| Identification code | 3202 |
| Empirical formula | C89H119Fe4N4O6Si8 |
| Formula weight | 1788.99 |
| Temperature/K | 173 |
| Crystal system | monoclinic |
| Space group | P21/n |
| a/Å | 10.9706(5) |
| b/Å | 23.7261(9) |
| c/Å | 17.2222(7) |
| α/° | 90.0 |
| β/° | 91.143(4) |
| γ/° | 90.0 |
| Volume/Å3 | 4481.8(3) |
| Z | 2 |
| ρcalcg/cm3 | 1.326 |
| μ/mm‑1 | 0.795 |
| F(000) | 1890.0 |
| Crystal size/mm3 | 0.2 × 0.2 × 0.02 |
| Radiation | MoKα (λ = 0.71073) |
| 2Θ range for data collection/° | 4.362 to 51.994 |
| Index ranges | -13 ≤ h ≤ 13, -29 ≤ k ≤ 29, -20 ≤ l ≤ 21 |
| Reflections collected | 36392 |
| Independent reflections | 8814 [Rint = 0.0490, Rsigma = 0.0475] |
| Data/restraints/parameters | 8814/0/514 |
| Goodness-of-fit on F2 | 1.040 |
| Final R indexes [I>=2σ (I)] | R1 = 0.0387, wR2 = 0.0783 |
| Final R indexes [all data] | R1 = 0.0556, wR2 = 0.0855 |
| Largest diff. peak/hole / e Å-3 | 0.41/-0.29 |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| Fe1 | 5563.2(3) | 5609.5(2) | 8671.3(2) | 21.17(9) |
| Fe2 | 7224.8(3) | 2854.8(2) | 6656.3(2) | 21.44(9) |
| Si1 | 5213.9(6) | 4610.4(3) | 7174.7(4) | 16.97(14) |
| Si2 | 5457.7(6) | 3508.1(3) | 8094.1(4) | 17.89(15) |
| Si3 | 2683.8(6) | 3443.9(3) | 7904.3(4) | 22.10(16) |
| Si4 | 2620.8(6) | 4106.7(3) | 6871.0(4) | 20.81(15) |
| O1 | 5783.2(15) | 4140.9(6) | 7781.5(9) | 20.4(4) |
| O2 | 4023.3(15) | 4341.7(6) | 6728.6(9) | 20.1(4) |
| O3 | 4035.2(15) | 3492.8(7) | 8347.4(9) | 22.0(4) |
| N1 | 4887(2) | 6107.4(9) | 6215.8(12) | 28.1(5) |
| N2 | 5233(2) | 1854.6(10) | 8414.8(15) | 42.6(7) |
| C1 | 4717(2) | 5229.7(9) | 7738.5(13) | 18.2(5) |
| C2 | 4853(2) | 5830.7(9) | 7603.9(13) | 19.2(5) |
| C3 | 4227(2) | 6121.2(10) | 8200.6(14) | 25.3(6) |
| C4 | 3712(2) | 5721.8(11) | 8707.3(15) | 28.1(6) |
| C5 | 4003(2) | 5176.3(10) | 8429.7(14) | 24.1(6) |
| C6 | 7169(2) | 5186.7(11) | 8850.6(15) | 27.6(6) |
| C7 | 7391(2) | 5760.6(11) | 8666.1(15) | 29.2(6) |
| C8 | 6840(3) | 6098.3(11) | 9239.3(15) | 31.9(6) |
| C9 | 6262(3) | 5736.0(11) | 9773.0(15) | 32.0(6) |
| C10 | 6467(3) | 5171.9(11) | 9531.6(15) | 30.5(6) |
| C11 | 5543(2) | 6104.7(10) | 6962.7(13) | 22.0(5) |
| C12 | 5701(3) | 6307.8(12) | 5613.1(15) | 39.7(7) |
| C13 | 3820(3) | 6467.2(15) | 6240.5(19) | 53.8(9) |
| C14 | 6385(2) | 4750.3(9) | 6425.1(13) | 18.4(5) |
| C15 | 7584(2) | 4901.3(10) | 6628.4(15) | 23.5(5) |
| C16 | 8455(2) | 4983.8(11) | 6061.7(16) | 28.7(6) |
| C17 | 8148(2) | 4913.7(11) | 5286.2(16) | 31.1(6) |
| C18 | 6967(2) | 4768.5(11) | 5067.7(15) | 30.3(6) |
| C19 | 6103(2) | 4689.3(10) | 5636.5(14) | 25.0(6) |
| C20 | 5686(2) | 3000.7(9) | 7288.2(14) | 20.3(5) |
| C21 | 6019(2) | 2409.8(10) | 7312.7(15) | 22.6(5) |
| C22 | 6011(2) | 2201.5(10) | 6537.5(15) | 26.0(6) |
| C23 | 5693(2) | 2646.3(10) | 6023.5(15) | 25.2(6) |
| C24 | 5485(2) | 3136.1(10) | 6480.9(14) | 21.4(5) |
| C25 | 8521(2) | 3441.1(11) | 6965.0(16) | 30.1(6) |
| C26 | 8869(2) | 2898.6(11) | 7237.2(17) | 32.9(6) |
| C27 | 8949(2) | 2539.5(12) | 6583.5(18) | 35.1(7) |
| C28 | 8648(3) | 2857.5(11) | 5907.6(17) | 35.2(7) |
| C29 | 8387(3) | 3420.1(11) | 6146.2(16) | 32.5(7) |
| C30 | 6321(2) | 2063.6(10) | 8022.0(15) | 29.5(6) |
| C31 | 4577(3) | 1452.6(14) | 7922(2) | 57.3(10) |
