| Identification code | 3021 |
| Empirical formula | C52H69Fe4N4O9Si4 |
| Formula weight | 1229.87 |
| Temperature/K | 173 |
| Crystal system | monoclinic |
| Space group | P21/n |
| a/Å | 13.2912(7) |
| b/Å | 13.5363(7) |
| c/Å | 30.9964(18) |
| α/° | 90 |
| β/° | 96.859(5) |
| γ/° | 90 |
| Volume/Å3 | 5536.8(5) |
| Z | 4 |
| ρcalcg/cm3 | 1.475 |
| μ/mm‑1 | 1.171 |
| F(000) | 2564.0 |
| Crystal size/mm3 | 0.14 × 0.11 × 0.06 |
| Radiation | MoKα (λ = 0.71073) |
| 2Θ range for data collection/° | 4.31 to 53.998 |
| Index ranges | -16 ≤ h ≤ 16, -17 ≤ k ≤ 17, -38 ≤ l ≤ 39 |
| Reflections collected | 42828 |
| Independent reflections | 11995 [Rint = 0.0745, Rsigma = 0.0936] |
| Data/restraints/parameters | 11995/5/686 |
| Goodness-of-fit on F2 | 1.017 |
| Final R indexes [I>=2σ (I)] | R1 = 0.0634, wR2 = 0.1325 |
| Final R indexes [all data] | R1 = 0.1265, wR2 = 0.1626 |
| Largest diff. peak/hole / e Å-3 | 0.81/-0.64 |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| Fe1 | 823.1(5) | 3237.9(5) | 5927.8(2) | 40.0(2) |
| Fe2 | -366.1(6) | 8541.0(6) | 6074.4(3) | 44.0(2) |
| Fe3 | 5218.9(5) | 9798.9(5) | 6352.8(2) | 36.37(19) |
| Fe4 | 6294.2(6) | 4351.4(5) | 6639.7(2) | 42.5(2) |
| Si1 | 2410.2(10) | 5076.4(10) | 6345.6(4) | 30.8(3) |
| Si2 | 1632.8(10) | 7052.6(10) | 5960.4(4) | 30.6(3) |
| Si3 | 3570.7(10) | 7898.5(10) | 6451.9(4) | 28.1(3) |
| Si4 | 4471.5(9) | 5925.9(10) | 6201.8(4) | 26.7(3) |
| O1 | 1943(3) | 5121(3) | 6799.8(11) | 47.7(10) |
| O2 | 1895(2) | 5887(2) | 6001.8(10) | 34.0(8) |
| O3 | 1762(3) | 7416(3) | 5473.4(10) | 44.6(9) |
| O4 | 2371(2) | 7649(2) | 6324.9(9) | 32.6(8) |
| O5 | 3804(3) | 7859(3) | 6971.5(10) | 40.0(8) |
| O6 | 4226(2) | 7102(2) | 6212.5(9) | 30.1(7) |
| O7 | 4513(2) | 5597(2) | 5705.9(10) | 36.0(8) |
| O8 | 3614(2) | 5327(2) | 6428.6(9) | 32.4(7) |
| N1 | 3161(3) | 4495(4) | 5180.3(13) | 49.3(12) |
| N2 | 869(3) | 6537(3) | 7126.4(13) | 45.4(11) |
| N3 | 3281(4) | 8602(4) | 5212.7(14) | 63.9(15) |
| N4 | 5050(3) | 6621(3) | 7457.4(13) | 48.0(12) |
| C1 | 2223(3) | 3836(4) | 6108.4(16) | 35.7(12) |
| C2 | 2107(4) | 3552(4) | 5653.1(17) | 42.6(13) |
| C3 | 1910(4) | 2529(4) | 5629(2) | 54.8(15) |
| C4 | 1897(4) | 2164(4) | 6053(2) | 61.8(18) |
| C5 | 2092(4) | 2948(4) | 6347.5(19) | 48.9(14) |
| C6 | -348(4) | 3929(6) | 5573(2) | 66.2(19) |
| C7 | -555(4) | 2922(6) | 5590(2) | 68.8(19) |
| C8 | -543(4) | 2667(5) | 6029(2) | 62.4(18) |
| C9 | -348(4) | 3533(5) | 6279.5(19) | 50.9(15) |
| C10 | -221(4) | 4312(4) | 5994(2) | 54.2(16) |
| C11 | 2130(4) | 4234(4) | 5276.1(16) | 44.2(14) |
| C12 | 3712(4) | 3619(5) | 5069(2) | 75(2) |
| C13 | 3060(5) | 5225(5) | 4821.0(16) | 72(2) |
| C14 | 314(4) | 7206(3) | 6070.6(16) | 35.5(12) |
| C15 | -85(4) | 7402(4) | 6482.8(15) | 38.1(12) |
| C16 | -1121(4) | 7528(4) | 6396.4(18) | 46.9(14) |
| C17 | -1419(4) | 7450(4) | 5944.3(19) | 50.3(14) |
| C18 | -543(4) | 7235(4) | 5748.1(18) | 46.8(14) |
| C19 | 714(5) | 9555(4) | 5979(2) | 64.0(18) |
| C20 | 394(5) | 9703(4) | 6377(3) | 67.5(19) |
| C21 | -668(5) | 9888(4) | 6332(2) | 60.4(17) |
| C22 | -975(5) | 9875(4) | 5882(2) | 64.1(18) |
| C23 | -128(6) | 9659(5) | 5663(2) | 77(2) |
| C24 | 550(4) | 7479(4) | 6919.5(16) | 43.2(13) |
| C25 | 6(5) | 5970(5) | 7238(2) | 69.0(19) |
| C26 | 1573(5) | 6723(5) | 7523.3(17) | 61.8(17) |
| C27 | 3821(3) | 9147(4) | 6267.5(15) | 33.2(11) |
| C28 | 4117(4) | 9489(4) | 5854.4(16) | 37.2(12) |
| C29 | 4279(4) | 10527(4) | 5890(2) | 50.6(15) |
| C30 | 4089(4) | 10843(4) | 6301(2) | 54.6(16) |
| C31 | 3801(4) | 10016(4) | 6533.7(19) | 44.6(14) |
| C32 | 6254(4) | 8732(4) | 6550(2) | 49.0(15) |
| C33 | 6554(4) | 9250(5) | 6193(2) | 55.6(16) |
| C34 | 6667(4) | 10256(4) | 6313(2) | 51.4(15) |
| C35 | 6447(4) | 10351(4) | 6743.4(19) | 51.8(15) |
| C36 | 6171(4) | 9411(4) | 6889.9(19) | 54.1(15) |
| C37 | 4247(4) | 8848(4) | 5472.2(16) | 47.3(14) |
| C38 | 3473(6) | 7969(6) | 4848.8(19) | 106(3) |
| C39 | 2728(5) | 9488(6) | 5067(2) | 104(3) |
| C40 | 5714(3) | 5734(3) | 6516.2(14) | 28.5(10) |
| C41 | 5980(4) | 5569(4) | 6977.7(15) | 35.7(11) |
| C42 | 7018(4) | 5363(4) | 7051.1(19) | 51.9(15) |
| C43 | 7425(4) | 5377(4) | 6650(2) | 54.7(16) |
| C44 | 6632(4) | 5611(4) | 6322.4(17) | 42.3(13) |
| C45 | 5227(5) | 3356(4) | 6385(2) | 65.2(18) |
| C46 | 5408(6) | 3256(5) | 6831(2) | 74(2) |
| C47 | 6416(7) | 3018(5) | 6938(3) | 84(2) |
| C48 | 6891(5) | 2984(4) | 6556(3) | 75(2) |
| C49 | 6126(7) | 3219(4) | 6203(2) | 78(2) |
| C50 | 5268(4) | 5607(4) | 7319.8(15) | 46.1(14) |
