(8) | 16.2(3) |
| C12 | 1941.0(16) | 4433.4(10) | 1169.8(9) | 26.5(4) |
| C13 | 2107.6(17) | 5496.9(8) | 1882.2(10) | 25.6(3) |
| C14 | 5113.6(14) | 3435.5(7) | 4683.6(8) | 14.8(3) |
| C15 | 5923.9(14) | 2819.5(7) | 4630.2(8) | 15.0(3) |
| C16 | 7138.3(15) | 2894.2(8) | 4526.0(9) | 22.0(3) |
| C17 | 7885.4(16) | 2323.9(9) | 4487.7(10) | 26.0(3) |
| C18 | 7426.0(16) | 1666.3(8) | 4537.1(9) | 24.1(3) |
| C19 | 6213.7(17) | 1583.7(8) | 4615(1) | 25.1(3) |
| C20 | 5472.2(15) | 2153.0(8) | 4665.5(9) | 21.3(3) |
| C21 | 6956.1(14) | 3796.7(7) | 2268.9(8) | 14.4(3) |
| C22 | 6635.9(14) | 3177.9(7) | 1813.5(8) | 15.5(3) |
| C23 | 7753.4(15) | 2890.1(7) | 1649.7(9) | 18.4(3) |
| C24 | 8754.6(14) | 3322.3(8) | 1979.3(9) | 18.4(3) |
| C25 | 8275.2(14) | 3874.2(7) | 2362.0(8) | 16.4(3) |
| C26 | 6202.9(17) | 4102.2(9) | 227.5(9) | 26.0(3) |
| C27 | 7267.2(17) | 3797.9(9) | 30.6(9) | 25.8(3) |
| C28 | 8302.9(16) | 4212.3(9) | 348.9(9) | 25.6(3) |
| C29 | 7878.5(17) | 4776.4(8) | 739.7(9) | 25.7(4) |
| C30 | 6574.8(17) | 4708.5(9) | 661.8(9) | 25.6(4) |
| C31 | 5374.4(14) | 2887.2(8) | 1520.2(9) | 17.7(3) |
| C32 | 5734.8(17) | 1949.8(9) | 2463.9(10) | 27.2(4) |
| C33 | 3706.4(16) | 2169.3(9) | 1716(1) | 26.8(4) |
| C34 | 6768.5(14) | 5275.9(7) | 2816.4(9) | 18.2(3) |
| C35 | 5896.0(14) | 5880.0(7) | 2723.8(9) | 16.9(3) |
| C36 | 5658.5(18) | 6257.9(8) | 2032.9(10) | 25.9(4) |
| C37 | 4803.5(18) | 6789.4(8) | 1918(1) | 27.3(4) |
| C38 | 4168.7(16) | 6965.9(8) | 2494.6(10) | 23.1(3) |
| C39 | 4399.0(15) | 6602.1(8) | 3188.1(9) | 22.3(3) |
| C40 | 5245.6(15) | 6062.4(8) | 3297.7(9) | 19.3(3) |
| Atom | U11 | U22 | U33 | U23 | U13 | U12 |
|---|---|---|---|---|---|---|
| Fe1 | 12.68(10) | 9.96(9) | 12.09(9) | -0.18(7) | 4.97(7) | -0.75(7) |
| Fe2 | 15.29(11) | 13.2(1) | 12.78(10) | 0.14(7) | 5.00(8) | 0.04(7) |
| Si1 | 13.64(19) | 11.61(17) | 12.21(17) | 0.19(13) | 5.52(14) | 0.96(14) |
| Si2 | 14.9(2) | 12.46(17) | 14.03(18) | -0.33(14) | 5.64(15) | -0.87(14) |
| O2 | 18.3(5) | 15.9(5) | 17.8(5) | -4.3(4) | 5.6(4) | -0.5(4) |
| O1 | 15.4(5) | 18.2(5) | 15.6(5) | 1.0(4) | 7.3(4) | -0.3(4) |
| O3 | 15.2(5) | 22.0(5) | 18.2(5) | 1.1(4) | 4.8(4) | 2.8(4) |
| N1 | 18.1(6) | 21.2(6) | 12.7(6) | 2.1(5) | 4.6(5) | 0.3(5) |
| N2 | 19.0(7) | 14.6(6) | 18.8(6) | -2.4(5) | 6.7(5) | -4.4(5) |
| C1 | 13.9(7) | 11.5(6) | 15.2(6) | 0.3(5) | 6.9(5) | -1.6(5) |
| C2 | 15.3(7) | 12.2(6) | 15.4(6) | 2.3(5) | 7.1(5) | -0.2(5) |
| C3 | 17.5(7) | 11.1(6) | 21.3(7) | 3.2(5) | 8.2(6) | 1.8(5) |
| C4 | 19.4(8) | 10.5(6) | 21.7(7) | -2.3(5) | 9.2(6) | -1.4(5) |
| C5 | 15.3(7) | 13.5(6) | 15.4(6) | -1.9(5) | 5.5(5) | -2.9(5) |
| C6 | 19.6(8) | 11.0(6) | 24.4(7) | 2.8(5) | 4.8(6) | -1.9(5) |