| C32 | 5600(4) | 1581.6(13) | 9145.5(19) | 58.6(11) |
| C33 | 6387(2) | 3351.1(10) | 8987.4(13) | 20.5(5) |
| C34 | 7632(2) | 3473.6(11) | 9052.9(15) | 27.9(6) |
| C35 | 8325(3) | 3303.6(12) | 9692.4(16) | 34.9(7) |
| C36 | 7783(3) | 3010.1(11) | 10289.2(15) | 32.3(6) |
| C37 | 6555(3) | 2892.9(11) | 10247.0(15) | 29.2(6) |
| C38 | 5866(2) | 3061.1(10) | 9604.5(14) | 24.8(6) |
| C39 | 2488(3) | 2717.6(11) | 7504.1(17) | 35.6(7) |
| C40 | 1524(3) | 3573.5(13) | 8659.7(16) | 38.5(7) |
| C41 | 2087(2) | 3740.6(11) | 5969.5(14) | 30.6(6) |
| C42 | 1609(3) | 4723.8(12) | 7057.6(16) | 35.6(7) |
| C43 | 704(6) | 5743(3) | 8712(4) | 46.2(16) |
| C44 | 568(4) | 5246(2) | 8999(3) | 85.7(15) |
| C46 | 130(4) | 5282.8(16) | 9830(2) | 75.4(13) |
| Atom | U11 | U22 | U33 | U23 | U13 | U12 |
|---|---|---|---|---|---|---|
| Fe1 | 24.8(2) | 21.33(18) | 17.36(19) | -0.67(14) | 0.63(15) | -4.24(15) |
| Fe2 | 21.3(2) | 19.67(18) | 23.4(2) | 1.10(14) | 3.53(15) | 2.83(15) |
| Si1 | 17.6(3) | 15.8(3) | 17.5(3) | 0.9(3) | 0.0(3) | -0.9(3) |
| Si2 | 18.3(3) | 18.7(3) | 16.6(3) | 2.8(3) | 1.0(3) | 0.7(3) |
| Si3 | 18.5(4) | 26.3(4) | 21.6(4) | 0.5(3) | 3.1(3) | -3.1(3) |
| Si4 | 18.3(4) | 25.2(4) | 18.9(4) | -1.3(3) | -0.9(3) | -0.7(3) |
| O1 | 21.4(9) | 18.8(8) | 20.9(9) | 3.1(7) | -1.8(7) | -2.3(7) |
| O2 | 21.2(9) | 18.7(8) | 20.4(9) | -0.3(7) | -0.3(7) | -2.5(7) |
| O3 | 19.3(9) | 26.5(9) | 20.2(9) | 2.1(7) | 1.8(7) | 0.0(7) |
| N1 | 32.0(13) | 30.8(12) | 21.4(11) | 1.2(9) | -3.5(10) | 2.5(10) |
| N2 | 47.8(16) | 34.5(13) | 46.3(16) | 19.2(12) | 21.0(13) | 14.0(12) |
| C1 | 16.5(12) | 19.5(12) | 18.5(12) | -2.2(10) | -2.2(10) | -2.1(10) |
| C2 | 18.5(13) | 20.6(12) | 18.3(12) | 0.7(10) | -3.1(10) | -0.6(10) |
| C3 | 27.2(15) | 20.5(12) | 28.1(14) | -6.1(11) | 0.4(11) | 0.6(11) |
| C4 | 25.6(15) | 33.0(14) | 25.9(14) | -4.9(11) | 8.1(12) | 0.3(12) |
| C5 | 25.6(14) | 25.1(13) | 21.8(13) | 0.6(10) | 2.0(11) | -4.6(11) |
| C6 | 27.4(15) | 30.4(14) | 24.8(14) | -1.5(11) | -4.8(11) | 1.6(12) |
| C7 | 25.0(15) | 37.6(15) | 25.0(14) | 4.7(12) | -2.2(11) | -8.9(12) |
| C8 | 39.5(17) | 27.3(14) | 28.5(15) | 0.8(12) | -12.1(13) | -9.7(13) |
| C9 | 40.0(17) | 38.1(15) | 17.9(13) | -1.3(12) | -1.9(12) | -4.0(13) |
| C10 | 38.3(17) | 30.7(14) | 22.4(14) | 8.3(11) | -3.9(12) | -7.3(13) |
| C11 | 25.3(14) | 19.5(12) | 21.2(13) | -0.4(10) | -1.2(11) | -0.1(10) |
| C12 | 57(2) | 40.0(16) | 22.0(15) | 6.2(12) | 1.4(14) | -2.7(15) |
| C13 | 47(2) | 72(2) | 41.9(19) | 8.7(17) | -8.2(16) | 26.0(18) |
| C14 | 20.5(13) | 13.8(11) | 20.7(13) | 1.1(9) | 0.6(10) | 2.4(10) |
| C15 | 24.3(14) | 23.6(13) | 22.4(13) | 1.4(10) | -3.1(11) | -1.9(11) |
| C16 | 17.4(13) | 30.8(14) | 38.0(16) | 9.3(12) | 1.6(12) | 0.1(11) |
| C17 | 27.3(15) | 36.9(15) | 29.4(15) | 11.9(12) | 11.4(12) | 5.1(12) |
| C18 | 31.4(16) | 40.1(16) | 19.3(13) | 4.8(12) | 1.9(12) | 5.2(13) |
| C19 | 21.0(14) | 28.9(14) | 25.0(14) | 4.8(11) | -2.1(11) | 3.0(11) |
| C20 | 18.7(13) | 19.8(12) | 22.4(13) | 2.8(10) | 2.9(10) | 2.3(10) |
| C21 | 18.9(13) | 19.4(12) | 29.8(14) | 2.4(10) | 5.3(11) | 0.6(10) |
| C22 | 24.9(14) | 18.2(12) | 34.9(15) | -4.6(11) | 4.4(12) | -1.0(11) |
| C23 | 25.0(14) | 27.8(13) | 22.8(13) | -3.1(11) | 0.6(11) | 0.0(11) |
