| Identification code | 3207_twin1_hklf4 |
| Empirical formula | C36H58Fe2Li2N2OSi2 |
| Formula weight | 716.60 |
| Temperature/K | 173.15 |
| Crystal system | triclinic |
| Space group | P-1 |
| a/Å | 9.3542(8) |
| b/Å | 9.9397(8) |
| c/Å | 22.1527(17) |
| α/° | 79.942(7) |
| β/° | 78.411(7) |
| γ/° | 70.771(7) |
| Volume/Å3 | 1892.0(3) |
| Z | 2 |
| ρcalcg/cm3 | 1.258 |
| μ/mm‑1 | 0.859 |
| F(000) | 764.0 |
| Crystal size/mm3 | 0.14 × 0.06 × 0.045 |
| Radiation | MoKα (λ = 0.71073) |
| 2Θ range for data collection/° | 4.37 to 51.998 |
| Index ranges | -11 ≤ h ≤ 11, -12 ≤ k ≤ 12, -27 ≤ l ≤ 27 |
| Reflections collected | 8461 |
| Independent reflections | 8461 [Rint = 0.1294, Rsigma = 0.1020] |
| Data/restraints/parameters | 8461/6/431 |
| Goodness-of-fit on F2 | 1.034 |
| Final R indexes [I>=2σ (I)] | R1 = 0.0506, wR2 = 0.1223 |
| Final R indexes [all data] | R1 = 0.0805, wR2 = 0.1391 |
| Largest diff. peak/hole / e Å-3 | 0.48/-0.48 |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| Fe1 | 4141.6(9) | 4453.4(9) | 8892.7(4) | 26.5(2) |
| Fe2 | 4920.7(9) | 6107.2(9) | 6258.3(4) | 24.9(2) |
| Si2 | 7760.5(18) | 7404.1(18) | 5268.9(8) | 28.4(4) |
| Si1 | 2171(2) | 1983.6(19) | 9573.3(8) | 33.1(4) |
| N1 | 4571(5) | 1633(5) | 7522(2) | 24.8(11) |
| O1 | 8473(4) | 689(4) | 7389(2) | 39.4(11) |
| C1 | 3894(6) | 2442(6) | 9120(3) | 23.1(13) |
| C7 | 2388(7) | 6204(6) | 8630(3) | 33.0(15) |
| N2 | 7974(5) | 5436(5) | 7450(2) | 27.6(12) |
| C14 | 3525(7) | 2645(7) | 7948(3) | 24.9(13) |
| C19 | 6539(6) | 4308(6) | 6675(3) | 25.7(14) |
| C16 | 3809(7) | 1737(7) | 6990(3) | 36.8(16) |
| C15 | 4910(7) | 164(6) | 7828(3) | 34.2(15) |
| C20 | 6135(6) | 4036(6) | 6124(3) | 27.6(15) |
| C18 | 7138(6) | 5516(6) | 6447(3) | 24.5(14) |
| C30 | 7717(7) | 6270(7) | 6849(3) | 30.7(15) |
| C12 | 349(6) | 3070(7) | 9259(3) | 39.6(17) |
| C17 | 7093(6) | 5986(6) | 5793(3) | 24.8(13) |
| C6 | 2177(7) | 5867(6) | 9278(3) | 34.3(16) |
| C3 | 5822(6) | 3009(6) | 8312(3) | 27.9(14) |
| C21 | 6455(6) | 5027(6) | 5593(3) | 25.5(14) |
| C13 | 2054(7) | 2297(8) | 10407(3) | 49.5(19) |
| C8 | 3815(7) | 6510(6) | 8448(3) | 37.4(16) |
| C26 | 2991(6) | 7211(7) | 5862(3) | 37.6(16) |
| C23 | 3538(7) | 7772(6) | 6728(3) | 39.7(18) |
| C5 | 5106(6) | 2563(6) | 9397(3) | 27.0(14) |
| C2 | 4339(6) | 2721(5) | 8463(3) | 21.5(13) |