| C7 | 19.5(8) | 14.5(6) | 18.2(7) | -1.1(5) | 3.1(6) | -5.0(6) |
| C8 | 15.0(7) | 18.4(7) | 21.3(7) | 1.8(6) | 6.5(6) | -2.5(6) |
| C9 | 23.2(8) | 21.4(7) | 16.8(7) | -0.1(6) | 10.8(6) | -5.9(6) |
| C10 | 21.9(8) | 20.1(7) | 16.0(7) | 5.8(6) | 2.2(6) | -5.9(6) |
| C11 | 15.9(7) | 18.1(7) | 15.3(7) | 1.7(5) | 4.7(5) | -0.1(5) |
| C12 | 24.2(9) | 39.9(10) | 14.8(7) | -1.9(7) | 2.4(6) | -3.0(7) |
| C13 | 30.4(9) | 22.7(8) | 24.3(8) | 8.5(6) | 7.1(7) | 0.6(7) |
| C14 | 17.6(7) | 13.7(6) | 14.2(6) | 0.3(5) | 5.8(5) | 1.3(5) |
| C15 | 17.6(7) | 16.1(6) | 11.6(6) | 0.8(5) | 3.3(5) | 3.1(5) |
| C16 | 20.1(8) | 19.0(7) | 28.7(8) | -4.1(6) | 9.0(6) | -1.8(6) |
| C17 | 17.9(8) | 28.9(8) | 32.9(9) | -3.3(7) | 9.4(7) | 3.0(7) |
| C18 | 27.1(9) | 22.7(8) | 24.2(8) | 3.7(6) | 8.9(7) | 11.4(7) |
| C19 | 32.4(10) | 15.3(7) | 30.7(9) | 7.1(6) | 14.0(7) | 3.5(6) |
| C20 | 19.9(8) | 18.5(7) | 28.0(8) | 4.9(6) | 11.0(6) | 2.2(6) |
| C21 | 16.2(7) | 14.0(6) | 13.5(6) | 2.4(5) | 4.3(5) | 0.8(5) |
| C22 | 18.2(7) | 13.3(6) | 15.8(6) | 1.2(5) | 5.1(5) | 0.4(5) |
| C23 | 21.9(8) | 13.3(6) | 20.9(7) | 0.5(5) | 6.4(6) | 3.6(6) |
| C24 | 15.6(7) | 19.3(7) | 20.2(7) | 1.3(6) | 3.6(6) | 5.2(6) |
| C25 | 15.4(7) | 17.2(7) | 16.1(7) | 0.5(5) | 1.7(5) | 1.4(5) |
| C26 | 22.8(9) | 34.0(9) | 19.3(8) | 8.2(7) | -0.5(6) | 0.5(7) |
| C27 | 33.7(10) | 29.4(8) | 14.5(7) | 0.1(6) | 5.0(7) | 0.4(7) |
| C28 | 23.7(9) | 35.3(9) | 20.7(8) | 6.3(7) | 11.6(7) | -0.3(7) |
| C29 | 35.9(10) | 21.0(8) | 20.9(8) | 5.9(6) | 7.4(7) | -6.8(7) |
| C30 | 32.2(10) | 24.2(8) | 22.5(8) | 10.6(6) | 10.6(7) | 9.8(7) |
| C31 | 19.8(8) | 15.7(7) | 18.5(7) | -1.3(5) | 6.0(6) | -2.8(6) |
| C32 | 34.6(10) | 20.1(8) | 27.8(8) | 4.8(6) | 8.8(7) | 0.4(7) |
| C33 | 27.0(9) | 22.7(8) | 31.5(9) | -7.5(7) | 8.0(7) | -10.5(7) |
| C34 | 18.2(8) | 14.5(6) | 23.3(7) | -2.2(6) | 7.9(6) | -2.0(6) |
| C35 | 19.0(8) | 12.4(6) | 20.0(7) | -2.3(5) | 5.9(6) | -3.5(5) |
| C36 | 42.2(11) | 16.6(7) | 23.9(8) | 1.7(6) | 18.8(7) | 1.0(7) |
| C37 | 43.8(11) | 15.7(7) | 23.4(8) | 5.1(6) | 9.4(7) | 0.5(7) |
| C38 | 23.4(9) | 16.2(7) | 27.9(8) | -1.6(6) | 0.7(7) | 1.3(6) |
| C39 | 20.1(8) | 27.1(8) | 20.0(7) | -3.6(6) | 4.8(6) | 3.8(6) |
| C40 | 19.3(8) | 23.3(7) | 15.3(7) | 0.3(6) | 3.5(6) | 1.6(6) |
| Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
|---|---|---|---|---|---|---|
| Fe1 | C1 | 2.0570(13) | C1 | C5 | 1.4437(19) | |
| Fe1 | C2 | 2.0432(13) | C2 | C3 | 1.4297(19) | |
| Fe1 | C3 | 2.0477(14) | C2 | C11 | 1.497(2) | |
| Fe1 | C4 | 2.0494(14) | C3 | C4 | 1.420(2) | |
| Fe1 | C5 | 2.0382(14) | C4 | C5 | 1.421(2) | |
| Fe1 | C6 | 2.0457(14) | C6 | C7 | 1.423(2) | |
| Fe1 | C7 | 2.0466(15) | C6 | C10 | 1.427(2) | |
| Fe1 | C8 | 2.0498(15) | C7 | C8 | 1.424(2) | |