| C24 | 22.2(13) | 21.1(12) | 20.8(13) | 1.5(10) | -0.7(10) | 2.7(10) |
| C25 | 23.3(14) | 27.6(14) | 39.5(17) | -3.2(12) | 4.0(12) | -3.3(12) |
| C26 | 24.2(15) | 37.7(16) | 36.8(16) | 3.3(13) | -0.5(12) | 1.2(12) |
| C27 | 21.0(14) | 28.0(14) | 57(2) | 0.6(14) | 5.2(13) | 7.5(12) |
| C28 | 29.3(16) | 39.6(16) | 37.1(17) | -6.8(13) | 15.4(13) | -2.6(13) |
| C29 | 30.3(16) | 30.2(14) | 37.5(17) | 6.6(12) | 11.0(13) | -2.0(12) |
| C30 | 32.2(16) | 21.9(13) | 34.7(16) | 5.9(11) | 6.0(13) | 7.9(11) |
| C31 | 38(2) | 48(2) | 86(3) | 29.8(19) | 13.0(19) | -3.1(16) |
| C32 | 89(3) | 40.6(18) | 47(2) | 24.6(16) | 28(2) | 23.8(19) |
| C33 | 23.7(13) | 19.4(12) | 18.4(13) | 0.9(10) | -0.9(10) | 3(1) |
| C34 | 28.5(15) | 32.9(14) | 22.4(14) | 6.1(11) | 1.7(12) | -1.0(12) |
| C35 | 21.6(15) | 49.1(17) | 33.9(16) | 3.0(14) | -2.5(12) | 0.2(13) |
| C36 | 33.8(16) | 40.7(16) | 22.2(14) | 5.8(12) | -5.9(12) | 9.3(13) |
| C37 | 38.2(17) | 28.3(14) | 21.4(14) | 6.8(11) | 5.1(12) | 5.1(12) |
| C38 | 23.2(14) | 28.1(13) | 23.1(13) | 3.3(11) | 2.9(11) | 0.7(11) |
| C39 | 36.1(17) | 29.5(15) | 41.3(17) | 0.0(13) | 2.1(13) | -8.4(13) |
| C40 | 24.5(15) | 59.1(19) | 32.2(16) | 1.7(14) | 6.3(13) | -0.3(14) |
| C41 | 29.3(15) | 39.1(15) | 23.1(14) | -2.0(12) | -4.4(12) | -11.2(13) |
| C42 | 27.3(16) | 45.4(17) | 33.9(16) | -1.2(13) | -3.5(13) | 9.9(13) |
| C43 | 35(4) | 44(4) | 59(4) | -2(3) | -1(3) | 9(3) |
| C44 | 43(2) | 112(4) | 103(4) | -49(3) | 10(2) | -3(2) |
| C46 | 40(2) | 100(3) | 85(3) | -47(3) | -11(2) | 8(2) |
| Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
|---|---|---|---|---|---|---|
| Fe1 | C1 | 2.048(2) | N2 | C31 | 1.458(4) | |
| Fe1 | C2 | 2.050(2) | N2 | C32 | 1.465(4) | |
| Fe1 | C3 | 2.057(3) | C1 | C2 | 1.453(3) | |
| Fe1 | C4 | 2.050(3) | C1 | C5 | 1.443(3) | |
| Fe1 | C5 | 2.032(3) | C2 | C3 | 1.425(3) | |
| Fe1 | C6 | 2.045(3) | C2 | C11 | 1.499(3) | |
| Fe1 | C7 | 2.038(3) | C3 | C4 | 1.414(3) | |
| Fe1 | C8 | 2.051(3) | C4 | C5 | 1.418(3) | |
| Fe1 | C9 | 2.054(3) | C6 | C7 | 1.421(4) | |
| Fe1 | C10 | 2.049(3) | C6 | C10 | 1.416(4) | |
| Fe2 | C20 | 2.056(2) | C7 | C8 | 1.416(4) | |
| Fe2 | C21 | 2.050(2) | C8 | C9 | 1.417(4) | |
| Fe2 | C22 | 2.051(2) | C9 | C10 | 1.421(4) | |
| Fe2 | C23 | 2.046(3) | C14 | C15 | 1.401(3) | |
| Fe2 | C24 | 2.038(2) | C14 | C19 | 1.394(3) | |
| Fe2 | C25 | 2.052(3) | C15 | C16 | 1.394(3) | |
| Fe2 | C26 | 2.048(3) | C16 | C17 | 1.381(4) | |
| Fe2 | C27 | 2.040(3) | C17 | C18 | 1.385(4) | |
| Fe2 | C28 | 2.045(3) | C18 | C19 | 1.390(3) | |
| Fe2 | C29 | 2.059(3) | C20 | C21 | 1.449(3) | |
| Si1 | O1 | 1.6422(17) | C20 | C24 | 1.440(3) | |
| Si1 | O2 | 1.6318(17) | C21 | C22 | 1.423(3) | |
| Si1 | C1 | 1.849(2) | C21 | C30 | 1.504(3) | |
| Si1 | C14 | 1.869(2) | C22 | C23 | 1.417(3) | |
| Si2 | O1 | 1.6368(16) | C23 | C24 | 1.425(3) | |
| Si2 | O3 | 1.6292(17) | C25 | C26 | 1.420(4) | |
| Si2 | C20 | 1.858(2) | C25 | C29 | 1.416(4) | |
| Si2 | C33 | 1.866(3) | C26 | C27 | 1.416(4) | |
| Si3 | Si4 | 2.3748(10) | C27 | C28 | 1.420(4) | |
| Si3 | O3 | 1.6578(18) | C28 | C29 | 1.427(4) | |
| Si3 | C39 | 1.867(3) | C33 | C34 | 1.399(3) | |
| Si3 | C40 | 1.863(3) | C33 | C38 | 1.398(3) | |
| Si4 | O2 | 1.6593(17) | C34 | C35 | 1.386(4) | |
| Si4 | C41 | 1.863(3) | C35 | C36 | 1.385(4) | |
