| Identification code | 3116 |
| Empirical formula | C46H52Fe4N2O3Si2 |
| Formula weight | 960.47 |
| Temperature/K | 150 |
| Crystal system | monoclinic |
| Space group | P21/n |
| a/Å | 12.8025(4) |
| b/Å | 18.1923(6) |
| c/Å | 17.9925(7) |
| α/° | 90 |
| β/° | 90.855(3) |
| γ/° | 90 |
| Volume/Å3 | 4190.1(2) |
| Z | 4 |
| ρcalcg/cm3 | 1.523 |
| μ/mm‑1 | 1.458 |
| F(000) | 1992.0 |
| Crystal size/mm3 | 0.2 × 0.1 × 0.05 |
| Radiation | MoKα (λ = 0.71073) |
| 2Θ range for data collection/° | 4.478 to 54 |
| Index ranges | -16 ≤ h ≤ 16, -23 ≤ k ≤ 23, -22 ≤ l ≤ 22 |
| Reflections collected | 31598 |
| Independent reflections | 9116 [Rint = 0.0358, Rsigma = 0.0398] |
| Data/restraints/parameters | 9116/0/526 |
| Goodness-of-fit on F2 | 1.028 |
| Final R indexes [I>=2σ (I)] | R1 = 0.0431, wR2 = 0.0946 |
| Final R indexes [all data] | R1 = 0.0611, wR2 = 0.1035 |
| Largest diff. peak/hole / e Å-3 | 0.96/-0.50 |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| Fe1 | 2922.8(4) | 748.9(2) | 933.5(3) | 28.67(11) |
| Fe2 | -495.8(3) | 2297.3(2) | -917.7(2) | 22.57(10) |
| Fe3 | 3517.5(4) | 4272.7(2) | -2583.3(3) | 29.95(12) |
| Fe4 | 2220.9(4) | 4702.9(2) | 637.0(3) | 30.41(12) |
| Si1 | 2103.4(6) | 2053.6(4) | -348.7(5) | 21.58(17) |
| Si2 | 3016.0(6) | 3579.1(4) | -849.1(5) | 21.79(17) |
| O1 | 2339.5(15) | 2918.2(10) | -496.0(11) | 24.5(4) |
| O2 | 2512.6(17) | 1536.9(12) | -1008.5(13) | 31.0(5) |
| O3 | 4246.6(17) | 3459.5(13) | -694.4(14) | 32.2(5) |
| N1 | 5173.6(19) | 2431.7(14) | 192.3(16) | 31.7(6) |
| N2 | 3603(2) | 1869.8(14) | -2251.4(15) | 34.1(6) |
| C1 | 2725(2) | 1796.1(15) | 555.2(16) | 23.1(6) |
| C2 | 3802(2) | 1657.8(16) | 766.6(17) | 27.7(7) |
| C3 | 3829(3) | 1468.7(18) | 1538.8(19) | 37.4(8) |
| C4 | 2795(3) | 1471.5(18) | 1808.6(19) | 36.5(8) |
| C5 | 2126(3) | 1679.7(16) | 1213.3(17) | 28.4(7) |
| C6 | 2972(8) | 44(2) | 83(3) | 102(3) |
| C7 | 3707(4) | -163(2) | 619(3) | 68.8(15) |
| C8 | 3193(3) | -309.8(18) | 1269(2) | 46.8(9) |
| C9 | 2147(3) | -201.9(18) | 1159(3) | 53.3(11) |
| C10 | 1973(5) | 16(2) | 440(4) | 92(2) |
| C11 | 4723(2) | 1685.6(17) | 277.4(19) | 32.0(7) |
| C12 | 5429(3) | 2777(2) | 901(2) | 51.4(10) |
| C13 | 6122(3) | 2353(2) | -253(3) | 53.5(11) |
| C14 | 691(2) | 2003.1(15) | -201.3(16) | 22.5(6) |
| C15 | -46(2) | 1417.9(16) | -293.8(16) | 24.1(6) |
| C16 | -1050(2) | 1664.2(17) | -76.3(17) | 27.7(7) |
| C17 | -955(2) | 2403.7(17) | 158.5(17) | 28.0(7) |
| C18 | 105(2) | 2614.3(16) | 83.0(16) | 25.2(6) |
| C19 | 168(3) | 2532(2) | -1913.8(19) | 45.1(9) |
| C20 | -584(3) | 1976(2) | -2003.8(19) | 43.5(9) |
| C21 | -1559(3) | 2250(2) | -1773(2) | 40.4(8) |
| C22 | -1397(3) | 2984(2) | -1537(2) | 42.3(9) |
| C23 | -328(3) | 3152(2) | -1631.4(19) | 42.3(9) |
| C24 | 2738(2) | 3611.9(15) | -1861.0(16) | 23.6(6) |
| C25 | 3193(2) | 3193.0(17) | -2457.2(17) | 29.0(7) |
| C26 | 2769(3) | 3454.4(19) | -3145.9(18) | 35.5(8) |
| C27 | 2060(3) | 4032.2(19) | -2995.9(18) | 35.2(8) |
| C28 | 2038(2) | 4126.4(17) | -2214.6(18) | 29.4(7) |
| C29 | 4794(3) | 4665(2) | -2024(2) | 42.4(9) |
| C30 | 5095(3) | 4322(2) | -2687(2) | 47(1) |
| C31 | 4594(3) | 4693(2) | -3285(2) | 55.3(11) |
| C32 | 3992(3) | 5268(2) | -2993(2) | 51(1) |
| C33 | 4108(3) | 5248.1(19) | -2206(2) | 44.5(9) |
| C34 | 4021(3) | 2612.9(18) | -2372.9(18) | 33.6(7) |
| C35 | 3027(3) | 1604(2) | -2901(2) | 53.4(10) |
| C36 | 4470(3) | 1364(2) | -2080(2) | 46.4(9) |
| C37 | 2587(2) | 4462.1(16) | -449.0(18) | 29.1(7) |
| C38 | 1547(3) | 4750(2) | -393(2) | 43.5(9) |
| C39 | 1588(5) | 5457(2) | -73(3) | 68.9(15) |
| C40 | 2628(5) | 5624(2) | 68(3) | 78.0(19) |
| C41 | 3254(4) | 5016(2) | -155(2) | 55.3(12) |
| C42 | 2224(4) | 3757(2) | 1236(2) | 56.4(12) |
| C43 | 1263(4) | 4118(2) | 1304(2) | 53.8(11) |
| C44 | 1455(3) | 4817(2) | 1619(2) | 46.1(9) |
| C45 | 2539(3) | 4878(2) | 1737(2) | 47.4(10) |
| C46 | 3019(4) | 4228(2) | 1502(2) | 57.2(11) |