| C51 | 4353(5) | 6580(5) | 7795.3(17) | 74(2) |
| C52 | 5993(5) | 7136(5) | 7620.2(18) | 62.3(17) |
| O9 | 2580(4) | 4181(4) | 7604.0(15) | 92.5(16) |
| Atom | U11 | U22 | U33 | U23 | U13 | U12 |
|---|---|---|---|---|---|---|
| Fe1 | 28.0(4) | 35.6(4) | 56.0(5) | 2.4(4) | 3.9(3) | -7.2(3) |
| Fe2 | 32.3(4) | 38.6(4) | 59.1(5) | 1.7(4) | -2.3(4) | 0.4(4) |
| Fe3 | 27.4(4) | 33.0(4) | 48.0(4) | -3.6(3) | 1.2(3) | -1.7(3) |
| Fe4 | 36.7(4) | 34.7(4) | 53.5(5) | 3.4(4) | -5.2(4) | 2.5(4) |
| Si1 | 29.4(7) | 36.0(8) | 27.7(7) | -0.4(6) | 5.8(5) | -7.3(6) |
| Si2 | 26.8(7) | 35.2(7) | 29.3(7) | -2.2(6) | 1.4(5) | -0.8(6) |
| Si3 | 27.4(7) | 29.8(7) | 26.7(6) | -2.0(6) | 1.7(5) | -3.3(6) |
| Si4 | 24.6(7) | 30.1(7) | 24.9(6) | -0.6(6) | 0.9(5) | -3.6(6) |
| O1 | 55(2) | 54(2) | 37(2) | 8.6(19) | 16.0(18) | 0(2) |
| O2 | 29.7(18) | 36.9(19) | 34.2(18) | -4.4(15) | -0.9(14) | -5.8(16) |
| O3 | 44(2) | 53(2) | 35.7(19) | 5.1(18) | 0.2(16) | -9(2) |
| O4 | 29.1(17) | 35.2(19) | 34.1(17) | -5.2(15) | 6.7(14) | -3.8(15) |
| O5 | 46(2) | 42(2) | 30.4(18) | -4.1(16) | -1.7(16) | 1.9(18) |
| O6 | 28.0(17) | 29.9(17) | 32.3(17) | 0.5(14) | 2.7(14) | -0.8(15) |
| O7 | 32.9(19) | 46(2) | 29.1(17) | -7.3(16) | 3.1(15) | -7.4(17) |
| O8 | 29.3(17) | 39.1(19) | 28.2(16) | 1.8(15) | 0.3(13) | -6.1(16) |
| N1 | 40(3) | 72(3) | 37(2) | -15(2) | 10(2) | -22(3) |
| N2 | 40(3) | 58(3) | 39(2) | 2(2) | 8(2) | -2(2) |
| N3 | 65(3) | 93(4) | 32(3) | 12(3) | -2(2) | -36(3) |
| N4 | 52(3) | 61(3) | 30(2) | 1(2) | -1(2) | 5(3) |
| C1 | 23(2) | 33(3) | 50(3) | 2(2) | 3(2) | -5(2) |
| C2 | 28(3) | 47(3) | 54(3) | -11(3) | 10(2) | -12(3) |
| C3 | 41(3) | 41(3) | 83(4) | -17(3) | 9(3) | -5(3) |
| C4 | 38(3) | 24(3) | 122(6) | -4(4) | 5(4) | -2(3) |
| C5 | 33(3) | 44(3) | 68(4) | 14(3) | -2(3) | -1(3) |
| C6 | 31(3) | 103(6) | 65(4) | 35(4) | 6(3) | 5(4) |
| C7 | 33(3) | 101(6) | 71(5) | -14(4) | 0(3) | -17(4) |
| C8 | 32(3) | 50(4) | 108(6) | 18(4) | 16(3) | -10(3) |
| C9 | 34(3) | 66(4) | 54(3) | 12(3) | 10(3) | 1(3) |
| C10 | 31(3) | 44(3) | 88(5) | 12(3) | 8(3) | 4(3) |
| C11 | 36(3) | 61(4) | 37(3) | -19(3) | 10(2) | -19(3) |
| C12 | 43(4) | 107(6) | 78(5) | -49(4) | 18(3) | -20(4) |
| C13 | 66(4) | 123(6) | 27(3) | 0(3) | 6(3) | -40(4) |
| C14 | 29(3) | 34(3) | 43(3) | -7(2) | -1(2) | -6(2) |
| C15 | 43(3) | 37(3) | 35(3) | -5(2) | 10(2) | -11(3) |
| C16 | 41(3) | 44(3) | 58(4) | -4(3) | 16(3) | 3(3) |
| C17 | 29(3) | 51(3) | 71(4) | -6(3) | 2(3) | -3(3) |
| C18 | 40(3) | 48(3) | 50(3) | -12(3) | -2(3) | -5(3) |
| C19 | 42(4) | 46(4) | 105(6) | 10(4) | 12(4) | -7(3) |
| C20 | 50(4) | 36(3) | 112(6) | -9(4) | -10(4) | -5(3) |
| C21 | 58(4) | 39(3) | 82(5) | -4(3) | 0(3) | 6(3) |
| C22 | 54(4) | 52(4) | 84(5) | 20(4) | -1(4) | 15(3) |
| C23 | 89(6) | 69(5) | 75(5) | 22(4) | 14(4) | 0(4) |
| C24 | 41(3) | 52(3) | 38(3) | -7(3) | 11(2) | 4(3) |
| C25 | 61(4) | 80(5) | 70(4) | 9(4) | 20(3) | -11(4) |
| C26 | 62(4) | 78(5) | 45(3) | 0(3) | 4(3) | -3(4) |
| C27 | 18(2) | 36(3) | 45(3) | -6(2) | 1(2) | -2(2) |
| C28 | 27(3) | 41(3) | 42(3) | 3(2) | -3(2) | -6(2) |
| C29 | 35(3) | 42(3) | 73(4) | 16(3) | 0(3) | -2(3) |
| C30 | 37(3) | 28(3) | 97(5) | -4(3) | 1(3) | 3(3) |
| C31 | 28(3) | 41(3) | 66(4) | -12(3) | 10(3) | 2(2) |
| C32 | 28(3) | 35(3) | 81(4) | -2(3) | -8(3) | 5(2) |
| C33 | 31(3) | 70(4) | 65(4) | -10(4) | 5(3) | 11(3) |
| C34 | 32(3) | 53(4) | 68(4) | 6(3) | 6(3) | -4(3) |
| C35 | 39(3) | 47(3) | 65(4) | -12(3) | -11(3) | -11(3) |
| C36 | 44(3) | 60(4) | 55(4) | -8(3) | -11(3) | -8(3) |
| C37 | 45(3) | 62(4) | 35(3) | 10(3) | 4(2) | -16(3) |
| C38 | 107(6) | 173(9) | 43(4) | -34(5) | 28(4) | -87(6) |
| C39 | 78(5) | 141(8) | 81(5) | 70(5) | -42(4) | -35(5) |
| C40 | 28(2) | 24(2) | 32(2) | -2(2) | -3(2) | -3(2) |
| C41 | 35(3) | 34(3) | 37(3) | -2(2) | -3(2) | -2(2) |
| C42 | 41(3) | 57(4) | 52(3) | -3(3) | -17(3) | 1(3) |
| C43 | 23(3) | 63(4) | 76(4) | -5(3) | -2(3) | -4(3) |
| C44 | 30(3) | 46(3) | 51(3) | 0(3) | 5(2) | -6(3) |
| C45 | 62(4) | 35(3) | 94(5) | -10(4) | -8(4) | -12(3) |
| C46 | 103(6) | 43(4) | 80(5) | 3(4) | 18(5) | -15(4) |
| C47 | 102(6) | 45(4) | 99(6) | 21(4) | -11(5) | 8(4) |
| C48 | 59(4) | 42(4) | 123(7) | -3(4) | 9(5) | 14(3) |
| C49 | 132(7) | 40(4) | 64(4) | -9(3) | 20(5) | -5(4) |
| C50 | 51(3) | 52(3) | 32(3) | 11(3) | -8(2) | -5(3) |
| C51 | 87(5) | 102(6) | 34(3) | 6(3) | 14(3) | 19(4) |
| C52 | 70(4) | 67(4) | 45(3) | -14(3) | -12(3) | -2(4) |
| O9 | 99(4) | 92(4) | 83(3) | 17(3) | 0(3) | 2(3) |
| Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