| Fe1 | C9 | 2.0502(14) | C8 | C9 | 1.426(2) | |
| Fe1 | C10 | 2.0464(14) | C9 | C10 | 1.421(2) | |
| Fe2 | C21 | 2.0502(14) | C14 | C15 | 1.5060(19) | |
| Fe2 | C22 | 2.0332(14) | C15 | C16 | 1.396(2) | |
| Fe2 | C23 | 2.0487(14) | C15 | C20 | 1.391(2) | |
| Fe2 | C24 | 2.0506(15) | C16 | C17 | 1.389(2) | |
| Fe2 | C25 | 2.0414(15) | C17 | C18 | 1.381(2) | |
| Fe2 | C26 | 2.0403(17) | C18 | C19 | 1.381(2) | |
| Fe2 | C27 | 2.0461(16) | C19 | C20 | 1.387(2) | |
| Fe2 | C28 | 2.0396(15) | C21 | C22 | 1.446(2) | |
| Fe2 | C29 | 2.0364(15) | C21 | C25 | 1.440(2) | |
| Fe2 | C30 | 2.0410(16) | C22 | C23 | 1.434(2) | |
| Si1 | O2 | 1.6179(11) | C22 | C31 | 1.495(2) | |
| Si1 | O1 | 1.6359(11) | C23 | C24 | 1.415(2) | |
| Si1 | C1 | 1.8533(14) | C24 | C25 | 1.421(2) | |
| Si1 | C14 | 1.8727(15) | C26 | C27 | 1.418(2) | |
| Si2 | O1 | 1.6376(10) | C26 | C30 | 1.417(3) | |
| Si2 | O3 | 1.6101(12) | C27 | C28 | 1.417(3) | |
| Si2 | C21 | 1.8492(15) | C28 | C29 | 1.420(2) | |
| Si2 | C34 | 1.8823(15) | C29 | C30 | 1.424(3) | |
| N1 | C11 | 1.4774(18) | C34 | C35 | 1.504(2) | |
| N1 | C12 | 1.464(2) | C35 | C36 | 1.397(2) | |
| N1 | C13 | 1.461(2) | C35 | C40 | 1.395(2) | |
| N2 | C31 | 1.4838(18) | C36 | C37 | 1.385(2) | |
| N2 | C32 | 1.462(2) | C37 | C38 | 1.385(2) | |
| N2 | C33 | 1.466(2) | C38 | C39 | 1.387(2) | |
| C1 | C2 | 1.442(2) | C39 | C40 | 1.390(2) |
| Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|
| C2 | Fe1 | C1 | 41.18(6) | C21 | Si2 | C34 | 109.39(7) | |
| C2 | Fe1 | C3 | 40.91(5) | Si1 | O1 | Si2 | 139.71(7) | |
| C2 | Fe1 | C4 | 68.72(6) | C12 | N1 | C11 | 109.20(12) | |
| C2 | Fe1 | C6 | 122.42(6) | C13 | N1 | C11 | 112.00(12) | |
| C2 | Fe1 | C7 | 107.54(6) | C13 | N1 | C12 | 110.30(13) | |
| C2 | Fe1 | C8 | 123.31(6) | C32 | N2 | C31 | 111.74(12) | |
| C2 | Fe1 | C9 | 159.60(6) | C32 | N2 | C33 | 109.84(13) | |
| C2 | Fe1 | C10 | 158.42(6) | C33 | N2 | C31 | 108.04(12) | |
| C3 | Fe1 | C1 | 69.25(6) | Si1 | C1 | Fe1 | 126.20(7) | |
| C3 | Fe1 | C4 | 40.56(6) | C2 | C1 | Fe1 | 68.90(8) | |
| C3 | Fe1 | C8 | 107.68(6) | C2 | C1 | Si1 | 129.58(10) | |
| C3 | Fe1 | C9 | 123.15(6) | C2 | C1 | C5 | 105.95(12) | |
| C4 | Fe1 | C1 | 69.35(5) | C5 | C1 | Fe1 | 68.66(8) | |
| C4 | Fe1 | C8 | 122.35(6) | C5 | C1 | Si1 | 124.47(11) | |
| C4 | Fe1 | C9 | 107.23(6) | C1 | C2 | Fe1 | 69.93(7) | |
| C5 | Fe1 | C1 | 41.28(5) | C1 | C2 | C11 | 126.38(12) | |
| C5 | Fe1 | C2 | 68.73(6) | C3 | C2 | Fe1 | 69.71(8) | |
| C5 | Fe1 | C3 | 68.36(6) | C3 | C2 | C1 | 108.62(12) | |
| C5 | Fe1 | C4 | 40.67(6) | C3 | C2 | C11 | 124.99(13) | |
| C5 | Fe1 | C6 | 123.12(6) | C11 | C2 | Fe1 | 127.06(10) | |
| C5 | Fe1 | C7 | 159.61(6) | C2 | C3 | Fe1 | 69.38(8) | |