| C29 | 6977(8) | 9218(7) | 5567(3) | 52(2) |
| C32 | 8205(7) | 6297(7) | 7874(3) | 42.8(18) |
| C10 | 3448(7) | 5959(6) | 9502(3) | 37.5(17) |
| C25 | 2664(6) | 6246(7) | 6363(3) | 38.7(17) |
| C31 | 9318(6) | 4169(6) | 7382(3) | 37.8(17) |
| C4 | 6211(6) | 2916(6) | 8914(3) | 32.0(15) |
| C22 | 3535(6) | 8167(7) | 6095(4) | 42.4(19) |
| C24 | 2997(6) | 6559(6) | 6913(3) | 34.3(16) |
| C27 | 9890(7) | 6928(7) | 5187(4) | 51(2) |
| C33 | 8776(7) | -69(7) | 7995(4) | 48(2) |
| C9 | 4452(7) | 6347(6) | 8995(3) | 38.3(17) |
| C34 | 10176(9) | 64(8) | 8172(5) | 77(3) |
| C28 | 7194(8) | 7534(7) | 4499(3) | 49.3(19) |
| Li1 | 6572(11) | 2339(10) | 7364(5) | 30(2) |
| C36 | 9378(9) | 720(9) | 6329(4) | 74(2) |
| C11 | 2377(8) | 59(7) | 9548(4) | 59(2) |
| C35 | 9446(11) | -91(10) | 6917(5) | 95(3) |
| Li2 | 6131(10) | 4682(11) | 7632(5) | 32(3) |
| Atom | U11 | U22 | U33 | U23 | U13 | U12 |
|---|---|---|---|---|---|---|
| Fe1 | 26.2(5) | 31.3(5) | 23.7(5) | -8.8(4) | -4.8(4) | -7.8(4) |
| Fe2 | 21.8(4) | 26.7(5) | 25.6(5) | -4.6(4) | -4.7(4) | -5.3(4) |
| Si2 | 28.5(9) | 32(1) | 24.8(10) | -1.8(8) | -4.8(8) | -9.9(8) |
| Si1 | 31.4(10) | 39.5(11) | 26.7(11) | 1.5(9) | -6.4(9) | -10.0(8) |
| N1 | 26(3) | 23(3) | 27(3) | -9(2) | -7(2) | -6(2) |
| O1 | 27(2) | 32(3) | 50(3) | -11(2) | -4(2) | 5(2) |
| C1 | 24(3) | 23(3) | 23(3) | -7(3) | -6(3) | -5(3) |
| C7 | 36(4) | 33(4) | 24(4) | -9(3) | -8(3) | 3(3) |
| N2 | 37(3) | 24(3) | 25(3) | 4(2) | -12(2) | -13(2) |
| C14 | 21(3) | 35(4) | 20(3) | -1(3) | -9(3) | -8(3) |
| C19 | 21(3) | 18(3) | 35(4) | -5(3) | -7(3) | 0(2) |
| C16 | 42(4) | 42(4) | 28(4) | -12(3) | -7(3) | -11(3) |
| C15 | 47(4) | 27(3) | 36(4) | -4(3) | -20(3) | -11(3) |
| C20 | 21(3) | 19(3) | 45(4) | -13(3) | -7(3) | -4(2) |
| C18 | 18(3) | 23(3) | 30(4) | -9(3) | -1(3) | -1(2) |
| C30 | 31(4) | 35(4) | 33(4) | 1(3) | -14(3) | -17(3) |
| C12 | 30(4) | 60(5) | 32(4) | -7(3) | 0(3) | -20(3) |
| C17 | 20(3) | 26(3) | 28(4) | -10(3) | -6(3) | -1(2) |
| C6 | 30(4) | 28(3) | 42(4) | -20(3) | 3(3) | -3(3) |
| C3 | 23(3) | 37(4) | 26(4) | -12(3) | -2(3) | -10(3) |
| C21 | 25(3) | 31(3) | 22(3) | -6(3) | -8(3) | -6(3) |
| C13 | 40(4) | 79(5) | 25(4) | 9(4) | -12(3) | -15(4) |
| C8 | 51(4) | 25(3) | 31(4) | -2(3) | -4(4) | -8(3) |