|---|---|---|---|---|---|---|
| Fe1 | C1 | 2.044(5) | N1 | C11 | 1.479(6) | |
| Fe1 | C2 | 2.040(5) | N1 | C12 | 1.457(7) | |
| Fe1 | C3 | 2.045(6) | N1 | C13 | 1.483(7) | |
| Fe1 | C4 | 2.042(6) | N2 | C24 | 1.467(6) | |
| Fe1 | C5 | 2.042(5) | N2 | C25 | 1.456(7) | |
| Fe1 | C6 | 2.025(6) | N2 | C26 | 1.476(7) | |
| Fe1 | C7 | 2.043(6) | N3 | C37 | 1.470(7) | |
| Fe1 | C8 | 2.032(5) | N3 | C38 | 1.463(8) | |
| Fe1 | C9 | 2.043(5) | N3 | C39 | 1.451(9) | |
| Fe1 | C10 | 2.037(6) | N4 | C50 | 1.476(7) | |
| Fe2 | C14 | 2.021(5) | N4 | C51 | 1.480(6) | |
| Fe2 | C15 | 2.001(5) | N4 | C52 | 1.470(7) | |
| Fe2 | C16 | 2.030(5) | C1 | C2 | 1.453(7) | |
| Fe2 | C17 | 2.042(5) | C1 | C5 | 1.433(7) | |
| Fe2 | C18 | 2.036(5) | C2 | C3 | 1.409(7) | |
| Fe2 | C19 | 2.034(6) | C2 | C11 | 1.493(7) | |
| Fe2 | C20 | 2.036(6) | C3 | C4 | 1.405(8) | |
| Fe2 | C21 | 2.049(6) | C4 | C5 | 1.404(8) | |
| Fe2 | C22 | 2.038(6) | C6 | C7 | 1.393(9) | |
| Fe2 | C23 | 2.027(6) | C6 | C10 | 1.397(8) | |
| Fe3 | C27 | 2.045(5) | C7 | C8 | 1.402(8) | |
| Fe3 | C28 | 2.041(5) | C8 | C9 | 1.413(8) | |
| Fe3 | C29 | 2.040(5) | C9 | C10 | 1.399(7) | |
| Fe3 | C30 | 2.055(5) | C14 | C15 | 1.465(6) | |
| Fe3 | C31 | 2.051(5) | C14 | C18 | 1.424(7) | |
| Fe3 | C32 | 2.038(5) | C15 | C16 | 1.381(7) | |
| Fe3 | C33 | 2.039(5) | C15 | C24 | 1.510(7) | |
| Fe3 | C34 | 2.040(5) | C16 | C17 | 1.414(7) | |
| Fe3 | C35 | 2.054(5) | C17 | C18 | 1.407(7) | |
| Fe3 | C36 | 2.036(6) | C19 | C20 | 1.366(8) | |
| Fe4 | C40 | 2.043(4) | C19 | C23 | 1.403(9) | |
| Fe4 | C41 | 2.024(5) | C20 | C21 | 1.423(8) | |
| Fe4 | C42 | 2.033(5) | C21 | C22 | 1.404(8) | |
| Fe4 | C43 | 2.043(5) | C22 | C23 | 1.414(9) | |
| Fe4 | C44 | 2.045(5) | C27 | C28 | 1.459(6) | |
| Fe4 | C45 | 2.046(6) | C27 | C31 | 1.439(7) | |
| Fe4 | C46 | 2.026(6) | C28 | C29 | 1.424(7) | |
| Fe4 | C47 | 2.026(7) | C28 | C37 | 1.495(7) | |
| Fe4 | C48 | 2.042(6) | C29 | C30 | 1.394(8) | |
| Fe4 | C49 | 2.040(6) | C30 | C31 | 1.410(7) | |
| Si1 | O1 | 1.606(3) | C32 | C33 | 1.409(8) | |
| Si1 | O2 | 1.623(3) | C32 | C36 | 1.412(7) | |
| Si1 | O8 | 1.626(3) | C33 | C34 | 1.415(8) | |
| Si1 | C1 | 1.839(5) | C34 | C35 | 1.405(7) | |
| Si2 | O2 | 1.618(3) | C35 | C36 | 1.414(8) | |
| Si2 | O3 | 1.616(3) | C40 | C41 | 1.449(6) | |
| Si2 | O4 | 1.620(3) | C40 | C44 | 1.433(6) | |
| Si2 | C14 | 1.837(5) | C41 | C42 | 1.400(7) | |
| Si3 | O4 | 1.631(3) | C41 | C50 | 1.503(7) | |
| Si3 | O5 | 1.604(3) | C42 | C43 | 1.413(7) | |
| Si3 | O6 | 1.621(3) | C43 | C44 | 1.410(7) | |
| Si3 | C27 | 1.827(5) | C45 | C46 | 1.382(9) | |
| Si4 | O6 | 1.626(3) | C45 | C49 | 1.392(9) | |
| Si4 | O7 | 1.607(3) | C46 | C47 | 1.379(10) | |
| Si4 | O8 | 1.625(3) | C47 | C48 | 1.407(10) | |
| Si4 | C40 | 1.833(5) | C48 | C49 | 1.438(10) |
| Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|
| C1 | Fe1 | C3 | 69.0(2) | O2 | Si1 | C1 | 109.2(2) | |
| C2 | Fe1 | C1 | 41.67(19) | O8 | Si1 | C1 | 109.76(19) | |
| C2 | Fe1 | C3 | 40.4(2) | O2 | Si2 | O4 | 108.86(17) | |
| C2 | Fe1 | C4 | 68.1(2) | O2 | Si2 | C14 | 107.3(2) | |
| C2 | Fe1 | C5 | 68.7(2) | O3 | Si2 | O2 | 108.98(19) | |
| C2 | Fe1 | C7 | 125.0(2) | O3 | Si2 | O4 | 112.13(18) | |
| C2 | Fe1 | C9 | 155.5(2) | O3 | Si2 | C14 | 110.4(2) | |
| C4 | Fe1 | C1 | 68.7(2) | O4 | Si2 | C14 | 109.01(19) | |
| C4 | Fe1 | C3 | 40.2(2) | O4 | Si3 | C27 | 108.99(19) | |
| C4 | Fe1 | C7 | 120.8(3) | O5 | Si3 | O4 | 107.55(17) | |
| C4 | Fe1 | C9 | 126.7(3) | O5 | Si3 | O6 | 112.80(18) | |
| C5 | Fe1 | C1 | 41.1(2) | O5 | Si3 | C27 | 108.9(2) | |
| C5 | Fe1 | C3 | 67.9(2) | O6 | Si3 | O4 | 108.36(17) | |
| C5 | Fe1 | C4 | 40.2(2) | O6 | Si3 | C27 | 110.11(19) | |
| C5 | Fe1 | C7 | 155.2(3) | O6 | Si4 | C40 | 107.33(18) | |
| C5 | Fe1 | C9 | 108.8(2) | O7 | Si4 | O6 | 108.67(17) | |
| C6 | Fe1 | C1 | 125.5(3) | O7 | Si4 | O8 | 112.44(17) | |
| C6 | Fe1 | C2 | 107.7(2) | O7 | Si4 | C40 | 109.72(19) | |
| C6 | Fe1 | C3 | 120.6(3) | O8 | Si4 | O6 | 109.07(17) | |
| C6 | Fe1 | C4 | 155.0(3) | O8 | Si4 | C40 | 109.48(18) | |
| C6 | Fe1 | C5 | 163.4(3) | Si2 | O2 | Si1 | 141.4(2) | |
| C6 | Fe1 | C7 | 40.0(3) | Si2 | O4 | Si3 | 139.9(2) | |
| C6 | Fe1 | C8 | 67.5(2) | Si3 | O6 | Si4 | 141.3(2) | |
| C6 | Fe1 | C9 | 67.3(2) | Si4 | O8 | Si1 | 139.8(2) | |
| C6 | Fe1 | C10 | 40.2(2) | C11 | N1 | C13 | 107.9(4) | |
| C7 | Fe1 | C1 | 162.5(3) | C12 | N1 | C11 | 110.9(4) | |
| C7 | Fe1 | C3 | 108.0(3) | C12 | N1 | C13 | 111.6(5) | |
| C8 | Fe1 | C1 | 155.3(3) | C24 | N2 | C26 | 109.7(4) | |