| Atom | U11 | U22 | U33 | U23 | U13 | U12 |
|---|---|---|---|---|---|---|
| Fe1 | 36.5(3) | 19.7(2) | 29.7(3) | 0.69(18) | -3.15(19) | -2.79(18) |
| Fe2 | 21.4(2) | 25.8(2) | 20.4(2) | -0.90(17) | -0.71(16) | 0.99(17) |
| Fe3 | 31.7(2) | 32.3(2) | 25.9(2) | 8.87(19) | 2.96(18) | -4.51(19) |
| Fe4 | 37.1(3) | 23.9(2) | 30.4(3) | -5.59(18) | 6.3(2) | -3.63(19) |
| Si1 | 19.9(4) | 20.4(4) | 24.5(4) | -0.1(3) | 0.2(3) | -1.2(3) |
| Si2 | 24.0(4) | 20.1(4) | 21.3(4) | 1.6(3) | 3.2(3) | -1.6(3) |
| O1 | 29.2(11) | 22.7(10) | 21.7(11) | 3.0(8) | 2.2(8) | -3.1(8) |
| O2 | 38.4(12) | 29.6(11) | 25.1(12) | -2.6(9) | 3.8(10) | -0.4(10) |
| O3 | 27.8(12) | 35.1(13) | 33.7(14) | 9.3(11) | -0.4(10) | -0.7(10) |
| N1 | 21.3(13) | 32.5(14) | 41.1(17) | 2.6(12) | -4.9(11) | -4.5(11) |
| N2 | 42.5(16) | 31.5(14) | 28.6(15) | -1.5(11) | 6.4(12) | 6.8(12) |
| C1 | 27.8(15) | 19.9(13) | 21.7(15) | -1.9(11) | 0.0(12) | -1.2(12) |
| C2 | 33.3(16) | 21.7(14) | 27.8(17) | -0.9(12) | -6.6(13) | -1.6(12) |
| C3 | 47(2) | 33.4(17) | 30.9(19) | 0.3(14) | -14.6(15) | -5.1(15) |
| C4 | 53(2) | 35.1(18) | 21.6(17) | 1.4(14) | -2.2(15) | -4.6(16) |
| C5 | 34.4(17) | 27.0(15) | 23.7(16) | -3.0(12) | 2.6(13) | -4.6(13) |
| C6 | 253(9) | 23(2) | 29(3) | -5.3(18) | 9(4) | -25(4) |
| C7 | 74(3) | 35(2) | 98(4) | -18(2) | 42(3) | -4(2) |
| C8 | 64(3) | 26.3(17) | 50(2) | 6.7(16) | -5(2) | 7.7(17) |
| C9 | 48(2) | 22.0(17) | 90(4) | 3.9(19) | 14(2) | -2.1(16) |
| C10 | 117(5) | 18.2(19) | 139(6) | -5(3) | -85(4) | -7(2) |
| C11 | 26.2(16) | 28.9(16) | 41(2) | -1.4(14) | -6.3(14) | 1.1(13) |
| C12 | 51(2) | 45(2) | 58(3) | -4.7(19) | -16.5(19) | -10.4(18) |
| C13 | 26.3(18) | 48(2) | 86(3) | -2(2) | 8.0(19) | -2.4(17) |
| C14 | 23.1(14) | 23.9(14) | 20.4(15) | -0.5(11) | -2.5(11) | -0.5(11) |
| C15 | 24.8(15) | 23.4(14) | 24.1(16) | 1.1(12) | 0.6(12) | 0.2(12) |
| C16 | 23.1(15) | 31.1(16) | 28.8(17) | 3.3(13) | 2.0(12) | -3.1(12) |
| C17 | 27.4(15) | 33.3(16) | 23.3(16) | -1.1(13) | 5.6(12) | 3.7(13) |
| C18 | 30.2(15) | 24.3(14) | 21.0(15) | -2.3(12) | -1.4(12) | -1.2(12) |
| C19 | 38.4(19) | 75(3) | 21.7(18) | 8.7(18) | 3.4(14) | 4.6(19) |
| C20 | 60(2) | 48(2) | 22.3(18) | -4.5(15) | -7.1(16) | 15.8(19) |
| C21 | 35.9(18) | 53(2) | 32.0(19) | 2.5(16) | -13.2(15) | -1.5(17) |
| C22 | 50(2) | 47(2) | 29.2(19) | 4.9(16) | -9.0(16) | 19.9(17) |
| C23 | 56(2) | 42(2) | 28.2(19) | 15.2(15) | -5.9(16) | -9.6(17) |
| C24 | 24.1(14) | 23.8(14) | 22.9(16) | 5.9(12) | 1.8(12) | -2.3(12) |
| C25 | 30.8(16) | 31.3(16) | 25.1(16) | 1.2(13) | 3.5(13) | -6.9(13) |
| C26 | 42.2(19) | 44.0(19) | 20.5(17) | 0.5(14) | 3.1(14) | -7.1(16) |
| C27 | 35.4(18) | 44.0(19) | 26.1(18) | 11.5(15) | -4.9(14) | -6.2(15) |
| C28 | 26.4(15) | 32.2(16) | 29.5(17) | 7.3(13) | 0.1(13) | -1.9(13) |
| C29 | 29.8(17) | 46(2) | 51(2) | 12.3(18) | -4.2(16) | -13.6(16) |
| C30 | 29.9(18) | 52(2) | 60(3) | 5.5(19) | 14.0(17) | -6.5(17) |
| C31 | 52(2) | 70(3) | 45(2) | 13(2) | 15.5(19) | -24(2) |
| C32 | 54(2) | 42(2) | 57(3) | 24.3(19) | -4(2) | -14.5(18) |
| C33 | 43(2) | 32.7(18) | 57(3) | 4.4(17) | 3.6(18) | -10.9(16) |
| C34 | 34.3(17) | 41.2(18) | 25.4(17) | -2.6(14) | 8.1(13) | 2.9(15) |
| C35 | 71(3) | 43(2) | 46(2) | -8.7(18) | -4(2) | -7(2) |
| C36 | 52(2) | 43(2) | 45(2) | 0.5(17) | 14.8(18) | 17.6(18) |
| C37 | 37.0(17) | 23.0(14) | 27.4(17) | 1.6(12) | 10.3(13) | -2.0(13) |
| C38 | 51(2) | 50(2) | 30(2) | 7.0(16) | 5.4(16) | 19.8(18) |
| C39 | 112(4) | 41(2) | 54(3) | 15(2) | 39(3) | 35(3) |
| C40 | 139(5) | 20.7(18) | 77(4) | -7.9(19) | 64(4) | -18(2) |
| C41 | 66(3) | 38(2) | 63(3) | -15.8(19) | 35(2) | -26.1(19) |
| C42 | 119(4) | 28.4(18) | 22.3(19) | 1.2(14) | 0(2) | -4(2) |
| C43 | 71(3) | 64(3) | 27(2) | -5.2(18) | 11.8(19) | -31(2) |
| C44 | 53(2) | 55(2) | 30(2) | -8.8(17) | 9.5(17) | -0.9(19) |
| C45 | 61(2) | 45(2) | 37(2) | -21.9(17) | -4.6(18) | -4.5(18) |
| C46 | 68(3) | 60(3) | 43(2) | -14(2) | -15(2) | 19(2) |
| Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
|---|---|---|---|---|---|---|
| Fe1 | C1 | 2.038(3) | N1 | C11 | 1.484(4) | |
| Fe1 | C2 | 2.025(3) | N1 | C12 | 1.454(5) | |
| Fe1 | C3 | 2.052(3) | N1 | C13 | 1.472(4) | |
| Fe1 | C4 | 2.060(3) | N2 | C34 | 1.472(4) | |
| Fe1 | C5 | 2.044(3) | N2 | C35 | 1.456(5) | |
| Fe1 | C6 | 1.998(4) | N2 | C36 | 1.471(4) | |
| Fe1 | C7 | 2.024(4) | C1 | C2 | 1.446(4) | |
| Fe1 | C8 | 2.046(3) | C1 | C5 | 1.437(4) | |
| Fe1 | C9 | 2.038(4) | C2 | C3 | 1.431(4) | |
| Fe1 | C10 | 2.002(4) | C2 | C11 | 1.483(4) | |
| Fe2 | C14 | 2.048(3) | C3 | C4 | 1.418(5) | |
| Fe2 | C15 | 2.033(3) | C4 | C5 | 1.413(5) | |
| Fe2 | C16 | 2.038(3) | C6 | C7 | 1.389(8) | |
| Fe2 | C17 | 2.041(3) | C6 | C10 | 1.440(9) | |
| Fe2 | C18 | 2.031(3) | C7 | C8 | 1.377(6) | |
| Fe2 | C19 | 2.040(3) | C8 | C9 | 1.364(5) | |
| Fe2 | C20 | 2.041(3) | C9 | C10 | 1.368(7) | |
| Fe2 | C21 | 2.042(3) | C14 | C15 | 1.430(4) | |
| Fe2 | C22 | 2.024(3) | C14 | C18 | 1.439(4) | |
| Fe2 | C23 | 2.030(3) | C15 | C16 | 1.422(4) | |
| Fe3 | C24 | 2.042(3) | C16 | C17 | 1.415(4) | |
| Fe3 | C25 | 2.021(3) | C17 | C18 | 1.418(4) | |
| Fe3 | C26 | 2.032(3) | C19 | C20 | 1.404(5) | |
| Fe3 | C27 | 2.045(3) | C19 | C23 | 1.394(5) | |
| Fe3 | C28 | 2.034(3) | C20 | C21 | 1.412(5) | |
| Fe3 | C29 | 2.036(4) | C21 | C22 | 1.417(5) | |
| Fe3 | C30 | 2.033(3) | C22 | C23 | 1.414(5) | |
| Fe3 | C31 | 2.033(3) | C24 | C25 | 1.445(4) | |
| Fe3 | C32 | 2.050(3) | C24 | C28 | 1.438(4) | |
| Fe3 | C33 | 2.041(4) | C25 | C26 | 1.427(5) | |
| Fe4 | C37 | 2.063(3) | C25 | C34 | 1.502(4) | |
| Fe4 | C38 | 2.035(4) | C26 | C27 | 1.417(5) | |
| Fe4 | C39 | 2.035(4) | C27 | C28 | 1.417(5) | |
| Fe4 | C40 | 2.035(4) | C29 | C30 | 1.405(5) | |
| Fe4 | C41 | 2.040(4) | C29 | C33 | 1.412(5) | |
| Fe4 | C42 | 2.031(4) | C30 | C31 | 1.416(6) | |
| Fe4 | C43 | 2.029(4) | C31 | C32 | 1.406(6) | |
| Fe4 | C44 | 2.043(3) | C32 | C33 | 1.422(6) | |
| Fe4 | C45 | 2.039(4) | C37 | C38 | 1.436(5) | |
| Fe4 | C46 | 2.040(4) | C37 | C41 | 1.418(5) | |
| Si1 | O1 | 1.624(2) | C38 | C39 | 1.410(6) | |
| Si1 | O2 | 1.608(2) | C39 | C40 | 1.386(8) | |
| Si1 | C1 | 1.860(3) | C40 | C41 | 1.427(6) | |
| Si1 | C14 | 1.834(3) | C42 | C43 | 1.401(6) | |
| Si2 | O1 | 1.617(2) | C42 | C46 | 1.409(6) | |
| Si2 | O3 | 1.611(2) | C43 | C44 | 1.412(5) | |
| Si2 | C24 | 1.851(3) | C44 | C45 | 1.406(5) | |
| Si2 | C37 | 1.847(3) | C45 | C46 | 1.401(5) |
| Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|
| C1 | Fe1 | C3 | 69.33(13) | C43 | Fe4 | C44 | 40.57(15) | |
| C1 | Fe1 | C4 | 69.37(12) | C43 | Fe4 | C45 | 67.83(16) | |
| C1 | Fe1 | C5 | 41.22(11) | C43 | Fe4 | C46 | 68.11(19) | |
| C1 | Fe1 | C8 | 176.53(14) | C44 | Fe4 | C37 | 163.52(15) | |
| C1 | Fe1 | C9 | 143.29(15) | C45 | Fe4 | C37 | 155.09(15) | |
| C2 | Fe1 | C1 | 41.70(12) | C45 | Fe4 | C41 | 120.77(17) | |
| C2 | Fe1 | C3 | 41.10(13) | C45 | Fe4 | C44 | 40.28(15) | |
| C2 | Fe1 | C4 | 69.08(13) | C45 | Fe4 | C46 | 40.17(15) | |
| C2 | Fe1 | C5 | 68.94(12) | C46 | Fe4 | C37 | 120.93(15) | |
| C2 | Fe1 | C8 | 136.10(15) | C46 | Fe4 | C44 | 67.97(17) | |
| C2 | Fe1 | C9 | 174.80(16) | O1 | Si1 | C1 | 107.95(12) | |
| C3 | Fe1 | C4 | 40.34(14) | O1 | Si1 | C14 | 104.97(12) | |
| C5 | Fe1 | C3 | 67.74(13) | O2 | Si1 | O1 | 112.47(12) | |
| C5 | Fe1 | C4 | 40.29(13) | O2 | Si1 | C1 | 110.99(13) | |
| C5 | Fe1 | C8 | 142.19(14) | O2 | Si1 | C14 | 114.22(13) | |
| C6 | Fe1 | C1 | 110.46(17) | C14 | Si1 | C1 | 105.74(13) | |
| C6 | Fe1 | C2 | 112.8(2) | O1 | Si2 | C24 | 108.32(12) | |
| C6 | Fe1 | C3 | 142.4(3) | O1 | Si2 | C37 | 109.24(12) | |
| C6 | Fe1 | C4 | 177.2(3) | O3 | Si2 | O1 | 111.09(12) | |
| C6 | Fe1 | C5 | 137.9(3) | O3 | Si2 | C24 | 110.33(13) | |
| C6 | Fe1 | C7 | 40.4(2) | O3 | Si2 | C37 | 110.22(14) | |
| C6 | Fe1 | C8 | 67.32(19) | C37 | Si2 | C24 | 107.55(14) | |
| C6 | Fe1 | C9 | 68.2(2) | Si2 | O1 | Si1 | 152.38(14) | |