| C5 | Fe1 | C8 | 158.11(6) | C4 | C3 | Fe1 | 69.79(8) | |
| C5 | Fe1 | C9 | 122.07(6) | C4 | C3 | C2 | 108.31(13) | |
| C5 | Fe1 | C10 | 107.12(6) | C3 | C4 | Fe1 | 69.66(8) | |
| C6 | Fe1 | C1 | 106.63(6) | C3 | C4 | C5 | 107.81(12) | |
| C6 | Fe1 | C3 | 158.75(6) | C5 | C4 | Fe1 | 69.24(8) | |
| C6 | Fe1 | C4 | 159.29(6) | C1 | C5 | Fe1 | 70.06(8) | |
| C6 | Fe1 | C7 | 40.69(6) | C4 | C5 | Fe1 | 70.09(8) | |
| C6 | Fe1 | C8 | 68.46(6) | C4 | C5 | C1 | 109.31(13) | |
| C6 | Fe1 | C9 | 68.46(6) | C7 | C6 | Fe1 | 69.69(8) | |
| C6 | Fe1 | C10 | 40.83(6) | C7 | C6 | C10 | 107.98(13) | |
| C7 | Fe1 | C1 | 122.71(6) | C10 | C6 | Fe1 | 69.62(8) | |
| C7 | Fe1 | C3 | 122.80(6) | C6 | C7 | Fe1 | 69.62(8) | |
| C7 | Fe1 | C4 | 158.45(6) | C6 | C7 | C8 | 108.04(13) | |
| C7 | Fe1 | C8 | 40.69(6) | C8 | C7 | Fe1 | 69.78(8) | |
| C7 | Fe1 | C9 | 68.47(6) | C7 | C8 | Fe1 | 69.53(8) | |
| C8 | Fe1 | C1 | 159.45(6) | C7 | C8 | C9 | 107.94(14) | |
| C8 | Fe1 | C9 | 40.70(6) | C9 | C8 | Fe1 | 69.66(8) | |
| C9 | Fe1 | C1 | 157.96(6) | C8 | C9 | Fe1 | 69.64(8) | |
| C10 | Fe1 | C1 | 121.72(6) | C10 | C9 | Fe1 | 69.56(8) | |
| C10 | Fe1 | C3 | 159.09(6) | C10 | C9 | C8 | 108.07(13) | |
| C10 | Fe1 | C4 | 122.80(6) | C6 | C10 | Fe1 | 69.56(8) | |
| C10 | Fe1 | C7 | 68.56(6) | C9 | C10 | Fe1 | 69.84(8) | |
| C10 | Fe1 | C8 | 68.47(6) | C9 | C10 | C6 | 107.96(14) | |
| C10 | Fe1 | C9 | 40.60(6) | N1 | C11 | C2 | 112.21(12) | |
| C21 | Fe2 | C24 | 69.39(6) | C15 | C14 | Si1 | 112.83(9) | |
| C22 | Fe2 | C21 | 41.48(5) | C16 | C15 | C14 | 121.56(13) | |
| C22 | Fe2 | C23 | 41.14(6) | C20 | C15 | C14 | 120.77(13) | |
| C22 | Fe2 | C24 | 69.05(6) | C20 | C15 | C16 | 117.65(13) | |
| C22 | Fe2 | C25 | 69.00(6) | C17 | C16 | C15 | 121.23(15) | |
| C22 | Fe2 | C26 | 106.64(7) | C18 | C17 | C16 | 120.20(15) | |
| C22 | Fe2 | C27 | 121.09(6) | C19 | C18 | C17 | 119.22(15) | |
| C22 | Fe2 | C28 | 156.94(7) | C18 | C19 | C20 | 120.63(15) | |
| C22 | Fe2 | C29 | 160.42(7) | C19 | C20 | C15 | 121.01(15) | |
| C22 | Fe2 | C30 | 123.27(7) | Si2 | C21 | Fe2 | 121.92(7) | |
| C23 | Fe2 | C21 | 69.30(6) | C22 | C21 | Fe2 | 68.63(8) | |
| C23 | Fe2 | C24 | 40.38(6) | C22 | C21 | Si2 | 128.81(11) | |
| C25 | Fe2 | C21 | 41.20(6) | C25 | C21 | Fe2 | 69.07(8) | |
| C25 | Fe2 | C23 | 68.14(6) | C25 | C21 | Si2 | 124.66(11) | |
| C25 | Fe2 | C24 | 40.65(6) | C25 | C21 | C22 | 106.20(12) | |
| C25 | Fe2 | C27 | 160.17(7) | C21 | C22 | Fe2 | 69.89(8) | |
| C26 | Fe2 | C21 | 121.30(7) | C21 | C22 | C31 | 127.67(13) | |
| C26 | Fe2 | C23 | 123.58(7) | C23 | C22 | Fe2 | 70.01(8) | |
| C26 | Fe2 | C24 | 159.76(7) | C23 | C22 | C21 | 108.01(13) | |
| C26 | Fe2 | C25 | 158.03(7) | C23 | C22 | C31 | 124.26(13) | |