| C8 | Fe1 | C2 | 162.0(3) | C25 | N2 | C24 | 111.5(4) | |
| C8 | Fe1 | C3 | 125.7(3) | C25 | N2 | C26 | 109.4(4) | |
| C8 | Fe1 | C4 | 108.5(2) | C38 | N3 | C37 | 109.5(5) | |
| C8 | Fe1 | C5 | 120.9(2) | C39 | N3 | C37 | 111.1(5) | |
| C8 | Fe1 | C7 | 40.2(2) | C39 | N3 | C38 | 111.9(6) | |
| C8 | Fe1 | C9 | 40.6(2) | C50 | N4 | C51 | 109.4(4) | |
| C8 | Fe1 | C10 | 67.9(2) | C52 | N4 | C50 | 110.6(4) | |
| C9 | Fe1 | C1 | 120.2(2) | C52 | N4 | C51 | 110.8(4) | |
| C9 | Fe1 | C3 | 163.2(2) | Si1 | C1 | Fe1 | 123.1(2) | |
| C9 | Fe1 | C7 | 67.7(2) | C2 | C1 | Fe1 | 69.0(3) | |
| C10 | Fe1 | C1 | 107.4(2) | C2 | C1 | Si1 | 128.6(4) | |
| C10 | Fe1 | C2 | 120.5(2) | C5 | C1 | Fe1 | 69.4(3) | |
| C10 | Fe1 | C3 | 155.1(3) | C5 | C1 | Si1 | 125.3(4) | |
| C10 | Fe1 | C4 | 163.4(3) | C5 | C1 | C2 | 106.0(5) | |
| C10 | Fe1 | C5 | 126.4(3) | C1 | C2 | Fe1 | 69.3(3) | |
| C10 | Fe1 | C7 | 67.7(3) | C1 | C2 | C11 | 126.0(5) | |
| C10 | Fe1 | C9 | 40.1(2) | C3 | C2 | Fe1 | 70.0(3) | |
| C14 | Fe2 | C16 | 69.3(2) | C3 | C2 | C1 | 107.9(5) | |
| C14 | Fe2 | C17 | 69.4(2) | C3 | C2 | C11 | 126.0(5) | |
| C14 | Fe2 | C18 | 41.10(19) | C11 | C2 | Fe1 | 123.5(4) | |
| C14 | Fe2 | C19 | 106.2(2) | C2 | C3 | Fe1 | 69.6(3) | |
| C14 | Fe2 | C20 | 119.7(2) | C4 | C3 | Fe1 | 69.8(3) | |
| C14 | Fe2 | C21 | 155.0(2) | C4 | C3 | C2 | 108.7(5) | |
| C14 | Fe2 | C22 | 162.3(2) | C3 | C4 | Fe1 | 70.0(3) | |
| C14 | Fe2 | C23 | 124.1(3) | C5 | C4 | Fe1 | 69.9(3) | |
| C15 | Fe2 | C14 | 42.72(19) | C5 | C4 | C3 | 108.7(5) | |
| C15 | Fe2 | C16 | 40.1(2) | C1 | C5 | Fe1 | 69.6(3) | |
| C15 | Fe2 | C17 | 68.9(2) | C4 | C5 | Fe1 | 69.9(3) | |
| C15 | Fe2 | C18 | 69.4(2) | C4 | C5 | C1 | 108.8(5) | |
| C15 | Fe2 | C19 | 122.0(2) | C7 | C6 | Fe1 | 70.7(4) | |
| C15 | Fe2 | C20 | 105.0(3) | C7 | C6 | C10 | 109.2(6) | |
| C15 | Fe2 | C21 | 118.0(2) | C10 | C6 | Fe1 | 70.4(3) | |
| C15 | Fe2 | C22 | 154.8(2) | C6 | C7 | Fe1 | 69.3(3) | |
| C15 | Fe2 | C23 | 160.2(3) | C6 | C7 | C8 | 107.5(6) | |
| C16 | Fe2 | C17 | 40.6(2) | C8 | C7 | Fe1 | 69.5(3) | |
| C16 | Fe2 | C18 | 67.9(2) | C7 | C8 | Fe1 | 70.3(3) | |
| C16 | Fe2 | C19 | 157.9(3) | C7 | C8 | C9 | 108.0(5) | |
| C16 | Fe2 | C20 | 122.8(3) | C9 | C8 | Fe1 | 70.1(3) | |
| C16 | Fe2 | C21 | 106.2(2) | C8 | C9 | Fe1 | 69.3(3) | |
| C16 | Fe2 | C22 | 122.6(2) | C10 | C9 | Fe1 | 69.7(3) | |
| C17 | Fe2 | C21 | 124.0(2) | C10 | C9 | C8 | 107.9(5) | |
| C18 | Fe2 | C17 | 40.4(2) | C6 | C10 | Fe1 | 69.4(3) | |
| C18 | Fe2 | C20 | 157.0(2) | C6 | C10 | C9 | 107.5(6) | |
| C18 | Fe2 | C21 | 161.7(2) | C9 | C10 | Fe1 | 70.2(3) | |
| C18 | Fe2 | C22 | 127.3(3) | N1 | C11 | C2 | 114.3(4) | |
| C19 | Fe2 | C17 | 159.9(3) | Si2 | C14 | Fe2 | 122.7(2) | |
| C19 | Fe2 | C18 | 123.8(3) | C15 | C14 | Fe2 | 67.9(3) | |
| C19 | Fe2 | C20 | 39.2(2) | C15 | C14 | Si2 | 129.5(4) | |
| C19 | Fe2 | C21 | 68.3(3) | C18 | C14 | Fe2 | 70.0(3) | |
| C19 | Fe2 | C22 | 67.8(3) | C18 | C14 | Si2 | 125.0(4) | |
| C20 | Fe2 | C17 | 160.1(3) | C18 | C14 | C15 | 105.3(4) | |
| C20 | Fe2 | C21 | 40.8(2) | C14 | C15 | Fe2 | 69.4(3) | |
| C20 | Fe2 | C22 | 66.9(3) | C14 | C15 | C24 | 124.9(4) | |
| C22 | Fe2 | C17 | 110.1(3) | C16 | C15 | Fe2 | 71.1(3) | |
| C22 | Fe2 | C21 | 40.2(2) | C16 | C15 | C14 | 108.0(5) | |
| C23 | Fe2 | C16 | 159.5(3) | C16 | C15 | C24 | 127.1(4) | |
| C23 | Fe2 | C17 | 124.8(3) | C24 | C15 | Fe2 | 123.8(4) | |
| C23 | Fe2 | C18 | 110.7(3) | C15 | C16 | Fe2 | 68.8(3) | |
| C23 | Fe2 | C19 | 40.4(3) | C15 | C16 | C17 | 109.7(5) | |
| C23 | Fe2 | C20 | 66.8(3) | C17 | C16 | Fe2 | 70.1(3) | |
| C23 | Fe2 | C21 | 68.5(3) | C16 | C17 | Fe2 | 69.2(3) | |
| C23 | Fe2 | C22 | 40.7(2) | C18 | C17 | Fe2 | 69.6(3) | |
| C27 | Fe3 | C30 | 69.1(2) | C18 | C17 | C16 | 107.2(5) | |
| C27 | Fe3 | C31 | 41.12(18) | C14 | C18 | Fe2 | 68.9(3) | |
| C27 | Fe3 | C35 | 151.5(2) | C17 | C18 | Fe2 | 70.0(3) | |
| C28 | Fe3 | C27 | 41.83(18) | C17 | C18 | C14 | 109.7(5) | |
| C28 | Fe3 | C30 | 68.3(2) | C20 | C19 | Fe2 | 70.5(4) | |
| C28 | Fe3 | C31 | 68.7(2) | C20 | C19 | C23 | 107.8(6) | |
| C28 | Fe3 | C35 | 165.7(2) | C23 | C19 | Fe2 | 69.5(4) | |
| C29 | Fe3 | C27 | 69.3(2) | C19 | C20 | Fe2 | 70.3(4) | |
| C29 | Fe3 | C28 | 40.8(2) | C19 | C20 | C21 | 110.5(7) | |
| C29 | Fe3 | C30 | 39.8(2) | C21 | C20 | Fe2 | 70.1(3) | |
| C29 | Fe3 | C31 | 67.5(2) | C20 | C21 | Fe2 | 69.1(3) | |
| C29 | Fe3 | C35 | 128.0(2) | C22 | C21 | Fe2 | 69.5(3) | |
| C31 | Fe3 | C30 | 40.2(2) | C22 | C21 | C20 | 105.3(6) | |
| C31 | Fe3 | C35 | 118.6(2) | C21 | C22 | Fe2 | 70.3(3) | |