| C26 | 25(3) | 48(4) | 36(4) | -5(4) | -14(3) | -1(3) |
| C23 | 38(4) | 27(4) | 46(5) | -16(3) | -12(4) | 9(3) |
| C5 | 29(3) | 35(3) | 18(3) | -3(2) | -16(2) | -2(2) |
| C2 | 27(3) | 16(3) | 22(3) | -3(3) | -14(3) | 1(2) |
| C29 | 53(5) | 53(5) | 50(5) | -11(4) | 4(4) | -22(4) |
| C32 | 55(4) | 41(4) | 41(5) | -17(3) | -5(4) | -21(3) |
| C10 | 52(4) | 34(4) | 31(4) | -20(3) | -9(4) | -9(3) |
| C25 | 16(3) | 38(4) | 62(5) | -10(4) | -9(3) | -4(3) |
| C31 | 33(4) | 29(3) | 51(5) | -5(3) | -21(3) | 0(3) |
| C4 | 27(3) | 37(4) | 33(4) | -11(3) | -12(3) | -3(3) |
| C22 | 17(3) | 28(4) | 69(6) | 1(4) | -2(4) | 5(3) |
| C24 | 25(3) | 31(4) | 35(4) | -7(3) | 8(3) | 1(3) |
| C27 | 34(4) | 55(5) | 66(6) | 1(4) | -7(4) | -21(3) |
| C33 | 38(4) | 28(4) | 70(6) | 3(4) | -13(4) | -1(3) |
| C9 | 44(4) | 26(3) | 49(5) | -17(3) | -3(4) | -12(3) |
| C34 | 74(6) | 64(6) | 103(8) | 0(6) | -23(6) | -33(5) |
| C28 | 67(5) | 54(5) | 32(4) | 11(4) | -16(4) | -28(4) |
| Li1 | 28(5) | 34(6) | 34(6) | -17(5) | -9(5) | -8(5) |
| C36 | 66(6) | 70(6) | 64(6) | -6(5) | 1(5) | -1(4) |
| C11 | 62(5) | 44(4) | 67(6) | 19(4) | -12(5) | -22(4) |
| C35 | 88(7) | 78(7) | 80(8) | 2(6) | 5(6) | 12(6) |
| Li2 | 22(5) | 30(6) | 43(7) | -7(5) | 6(5) | -15(5) |
| Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
|---|---|---|---|---|---|---|
| Fe1 | C1 | 2.052(5) | O1 | C35 | 1.400(9) | |
| Fe1 | C7 | 2.051(6) | C1 | C5 | 1.439(7) | |
| Fe1 | C6 | 2.042(6) | C1 | C2 | 1.437(7) | |
| Fe1 | C3 | 2.130(6) | C7 | C6 | 1.405(8) | |
| Fe1 | C8 | 2.061(6) | C7 | C8 | 1.430(8) | |
| Fe1 | C5 | 2.036(6) | N2 | C30 | 1.459(7) | |
| Fe1 | C2 | 2.050(5) | N2 | C32 | 1.466(7) | |
| Fe1 | C10 | 2.049(6) | N2 | C31 | 1.462(7) | |
| Fe1 | C4 | 2.037(6) | N2 | Li2 | 2.040(10) | |
| Fe1 | C9 | 2.053(6) | C14 | C2 | 1.517(7) | |
| Fe2 | C19 | 2.132(6) | C19 | C20 | 1.441(8) | |
| Fe2 | C20 | 2.039(5) | C19 | C18 | 1.459(7) | |
| Fe2 | C18 | 2.069(5) | C19 | Li1 | 2.257(12) | |
| Fe2 | C17 | 2.061(5) | C19 | Li2 | 2.151(12) | |
| Fe2 | C21 | 2.019(6) | C20 | C21 | 1.447(8) | |
| Fe2 | C26 | 2.056(6) | C18 | C30 | 1.530(7) | |
| Fe2 | C23 | 2.036(6) | C18 | C17 | 1.446(8) | |
| Fe2 | C25 | 2.037(6) | C17 | C21 | 1.446(7) | |
| Fe2 | C22 | 2.045(6) | C6 | C10 | 1.411(8) | |
| Fe2 | C24 | 2.047(6) | C3 | C2 | 1.469(7) | |
| Si2 | C17 | 1.855(6) | C3 | C4 | 1.431(8) | |