| Si4 | C42 | 1.869(3) | C36 | C37 | 1.376(4) | |
| N1 | C11 | 1.461(3) | C37 | C38 | 1.386(4) | |
| N1 | C12 | 1.462(3) | C43 | C44 | 1.289(7) | |
| N1 | C13 | 1.450(4) | C44 | C46 | 1.521(5) | |
| N2 | C30 | 1.470(3) | C46 | C461 | 1.494(8) |
| Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|
| C1 | Fe1 | C2 | 41.52(9) | O2 | Si4 | Si3 | 108.67(7) | |
| C1 | Fe1 | C3 | 69.05(9) | O2 | Si4 | C41 | 108.08(10) | |
| C1 | Fe1 | C4 | 69.34(10) | O2 | Si4 | C42 | 108.53(11) | |
| C1 | Fe1 | C8 | 156.51(10) | C41 | Si4 | Si3 | 108.64(9) | |
| C1 | Fe1 | C9 | 160.68(10) | C41 | Si4 | C42 | 109.30(13) | |
| C1 | Fe1 | C10 | 123.33(10) | C42 | Si4 | Si3 | 113.48(9) | |
| C2 | Fe1 | C3 | 40.60(9) | Si2 | O1 | Si1 | 138.48(11) | |
| C2 | Fe1 | C8 | 121.76(10) | Si1 | O2 | Si4 | 142.89(11) | |
| C2 | Fe1 | C9 | 156.75(10) | Si2 | O3 | Si3 | 136.97(11) | |
| C4 | Fe1 | C2 | 68.60(10) | C11 | N1 | C12 | 109.2(2) | |
| C4 | Fe1 | C3 | 40.26(10) | C13 | N1 | C11 | 111.1(2) | |
| C4 | Fe1 | C8 | 125.40(11) | C13 | N1 | C12 | 109.5(2) | |
| C4 | Fe1 | C9 | 107.74(11) | C31 | N2 | C30 | 110.4(2) | |
| C5 | Fe1 | C1 | 41.43(9) | C31 | N2 | C32 | 109.6(2) | |
| C5 | Fe1 | C2 | 69.06(10) | C32 | N2 | C30 | 109.4(3) | |
| C5 | Fe1 | C3 | 68.12(10) | Si1 | C1 | Fe1 | 128.89(13) | |
| C5 | Fe1 | C4 | 40.66(10) | C2 | C1 | Fe1 | 69.32(13) | |
| C5 | Fe1 | C6 | 120.13(10) | C2 | C1 | Si1 | 131.59(17) | |
| C5 | Fe1 | C7 | 155.93(10) | C5 | C1 | Fe1 | 68.69(14) | |
| C5 | Fe1 | C8 | 161.38(10) | C5 | C1 | Si1 | 122.25(17) | |
| C5 | Fe1 | C9 | 124.07(10) | C5 | C1 | C2 | 106.07(19) | |
| C5 | Fe1 | C10 | 106.57(10) | C1 | C2 | Fe1 | 69.15(13) | |
| C6 | Fe1 | C1 | 106.14(10) | C1 | C2 | C11 | 126.7(2) | |
| C6 | Fe1 | C2 | 124.86(10) | C3 | C2 | Fe1 | 69.96(14) | |
| C6 | Fe1 | C3 | 162.51(10) | C3 | C2 | C1 | 107.9(2) | |
| C6 | Fe1 | C4 | 155.46(10) | C3 | C2 | C11 | 125.4(2) | |
| C6 | Fe1 | C8 | 68.14(11) | C11 | C2 | Fe1 | 125.66(17) | |
| C6 | Fe1 | C9 | 68.15(11) | C2 | C3 | Fe1 | 69.44(14) | |
| C6 | Fe1 | C10 | 40.47(10) | C4 | C3 | Fe1 | 69.61(15) | |
| C7 | Fe1 | C1 | 120.31(10) | C4 | C3 | C2 | 109.0(2) | |
| C7 | Fe1 | C2 | 107.90(10) | C3 | C4 | Fe1 | 70.13(15) | |
| C7 | Fe1 | C3 | 126.03(10) | C3 | C4 | C5 | 107.9(2) | |
| C7 | Fe1 | C4 | 162.34(11) | C5 | C4 | Fe1 | 68.98(15) | |
| C7 | Fe1 | C6 | 40.72(10) | C1 | C5 | Fe1 | 69.88(14) | |
| C7 | Fe1 | C8 | 40.53(11) | C4 | C5 | Fe1 | 70.37(15) | |
| C7 | Fe1 | C9 | 68.23(11) | C4 | C5 | C1 | 109.1(2) | |
| C7 | Fe1 | C10 | 68.29(11) | C7 | C6 | Fe1 | 69.34(15) | |
| C8 | Fe1 | C3 | 109.19(11) | C10 | C6 | Fe1 | 69.90(16) | |
| C8 | Fe1 | C9 | 40.39(10) | C10 | C6 | C7 | 107.9(2) | |
| C9 | Fe1 | C3 | 121.84(11) | C6 | C7 | Fe1 | 69.93(15) | |
| C10 | Fe1 | C2 | 161.39(10) | C8 | C7 | Fe1 | 70.26(16) | |
| C10 | Fe1 | C3 | 156.17(10) | C8 | C7 | C6 | 108.0(2) | |
| C10 | Fe1 | C4 | 120.61(11) | C7 | C8 | Fe1 | 69.21(15) | |
| C10 | Fe1 | C8 | 68.02(11) | C7 | C8 | C9 | 108.2(2) | |
| C10 | Fe1 | C9 | 40.52(10) | C9 | C8 | Fe1 | 69.91(15) | |
| C20 | Fe2 | C29 | 129.65(10) | C8 | C9 | Fe1 | 69.70(15) | |
| C21 | Fe2 | C20 | 41.33(9) | C8 | C9 | C10 | 107.8(2) | |
| C21 | Fe2 | C22 | 40.62(10) | C10 | C9 | Fe1 | 69.54(15) | |