| C26 | Fe2 | C27 | 40.60(7) | C31 | C22 | Fe2 | 123.58(10) | |
| C26 | Fe2 | C30 | 40.63(7) | C22 | C23 | Fe2 | 68.85(8) | |
| C27 | Fe2 | C21 | 157.18(7) | C24 | C23 | Fe2 | 69.88(8) | |
| C27 | Fe2 | C23 | 107.23(6) | C24 | C23 | C22 | 108.65(13) | |
| C27 | Fe2 | C24 | 123.44(7) | C23 | C24 | Fe2 | 69.73(9) | |
| C28 | Fe2 | C21 | 160.47(7) | C23 | C24 | C25 | 107.79(13) | |
| C28 | Fe2 | C23 | 121.47(7) | C25 | C24 | Fe2 | 69.33(8) | |
| C28 | Fe2 | C24 | 107.36(7) | C21 | C25 | Fe2 | 69.73(8) | |
| C28 | Fe2 | C25 | 124.00(7) | C24 | C25 | Fe2 | 70.02(9) | |
| C28 | Fe2 | C26 | 68.43(7) | C24 | C25 | C21 | 109.35(13) | |
| C28 | Fe2 | C27 | 40.60(7) | C27 | C26 | Fe2 | 69.92(10) | |
| C28 | Fe2 | C30 | 68.57(7) | C30 | C26 | Fe2 | 69.72(9) | |
| C29 | Fe2 | C21 | 123.49(6) | C30 | C26 | C27 | 108.18(16) | |
| C29 | Fe2 | C23 | 157.30(7) | C26 | C27 | Fe2 | 69.48(9) | |
| C29 | Fe2 | C24 | 122.05(7) | C28 | C27 | Fe2 | 69.45(9) | |
| C29 | Fe2 | C25 | 107.95(6) | C28 | C27 | C26 | 108.04(15) | |
| C29 | Fe2 | C26 | 68.55(7) | C27 | C28 | Fe2 | 69.95(9) | |
| C29 | Fe2 | C27 | 68.43(7) | C27 | C28 | C29 | 108.03(15) | |
| C29 | Fe2 | C28 | 40.77(7) | C29 | C28 | Fe2 | 69.49(9) | |
| C29 | Fe2 | C30 | 40.87(7) | C28 | C29 | Fe2 | 69.74(9) | |
| C30 | Fe2 | C21 | 106.88(6) | C28 | C29 | C30 | 107.89(15) | |
| C30 | Fe2 | C23 | 160.22(7) | C30 | C29 | Fe2 | 69.74(9) | |
| C30 | Fe2 | C24 | 158.13(7) | C26 | C30 | Fe2 | 69.66(9) | |
| C30 | Fe2 | C25 | 122.55(6) | C26 | C30 | C29 | 107.86(15) | |
| C30 | Fe2 | C27 | 68.35(7) | C29 | C30 | Fe2 | 69.39(9) | |
| O2 | Si1 | O1 | 111.61(5) | N2 | C31 | C22 | 114.20(12) | |
| O2 | Si1 | C1 | 109.36(6) | C35 | C34 | Si2 | 111.74(10) | |
| O2 | Si1 | C14 | 112.44(6) | C36 | C35 | C34 | 120.47(13) | |
| O1 | Si1 | C1 | 108.94(6) | C40 | C35 | C34 | 122.01(14) | |
| O1 | Si1 | C14 | 105.61(6) | C40 | C35 | C36 | 117.43(14) | |
| C1 | Si1 | C14 | 108.75(6) | C37 | C36 | C35 | 121.40(15) | |
| O1 | Si2 | C21 | 110.20(6) | C36 | C37 | C38 | 120.46(15) | |
| O1 | Si2 | C34 | 105.84(6) | C37 | C38 | C39 | 119.10(15) | |
| O3 | Si2 | O1 | 111.47(6) | C38 | C39 | C40 | 120.30(14) | |
| O3 | Si2 | C21 | 107.58(6) | C39 | C40 | C35 | 121.29(14) | |
| O3 | Si2 | C34 | 112.37(7) |
| D | H | A | d(D-H)/Å | d(H-A)/Å | d(D-A)/Å | D-H-A/° |
|---|---|---|---|---|---|---|
| O2 | H2 | N2 | 0.902(16) | 1.847(16) | 2.7376(16) | 169(2) |
| O3 | H3 | N1 | 0.958(16) | 1.773(18) | 2.6740(17) | 156(2) |
| A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|---|---|
| Fe1 | C1 | C2 | C3 | 59.16(9) | C5 | C1 | C2 | C3 | 0.22(15) | |
| Fe1 | C1 | C2 | C11 | -121.85(14) | C5 | C1 | C2 | C11 | 179.21(13) | |
| Fe1 | C1 | C5 | C4 | -59.27(10) | C6 | C7 | C8 | Fe1 | 59.32(10) | |