| Si2 | C29 | 1.891(6) | C3 | Li1 | 2.220(11) | |
| Si2 | C27 | 1.868(6) | C3 | Li2 | 2.094(12) | |
| Si2 | C28 | 1.858(7) | C8 | C9 | 1.417(9) | |
| Si1 | C1 | 1.868(6) | C26 | C25 | 1.389(9) | |
| Si1 | C12 | 1.886(6) | C26 | C22 | 1.422(8) | |
| Si1 | C13 | 1.901(7) | C23 | C22 | 1.390(9) | |
| Si1 | C11 | 1.869(7) | C23 | C24 | 1.423(8) | |
| N1 | C14 | 1.473(7) | C5 | C4 | 1.414(8) | |
| N1 | C16 | 1.469(7) | C10 | C9 | 1.399(9) | |
| N1 | C15 | 1.459(7) | C25 | C24 | 1.423(9) | |
| N1 | Li1 | 2.153(10) | C33 | C34 | 1.493(9) | |
| O1 | C33 | 1.451(8) | C36 | C35 | 1.410(11) | |
| O1 | Li1 | 1.985(10) |
| Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|
| C1 | Fe1 | C3 | 70.3(2) | C33 | O1 | Li1 | 117.1(5) | |
| C1 | Fe1 | C8 | 158.3(2) | C35 | O1 | C33 | 110.7(6) | |
| C1 | Fe1 | C9 | 159.5(2) | C35 | O1 | Li1 | 130.8(6) | |
| C7 | Fe1 | C1 | 122.0(2) | Si1 | C1 | Fe1 | 126.6(3) | |
| C7 | Fe1 | C3 | 127.5(2) | C5 | C1 | Fe1 | 68.8(3) | |
| C7 | Fe1 | C8 | 40.7(2) | C5 | C1 | Si1 | 123.9(4) | |
| C7 | Fe1 | C9 | 67.9(3) | C2 | C1 | Fe1 | 69.4(3) | |
| C6 | Fe1 | C1 | 107.4(2) | C2 | C1 | Si1 | 130.7(4) | |
| C6 | Fe1 | C7 | 40.2(2) | C2 | C1 | C5 | 105.4(5) | |
| C6 | Fe1 | C3 | 164.7(2) | C6 | C7 | Fe1 | 69.6(3) | |
| C6 | Fe1 | C8 | 67.8(3) | C6 | C7 | C8 | 107.7(6) | |
| C6 | Fe1 | C2 | 127.6(2) | C8 | C7 | Fe1 | 70.0(3) | |
| C6 | Fe1 | C10 | 40.4(2) | C30 | N2 | C32 | 111.0(5) | |
| C6 | Fe1 | C9 | 67.5(2) | C30 | N2 | C31 | 111.0(5) | |
| C8 | Fe1 | C3 | 108.5(2) | C30 | N2 | Li2 | 99.3(5) | |
| C5 | Fe1 | C1 | 41.2(2) | C32 | N2 | Li2 | 121.2(5) | |
| C5 | Fe1 | C7 | 155.8(2) | C31 | N2 | C32 | 108.5(5) | |
| C5 | Fe1 | C6 | 119.6(3) | C31 | N2 | Li2 | 105.5(4) | |
| C5 | Fe1 | C3 | 69.2(2) | N1 | C14 | C2 | 110.0(5) | |
| C5 | Fe1 | C8 | 160.0(2) | Fe2 | C19 | Li1 | 139.2(4) | |
| C5 | Fe1 | C2 | 68.1(2) | Fe2 | C19 | Li2 | 103.8(3) | |
| C5 | Fe1 | C10 | 105.2(2) | C20 | C19 | Fe2 | 66.3(3) | |
| C5 | Fe1 | C4 | 40.6(2) | C20 | C19 | C18 | 102.3(5) | |
| C5 | Fe1 | C9 | 122.4(3) | C20 | C19 | Li1 | 105.8(4) | |
| C2 | Fe1 | C1 | 41.0(2) | C20 | C19 | Li2 | 154.7(5) | |
| C2 | Fe1 | C7 | 111.4(2) | C18 | C19 | Fe2 | 67.4(3) | |
| C2 | Fe1 | C3 | 41.1(2) | C18 | C19 | Li1 | 148.0(5) | |
| C2 | Fe1 | C8 | 124.0(2) | C18 | C19 | Li2 | 94.2(4) | |