| C21 | Fe2 | C25 | 131.14(10) | C6 | C10 | Fe1 | 69.63(15) | |
| C21 | Fe2 | C29 | 169.27(10) | C6 | C10 | C9 | 108.1(2) | |
| C22 | Fe2 | C20 | 69.01(9) | C9 | C10 | Fe1 | 69.94(15) | |
| C22 | Fe2 | C25 | 169.56(11) | N1 | C11 | C2 | 113.8(2) | |
| C22 | Fe2 | C29 | 148.86(11) | C15 | C14 | Si1 | 121.84(18) | |
| C23 | Fe2 | C20 | 69.40(10) | C19 | C14 | Si1 | 120.79(19) | |
| C23 | Fe2 | C21 | 68.70(10) | C19 | C14 | C15 | 117.3(2) | |
| C23 | Fe2 | C22 | 40.47(10) | C16 | C15 | C14 | 121.0(2) | |
| C23 | Fe2 | C25 | 149.31(10) | C17 | C16 | C15 | 120.1(3) | |
| C23 | Fe2 | C26 | 168.22(10) | C16 | C17 | C18 | 120.1(2) | |
| C23 | Fe2 | C29 | 116.07(11) | C17 | C18 | C19 | 119.3(2) | |
| C24 | Fe2 | C20 | 41.17(9) | C18 | C19 | C14 | 122.1(2) | |
| C24 | Fe2 | C21 | 68.76(10) | Si2 | C20 | Fe2 | 128.96(13) | |
| C24 | Fe2 | C22 | 68.21(10) | C21 | C20 | Fe2 | 69.12(13) | |
| C24 | Fe2 | C23 | 40.83(9) | C21 | C20 | Si2 | 130.00(18) | |
| C24 | Fe2 | C25 | 117.29(10) | C24 | C20 | Fe2 | 68.76(13) | |
| C24 | Fe2 | C26 | 150.31(10) | C24 | C20 | Si2 | 123.82(17) | |
| C24 | Fe2 | C27 | 167.75(11) | C24 | C20 | C21 | 106.1(2) | |
| C24 | Fe2 | C28 | 129.05(11) | C20 | C21 | Fe2 | 69.55(13) | |
| C24 | Fe2 | C29 | 108.02(10) | C20 | C21 | C30 | 127.1(2) | |
| C25 | Fe2 | C20 | 108.72(10) | C22 | C21 | Fe2 | 69.72(14) | |
| C25 | Fe2 | C29 | 40.29(11) | C22 | C21 | C20 | 108.2(2) | |
| C26 | Fe2 | C20 | 117.22(11) | C22 | C21 | C30 | 124.7(2) | |
| C26 | Fe2 | C21 | 109.19(11) | C30 | C21 | Fe2 | 126.52(18) | |
| C26 | Fe2 | C22 | 130.60(11) | C21 | C22 | Fe2 | 69.66(14) | |
| C26 | Fe2 | C25 | 40.52(10) | C23 | C22 | Fe2 | 69.57(14) | |
| C26 | Fe2 | C29 | 68.19(11) | C23 | C22 | C21 | 108.9(2) | |
| C27 | Fe2 | C20 | 150.02(11) | C22 | C23 | Fe2 | 69.96(15) | |
| C27 | Fe2 | C21 | 117.01(11) | C22 | C23 | C24 | 107.6(2) | |
| C27 | Fe2 | C22 | 108.50(11) | C24 | C23 | Fe2 | 69.31(14) | |
| C27 | Fe2 | C23 | 129.16(11) | C20 | C24 | Fe2 | 70.07(14) | |
| C27 | Fe2 | C25 | 68.04(11) | C23 | C24 | Fe2 | 69.86(14) | |
| C27 | Fe2 | C26 | 40.53(11) | C23 | C24 | C20 | 109.2(2) | |
| C27 | Fe2 | C28 | 40.70(11) | C26 | C25 | Fe2 | 69.60(16) | |
| C27 | Fe2 | C29 | 68.29(11) | C29 | C25 | Fe2 | 70.14(15) | |
| C28 | Fe2 | C20 | 168.14(11) | C29 | C25 | C26 | 108.6(2) | |
| C28 | Fe2 | C21 | 149.16(10) | C25 | C26 | Fe2 | 69.88(16) | |
| C28 | Fe2 | C22 | 116.21(11) | C27 | C26 | Fe2 | 69.42(16) | |
| C28 | Fe2 | C23 | 107.13(11) | C27 | C26 | C25 | 107.7(2) | |
| C28 | Fe2 | C25 | 68.12(11) | C26 | C27 | Fe2 | 70.05(15) | |
| C28 | Fe2 | C26 | 68.38(12) | C26 | C27 | C28 | 108.4(2) | |
| C28 | Fe2 | C29 | 40.71(10) | C28 | C27 | Fe2 | 69.83(15) | |
| O1 | Si1 | C1 | 108.49(10) | C27 | C28 | Fe2 | 69.47(15) | |
| O1 | Si1 | C14 | 107.58(10) | C27 | C28 | C29 | 107.8(2) | |
| O2 | Si1 | O1 | 108.99(8) | C29 | C28 | Fe2 | 70.20(14) | |
| O2 | Si1 | C1 | 108.43(10) | C25 | C29 | Fe2 | 69.57(14) | |
| O2 | Si1 | C14 | 107.39(10) | C25 | C29 | C28 | 107.6(2) | |
| C1 | Si1 | C14 | 115.80(10) | C28 | C29 | Fe2 | 69.10(15) | |
| O1 | Si2 | C20 | 108.36(9) | N2 | C30 | C21 | 113.0(2) | |
| O1 | Si2 | C33 | 109.58(10) | C34 | C33 | Si2 | 122.79(18) | |
| O3 | Si2 | O1 | 108.97(9) | C38 | C33 | Si2 | 119.99(19) | |