| C6 | Fe1 | C10 | 42.2(3) | C12 | N1 | C11 | 112.8(3) | |
| C7 | Fe1 | C1 | 137.07(17) | C12 | N1 | C13 | 110.0(3) | |
| C7 | Fe1 | C2 | 110.39(15) | C13 | N1 | C11 | 107.0(3) | |
| C7 | Fe1 | C3 | 113.09(19) | C35 | N2 | C34 | 111.5(3) | |
| C7 | Fe1 | C4 | 141.5(2) | C35 | N2 | C36 | 109.4(3) | |
| C7 | Fe1 | C5 | 178.0(2) | C36 | N2 | C34 | 109.3(3) | |
| C7 | Fe1 | C8 | 39.55(17) | Si1 | C1 | Fe1 | 125.23(15) | |
| C7 | Fe1 | C9 | 66.78(17) | C2 | C1 | Fe1 | 68.68(16) | |
| C8 | Fe1 | C3 | 110.64(15) | C2 | C1 | Si1 | 131.9(2) | |
| C8 | Fe1 | C4 | 112.99(15) | C5 | C1 | Fe1 | 69.63(17) | |
| C9 | Fe1 | C3 | 135.17(18) | C5 | C1 | Si1 | 122.0(2) | |
| C9 | Fe1 | C4 | 110.17(16) | C5 | C1 | C2 | 106.1(3) | |
| C9 | Fe1 | C5 | 114.05(14) | C1 | C2 | Fe1 | 69.62(16) | |
| C9 | Fe1 | C8 | 39.03(16) | C1 | C2 | C11 | 126.9(3) | |
| C10 | Fe1 | C1 | 113.75(16) | C3 | C2 | Fe1 | 70.46(18) | |
| C10 | Fe1 | C2 | 144.4(2) | C3 | C2 | C1 | 107.9(3) | |
| C10 | Fe1 | C3 | 174.2(3) | C3 | C2 | C11 | 125.2(3) | |
| C10 | Fe1 | C4 | 135.2(3) | C11 | C2 | Fe1 | 124.4(2) | |
| C10 | Fe1 | C5 | 111.0(2) | C2 | C3 | Fe1 | 68.44(18) | |
| C10 | Fe1 | C7 | 68.4(2) | C4 | C3 | Fe1 | 70.13(19) | |
| C10 | Fe1 | C8 | 66.60(18) | C4 | C3 | C2 | 108.8(3) | |
| C10 | Fe1 | C9 | 39.6(2) | C3 | C4 | Fe1 | 69.54(19) | |
| C15 | Fe2 | C14 | 41.02(11) | C5 | C4 | Fe1 | 69.26(18) | |
| C15 | Fe2 | C16 | 40.89(11) | C5 | C4 | C3 | 107.5(3) | |
| C15 | Fe2 | C17 | 68.53(12) | C1 | C5 | Fe1 | 69.15(16) | |
| C15 | Fe2 | C19 | 122.10(14) | C4 | C5 | Fe1 | 70.45(19) | |
| C15 | Fe2 | C20 | 108.32(13) | C4 | C5 | C1 | 109.8(3) | |
| C15 | Fe2 | C21 | 124.28(14) | C7 | C6 | Fe1 | 70.8(3) | |
| C16 | Fe2 | C14 | 69.39(12) | C7 | C6 | C10 | 106.2(4) | |
| C16 | Fe2 | C17 | 40.59(12) | C10 | C6 | Fe1 | 69.1(3) | |
| C16 | Fe2 | C19 | 157.67(15) | C6 | C7 | Fe1 | 68.8(3) | |
| C16 | Fe2 | C20 | 122.30(15) | C8 | C7 | Fe1 | 71.1(2) | |
| C16 | Fe2 | C21 | 107.49(14) | C8 | C7 | C6 | 108.3(5) | |
| C17 | Fe2 | C14 | 69.46(12) | C7 | C8 | Fe1 | 69.4(2) | |
| C17 | Fe2 | C21 | 121.43(14) | C9 | C8 | Fe1 | 70.2(2) | |
| C18 | Fe2 | C14 | 41.31(11) | C9 | C8 | C7 | 109.3(4) | |
| C18 | Fe2 | C15 | 68.49(12) | C8 | C9 | Fe1 | 70.8(2) | |
| C18 | Fe2 | C16 | 68.49(12) | C8 | C9 | C10 | 108.9(4) | |
| C18 | Fe2 | C17 | 40.77(12) | C10 | C9 | Fe1 | 68.8(2) | |
| C18 | Fe2 | C19 | 124.21(14) | C6 | C10 | Fe1 | 68.7(3) | |
| C18 | Fe2 | C20 | 160.87(14) | C9 | C10 | Fe1 | 71.6(3) | |
| C18 | Fe2 | C21 | 156.94(13) | C9 | C10 | C6 | 107.4(5) | |
| C19 | Fe2 | C14 | 107.02(13) | C2 | C11 | N1 | 114.0(3) | |
| C19 | Fe2 | C17 | 160.59(15) | Si1 | C14 | Fe2 | 128.27(16) | |
| C19 | Fe2 | C20 | 40.24(15) | C15 | C14 | Fe2 | 68.90(16) | |
| C19 | Fe2 | C21 | 68.17(15) | C15 | C14 | Si1 | 132.1(2) | |
| C20 | Fe2 | C14 | 123.87(13) | C15 | C14 | C18 | 105.7(2) | |
| C20 | Fe2 | C17 | 157.35(15) | C18 | C14 | Fe2 | 68.69(16) | |
| C20 | Fe2 | C21 | 40.47(14) | C18 | C14 | Si1 | 122.2(2) | |
| C21 | Fe2 | C14 | 160.58(13) | C14 | C15 | Fe2 | 70.08(16) | |
| C22 | Fe2 | C14 | 156.78(14) | C16 | C15 | Fe2 | 69.76(17) | |
| C22 | Fe2 | C15 | 160.84(14) | C16 | C15 | C14 | 109.3(3) | |
| C22 | Fe2 | C16 | 123.80(14) | C15 | C16 | Fe2 | 69.35(16) | |
| C22 | Fe2 | C17 | 107.12(14) | C17 | C16 | Fe2 | 69.82(17) | |
| C22 | Fe2 | C18 | 121.21(14) | C17 | C16 | C15 | 107.9(3) | |
| C22 | Fe2 | C19 | 68.18(15) | C16 | C17 | Fe2 | 69.59(17) | |
| C22 | Fe2 | C20 | 68.08(15) | C16 | C17 | C18 | 107.8(3) | |
| C22 | Fe2 | C21 | 40.79(15) | C18 | C17 | Fe2 | 69.23(17) | |
| C22 | Fe2 | C23 | 40.83(15) | C14 | C18 | Fe2 | 70.00(17) | |
| C23 | Fe2 | C14 | 120.92(13) | C17 | C18 | Fe2 | 70.01(17) | |
| C23 | Fe2 | C15 | 156.97(14) | C17 | C18 | C14 | 109.2(3) | |
| C23 | Fe2 | C16 | 160.74(14) | C20 | C19 | Fe2 | 69.9(2) | |
| C23 | Fe2 | C17 | 124.21(14) | C23 | C19 | Fe2 | 69.6(2) | |