| C32 | Fe3 | C27 | 107.7(2) | C21 | C22 | C23 | 108.9(6) | |
| C32 | Fe3 | C28 | 118.7(2) | C23 | C22 | Fe2 | 69.2(4) | |
| C32 | Fe3 | C29 | 152.7(2) | C19 | C23 | Fe2 | 70.0(4) | |
| C32 | Fe3 | C30 | 166.4(3) | C19 | C23 | C22 | 107.5(6) | |
| C32 | Fe3 | C31 | 129.0(2) | C22 | C23 | Fe2 | 70.1(4) | |
| C32 | Fe3 | C33 | 40.5(2) | N2 | C24 | C15 | 115.7(4) | |
| C32 | Fe3 | C34 | 68.0(2) | Si3 | C27 | Fe3 | 123.7(2) | |
| C32 | Fe3 | C35 | 67.7(2) | C28 | C27 | Fe3 | 68.9(3) | |
| C33 | Fe3 | C27 | 127.9(2) | C28 | C27 | Si3 | 130.3(4) | |
| C33 | Fe3 | C28 | 107.9(2) | C31 | C27 | Fe3 | 69.6(3) | |
| C33 | Fe3 | C29 | 118.9(2) | C31 | C27 | Si3 | 124.0(4) | |
| C33 | Fe3 | C30 | 151.7(3) | C31 | C27 | C28 | 105.6(4) | |
| C33 | Fe3 | C31 | 166.8(2) | C27 | C28 | Fe3 | 69.2(3) | |
| C33 | Fe3 | C34 | 40.6(2) | C27 | C28 | C37 | 125.5(4) | |
| C33 | Fe3 | C35 | 67.8(2) | C29 | C28 | Fe3 | 69.5(3) | |
| C34 | Fe3 | C27 | 166.5(2) | C29 | C28 | C27 | 107.4(5) | |
| C34 | Fe3 | C28 | 127.9(2) | C29 | C28 | C37 | 127.1(5) | |
| C34 | Fe3 | C29 | 108.3(2) | C37 | C28 | Fe3 | 125.3(4) | |
| C34 | Fe3 | C30 | 118.2(2) | C28 | C29 | Fe3 | 69.6(3) | |
| C34 | Fe3 | C31 | 151.4(2) | C30 | C29 | Fe3 | 70.7(3) | |
| C34 | Fe3 | C35 | 40.1(2) | C30 | C29 | C28 | 109.4(5) | |
| C35 | Fe3 | C30 | 108.5(2) | C29 | C30 | Fe3 | 69.5(3) | |
| C36 | Fe3 | C27 | 117.4(2) | C29 | C30 | C31 | 108.3(5) | |
| C36 | Fe3 | C28 | 152.3(2) | C31 | C30 | Fe3 | 69.7(3) | |
| C36 | Fe3 | C29 | 165.5(2) | C27 | C31 | Fe3 | 69.2(3) | |
| C36 | Fe3 | C30 | 128.2(3) | C30 | C31 | Fe3 | 70.1(3) | |
| C36 | Fe3 | C31 | 108.4(2) | C30 | C31 | C27 | 109.3(5) | |
| C36 | Fe3 | C32 | 40.5(2) | C33 | C32 | Fe3 | 69.8(3) | |
| C36 | Fe3 | C33 | 68.4(2) | C33 | C32 | C36 | 108.5(5) | |
| C36 | Fe3 | C34 | 68.2(2) | C36 | C32 | Fe3 | 69.7(3) | |
| C36 | Fe3 | C35 | 40.5(2) | C32 | C33 | Fe3 | 69.7(3) | |
| C40 | Fe4 | C43 | 69.0(2) | C32 | C33 | C34 | 107.6(5) | |
| C40 | Fe4 | C44 | 41.04(18) | C34 | C33 | Fe3 | 69.7(3) | |
| C40 | Fe4 | C45 | 107.6(2) | C33 | C34 | Fe3 | 69.7(3) | |
| C41 | Fe4 | C40 | 41.75(18) | C35 | C34 | Fe3 | 70.5(3) | |
| C41 | Fe4 | C42 | 40.36(19) | C35 | C34 | C33 | 108.1(5) | |
| C41 | Fe4 | C43 | 68.6(2) | C34 | C35 | Fe3 | 69.4(3) | |
| C41 | Fe4 | C44 | 68.9(2) | C34 | C35 | C36 | 108.3(5) | |
| C41 | Fe4 | C45 | 124.1(2) | C36 | C35 | Fe3 | 69.1(3) | |
| C41 | Fe4 | C46 | 106.4(2) | C32 | C36 | Fe3 | 69.8(3) | |
| C41 | Fe4 | C47 | 120.0(3) | C32 | C36 | C35 | 107.5(5) | |
| C41 | Fe4 | C48 | 155.7(3) | C35 | C36 | Fe3 | 70.4(3) | |
| C41 | Fe4 | C49 | 160.5(3) | N3 | C37 | C28 | 112.9(5) | |
| C42 | Fe4 | C40 | 68.9(2) | Si4 | C40 | Fe4 | 121.7(2) | |
| C42 | Fe4 | C43 | 40.6(2) | C41 | C40 | Fe4 | 68.4(3) | |
| C42 | Fe4 | C44 | 68.0(2) | C41 | C40 | Si4 | 130.1(3) | |
| C42 | Fe4 | C45 | 160.1(3) | C44 | C40 | Fe4 | 69.5(3) | |
| C42 | Fe4 | C48 | 121.9(3) | C44 | C40 | Si4 | 123.5(3) | |
| C42 | Fe4 | C49 | 158.2(3) | C44 | C40 | C41 | 106.1(4) | |
| C43 | Fe4 | C44 | 40.4(2) | C40 | C41 | Fe4 | 69.8(3) | |
| C43 | Fe4 | C45 | 158.2(3) | C40 | C41 | C50 | 126.3(4) | |
| C44 | Fe4 | C45 | 123.1(3) | C42 | C41 | Fe4 | 70.2(3) | |
| C46 | Fe4 | C40 | 120.4(3) | C42 | C41 | C40 | 108.1(4) | |
| C46 | Fe4 | C42 | 123.9(3) | C42 | C41 | C50 | 125.7(5) | |
| C46 | Fe4 | C43 | 160.9(3) | C50 | C41 | Fe4 | 125.4(3) | |
| C46 | Fe4 | C44 | 156.9(3) | C41 | C42 | Fe4 | 69.4(3) | |
| C46 | Fe4 | C45 | 39.7(3) | C41 | C42 | C43 | 109.2(5) | |
| C46 | Fe4 | C47 | 39.8(3) | C43 | C42 | Fe4 | 70.1(3) | |
| C46 | Fe4 | C48 | 67.8(3) | C42 | C43 | Fe4 | 69.3(3) | |
| C46 | Fe4 | C49 | 67.8(3) | C44 | C43 | Fe4 | 69.9(3) | |
| C47 | Fe4 | C40 | 155.5(3) | C44 | C43 | C42 | 107.8(5) | |
| C47 | Fe4 | C42 | 107.9(3) | C40 | C44 | Fe4 | 69.4(3) | |
| C47 | Fe4 | C43 | 125.4(3) | C43 | C44 | Fe4 | 69.8(3) | |
| C47 | Fe4 | C44 | 162.2(3) | C43 | C44 | C40 | 108.9(5) | |
| C47 | Fe4 | C45 | 66.6(3) | C46 | C45 | Fe4 | 69.4(4) | |
| C47 | Fe4 | C48 | 40.5(3) | C46 | C45 | C49 | 109.7(7) | |
| C47 | Fe4 | C49 | 68.3(3) | C49 | C45 | Fe4 | 69.8(4) | |
| C48 | Fe4 | C40 | 161.9(3) | C45 | C46 | Fe4 | 70.9(4) | |
| C48 | Fe4 | C43 | 108.8(3) | C47 | C46 | Fe4 | 70.1(4) | |
| C48 | Fe4 | C44 | 125.7(3) | C47 | C46 | C45 | 108.2(7) | |
| C48 | Fe4 | C45 | 67.4(3) | C46 | C47 | Fe4 | 70.1(4) | |
| C49 | Fe4 | C40 | 123.7(3) | C46 | C47 | C48 | 108.9(7) | |
| C49 | Fe4 | C43 | 122.9(3) | C48 | C47 | Fe4 | 70.4(4) | |
| C49 | Fe4 | C44 | 108.7(2) | C47 | C48 | Fe4 | 69.2(4) | |