| O3 | Si2 | C20 | 109.24(10) | C38 | C33 | C34 | 117.0(2) | |
| O3 | Si2 | C33 | 106.58(10) | C35 | C34 | C33 | 121.5(2) | |
| C20 | Si2 | C33 | 114.01(11) | C36 | C35 | C34 | 119.9(3) | |
| O3 | Si3 | Si4 | 108.12(6) | C37 | C36 | C35 | 119.8(3) | |
| O3 | Si3 | C39 | 109.26(12) | C36 | C37 | C38 | 120.1(2) | |
| O3 | Si3 | C40 | 106.50(11) | C37 | C38 | C33 | 121.6(2) | |
| C39 | Si3 | Si4 | 109.46(10) | C43 | C44 | C46 | 110.5(4) | |
| C40 | Si3 | Si4 | 113.81(10) | C461 | C46 | C44 | 112.5(4) | |
| C40 | Si3 | C39 | 109.57(13) |
| A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|---|---|
| Fe1 | C1 | C2 | C3 | -59.46(17) | C3 | C4 | C5 | C1 | 0.2(3) | |
| Fe1 | C1 | C2 | C11 | 119.6(2) | C5 | C1 | C2 | Fe1 | 59.14(17) | |
| Fe1 | C1 | C5 | C4 | 59.62(19) | C5 | C1 | C2 | C3 | -0.3(3) | |
| Fe1 | C2 | C3 | C4 | -58.50(19) | C5 | C1 | C2 | C11 | 178.8(2) | |
| Fe1 | C2 | C11 | N1 | 167.81(16) | C6 | C7 | C8 | Fe1 | -60.02(18) | |
| Fe1 | C3 | C4 | C5 | -58.81(19) | C6 | C7 | C8 | C9 | -0.8(3) | |
| Fe1 | C4 | C5 | C1 | -59.32(18) | C7 | C6 | C10 | Fe1 | 59.13(18) | |
| Fe1 | C6 | C7 | C8 | 60.23(19) | C7 | C6 | C10 | C9 | -0.4(3) | |
| Fe1 | C6 | C10 | C9 | -59.6(2) | C7 | C8 | C9 | Fe1 | -58.81(19) | |
| Fe1 | C7 | C8 | C9 | 59.3(2) | C7 | C8 | C9 | C10 | 0.5(3) | |
| Fe1 | C8 | C9 | C10 | 59.31(19) | C8 | C9 | C10 | Fe1 | -59.41(19) | |
| Fe1 | C9 | C10 | C6 | 59.38(19) | C8 | C9 | C10 | C6 | 0.0(3) | |
| Fe2 | C20 | C21 | C22 | -59.22(17) | C10 | C6 | C7 | Fe1 | -59.48(19) | |
| Fe2 | C20 | C21 | C30 | 120.9(3) | C10 | C6 | C7 | C8 | 0.7(3) | |
| Fe2 | C20 | C24 | C23 | 59.06(17) | C11 | C2 | C3 | Fe1 | -120.1(2) | |
| Fe2 | C21 | C22 | C23 | -58.64(18) | C11 | C2 | C3 | C4 | -178.6(2) | |
| Fe2 | C21 | C30 | N2 | 172.88(18) | C12 | N1 | C11 | C2 | -171.9(2) | |
| Fe2 | C22 | C23 | C24 | -59.32(17) | C13 | N1 | C11 | C2 | 67.2(3) | |
| Fe2 | C23 | C24 | C20 | -59.19(17) | C14 | Si1 | O1 | Si2 | -120.58(16) | |
| Fe2 | C25 | C26 | C27 | 59.37(19) | C14 | Si1 | O2 | Si4 | -178.54(16) | |
| Fe2 | C25 | C29 | C28 | -58.84(19) | C14 | Si1 | C1 | Fe1 | -80.42(17) | |
| Fe2 | C26 | C27 | C28 | 59.53(19) | C14 | Si1 | C1 | C2 | 15.9(3) | |
| Fe2 | C27 | C28 | C29 | 60.00(19) | C14 | Si1 | C1 | C5 | -167.9(2) | |
| Fe2 | C28 | C29 | C25 | 59.14(18) | C14 | C15 | C16 | C17 | -0.4(4) | |
| Si1 | C1 | C2 | Fe1 | -124.2(2) | C15 | C14 | C19 | C18 | 0.5(3) | |
| Si1 | C1 | C2 | C3 | 176.3(2) | C15 | C16 | C17 | C18 | 0.9(4) | |
| Si1 | C1 | C2 | C11 | -4.6(4) | C16 | C17 | C18 | C19 | -0.6(4) | |
| Si1 | C1 | C5 | Fe1 | 123.41(18) | C17 | C18 | C19 | C14 | -0.1(4) | |
| Si1 | C1 | C5 | C4 | -176.97(18) | C19 | C14 | C15 | C16 | -0.3(3) | |
| Si1 | C14 | C15 | C16 | 177.62(18) | C20 | Si2 | O1 | Si1 | 69.87(18) | |
| Si1 | C14 | C19 | C18 | -177.39(19) | C20 | Si2 | O3 | Si3 | -39.46(18) | |
| Si2 | C20 | C21 | Fe2 | -123.9(2) | C20 | Si2 | C33 | C34 | 77.1(2) | |
| Si2 | C20 | C21 | C22 | 176.84(19) | C20 | Si2 | C33 | C38 | -97.9(2) | |
| Si2 | C20 | C21 | C30 | -3.0(4) | C20 | C21 | C22 | Fe2 | 59.11(17) | |
| Si2 | C20 | C24 | Fe2 | 123.48(18) | C20 | C21 | C22 | C23 | 0.5(3) | |
| Si2 | C20 | C24 | C23 | -177.46(18) | C20 | C21 | C30 | N2 | 82.0(3) | |