| C23 | Fe2 | C18 | 107.53(14) | C23 | C19 | C20 | 108.0(3) | |
| C23 | Fe2 | C19 | 40.05(15) | C19 | C20 | Fe2 | 69.8(2) | |
| C23 | Fe2 | C20 | 67.57(16) | C19 | C20 | C21 | 108.6(3) | |
| C23 | Fe2 | C21 | 68.35(15) | C21 | C20 | Fe2 | 69.8(2) | |
| C24 | Fe3 | C27 | 69.71(12) | C20 | C21 | Fe2 | 69.75(19) | |
| C24 | Fe3 | C32 | 154.04(15) | C20 | C21 | C22 | 107.1(3) | |
| C25 | Fe3 | C24 | 41.68(12) | C22 | C21 | Fe2 | 68.95(19) | |
| C25 | Fe3 | C26 | 41.22(13) | C21 | C22 | Fe2 | 70.26(19) | |
| C25 | Fe3 | C27 | 69.20(13) | C23 | C22 | Fe2 | 69.78(19) | |
| C25 | Fe3 | C28 | 69.03(12) | C23 | C22 | C21 | 107.8(3) | |
| C25 | Fe3 | C29 | 116.77(14) | C19 | C23 | Fe2 | 70.4(2) | |
| C25 | Fe3 | C30 | 105.02(15) | C19 | C23 | C22 | 108.5(3) | |
| C25 | Fe3 | C31 | 125.27(16) | C22 | C23 | Fe2 | 69.38(19) | |
| C25 | Fe3 | C32 | 163.94(16) | Si2 | C24 | Fe3 | 123.83(15) | |
| C25 | Fe3 | C33 | 152.04(15) | C25 | C24 | Fe3 | 68.41(16) | |
| C26 | Fe3 | C24 | 69.79(12) | C25 | C24 | Si2 | 129.8(2) | |
| C26 | Fe3 | C27 | 40.68(14) | C28 | C24 | Fe3 | 69.06(16) | |
| C26 | Fe3 | C28 | 68.42(13) | C28 | C24 | Si2 | 124.4(2) | |
| C26 | Fe3 | C29 | 150.71(15) | C28 | C24 | C25 | 105.7(3) | |
| C26 | Fe3 | C30 | 116.62(15) | C24 | C25 | Fe3 | 69.92(17) | |
| C26 | Fe3 | C31 | 106.55(16) | C24 | C25 | C34 | 125.9(3) | |
| C26 | Fe3 | C32 | 127.42(16) | C26 | C25 | Fe3 | 69.80(19) | |
| C26 | Fe3 | C33 | 166.44(15) | C26 | C25 | C24 | 108.5(3) | |
| C27 | Fe3 | C32 | 109.38(15) | C26 | C25 | C34 | 125.5(3) | |
| C28 | Fe3 | C24 | 41.32(11) | C34 | C25 | Fe3 | 123.2(2) | |
| C28 | Fe3 | C27 | 40.65(13) | C25 | C26 | Fe3 | 68.98(18) | |
| C28 | Fe3 | C29 | 129.02(15) | C27 | C26 | Fe3 | 70.1(2) | |
| C28 | Fe3 | C32 | 121.01(15) | C27 | C26 | C25 | 108.6(3) | |
| C28 | Fe3 | C33 | 110.35(14) | C26 | C27 | Fe3 | 69.17(19) | |
| C29 | Fe3 | C24 | 106.76(14) | C28 | C27 | Fe3 | 69.25(18) | |
| C29 | Fe3 | C27 | 167.38(15) | C28 | C27 | C26 | 107.5(3) | |
| C29 | Fe3 | C32 | 68.16(16) | C24 | C28 | Fe3 | 69.62(16) | |
| C29 | Fe3 | C33 | 40.52(15) | C27 | C28 | Fe3 | 70.10(18) | |
| C30 | Fe3 | C24 | 125.43(14) | C27 | C28 | C24 | 109.8(3) | |
| C30 | Fe3 | C27 | 151.44(16) | C30 | C29 | Fe3 | 69.7(2) | |
| C30 | Fe3 | C28 | 165.24(15) | C30 | C29 | C33 | 108.3(4) | |
| C30 | Fe3 | C29 | 40.41(16) | C33 | C29 | Fe3 | 69.9(2) | |
| C30 | Fe3 | C32 | 68.18(16) | C29 | C30 | Fe3 | 69.9(2) | |
| C30 | Fe3 | C33 | 68.19(16) | C29 | C30 | C31 | 107.9(4) | |
| C31 | Fe3 | C24 | 163.59(16) | C31 | C30 | Fe3 | 69.6(2) | |
| C31 | Fe3 | C27 | 118.58(16) | C30 | C31 | Fe3 | 69.6(2) | |
| C31 | Fe3 | C28 | 153.58(16) | C32 | C31 | Fe3 | 70.5(2) | |
| C31 | Fe3 | C29 | 68.17(17) | C32 | C31 | C30 | 108.3(4) | |
| C31 | Fe3 | C30 | 40.76(17) | C31 | C32 | Fe3 | 69.2(2) | |
| C31 | Fe3 | C32 | 40.30(17) | C31 | C32 | C33 | 107.7(4) | |
| C31 | Fe3 | C33 | 68.19(17) | C33 | C32 | Fe3 | 69.3(2) | |
| C33 | Fe3 | C24 | 118.84(14) | C29 | C33 | Fe3 | 69.6(2) | |
| C33 | Fe3 | C27 | 129.67(15) | C29 | C33 | C32 | 107.8(4) | |
| C33 | Fe3 | C32 | 40.69(16) | C32 | C33 | Fe3 | 70.0(2) | |
| C38 | Fe4 | C37 | 41.03(13) | N2 | C34 | C25 | 113.7(3) | |
| C38 | Fe4 | C39 | 40.54(17) | Si2 | C37 | Fe4 | 128.82(16) | |
| C38 | Fe4 | C41 | 67.81(18) | C38 | C37 | Fe4 | 68.42(19) | |
| C38 | Fe4 | C44 | 125.51(16) | C38 | C37 | Si2 | 128.8(3) | |
| C38 | Fe4 | C45 | 162.39(15) | C41 | C37 | Fe4 | 68.9(2) | |
| C38 | Fe4 | C46 | 155.97(15) | C41 | C37 | Si2 | 125.6(3) | |
| C39 | Fe4 | C37 | 69.08(14) | C41 | C37 | C38 | 105.6(3) | |
| C39 | Fe4 | C41 | 68.3(2) | C37 | C38 | Fe4 | 70.6(2) | |
| C39 | Fe4 | C44 | 106.40(17) | C39 | C38 | Fe4 | 69.7(3) | |
| C39 | Fe4 | C45 | 125.12(17) | C39 | C38 | C37 | 109.4(4) | |
| C39 | Fe4 | C46 | 162.6(2) | C38 | C39 | Fe4 | 69.7(2) | |
| C40 | Fe4 | C37 | 68.60(15) | C40 | C39 | Fe4 | 70.1(3) | |
| C40 | Fe4 | C38 | 67.4(2) | C40 | C39 | C38 | 107.7(4) | |