| C49 | Fe4 | C45 | 39.9(3) | C47 | C48 | C49 | 106.7(6) | |
| C49 | Fe4 | C48 | 41.3(3) | C49 | C48 | Fe4 | 69.3(4) | |
| O1 | Si1 | O2 | 111.9(2) | C45 | C49 | Fe4 | 70.3(4) | |
| O1 | Si1 | O8 | 109.26(19) | C45 | C49 | C48 | 106.5(6) | |
| O1 | Si1 | C1 | 109.7(2) | C48 | C49 | Fe4 | 69.4(4) | |
| O2 | Si1 | O8 | 107.00(17) | N4 | C50 | C41 | 113.4(4) |
| D | H | A | d(D-H)/Å | d(H-A)/Å | d(D-A)/Å | D-H-A/° |
|---|---|---|---|---|---|---|
| O1 | H1A | N2 | 1.00(2) | 1.69(3) | 2.661(6) | 163(6) |
| O1 | H1B | O9 | 1.01(2) | 1.87(4) | 2.836(6) | 159(8) |
| O3 | H3 | N3 | 0.98(2) | 1.82(3) | 2.775(6) | 163(6) |
| O5 | H5 | N4 | 0.971(19) | 1.75(2) | 2.688(6) | 162(4) |
| O7 | H7 | N1 | 0.96(2) | 1.79(3) | 2.722(5) | 162(5) |
| A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|---|---|
| Fe1 | C1 | C2 | C3 | -59.6(4) | O8 | Si4 | C40 | C41 | -31.1(5) | |
| Fe1 | C1 | C2 | C11 | 117.1(5) | O8 | Si4 | C40 | C44 | 141.6(4) | |
| Fe1 | C1 | C5 | C4 | 59.1(4) | C1 | Si1 | O2 | Si2 | 173.0(3) | |
| Fe1 | C2 | C3 | C4 | -59.0(4) | C1 | Si1 | O8 | Si4 | 98.8(4) | |
| Fe1 | C2 | C11 | N1 | 169.5(3) | C1 | C2 | C3 | Fe1 | 59.1(3) | |
| Fe1 | C3 | C4 | C5 | -59.4(4) | C1 | C2 | C3 | C4 | 0.1(6) | |
| Fe1 | C4 | C5 | C1 | -58.9(4) | C1 | C2 | C11 | N1 | 82.0(6) | |
| Fe1 | C6 | C7 | C8 | 59.2(4) | C2 | C1 | C5 | Fe1 | -59.6(3) | |
| Fe1 | C6 | C10 | C9 | -60.1(4) | C2 | C1 | C5 | C4 | -0.6(6) | |
| Fe1 | C7 | C8 | C9 | 60.3(4) | C2 | C3 | C4 | Fe1 | 58.9(4) | |
| Fe1 | C8 | C9 | C10 | 59.3(4) | C2 | C3 | C4 | C5 | -0.5(6) | |
| Fe1 | C9 | C10 | C6 | 59.6(4) | C3 | C2 | C11 | N1 | -102.0(6) | |
| Fe2 | C14 | C15 | C16 | 60.9(4) | C3 | C4 | C5 | Fe1 | 59.5(4) | |
| Fe2 | C14 | C15 | C24 | -117.5(5) | C3 | C4 | C5 | C1 | 0.6(6) | |
| Fe2 | C14 | C18 | C17 | -58.2(4) | C5 | C1 | C2 | Fe1 | 59.8(3) | |
| Fe2 | C15 | C16 | C17 | 58.2(4) | C5 | C1 | C2 | C3 | 0.3(6) | |
| Fe2 | C15 | C24 | N2 | -166.2(3) | C5 | C1 | C2 | C11 | 176.9(5) | |
| Fe2 | C16 | C17 | C18 | 59.5(4) | C6 | C7 | C8 | Fe1 | -59.1(4) | |
| Fe2 | C17 | C18 | C14 | 57.5(4) | C6 | C7 | C8 | C9 | 1.2(7) | |
| Fe2 | C19 | C20 | C21 | -58.7(4) | C7 | C6 | C10 | Fe1 | 60.3(4) | |
| Fe2 | C19 | C23 | C22 | 60.3(5) | C7 | C6 | C10 | C9 | 0.2(7) | |
| Fe2 | C20 | C21 | C22 | -60.5(4) | C7 | C8 | C9 | Fe1 | -60.4(4) | |
| Fe2 | C21 | C22 | C23 | -58.6(5) | C7 | C8 | C9 | C10 | -1.1(6) | |
| Fe2 | C22 | C23 | C19 | -60.3(4) | C8 | C9 | C10 | Fe1 | -59.0(4) | |
| Fe3 | C27 | C28 | C29 | -59.3(3) | C8 | C9 | C10 | C6 | 0.6(6) | |
| Fe3 | C27 | C28 | C37 | 119.3(5) | C10 | C6 | C7 | Fe1 | -60.1(4) | |
| Fe3 | C27 | C31 | C30 | 58.7(4) | C10 | C6 | C7 | C8 | -0.9(7) | |
| Fe3 | C28 | C29 | C30 | -59.7(4) | C11 | C2 | C3 | Fe1 | -117.5(5) | |
| Fe3 | C28 | C37 | N3 | 168.6(4) | C11 | C2 | C3 | C4 | -176.5(5) | |
| Fe3 | C29 | C30 | C31 | -59.2(4) | C12 | N1 | C11 | C2 | 61.4(6) | |
| Fe3 | C30 | C31 | C27 | -58.2(4) | C13 | N1 | C11 | C2 | -176.1(4) | |
| Fe3 | C32 | C33 | C34 | 59.7(4) | C14 | Si2 | O2 | Si1 | -95.7(4) | |
| Fe3 | C32 | C36 | C35 | -60.7(4) | C14 | Si2 | O4 | Si3 | -178.4(3) | |
| Fe3 | C33 | C34 | C35 | 60.2(4) | C14 | C15 | C16 | Fe2 | -59.8(3) | |
| Fe3 | C34 | C35 | C36 | 58.3(4) | C14 | C15 | C16 | C17 | -1.5(6) | |
| Fe3 | C35 | C36 | C32 | 60.3(4) | C14 | C15 | C24 | N2 | -79.1(6) | |
| Fe4 | C40 | C41 | C42 | 60.0(4) | C15 | C14 | C18 | Fe2 | 59.0(3) | |
| Fe4 | C40 | C41 | C50 | -119.7(5) | C15 | C14 | C18 | C17 | 0.8(6) | |
| Fe4 | C40 | C44 | C43 | -58.7(4) | C15 | C16 | C17 | Fe2 | -57.5(4) | |
| Fe4 | C41 | C42 | C43 | 59.0(4) | C15 | C16 | C17 | C18 | 2.0(6) | |
| Fe4 | C41 | C50 | N4 | -170.0(3) | C16 | C15 | C24 | N2 | 102.8(6) | |
| Fe4 | C42 | C43 | C44 | 59.5(4) | C16 | C17 | C18 | Fe2 | -59.3(4) | |
| Fe4 | C43 | C44 | C40 | 58.5(3) | C16 | C17 | C18 | C14 | -1.7(6) | |
| Fe4 | C45 | C46 | C47 | -60.5(5) | C18 | C14 | C15 | Fe2 | -60.4(3) | |
| Fe4 | C45 | C49 | C48 | 60.3(4) | C18 | C14 | C15 | C16 | 0.4(6) | |
| Fe4 | C46 | C47 | C48 | -59.9(5) | C18 | C14 | C15 | C24 | -177.9(5) | |
| Fe4 | C47 | C48 | C49 | -59.4(4) | C19 | C20 | C21 | Fe2 | 58.8(4) | |
| Fe4 | C48 | C49 | C45 | -60.9(4) | C19 | C20 | C21 | C22 | -1.6(7) | |
| Si1 | C1 | C2 | Fe1 | -116.3(4) | C20 | C19 | C23 | Fe2 | -60.4(4) | |
| Si1 | C1 | C2 | C3 | -175.9(4) | C20 | C19 | C23 | C22 | 0.0(7) | |
| Si1 | C1 | C2 | C11 | 0.8(7) | C20 | C21 | C22 | Fe2 | 60.2(4) | |
| Si1 | C1 | C5 | Fe1 | 116.7(4) | C20 | C21 | C22 | C23 | 1.6(7) | |
| Si1 | C1 | C5 | C4 | 175.7(4) | C21 | C22 | C23 | Fe2 | 59.3(4) | |