| Fe1 | C2 | C3 | C4 | 59.11(10) | C6 | C7 | C8 | C9 | 0.03(16) | |
| Fe1 | C2 | C11 | N1 | -172.18(10) | C7 | C6 | C10 | Fe1 | -59.34(10) | |
| Fe1 | C3 | C4 | C5 | 58.92(10) | C7 | C6 | C10 | C9 | 0.16(16) | |
| Fe1 | C4 | C5 | C1 | 59.25(9) | C7 | C8 | C9 | Fe1 | 59.20(10) | |
| Fe1 | C6 | C7 | C8 | -59.41(10) | C7 | C8 | C9 | C10 | 0.07(16) | |
| Fe1 | C6 | C10 | C9 | 59.50(10) | C8 | C9 | C10 | Fe1 | 59.18(10) | |
| Fe1 | C7 | C8 | C9 | -59.29(10) | C8 | C9 | C10 | C6 | -0.14(16) | |
| Fe1 | C8 | C9 | C10 | -59.13(10) | C10 | C6 | C7 | Fe1 | 59.30(10) | |
| Fe1 | C9 | C10 | C6 | -59.33(10) | C10 | C6 | C7 | C8 | -0.12(16) | |
| Fe2 | C21 | C22 | C23 | 59.88(10) | C11 | C2 | C3 | Fe1 | 121.70(14) | |
| Fe2 | C21 | C22 | C31 | -117.48(15) | C11 | C2 | C3 | C4 | -179.19(13) | |
| Fe2 | C21 | C25 | C24 | -58.96(10) | C12 | N1 | C11 | C2 | 174.88(13) | |
| Fe2 | C22 | C23 | C24 | 58.68(10) | C13 | N1 | C11 | C2 | -62.65(16) | |
| Fe2 | C22 | C31 | N2 | -170.37(9) | C14 | Si1 | O1 | Si2 | 157.65(10) | |
| Fe2 | C23 | C24 | C25 | 59.09(10) | C14 | Si1 | C1 | Fe1 | -59.65(10) | |
| Fe2 | C24 | C25 | C21 | 58.78(10) | C14 | Si1 | C1 | C2 | -151.14(12) | |
| Fe2 | C26 | C27 | C28 | -58.93(11) | C14 | Si1 | C1 | C5 | 27.80(13) | |
| Fe2 | C26 | C30 | C29 | 59.08(11) | C14 | C15 | C16 | C17 | 179.13(15) | |
| Fe2 | C27 | C28 | C29 | -59.27(11) | C14 | C15 | C20 | C19 | 179.86(14) | |
| Fe2 | C28 | C29 | C30 | -59.54(11) | C15 | C16 | C17 | C18 | 1.3(3) | |
| Fe2 | C29 | C30 | C26 | -59.24(11) | C16 | C15 | C20 | C19 | 1.3(2) | |
| Si1 | C1 | C2 | Fe1 | 120.15(11) | C16 | C17 | C18 | C19 | 0.8(3) | |
| Si1 | C1 | C2 | C3 | 179.31(10) | C17 | C18 | C19 | C20 | -1.8(3) | |
| Si1 | C1 | C2 | C11 | -1.7(2) | C18 | C19 | C20 | C15 | 0.7(3) | |
| Si1 | C1 | C5 | Fe1 | -120.06(10) | C20 | C15 | C16 | C17 | -2.3(2) | |
| Si1 | C1 | C5 | C4 | -179.33(10) | C21 | Si2 | O1 | Si1 | -99.17(11) | |
| Si1 | C14 | C15 | C16 | 80.42(16) | C21 | Si2 | C34 | C35 | 153.98(10) | |
| Si1 | C14 | C15 | C20 | -98.06(14) | C21 | C22 | C23 | Fe2 | -59.80(10) | |
| Si2 | C21 | C22 | Fe2 | 114.45(12) | C21 | C22 | C23 | C24 | -1.12(16) | |
| Si2 | C21 | C22 | C23 | 174.32(11) | C21 | C22 | C31 | N2 | -80.87(18) | |
| Si2 | C21 | C22 | C31 | -3.0(2) | C22 | C21 | C25 | Fe2 | 58.84(9) | |
| Si2 | C21 | C25 | Fe2 | -115.07(11) | C22 | C21 | C25 | C24 | -0.11(16) | |
| Si2 | C21 | C25 | C24 | -174.03(10) | C22 | C23 | C24 | Fe2 | -58.05(10) | |
| Si2 | C34 | C35 | C36 | -96.00(15) | C22 | C23 | C24 | C25 | 1.04(17) | |
| Si2 | C34 | C35 | C40 | 80.47(16) | C23 | C22 | C31 | N2 | 102.17(16) | |
| O2 | Si1 | O1 | Si2 | 35.17(12) | C23 | C24 | C25 | Fe2 | -59.35(10) | |