| C40 | Fe4 | C39 | 39.8(2) | C39 | C40 | Fe4 | 70.1(2) | |
| C40 | Fe4 | C41 | 41.00(17) | C39 | C40 | C41 | 108.8(4) | |
| C40 | Fe4 | C44 | 118.75(16) | C41 | C40 | Fe4 | 69.7(2) | |
| C40 | Fe4 | C45 | 108.05(19) | C37 | C41 | Fe4 | 70.68(19) | |
| C40 | Fe4 | C46 | 127.1(2) | C37 | C41 | C40 | 108.5(4) | |
| C41 | Fe4 | C37 | 40.42(14) | C40 | C41 | Fe4 | 69.3(2) | |
| C41 | Fe4 | C44 | 154.17(15) | C43 | C42 | Fe4 | 69.8(2) | |
| C41 | Fe4 | C46 | 109.2(2) | C43 | C42 | C46 | 108.4(3) | |
| C42 | Fe4 | C37 | 108.89(14) | C46 | C42 | Fe4 | 70.1(2) | |
| C42 | Fe4 | C38 | 121.11(16) | C42 | C43 | Fe4 | 69.9(2) | |
| C42 | Fe4 | C39 | 154.5(2) | C42 | C43 | C44 | 108.0(4) | |
| C42 | Fe4 | C40 | 165.0(2) | C44 | C43 | Fe4 | 70.2(2) | |
| C42 | Fe4 | C41 | 127.67(19) | C43 | C44 | Fe4 | 69.2(2) | |
| C42 | Fe4 | C44 | 67.94(16) | C45 | C44 | Fe4 | 69.7(2) | |
| C42 | Fe4 | C45 | 67.62(16) | C45 | C44 | C43 | 107.3(4) | |
| C42 | Fe4 | C46 | 40.50(17) | C44 | C45 | Fe4 | 70.0(2) | |
| C43 | Fe4 | C37 | 126.60(14) | C46 | C45 | Fe4 | 70.0(2) | |
| C43 | Fe4 | C38 | 108.00(17) | C46 | C45 | C44 | 108.8(3) | |
| C43 | Fe4 | C39 | 119.1(2) | C42 | C46 | Fe4 | 69.4(2) | |
| C43 | Fe4 | C40 | 152.9(2) | C45 | C46 | Fe4 | 69.9(2) | |
| C43 | Fe4 | C41 | 164.37(16) | C45 | C46 | C42 | 107.4(4) | |
| C43 | Fe4 | C42 | 40.38(18) |
| D | H | A | d(D-H)/Å | d(H-A)/Å | d(D-A)/Å | D-H-A/° |
|---|---|---|---|---|---|---|
| O2 | H2 | N2 | 0.95(5) | 2.10(5) | 2.722(3) | 122(4) |
| O3 | H3 | N1 | 0.73(4) | 2.01(4) | 2.719(4) | 167(4) |
| A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|---|---|
| Fe1 | C1 | C2 | C3 | -60.3(2) | C3 | C2 | C11 | N1 | -96.3(4) | |
| Fe1 | C1 | C2 | C11 | 118.3(3) | C3 | C4 | C5 | Fe1 | 59.3(2) | |
| Fe1 | C1 | C5 | C4 | 58.8(2) | C3 | C4 | C5 | C1 | 1.2(4) | |
| Fe1 | C2 | C3 | C4 | -58.6(2) | C5 | C1 | C2 | Fe1 | 59.93(19) | |
| Fe1 | C2 | C11 | N1 | 174.5(2) | C5 | C1 | C2 | C3 | -0.4(3) | |
| Fe1 | C3 | C4 | C5 | -59.1(2) | C5 | C1 | C2 | C11 | 178.2(3) | |
| Fe1 | C4 | C5 | C1 | -58.0(2) | C6 | C7 | C8 | Fe1 | -58.9(3) | |
| Fe1 | C6 | C7 | C8 | 60.4(3) | C6 | C7 | C8 | C9 | 0.0(5) | |
| Fe1 | C6 | C10 | C9 | -61.6(3) | C7 | C6 | C10 | Fe1 | 61.5(3) | |
| Fe1 | C7 | C8 | C9 | 59.0(3) | C7 | C6 | C10 | C9 | -0.1(5) | |
| Fe1 | C8 | C9 | C10 | 58.4(3) | C7 | C8 | C9 | Fe1 | -58.5(3) | |
| Fe1 | C9 | C10 | C6 | 59.7(3) | C7 | C8 | C9 | C10 | -0.1(4) | |
| Fe2 | C14 | C15 | C16 | -58.9(2) | C8 | C9 | C10 | Fe1 | -59.6(3) | |
| Fe2 | C14 | C18 | C17 | 59.2(2) | C8 | C9 | C10 | C6 | 0.1(5) | |
| Fe2 | C15 | C16 | C17 | -59.4(2) | C10 | C6 | C7 | Fe1 | -60.4(3) | |
| Fe2 | C16 | C17 | C18 | -58.8(2) | C10 | C6 | C7 | C8 | 0.0(5) | |
| Fe2 | C17 | C18 | C14 | -59.2(2) | C11 | C2 | C3 | Fe1 | -118.9(3) | |
| Fe2 | C19 | C20 | C21 | 59.2(2) | C11 | C2 | C3 | C4 | -177.5(3) | |
| Fe2 | C19 | C23 | C22 | -59.1(2) | C12 | N1 | C11 | C2 | 54.2(4) | |
| Fe2 | C20 | C21 | C22 | 59.1(2) | C13 | N1 | C11 | C2 | 175.4(3) | |
| Fe2 | C21 | C22 | C23 | 60.0(2) | C14 | Si1 | O1 | Si2 | -153.3(3) | |
| Fe2 | C22 | C23 | C19 | 59.8(2) | C14 | Si1 | C1 | Fe1 | 80.19(19) | |
| Fe3 | C24 | C25 | C26 | -59.4(2) | C14 | Si1 | C1 | C2 | 172.2(3) | |
| Fe3 | C24 | C25 | C34 | 117.1(3) | C14 | Si1 | C1 | C5 | -6.3(3) | |
| Fe3 | C24 | C28 | C27 | 58.7(2) | C14 | C15 | C16 | Fe2 | 59.1(2) | |
| Fe3 | C25 | C26 | C27 | -59.2(2) | C14 | C15 | C16 | C17 | -0.3(3) | |
| Fe3 | C25 | C34 | N2 | 177.1(2) | C15 | C14 | C18 | Fe2 | -59.3(2) | |
| Fe3 | C26 | C27 | C28 | -58.8(2) | C15 | C14 | C18 | C17 | -0.1(3) | |
| Fe3 | C27 | C28 | C24 | -58.4(2) | C15 | C16 | C17 | Fe2 | 59.1(2) | |
| Fe3 | C29 | C30 | C31 | 59.5(3) | C15 | C16 | C17 | C18 | 0.2(3) | |
| Fe3 | C29 | C33 | C32 | -59.8(2) | C16 | C17 | C18 | Fe2 | 59.1(2) | |
| Fe3 | C30 | C31 | C32 | 60.1(3) | C16 | C17 | C18 | C14 | -0.1(4) | |
| Fe3 | C31 | C32 | C33 | 58.8(3) | C18 | C14 | C15 | Fe2 | 59.1(2) | |