| Si2 | C14 | C15 | Fe2 | 114.9(4) | C21 | C22 | C23 | C19 | -1.0(7) | |
| Si2 | C14 | C15 | C16 | 175.7(4) | C23 | C19 | C20 | Fe2 | 59.8(4) | |
| Si2 | C14 | C15 | C24 | -2.6(8) | C23 | C19 | C20 | C21 | 1.0(7) | |
| Si2 | C14 | C18 | Fe2 | -116.5(4) | C24 | C15 | C16 | Fe2 | 118.6(5) | |
| Si2 | C14 | C18 | C17 | -174.8(4) | C24 | C15 | C16 | C17 | 176.8(5) | |
| Si3 | C27 | C28 | Fe3 | -117.0(4) | C25 | N2 | C24 | C15 | -65.0(6) | |
| Si3 | C27 | C28 | C29 | -176.2(4) | C26 | N2 | C24 | C15 | 173.7(4) | |
| Si3 | C27 | C28 | C37 | 2.3(7) | C27 | Si3 | O4 | Si2 | 100.5(3) | |
| Si3 | C27 | C31 | Fe3 | 117.6(4) | C27 | Si3 | O6 | Si4 | 177.0(3) | |
| Si3 | C27 | C31 | C30 | 176.4(4) | C27 | C28 | C29 | Fe3 | 59.1(3) | |
| Si4 | C40 | C41 | Fe4 | 113.9(4) | C27 | C28 | C29 | C30 | -0.6(6) | |
| Si4 | C40 | C41 | C42 | 174.0(4) | C27 | C28 | C37 | N3 | 80.3(6) | |
| Si4 | C40 | C41 | C50 | -5.8(7) | C28 | C27 | C31 | Fe3 | -59.9(3) | |
| Si4 | C40 | C44 | Fe4 | -115.2(3) | C28 | C27 | C31 | C30 | -1.1(6) | |
| Si4 | C40 | C44 | C43 | -173.9(4) | C28 | C29 | C30 | Fe3 | 59.1(4) | |
| O1 | Si1 | O2 | Si2 | 51.4(4) | C28 | C29 | C30 | C31 | -0.1(6) | |
| O1 | Si1 | O8 | Si4 | -140.9(3) | C29 | C28 | C37 | N3 | -101.5(6) | |
| O1 | Si1 | C1 | Fe1 | 62.5(3) | C29 | C30 | C31 | Fe3 | 59.0(4) | |
| O1 | Si1 | C1 | C2 | 151.0(4) | C29 | C30 | C31 | C27 | 0.8(6) | |
| O1 | Si1 | C1 | C5 | -24.4(5) | C31 | C27 | C28 | Fe3 | 60.3(3) | |
| O2 | Si1 | O8 | Si4 | -19.6(4) | C31 | C27 | C28 | C29 | 1.1(5) | |
| O2 | Si1 | C1 | Fe1 | -60.4(3) | C31 | C27 | C28 | C37 | 179.6(5) | |
| O2 | Si1 | C1 | C2 | 28.1(5) | C32 | C33 | C34 | Fe3 | -59.7(4) | |
| O2 | Si1 | C1 | C5 | -147.4(4) | C32 | C33 | C34 | C35 | 0.5(6) | |
| O2 | Si2 | O4 | Si3 | 64.8(4) | C33 | C32 | C36 | Fe3 | 59.2(4) | |
| O2 | Si2 | C14 | Fe2 | 178.3(2) | C33 | C32 | C36 | C35 | -1.5(6) | |
| O2 | Si2 | C14 | C15 | 91.2(5) | C33 | C34 | C35 | Fe3 | -59.7(4) | |
| O2 | Si2 | C14 | C18 | -94.3(5) | C33 | C34 | C35 | C36 | -1.4(6) | |
| O3 | Si2 | O2 | Si1 | 144.7(3) | C34 | C35 | C36 | Fe3 | -58.5(4) | |
| O3 | Si2 | O4 | Si3 | -55.8(4) | C34 | C35 | C36 | C32 | 1.8(6) | |
| O3 | Si2 | C14 | Fe2 | -63.0(3) | C36 | C32 | C33 | Fe3 | -59.1(4) | |
| O3 | Si2 | C14 | C15 | -150.1(4) | C36 | C32 | C33 | C34 | 0.6(6) | |
| O3 | Si2 | C14 | C18 | 24.3(5) | C37 | C28 | C29 | Fe3 | -119.4(5) | |
| O4 | Si2 | O2 | Si1 | 22.1(4) | C37 | C28 | C29 | C30 | -179.1(5) | |
| O4 | Si2 | C14 | Fe2 | 60.6(3) | C38 | N3 | C37 | C28 | -179.5(5) | |
| O4 | Si2 | C14 | C15 | -26.5(5) | C39 | N3 | C37 | C28 | 56.4(6) | |
| O4 | Si2 | C14 | C18 | 147.9(4) | C40 | Si4 | O6 | Si3 | -101.4(3) | |
| O4 | Si3 | O6 | Si4 | -63.9(4) | C40 | Si4 | O8 | Si1 | -175.7(3) | |
| O4 | Si3 | C27 | Fe3 | 179.9(2) | C40 | C41 | C42 | Fe4 | -59.8(3) | |
| O4 | Si3 | C27 | C28 | -90.1(4) | C40 | C41 | C42 | C43 | -0.8(6) | |
| O4 | Si3 | C27 | C31 | 93.0(4) | C40 | C41 | C50 | N4 | -80.2(6) | |
| O5 | Si3 | O4 | Si2 | -141.5(3) | C41 | C40 | C44 | Fe4 | 58.9(3) | |
| O5 | Si3 | O6 | Si4 | 55.1(4) | C41 | C40 | C44 | C43 | 0.2(6) | |
| O5 | Si3 | C27 | Fe3 | 62.8(3) | C41 | C42 | C43 | Fe4 | -58.6(4) | |
| O5 | Si3 | C27 | C28 | 152.8(4) | C41 | C42 | C43 | C44 | 0.9(7) | |
| O5 | Si3 | C27 | C31 | -24.1(5) | C42 | C41 | C50 | N4 | 100.1(6) | |
| O6 | Si3 | O4 | Si2 | -19.3(4) | C42 | C43 | C44 | Fe4 | -59.2(4) | |
| O6 | Si3 | C27 | Fe3 | -61.4(3) | C42 | C43 | C44 | C40 | -0.7(6) | |
| O6 | Si3 | C27 | C28 | 28.6(5) | C44 | C40 | C41 | Fe4 | -59.7(3) | |
| O6 | Si3 | C27 | C31 | -148.3(4) | C44 | C40 | C41 | C42 | 0.4(5) | |
| O6 | Si4 | O8 | Si1 | 67.1(3) | C44 | C40 | C41 | C50 | -179.4(5) | |
| O6 | Si4 | C40 | Fe4 | 174.6(2) | C45 | C46 | C47 | Fe4 | 61.0(4) | |
| O6 | Si4 | C40 | C41 | 87.2(4) | C45 | C46 | C47 | C48 | 1.2(8) | |
| O6 | Si4 | C40 | C44 | -100.2(4) | C46 | C45 | C49 | Fe4 | -58.0(4) | |
| O7 | Si4 | O6 | Si3 | 140.0(3) | C46 | C45 | C49 | C48 | 2.3(7) | |
| O7 | Si4 | O8 | Si1 | -53.5(4) | C46 | C47 | C48 | Fe4 | 59.7(5) | |
| O7 | Si4 | C40 | Fe4 | -67.5(3) | C46 | C47 | C48 | C49 | 0.2(8) | |
| O7 | Si4 | C40 | C41 | -154.9(4) | C47 | C48 | C49 | Fe4 | 59.3(5) | |
| O7 | Si4 | C40 | C44 | 17.7(4) | C47 | C48 | C49 | C45 | -1.5(7) | |
| O8 | Si1 | O2 | Si2 | -68.3(4) | C49 | C45 | C46 | Fe4 | 58.3(4) | |
| O8 | Si1 | C1 | Fe1 | -177.4(2) | C49 | C45 | C46 | C47 | -2.2(7) | |
| O8 | Si1 | C1 | C2 | -88.9(5) | C50 | C41 | C42 | Fe4 | 119.9(5) | |
| O8 | Si1 | C1 | C5 | 95.6(4) | C50 | C41 | C42 | C43 | 178.9(5) | |