| O2 | Si1 | C1 | Fe1 | 63.48(10) | C23 | C24 | C25 | C21 | -0.57(17) | |
| O2 | Si1 | C1 | C2 | -28.01(14) | C25 | C21 | C22 | Fe2 | -59.13(9) | |
| O2 | Si1 | C1 | C5 | 150.93(11) | C25 | C21 | C22 | C23 | 0.75(15) | |
| O2 | Si1 | C14 | C15 | 49.72(12) | C25 | C21 | C22 | C31 | -176.60(14) | |
| O1 | Si1 | C1 | Fe1 | -174.29(8) | C26 | C27 | C28 | Fe2 | 58.95(11) | |
| O1 | Si1 | C1 | C2 | 94.22(13) | C26 | C27 | C28 | C29 | -0.33(18) | |
| O1 | Si1 | C1 | C5 | -86.84(12) | C27 | C26 | C30 | Fe2 | -59.57(11) | |
| O1 | Si1 | C14 | C15 | -72.22(11) | C27 | C26 | C30 | C29 | -0.49(18) | |
| O1 | Si2 | C21 | Fe2 | 172.77(7) | C27 | C28 | C29 | Fe2 | 59.56(11) | |
| O1 | Si2 | C21 | C22 | 85.64(13) | C27 | C28 | C29 | C30 | 0.02(18) | |
| O1 | Si2 | C21 | C25 | -101.87(12) | C28 | C29 | C30 | Fe2 | 59.53(11) | |
| O1 | Si2 | C34 | C35 | -87.31(11) | C28 | C29 | C30 | C26 | 0.29(18) | |
| O3 | Si2 | O1 | Si1 | 20.20(12) | C30 | C26 | C27 | Fe2 | 59.44(11) | |
| O3 | Si2 | C21 | Fe2 | 51.06(10) | C30 | C26 | C27 | C28 | 0.51(18) | |
| O3 | Si2 | C21 | C22 | -36.07(14) | C31 | C22 | C23 | Fe2 | 117.66(14) | |
| O3 | Si2 | C21 | C25 | 136.42(12) | C31 | C22 | C23 | C24 | 176.35(13) | |
| O3 | Si2 | C34 | C35 | 34.57(12) | C32 | N2 | C31 | C22 | -52.71(16) | |
| C1 | Si1 | O1 | Si2 | -85.69(11) | C33 | N2 | C31 | C22 | -173.66(13) | |
| C1 | Si1 | C14 | C15 | 170.99(10) | C34 | Si2 | O1 | Si1 | 142.65(10) | |
| C1 | C2 | C3 | Fe1 | -59.29(9) | C34 | Si2 | C21 | Fe2 | -71.26(10) | |
| C1 | C2 | C3 | C4 | -0.18(16) | C34 | Si2 | C21 | C22 | -158.39(12) | |
| C1 | C2 | C11 | N1 | -80.91(17) | C34 | Si2 | C21 | C25 | 14.10(14) | |
| C2 | C1 | C5 | Fe1 | 59.09(9) | C34 | C35 | C36 | C37 | 176.09(16) | |
| C2 | C1 | C5 | C4 | -0.18(15) | C34 | C35 | C40 | C39 | -176.94(15) | |
| C2 | C3 | C4 | Fe1 | -58.85(9) | C35 | C36 | C37 | C38 | 0.8(3) | |
| C2 | C3 | C4 | C5 | 0.07(16) | C36 | C35 | C40 | C39 | -0.4(2) | |
| C3 | C2 | C11 | N1 | 97.93(16) | C36 | C37 | C38 | C39 | -0.1(3) | |
| C3 | C4 | C5 | Fe1 | -59.18(10) | C37 | C38 | C39 | C40 | -0.7(2) | |
| C3 | C4 | C5 | C1 | 0.07(16) | C38 | C39 | C40 | C35 | 1.0(2) | |
| C5 | C1 | C2 | Fe1 | -58.94(9) | C40 | C35 | C36 | C37 | -0.5(2) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| H2 | 4220(20) | 3001(11) | 2811(12) | 47(7) |
| H3 | 3963(18) | 4653(13) | 2053(14) | 53(7) |
| H3A | 796 | 5426 | 3452 | 19 |
| H4 | 2064 | 5624 | 4806 | 20 |
| H5 | 3919 | 4830 | 4993 | 17 |
| H6 | 2217 | 2926 | 4418 | 22 |
| H7 | 263 | 3302 | 3485 | 21 |
| H8 | -795 | 4215 | 4160 | 21 |
| H9 | 509 | 4404 | 5510 | 23 |
| H10 | 2371 | 3611 | 5669 | 23 |
| H11A | 1835 | 3914 | 2485 | 19 |
| H11B | 799 | 4503 | 2340 | 19 |
| H12A | 2100 | 3936 | 1212 | 40 |