| C2 | Fe1 | C9 | 157.4(3) | Li2 | C19 | Li1 | 65.5(4) | |
| C10 | Fe1 | C1 | 123.4(3) | C19 | C20 | Fe2 | 73.3(3) | |
| C10 | Fe1 | C7 | 67.7(2) | C19 | C20 | C21 | 111.7(5) | |
| C10 | Fe1 | C3 | 153.5(2) | C21 | C20 | Fe2 | 68.4(3) | |
| C10 | Fe1 | C8 | 67.6(3) | C19 | C18 | Fe2 | 72.0(3) | |
| C10 | Fe1 | C2 | 162.5(2) | C19 | C18 | C30 | 124.7(5) | |
| C10 | Fe1 | C9 | 39.9(2) | C30 | C18 | Fe2 | 125.6(4) | |
| C4 | Fe1 | C1 | 68.7(2) | C17 | C18 | Fe2 | 69.2(3) | |
| C4 | Fe1 | C7 | 163.2(3) | C17 | C18 | C19 | 113.3(5) | |
| C4 | Fe1 | C6 | 154.3(3) | C17 | C18 | C30 | 121.9(5) | |
| C4 | Fe1 | C3 | 40.1(2) | N2 | C30 | C18 | 112.0(5) | |
| C4 | Fe1 | C8 | 125.1(3) | Si2 | C17 | Fe2 | 128.5(3) | |
| C4 | Fe1 | C2 | 67.1(2) | C18 | C17 | Fe2 | 69.8(3) | |
| C4 | Fe1 | C10 | 119.1(3) | C18 | C17 | Si2 | 131.2(4) | |
| C4 | Fe1 | C9 | 106.8(2) | C21 | C17 | Fe2 | 67.7(3) | |
| C9 | Fe1 | C3 | 120.0(2) | C21 | C17 | Si2 | 124.1(4) | |
| C9 | Fe1 | C8 | 40.3(2) | C21 | C17 | C18 | 104.6(5) | |
| C20 | Fe2 | C19 | 40.4(2) | C7 | C6 | Fe1 | 70.3(3) | |
| C20 | Fe2 | C18 | 66.7(2) | C7 | C6 | C10 | 108.4(6) | |
| C20 | Fe2 | C17 | 69.7(2) | C10 | C6 | Fe1 | 70.1(3) | |
| C20 | Fe2 | C26 | 122.4(2) | Fe1 | C3 | Li1 | 145.9(4) | |
| C20 | Fe2 | C22 | 159.9(3) | C2 | C3 | Fe1 | 66.5(3) | |
| C20 | Fe2 | C24 | 120.5(2) | C2 | C3 | Li1 | 99.7(4) | |
| C18 | Fe2 | C19 | 40.6(2) | C2 | C3 | Li2 | 120.4(5) | |
| C17 | Fe2 | C19 | 70.7(2) | C4 | C3 | Fe1 | 66.4(3) | |
| C17 | Fe2 | C18 | 41.0(2) | C4 | C3 | C2 | 102.2(5) | |
| C21 | Fe2 | C19 | 70.2(2) | C4 | C3 | Li1 | 147.1(5) | |
| C21 | Fe2 | C20 | 41.8(2) | C4 | C3 | Li2 | 119.8(5) | |
| C21 | Fe2 | C18 | 68.1(2) | Li2 | C3 | Fe1 | 92.4(4) | |
| C21 | Fe2 | C17 | 41.5(2) | Li2 | C3 | Li1 | 67.1(4) | |
| C21 | Fe2 | C26 | 106.1(2) | C20 | C21 | Fe2 | 69.8(3) | |
| C21 | Fe2 | C23 | 160.2(3) | C17 | C21 | Fe2 | 70.8(3) | |
| C21 | Fe2 | C25 | 120.7(2) | C17 | C21 | C20 | 108.0(5) | |
| C21 | Fe2 | C22 | 123.5(3) | C7 | C8 | Fe1 | 69.3(3) | |
| C21 | Fe2 | C24 | 156.6(2) | C9 | C8 | Fe1 | 69.5(3) | |
| C26 | Fe2 | C19 | 157.4(2) | C9 | C8 | C7 | 107.2(6) | |
| C26 | Fe2 | C18 | 160.2(2) | C25 | C26 | Fe2 | 69.4(4) | |
| C26 | Fe2 | C17 | 122.2(2) | C25 | C26 | C22 | 106.8(6) | |
| C23 | Fe2 | C19 | 122.8(2) | C22 | C26 | Fe2 | 69.3(3) | |