| Si2 | C33 | C34 | C35 | -173.7(2) | C21 | C20 | C24 | Fe2 | -59.31(16) | |
| Si2 | C33 | C38 | C37 | 174.14(19) | C21 | C20 | C24 | C23 | -0.3(3) | |
| Si3 | Si4 | O2 | Si1 | -50.91(18) | C21 | C22 | C23 | Fe2 | 58.69(18) | |
| Si4 | Si3 | O3 | Si2 | -48.59(16) | C21 | C22 | C23 | C24 | -0.6(3) | |
| O1 | Si1 | O2 | Si4 | 65.19(19) | C22 | C21 | C30 | N2 | -97.8(3) | |
| O1 | Si1 | C1 | Fe1 | 40.61(17) | C22 | C23 | C24 | Fe2 | 59.74(18) | |
| O1 | Si1 | C1 | C2 | 136.9(2) | C22 | C23 | C24 | C20 | 0.5(3) | |
| O1 | Si1 | C1 | C5 | -46.9(2) | C24 | C20 | C21 | Fe2 | 59.08(16) | |
| O1 | Si1 | C14 | C15 | -52.9(2) | C24 | C20 | C21 | C22 | -0.1(3) | |
| O1 | Si1 | C14 | C19 | 124.93(19) | C24 | C20 | C21 | C30 | -180.0(2) | |
| O1 | Si2 | O3 | Si3 | 78.76(17) | C25 | C26 | C27 | Fe2 | -59.66(19) | |
| O1 | Si2 | C20 | Fe2 | 56.74(17) | C25 | C26 | C27 | C28 | -0.1(3) | |
| O1 | Si2 | C20 | C21 | 151.3(2) | C26 | C25 | C29 | Fe2 | 59.17(19) | |
| O1 | Si2 | C20 | C24 | -32.2(2) | C26 | C25 | C29 | C28 | 0.3(3) | |
| O1 | Si2 | C33 | C34 | -44.5(2) | C26 | C27 | C28 | Fe2 | -59.67(19) | |
| O1 | Si2 | C33 | C38 | 140.45(18) | C26 | C27 | C28 | C29 | 0.3(3) | |
| O2 | Si1 | O1 | Si2 | -4.43(18) | C27 | C28 | C29 | Fe2 | -59.54(19) | |
| O2 | Si1 | C1 | Fe1 | 158.84(13) | C27 | C28 | C29 | C25 | -0.4(3) | |
| O2 | Si1 | C1 | C2 | -104.9(2) | C29 | C25 | C26 | Fe2 | -59.50(19) | |
| O2 | Si1 | C1 | C5 | 71.3(2) | C29 | C25 | C26 | C27 | -0.1(3) | |
| O2 | Si1 | C14 | C15 | -170.10(18) | C30 | C21 | C22 | Fe2 | -121.0(2) | |
| O2 | Si1 | C14 | C19 | 7.7(2) | C30 | C21 | C22 | C23 | -179.7(2) | |
| O3 | Si2 | O1 | Si1 | -48.90(18) | C31 | N2 | C30 | C21 | 66.0(3) | |
| O3 | Si2 | C20 | Fe2 | 175.34(13) | C32 | N2 | C30 | C21 | -173.2(2) | |
| O3 | Si2 | C20 | C21 | -90.1(2) | C33 | Si2 | O1 | Si1 | -165.17(15) | |
| O3 | Si2 | C20 | C24 | 86.4(2) | C33 | Si2 | O3 | Si3 | -163.07(15) | |
| O3 | Si2 | C33 | C34 | -162.3(2) | C33 | Si2 | C20 | Fe2 | -65.56(18) | |
| O3 | Si2 | C33 | C38 | 22.7(2) | C33 | Si2 | C20 | C21 | 29.0(3) | |
| C1 | Si1 | O1 | Si2 | 113.44(16) | C33 | Si2 | C20 | C24 | -154.5(2) | |
| C1 | Si1 | O2 | Si4 | -52.7(2) | C33 | C34 | C35 | C36 | -0.7(4) | |
| C1 | Si1 | C14 | C15 | 68.6(2) | C34 | C33 | C38 | C37 | -1.2(4) | |
| C1 | Si1 | C14 | C19 | -113.6(2) | C34 | C35 | C36 | C37 | -0.6(4) | |
| C1 | C2 | C3 | Fe1 | 58.95(16) | C35 | C36 | C37 | C38 | 0.9(4) | |
| C1 | C2 | C3 | C4 | 0.5(3) | C36 | C37 | C38 | C33 | 0.0(4) | |
| C1 | C2 | C11 | N1 | 78.4(3) | C38 | C33 | C34 | C35 | 1.5(4) | |
| C2 | C1 | C5 | Fe1 | -59.55(16) | C39 | Si3 | O3 | Si2 | 70.46(18) | |
| C2 | C1 | C5 | C4 | 0.1(3) | C40 | Si3 | O3 | Si2 | -171.27(16) | |
| C2 | C3 | C4 | Fe1 | 58.40(18) | C41 | Si4 | O2 | Si1 | -168.64(17) | |
| C2 | C3 | C4 | C5 | -0.4(3) | C42 | Si4 | O2 | Si1 | 72.9(2) | |
| C3 | C2 | C11 | N1 | -102.6(3) | C43 | C44 | C46 | C461 | 175.8(5) | |
| C3 | C4 | C5 | Fe1 | 59.52(19) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| H3 | 4166 | 6519 | 8250 | 30 |
| H4 | 3252 | 5804 | 9155 | 34 |
| H5 | 3767 | 4831 | 8662 | 29 |
| H6 | 7443 | 4869 | 8567 | 33 |
| H7 | 7832 | 5894 | 8234 | 35 |
| H8 | 6855 | 6498 | 9262 | 38 |
| H9 | 5817 | 5850 | 10214 | 38 |
| H10 | 6183 | 4842 | 9783 | 37 |