| O8 | Si4 | O6 | Si3 | 17.1(4) | C51 | N4 | C50 | C41 | -179.6(4) | |
| O8 | Si4 | C40 | Fe4 | 56.4(3) | C52 | N4 | C50 | C41 | -57.4(5) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| H1A | 1470(40) | 5660(30) | 6867(19) | 80(20) |
| H1B | 2160(70) | 4640(50) | 7040(20) | 190(40) |
| H3 | 2360(30) | 7830(40) | 5440(20) | 90(20) |
| H5 | 4240(30) | 7330(30) | 7093(14) | 43(15) |
| H7 | 3980(30) | 5180(30) | 5574(16) | 69(19) |
| H3A | 1804 | 2150 | 5370 | 66 |
| H4 | 1775 | 1497 | 6127 | 74 |
| H5A | 2132 | 2898 | 6655 | 59 |
| H6 | -300 | 4297 | 5315 | 79 |
| H7A | -682 | 2488 | 5349 | 83 |
| H8 | -648 | 2025 | 6139 | 75 |
| H9 | -309 | 3578 | 6587 | 61 |
| H10 | -75 | 4980 | 6073 | 65 |
| H11A | 1759 | 3922 | 5015 | 53 |
| H11B | 1766 | 4849 | 5335 | 53 |
| H12A | 3334 | 3290 | 4818 | 113 |
| H12B | 3789 | 3165 | 5317 | 113 |
| H12C | 4382 | 3812 | 4997 | 113 |
| H13A | 2755 | 5833 | 4918 | 108 |
| H13B | 2627 | 4952 | 4571 | 108 |
| H13C | 3731 | 5373 | 4736 | 108 |
| H16 | -1566 | 7649 | 6609 | 56 |
| H17 | -2086 | 7527 | 5800 | 60 |
| H18 | -526 | 7127 | 5446 | 56 |
| H19 | 1388 | 9409 | 5926 | 77 |
| H20 | 819 | 9684 | 6646 | 81 |
| H21 | -1080 | 9998 | 6557 | 72 |
| H22 | -1645 | 9991 | 5747 | 77 |
| H23 | -128 | 9595 | 5358 | 92 |
| H24A | 1164 | 7869 | 6883 | 52 |
| H24B | 159 | 7850 | 7119 | 52 |
| H25A | -460 | 5841 | 6974 | 104 |
| H25B | -347 | 6346 | 7444 | 104 |
| H25C | 243 | 5341 | 7370 | 104 |
| H26A | 1229 | 7113 | 7728 | 93 |
| H26B | 2165 | 7087 | 7448 | 93 |
| H26C | 1793 | 6091 | 7658 | 93 |
| H29 | 4484 | 10940 | 5669 | 61 |
| H30 | 4144 | 11503 | 6406 | 66 |
| H31 | 3622 | 10029 | 6821 | 54 |
| H32 | 6129 | 8042 | 6561 | 59 |
| H33 | 6660 | 8974 | 5920 | 67 |
| H34 | 6859 | 10777 | 6134 | 62 |
| H35 | 6479 | 10945 | 6908 | 62 |
| H36 | 5966 | 9264 | 7166 | 65 |
| H37A | 4689 | 9192 | 5285 | 57 |
| H37B | 4592 | 8229 | 5576 | 57 |
| H38A | 3814 | 7363 | 4961 | 159 |
| H38B | 3905 | 8320 | 4664 | 159 |
| H38C | 2828 | 7799 | 4678 | 159 |
| H39A | 3132 | 9878 | 4884 | 156 |
| H39B | 2594 | 9881 | 5319 | 156 |
| H39C | 2084 | 9304 | 4898 | 156 |
| H42 | 7390 | 5235 | 7326 | 62 |
| H43 | 8110 | 5251 | 6609 | 66 |
| H44 | 6696 | 5676 | 6022 | 51 |
| H45 | 4587 | 3497 | 6226 | 78 |
| H46 | 4923 | 3337 | 7030 | 89 |
| H47 | 6738 | 2897 | 7224 | 101 |
| H48 | 7582 | 2836 | 6536 | 90 |
| H49 | 6215 | 3270 | 5904 | 94 |
| H50A | 4624 | 5283 | 7206 | 55 |
| H50B | 5568 | 5228 | 7577 | 55 |
| H51A | 4670 | 6205 | 8046 | 111 |
| H51B | 3720 | 6256 | 7677 | 111 |
| H51C | 4207 | 7253 | 7887 | 111 |
| H52A | 6429 | 7183 | 7387 | 93 |
| H52B | 6346 | 6766 | 7865 | 93 |
| H52C | 5833 | 7801 | 7717 | 93 |
Experimental
Single crystals of C52H69Fe4N4O9Si4 [3021] were [The material was recrystallised from a mixture of acetone and water by slow evaporation]. A suitable crystal was selected and [The crystal was mounted on a MITIGEN holder oil] on a Xcalibur, Sapphire3 diffractometer. The crystal was kept at 173 K during data collection. Using Olex2 [1], the structure was solved with the XS [2] structure solution program using Direct Methods and refined with the XL [3] refinement package using Least Squares minimisation.
Crystal structure determination of [3021]
Crystal Data for C52H69Fe4N4O9Si4 (M =1229.87 g/mol): monoclinic, space group P21/n (no. 14), a = 13.2912(7) Å, b = 13.5363(7) Å, c = 30.9964(18) Å, β = 96.859(5)°, V = 5536.8(5) Å3, Z = 4, T = 173 K, μ(MoKα) = 1.171 mm-1, Dcalc = 1.475 g/cm3, 42828 reflections measured (4.31° ≤ 2Θ ≤ 53.998°), 11995 unique (Rint = 0.0745, Rsigma = 0.0936) which were used in all calculations. The final R1 was 0.0634 (I > 2σ(I)) and wR2 was 0.1626 (all data).
Refinement model description
Number of restraints - 5, 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
O7-H7 = O5-H5 = O3-H3 = O1-H1A
1 with sigma of 0.02
O1-H1B
1 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
C11(H11A,H11B), C24(H24A,H24B), C37(H37A,H37B), C50(H50A,H50B)
3.b Aromatic/amide H refined with riding coordinates:
C3(H3A), C4(H4), C5(H5A), C6(H6), C7(H7A), C8(H8), C9(H9), C10(H10), C16(H16),
C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23),
C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36),
C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49)
3.c Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C25(H25A,H25B,H25C), C26(H26A,H26B,
H26C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C51(H51A,H51B,H51C), C52(H52A,
H52B,H52C)
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.