| C23 | Fe2 | C20 | 157.5(3) | C22 | C23 | Fe2 | 70.4(4) | |
| C23 | Fe2 | C18 | 110.8(2) | C22 | C23 | C24 | 109.0(6) | |
| C23 | Fe2 | C17 | 124.3(2) | C24 | C23 | Fe2 | 70.0(3) | |
| C23 | Fe2 | C26 | 67.8(3) | C1 | C5 | Fe1 | 70.0(3) | |
| C23 | Fe2 | C25 | 67.6(3) | C4 | C5 | Fe1 | 69.7(3) | |
| C23 | Fe2 | C22 | 39.8(3) | C4 | C5 | C1 | 108.0(5) | |
| C23 | Fe2 | C24 | 40.8(2) | C1 | C2 | Fe1 | 69.6(3) | |
| C25 | Fe2 | C19 | 121.8(3) | C1 | C2 | C14 | 127.8(5) | |
| C25 | Fe2 | C20 | 106.5(2) | C1 | C2 | C3 | 111.9(5) | |
| C25 | Fe2 | C18 | 159.7(3) | C14 | C2 | Fe1 | 129.1(4) | |
| C25 | Fe2 | C17 | 157.1(3) | C3 | C2 | Fe1 | 72.4(3) | |
| C25 | Fe2 | C26 | 39.7(2) | C3 | C2 | C14 | 120.2(5) | |
| C25 | Fe2 | C22 | 67.1(3) | C6 | C10 | Fe1 | 69.5(3) | |
| C25 | Fe2 | C24 | 40.8(2) | C9 | C10 | Fe1 | 70.2(3) | |
| C22 | Fe2 | C19 | 159.4(3) | C9 | C10 | C6 | 108.2(6) | |
| C22 | Fe2 | C18 | 125.6(2) | C26 | C25 | Fe2 | 70.9(3) | |
| C22 | Fe2 | C17 | 108.4(2) | C26 | C25 | C24 | 110.1(6) | |
| C22 | Fe2 | C26 | 40.6(2) | C24 | C25 | Fe2 | 70.0(3) | |
| C22 | Fe2 | C24 | 68.0(3) | C3 | C4 | Fe1 | 73.4(3) | |
| C24 | Fe2 | C19 | 105.6(2) | C5 | C4 | Fe1 | 69.7(3) | |
| C24 | Fe2 | C18 | 124.5(2) | C5 | C4 | C3 | 112.6(5) | |
| C24 | Fe2 | C17 | 160.6(2) | C26 | C22 | Fe2 | 70.1(3) | |
| C24 | Fe2 | C26 | 68.4(3) | C23 | C22 | Fe2 | 69.8(4) | |
| C17 | Si2 | C29 | 113.5(3) | C23 | C22 | C26 | 108.6(6) | |
| C17 | Si2 | C27 | 109.9(3) | C23 | C24 | Fe2 | 69.2(3) | |
| C17 | Si2 | C28 | 108.2(3) | C25 | C24 | Fe2 | 69.3(3) | |
| C27 | Si2 | C29 | 105.7(3) | C25 | C24 | C23 | 105.5(6) | |
| C28 | Si2 | C29 | 109.9(3) | O1 | C33 | C34 | 112.8(6) | |
| C28 | Si2 | C27 | 109.7(3) | C8 | C9 | Fe1 | 70.2(3) | |
| C1 | Si1 | C12 | 112.8(3) | C10 | C9 | Fe1 | 69.9(3) | |
| C1 | Si1 | C13 | 106.8(3) | C10 | C9 | C8 | 108.5(6) | |
| C1 | Si1 | C11 | 110.4(3) | N1 | Li1 | C19 | 116.5(5) | |
| C12 | Si1 | C13 | 111.0(3) | N1 | Li1 | C3 | 86.7(4) | |
| C11 | Si1 | C12 | 106.5(3) | O1 | Li1 | N1 | 111.4(5) | |
| C11 | Si1 | C13 | 109.4(3) | O1 | Li1 | C19 | 120.5(5) | |
| C14 | N1 | Li1 | 100.7(4) | O1 | Li1 | C3 | 107.2(5) | |
| C16 | N1 | C14 | 108.2(4) | C3 | Li1 | C19 | 108.5(4) | |
| C16 | N1 | Li1 | 118.2(5) | O1 | C35 | C36 | 112.1(7) | |