| H12B | 2402 | 4635 | 802 | 40 |
| H12C | 1054 | 4514 | 984 | 40 |
| H13A | 1219 | 5580 | 1713 | 38 |
| H13B | 2551 | 5701 | 1507 | 38 |
| H13C | 2398 | 5707 | 2393 | 38 |
| H14A | 5612 | 3796 | 5001 | 18 |
| H14B | 4443 | 3298 | 4952 | 18 |
| H16 | 7460 | 3343 | 4480 | 26 |
| H17 | 8715 | 2386 | 4427 | 31 |
| H18 | 7938 | 1275 | 4518 | 29 |
| H19 | 5884 | 1133 | 4634 | 30 |
| H20 | 4643 | 2087 | 4725 | 26 |
| H23 | 7812 | 2478 | 1367 | 22 |
| H24 | 9597 | 3255 | 1950 | 22 |
| H25 | 8751 | 4237 | 2636 | 20 |
| H26 | 5382 | 3930 | 92 | 31 |
| H27 | 7283 | 3388 | -263 | 31 |
| H28 | 9135 | 4128 | 308 | 31 |
| H29 | 8376 | 5135 | 1006 | 31 |
| H30 | 6048 | 5015 | 865 | 31 |
| H31A | 4800 | 3271 | 1335 | 21 |
| H31B | 5404 | 2586 | 1070 | 21 |
| H32A | 5364 | 1687 | 2836 | 41 |
| H32B | 6505 | 2165 | 2735 | 41 |
| H32C | 5913 | 1639 | 2060 | 41 |
| H33A | 3124 | 2531 | 1491 | 40 |
| H33B | 3355 | 1903 | 2093 | 40 |
| H33C | 3861 | 1863 | 1302 | 40 |
| H34A | 7248 | 5264 | 3356 | 22 |
| H34B | 7359 | 5335 | 2465 | 22 |
| H36 | 6093 | 6148 | 1634 | 31 |
| H37 | 4651 | 7035 | 1440 | 33 |
| H38 | 3583 | 7331 | 2416 | 28 |
| H39 | 3976 | 6722 | 3590 | 27 |
| H40 | 5384 | 5813 | 3773 | 23 |
Experimental
Single crystals of C40H48Fe2N2O3Si2 [mo_B0129_0m] were [The material was recrystallised from Diethylether by slow evaporation]. A suitable crystal was selected and [The crystal was mounted on a MITIGEN holder in perfluoroether oil] on a Bruker D8 Venture diffractometer. The crystal was kept at 100.0 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_B0129_0m]
Crystal Data for C40H48Fe2N2O3Si2 (M =772.68 g/mol): monoclinic, space group P21/n (no. 14), a = 11.0354(10) Å, b = 19.3902(15) Å, c = 17.5694(12) Å, β = 101.549(3)°, V = 3683.4(5) Å3, Z = 4, T = 100.0 K, μ(MoKα) = 0.893 mm-1, Dcalc = 1.393 g/cm3, 42889 reflections measured (4.732° ≤ 2Θ ≤ 57.996°), 9768 unique (Rint = 0.0289, Rsigma = 0.0275) which were used in all calculations. The final R1 was 0.0297 (I > 2σ(I)) and wR2 was 0.0718 (all data).
Refinement model description
Number of restraints - 2, 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
O2-H2 = O3-H3
0.98 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
C11(H11A,H11B), C14(H14A,H14B), C31(H31A,H31B), C34(H34A,H34B)
3.b Aromatic/amide H refined with riding coordinates:
C3(H3A), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C16(H16),
C17(H17), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C25(H25), C26(H26),
C27(H27), C28(H28), C29(H29), C30(H30), C36(H36), C37(H37), C38(H38),
C39(H39), C40(H40)
3.c Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C32(H32A,H32B,H32C), C33(H33A,H33B,
H33C)
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.