| Fe3 | C32 | C33 | C29 | 59.5(2) | C18 | C14 | C15 | C16 | 0.2(3) | |
| Fe4 | C37 | C38 | C39 | 59.1(3) | C19 | C20 | C21 | Fe2 | -59.2(2) | |
| Fe4 | C37 | C41 | C40 | -59.2(3) | C19 | C20 | C21 | C22 | -0.2(4) | |
| Fe4 | C38 | C39 | C40 | 60.1(3) | C20 | C19 | C23 | Fe2 | 59.6(2) | |
| Fe4 | C39 | C40 | C41 | 59.2(3) | C20 | C19 | C23 | C22 | 0.4(4) | |
| Fe4 | C40 | C41 | C37 | 60.0(3) | C20 | C21 | C22 | Fe2 | -59.6(2) | |
| Fe4 | C42 | C43 | C44 | -60.1(3) | C20 | C21 | C22 | C23 | 0.4(4) | |
| Fe4 | C42 | C46 | C45 | 59.8(3) | C21 | C22 | C23 | Fe2 | -60.3(2) | |
| Fe4 | C43 | C44 | C45 | -59.5(3) | C21 | C22 | C23 | C19 | -0.5(4) | |
| Fe4 | C44 | C45 | C46 | -59.4(3) | C23 | C19 | C20 | Fe2 | -59.3(2) | |
| Fe4 | C45 | C46 | C42 | -59.5(3) | C23 | C19 | C20 | C21 | -0.2(4) | |
| Si1 | C1 | C2 | Fe1 | -118.8(3) | C24 | Si2 | O1 | Si1 | 74.1(3) | |
| Si1 | C1 | C2 | C3 | -179.1(2) | C24 | Si2 | C37 | Fe4 | 158.80(19) | |
| Si1 | C1 | C2 | C11 | -0.5(5) | C24 | Si2 | C37 | C38 | 66.5(3) | |
| Si1 | C1 | C5 | Fe1 | 119.6(2) | C24 | Si2 | C37 | C41 | -110.7(3) | |
| Si1 | C1 | C5 | C4 | 178.4(2) | C24 | C25 | C26 | Fe3 | 59.4(2) | |
| Si1 | C14 | C15 | Fe2 | -123.1(3) | C24 | C25 | C26 | C27 | 0.3(4) | |
| Si1 | C14 | C15 | C16 | 178.0(2) | C24 | C25 | C34 | N2 | 88.9(4) | |
| Si1 | C14 | C18 | Fe2 | 122.7(2) | C25 | C24 | C28 | Fe3 | -58.89(19) | |
| Si1 | C14 | C18 | C17 | -178.1(2) | C25 | C24 | C28 | C27 | -0.2(3) | |
| Si2 | C24 | C25 | Fe3 | -116.7(2) | C25 | C26 | C27 | Fe3 | 58.4(2) | |
| Si2 | C24 | C25 | C26 | -176.1(2) | C25 | C26 | C27 | C28 | -0.4(4) | |
| Si2 | C24 | C25 | C34 | 0.4(5) | C26 | C25 | C34 | N2 | -95.2(4) | |
| Si2 | C24 | C28 | Fe3 | 117.4(2) | C26 | C27 | C28 | Fe3 | 58.8(2) | |
| Si2 | C24 | C28 | C27 | 176.1(2) | C26 | C27 | C28 | C24 | 0.4(4) | |
| Si2 | C37 | C38 | Fe4 | 123.2(3) | C28 | C24 | C25 | Fe3 | 59.31(19) | |
| Si2 | C37 | C38 | C39 | -177.8(3) | C28 | C24 | C25 | C26 | 0.0(3) | |
| Si2 | C37 | C41 | Fe4 | -123.4(3) | C28 | C24 | C25 | C34 | 176.4(3) | |
| Si2 | C37 | C41 | C40 | 177.5(3) | C29 | C30 | C31 | Fe3 | -59.7(2) | |
| O1 | Si1 | C1 | Fe1 | -167.88(15) | C29 | C30 | C31 | C32 | 0.4(4) | |
| O1 | Si1 | C1 | C2 | -75.8(3) | C30 | C29 | C33 | Fe3 | 59.3(2) | |
| O1 | Si1 | C1 | C5 | 105.6(2) | C30 | C29 | C33 | C32 | -0.5(4) | |
| O1 | Si1 | C14 | Fe2 | 60.1(2) | C30 | C31 | C32 | Fe3 | -59.6(3) | |
| O1 | Si1 | C14 | C15 | 155.6(3) | C30 | C31 | C32 | C33 | -0.7(4) | |
| O1 | Si1 | C14 | C18 | -27.0(3) | C31 | C32 | C33 | Fe3 | -58.8(3) | |
| O1 | Si2 | C24 | Fe3 | -172.83(15) | C31 | C32 | C33 | C29 | 0.8(4) | |
| O1 | Si2 | C24 | C25 | -83.9(3) | C33 | C29 | C30 | Fe3 | -59.5(2) | |
| O1 | Si2 | C24 | C28 | 100.7(3) | C33 | C29 | C30 | C31 | 0.0(4) | |
| O1 | Si2 | C37 | Fe4 | 41.4(2) | C34 | C25 | C26 | Fe3 | -117.1(3) | |
| O1 | Si2 | C37 | C38 | -50.9(3) | C34 | C25 | C26 | C27 | -176.2(3) | |
| O1 | Si2 | C37 | C41 | 131.9(3) | C35 | N2 | C34 | C25 | 66.2(4) | |
| O2 | Si1 | O1 | Si2 | -28.5(4) | C36 | N2 | C34 | C25 | -172.7(3) | |
| O2 | Si1 | C1 | Fe1 | -44.2(2) | C37 | Si2 | O1 | Si1 | -169.0(3) | |
| O2 | Si1 | C1 | C2 | 47.8(3) | C37 | Si2 | C24 | Fe3 | 69.2(2) | |
| O2 | Si1 | C1 | C5 | -130.7(2) | C37 | Si2 | C24 | C25 | 158.1(3) | |
| O2 | Si1 | C14 | Fe2 | -63.5(2) | C37 | Si2 | C24 | C28 | -17.2(3) | |
| O2 | Si1 | C14 | C15 | 31.9(3) | C37 | C38 | C39 | Fe4 | -59.6(2) | |
| O2 | Si1 | C14 | C18 | -150.6(2) | C37 | C38 | C39 | C40 | 0.5(5) | |
| O3 | Si2 | O1 | Si1 | -47.2(4) | C38 | C37 | C41 | Fe4 | 58.9(2) | |
| O3 | Si2 | C24 | Fe3 | -51.0(2) | C38 | C37 | C41 | C40 | -0.3(4) | |
| O3 | Si2 | C24 | C25 | 37.9(3) | C38 | C39 | C40 | Fe4 | -59.8(3) | |
| O3 | Si2 | C24 | C28 | -137.5(2) | C38 | C39 | C40 | C41 | -0.7(5) | |
| O3 | Si2 | C37 | Fe4 | -80.9(2) | C39 | C40 | C41 | Fe4 | -59.4(3) | |
| O3 | Si2 | C37 | C38 | -173.2(3) | C39 | C40 | C41 | C37 | 0.6(5) | |