| C15 | N1 | C14 | 110.7(5) | N2 | Li2 | C19 | 88.7(4) | |
| C15 | N1 | C16 | 108.5(4) | N2 | Li2 | C3 | 126.0(6) | |
| C15 | N1 | Li1 | 110.3(4) | C3 | Li2 | C19 | 117.8(5) |
| A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|---|---|
| Fe1 | C1 | C5 | C4 | -59.6(4) | C6 | C10 | C9 | C8 | 0.4(7) | |
| Fe1 | C1 | C2 | C14 | -124.2(6) | C13 | Si1 | C1 | Fe1 | -70.4(4) | |
| Fe1 | C1 | C2 | C3 | 60.1(4) | C13 | Si1 | C1 | C5 | 17.2(5) | |
| Fe1 | C7 | C6 | C10 | 60.0(4) | C13 | Si1 | C1 | C2 | -163.9(5) | |
| Fe1 | C7 | C8 | C9 | -59.5(4) | C8 | C7 | C6 | Fe1 | -59.9(4) | |
| Fe1 | C6 | C10 | C9 | 59.8(4) | C8 | C7 | C6 | C10 | 0.1(7) | |
| Fe1 | C3 | C2 | C1 | -58.5(4) | C26 | C25 | C24 | Fe2 | -59.7(4) | |
| Fe1 | C3 | C2 | C14 | 125.5(5) | C26 | C25 | C24 | C23 | 0.3(7) | |
| Fe1 | C3 | C4 | C5 | 59.0(4) | C5 | C1 | C2 | Fe1 | -59.8(4) | |
| Fe1 | C8 | C9 | C10 | -59.6(4) | C5 | C1 | C2 | C14 | 176.0(5) | |
| Fe1 | C5 | C4 | C3 | -61.1(4) | C5 | C1 | C2 | C3 | 0.4(6) | |
| Fe1 | C10 | C9 | C8 | 59.7(4) | C2 | C1 | C5 | Fe1 | 60.2(4) | |
| Fe2 | C19 | C20 | C21 | 57.8(4) | C2 | C1 | C5 | C4 | 0.6(6) | |
| Fe2 | C19 | C18 | C30 | 121.3(5) | C2 | C3 | C4 | Fe1 | -57.4(4) | |
| Fe2 | C19 | C18 | C17 | -56.8(4) | C2 | C3 | C4 | C5 | 1.5(6) | |
| Fe2 | C20 | C21 | C17 | 60.8(4) | C29 | Si2 | C17 | Fe2 | 43.3(5) | |
| Fe2 | C18 | C30 | N2 | 106.5(5) | C29 | Si2 | C17 | C18 | -53.0(6) | |
| Fe2 | C18 | C17 | Si2 | 124.1(5) | C29 | Si2 | C17 | C21 | 130.6(5) | |
| Fe2 | C18 | C17 | C21 | -59.1(3) | C32 | N2 | C30 | C18 | -167.8(5) | |
| Fe2 | C17 | C21 | C20 | -60.2(4) | C25 | C26 | C22 | Fe2 | 59.6(4) | |
| Fe2 | C26 | C25 | C24 | 59.1(4) | C25 | C26 | C22 | C23 | 0.2(7) | |
| Fe2 | C26 | C22 | C23 | -59.4(4) | C31 | N2 | C30 | C18 | 71.5(6) | |
| Fe2 | C23 | C22 | C26 | 59.6(4) | C4 | C3 | C2 | Fe1 | 57.4(4) | |
| Fe2 | C23 | C24 | C25 | -60.1(4) | C4 | C3 | C2 | C1 | -1.1(6) | |
| Fe2 | C25 | C24 | C23 | 60.0(4) | C4 | C3 | C2 | C14 | -177.1(5) | |
| Si2 | C17 | C21 | Fe2 | -122.4(4) | C22 | C26 | C25 | Fe2 | -59.5(4) | |
| Si2 | C17 | C21 | C20 | 177.5(4) | C22 | C26 | C25 | C24 | -0.4(7) | |
| Si1 | C1 | C5 | Fe1 | -120.7(4) | C22 | C23 | C24 | Fe2 | 59.9(4) | |
| Si1 | C1 | C5 | C4 | 179.7(4) | C22 | C23 | C24 | C25 | -0.2(7) | |
| Si1 | C1 | C2 | Fe1 | 121.2(5) | C24 | C23 | C22 | Fe2 | -59.6(4) | |