| H11A | 5731 | 6498 | 7113 | 26 |
| H11B | 6327 | 5904 | 6902 | 26 |
| H12A | 5987 | 6688 | 5744 | 60 |
| H12B | 5261 | 6316 | 5113 | 60 |
| H12C | 6402 | 6053 | 5579 | 60 |
| H13A | 3270 | 6329 | 6639 | 81 |
| H13B | 3399 | 6462 | 5734 | 81 |
| H13C | 4072 | 6854 | 6365 | 81 |
| H15 | 7806 | 4948 | 7160 | 28 |
| H16 | 9263 | 5088 | 6209 | 34 |
| H17 | 8747 | 4965 | 4902 | 37 |
| H18 | 6751 | 4724 | 4534 | 36 |
| H19 | 5294 | 4590 | 5483 | 30 |
| H22 | 6191 | 1825 | 6389 | 31 |
| H23 | 5629 | 2622 | 5474 | 30 |
| H24 | 5252 | 3495 | 6284 | 26 |
| H25 | 8398 | 3764 | 7280 | 36 |
| H26 | 9022 | 2795 | 7763 | 39 |
| H27 | 9166 | 2152 | 6595 | 42 |
| H28 | 8625 | 2720 | 5389 | 42 |
| H29 | 8164 | 3725 | 5816 | 39 |
| H30A | 6828 | 1738 | 7869 | 35 |
| H30B | 6809 | 2296 | 8391 | 35 |
| H31A | 4309 | 1639 | 7440 | 86 |
| H31B | 3865 | 1311 | 8195 | 86 |
| H31C | 5116 | 1137 | 7798 | 86 |
| H32A | 6128 | 1259 | 9036 | 88 |
| H32B | 4874 | 1451 | 9415 | 88 |
| H32C | 6046 | 1852 | 9475 | 88 |
| H34 | 8011 | 3678 | 8650 | 34 |
| H35 | 9172 | 3388 | 9722 | 42 |
| H36 | 8258 | 2890 | 10726 | 39 |
| H37 | 6179 | 2696 | 10659 | 35 |
| H38 | 5019 | 2977 | 9583 | 30 |
| H39A | 1661 | 2676 | 7286 | 53 |
| H39B | 2619 | 2441 | 7920 | 53 |
| H39C | 3081 | 2654 | 7095 | 53 |
| H40A | 1697 | 3933 | 8919 | 58 |
| H40B | 1554 | 3268 | 9042 | 58 |
| H40C | 711 | 3588 | 8414 | 58 |
| H41A | 2629 | 3423 | 5863 | 46 |
| H41B | 2096 | 4005 | 5533 | 46 |
| H41C | 1256 | 3601 | 6039 | 46 |
| H42A | 774 | 4592 | 7135 | 53 |
| H42B | 1622 | 4980 | 6612 | 53 |
| H42C | 1900 | 4923 | 7524 | 53 |
| H43A | 1241 | 5965 | 9055 | 69 |
| H43B | -92 | 5928 | 8664 | 69 |
| H43C | 1067 | 5713 | 8198 | 69 |
| H44A | 1354 | 5041 | 8991 | 103 |
| H44B | -33 | 5032 | 8679 | 103 |
| H46A | 760 | 5474 | 10154 | 90 |
| H46B | -620 | 5515 | 9840 | 90 |
| Atom | Occupancy | Atom | Occupancy | Atom | Occupancy | ||
|---|---|---|---|---|---|---|---|
| C43 | 0.5 | H43A | 0.5 | H43B | 0.5 | ||
| H43C | 0.5 |
Experimental
Single crystals of C89H119Fe4N4O6Si8 [3202] 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 [3202]
Crystal Data for C89H119Fe4N4O6Si8 (M =1788.99 g/mol): monoclinic, space group P21/n (no. 14), a = 10.9706(5) Å, b = 23.7261(9) Å, c = 17.2222(7) Å, β = 91.143(4)°, V = 4481.8(3) Å3, Z = 2, T = 173 K, μ(MoKα) = 0.795 mm-1, Dcalc = 1.326 g/cm3, 36392 reflections measured (4.362° ≤ 2Θ ≤ 51.994°), 8814 unique (Rint = 0.0490, Rsigma = 0.0475) which were used in all calculations. The final R1 was 0.0387 (I > 2σ(I)) and wR2 was 0.0855 (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. Others
Fixed Sof: C43(0.5) H43A(0.5) H43B(0.5) H43C(0.5)
3.a Secondary CH2 refined with riding coordinates:
C11(H11A,H11B), C30(H30A,H30B), C44(H44A,H44B), C46(H46A,H46B)
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), C15(H15),
C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C24(H24), C25(H25),
C26(H26), C27(H27), C28(H28), C29(H29), C34(H34), C35(H35), C36(H36),
C37(H37), C38(H38)
3.c Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C31(H31A,H31B,H31C), C32(H32A,H32B,
H32C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,
H42B,H42C), C43(H43A,H43B,H43C)
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.