| O3 | Si2 | C37 | C41 | 9.6(4) | C41 | C37 | C38 | Fe4 | -59.2(3) | |
| C1 | Si1 | O1 | Si2 | 94.3(3) | C41 | C37 | C38 | C39 | -0.1(4) | |
| C1 | Si1 | C14 | Fe2 | 174.14(17) | C42 | C43 | C44 | Fe4 | 59.9(3) | |
| C1 | Si1 | C14 | C15 | -90.4(3) | C42 | C43 | C44 | C45 | 0.4(4) | |
| C1 | Si1 | C14 | C18 | 87.0(3) | C43 | C42 | C46 | Fe4 | -59.5(3) | |
| C1 | C2 | C3 | Fe1 | 59.8(2) | C43 | C42 | C46 | C45 | 0.3(5) | |
| C1 | C2 | C3 | C4 | 1.2(4) | C43 | C44 | C45 | Fe4 | 59.2(3) | |
| C1 | C2 | C11 | N1 | 85.3(4) | C43 | C44 | C45 | C46 | -0.2(5) | |
| C2 | C1 | C5 | Fe1 | -59.31(19) | C44 | C45 | C46 | Fe4 | 59.4(3) | |
| C2 | C1 | C5 | C4 | -0.5(3) | C44 | C45 | C46 | C42 | -0.1(5) | |
| C2 | C3 | C4 | Fe1 | 57.6(2) | C46 | C42 | C43 | Fe4 | 59.7(3) | |
| C2 | C3 | C4 | C5 | -1.5(4) | C46 | C42 | C43 | C44 | -0.4(4) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| H2 | 2430(30) | 1820(20) | -1450(30) | 73(15) |
| H3 | 4410(30) | 3160(20) | -450(20) | 37(12) |
| H3A | 4441 | 1359 | 1824 | 45 |
| H4 | 2589 | 1355 | 2300 | 44 |
| H5 | 1389 | 1734 | 1244 | 34 |
| H6 | 3101 | 177 | -417 | 122 |
| H7 | 4440 | -196 | 548 | 83 |
| H8 | 3515 | -462 | 1722 | 56 |
| H9 | 1625 | -268 | 1523 | 64 |
| H10 | 1315 | 129 | 218 | 111 |
| H11A | 4518 | 1497 | -220 | 38 |
| H11B | 5269 | 1355 | 482 | 38 |
| H12A | 4798 | 2812 | 1200 | 77 |
| H12B | 5707 | 3271 | 814 | 77 |
| H12C | 5954 | 2481 | 1166 | 77 |
| H13A | 6639 | 2060 | 23 | 80 |
| H13B | 6413 | 2841 | -355 | 80 |
| H13C | 5946 | 2108 | -723 | 80 |
| H15 | 111 | 940 | -473 | 29 |
| H16 | -1674 | 1382 | -87 | 33 |
| H17 | -1503 | 2706 | 335 | 34 |
| H18 | 384 | 3084 | 201 | 30 |
| H19 | 889 | 2493 | -2026 | 54 |
| H20 | -457 | 1496 | -2189 | 52 |
| H21 | -2203 | 1990 | -1776 | 49 |
| H22 | -1913 | 3307 | -1350 | 51 |
| H23 | -3 | 3609 | -1521 | 51 |
| H26 | 2935 | 3272 | -3625 | 43 |
| H27 | 1671 | 4306 | -3354 | 42 |
| H28 | 1622 | 4477 | -1962 | 35 |
| H29 | 5015 | 4529 | -1537 | 51 |
| H30 | 5553 | 3913 | -2726 | 56 |
| H31 | 4655 | 4573 | -3797 | 66 |
| H32 | 3581 | 5608 | -3271 | 61 |
| H33 | 3783 | 5570 | -1864 | 53 |
| H34A | 4451 | 2608 | -2826 | 40 |
| H34B | 4485 | 2744 | -1948 | 40 |
| H35A | 3483 | 1611 | -3334 | 80 |
| H35B | 2421 | 1921 | -2996 | 80 |
| H35C | 2790 | 1100 | -2812 | 80 |
| H36A | 4943 | 1344 | -2503 | 70 |
| H36B | 4192 | 872 | -1984 | 70 |
| H36C | 4853 | 1540 | -1639 | 70 |
| H38 | 927 | 4503 | -548 | 52 |
| H39 | 1007 | 5765 | 28 | 83 |
| H40 | 2883 | 6069 | 279 | 94 |
| H41 | 3994 | 4987 | -114 | 66 |
| H42 | 2322 | 3276 | 1043 | 68 |
| H43 | 599 | 3926 | 1162 | 65 |
| H44 | 946 | 5178 | 1730 | 55 |
| H45 | 2890 | 5293 | 1942 | 57 |
| H46 | 3746 | 4124 | 1519 | 69 |
Experimental
Single crystals of C46H52Fe4N2O3Si2 [3116] were []. A suitable crystal was selected and [] on a Xcalibur, Sapphire3 diffractometer. The crystal was kept at 150 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 [3116]
Crystal Data for C46H52Fe4N2O3Si2 (M =960.47 g/mol): monoclinic, space group P21/n (no. 14), a = 12.8025(4) Å, b = 18.1923(6) Å, c = 17.9925(7) Å, β = 90.855(3)°, V = 4190.1(2) Å3, Z = 4, T = 150 K, μ(MoKα) = 1.458 mm-1, Dcalc = 1.523 g/cm3, 31598 reflections measured (4.478° ≤ 2Θ ≤ 54°), 9116 unique (Rint = 0.0358, Rsigma = 0.0398) which were used in all calculations. The final R1 was 0.0431 (I > 2σ(I)) and wR2 was 0.1035 (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), C34(H34A,H34B)
2.b Aromatic/amide H refined with riding coordinates:
C3(H3A), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C15(H15),
C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23),
C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
C33(H33), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44),
C45(H45), C46(H46)
2.c Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C35(H35A,H35B,H35C), C36(H36A,H36B,
H36C)
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.