| Si1 | C1 | C2 | C14 | -3.1(9) | C24 | C23 | C22 | C26 | 0.0(7) | |
| Si1 | C1 | C2 | C3 | -178.7(4) | C27 | Si2 | C17 | Fe2 | 161.4(4) | |
| N1 | C14 | C2 | Fe1 | 143.6(4) | C27 | Si2 | C17 | C18 | 65.0(6) | |
| N1 | C14 | C2 | C1 | -123.0(6) | C27 | Si2 | C17 | C21 | -111.3(5) | |
| N1 | C14 | C2 | C3 | 52.3(7) | C33 | O1 | C35 | C36 | -169.3(7) | |
| C1 | C5 | C4 | Fe1 | 59.7(4) | C28 | Si2 | C17 | Fe2 | -78.9(4) | |
| C1 | C5 | C4 | C3 | -1.4(7) | C28 | Si2 | C17 | C18 | -175.3(5) | |
| C7 | C6 | C10 | Fe1 | -60.1(4) | C28 | Si2 | C17 | C21 | 8.4(5) | |
| C7 | C6 | C10 | C9 | -0.3(7) | Li1 | N1 | C14 | C2 | -48.0(6) | |
| C7 | C8 | C9 | Fe1 | 59.3(4) | Li1 | O1 | C33 | C34 | -114.9(6) | |
| C7 | C8 | C9 | C10 | -0.3(7) | Li1 | O1 | C35 | C36 | 25.4(12) | |
| C19 | C20 | C21 | Fe2 | -60.6(4) | Li1 | C19 | C20 | Fe2 | 137.3(4) | |
| C19 | C20 | C21 | C17 | 0.1(6) | Li1 | C19 | C20 | C21 | -165.0(4) | |
| C19 | C18 | C30 | N2 | 14.6(8) | Li1 | C19 | C18 | Fe2 | -151.5(8) | |
| C19 | C18 | C17 | Fe2 | 58.4(4) | Li1 | C19 | C18 | C30 | -30.2(11) | |
| C19 | C18 | C17 | Si2 | -177.5(4) | Li1 | C19 | C18 | C17 | 151.6(7) | |
| C19 | C18 | C17 | C21 | -0.7(6) | Li1 | C3 | C2 | Fe1 | -147.4(4) | |
| C16 | N1 | C14 | C2 | -172.6(5) | Li1 | C3 | C2 | C1 | 154.1(5) | |
| C15 | N1 | C14 | C2 | 68.7(6) | Li1 | C3 | C2 | C14 | -21.9(6) | |
| C20 | C19 | C18 | Fe2 | 57.6(3) | Li1 | C3 | C4 | Fe1 | 172.0(9) | |
| C20 | C19 | C18 | C30 | 178.9(5) | Li1 | C3 | C4 | C5 | -129.0(8) | |
| C20 | C19 | C18 | C17 | 0.7(6) | C11 | Si1 | C1 | Fe1 | 170.7(4) | |
| C18 | C19 | C20 | Fe2 | -58.3(3) | C11 | Si1 | C1 | C5 | -101.7(5) | |
| C18 | C19 | C20 | C21 | -0.5(6) | C11 | Si1 | C1 | C2 | 77.2(6) | |
| C18 | C17 | C21 | Fe2 | 60.5(4) | C35 | O1 | C33 | C34 | 77.5(8) | |
| C18 | C17 | C21 | C20 | 0.3(6) | Li2 | N2 | C30 | C18 | -39.1(6) | |
| C30 | C18 | C17 | Fe2 | -119.8(5) | Li2 | C19 | C20 | Fe2 | 71.6(11) | |
| C30 | C18 | C17 | Si2 | 4.3(8) | Li2 | C19 | C20 | C21 | 129.3(11) | |
| C30 | C18 | C17 | C21 | -178.9(5) | Li2 | C19 | C18 | Fe2 | -103.2(3) | |
| C12 | Si1 | C1 | Fe1 | 51.7(4) | Li2 | C19 | C18 | C30 | 18.1(6) | |
| C12 | Si1 | C1 | C5 | 139.3(5) | Li2 | C19 | C18 | C17 | -160.1(5) | |
| C12 | Si1 | C1 | C2 | -41.8(6) | Li2 | C3 | C2 | Fe1 | -78.3(5) | |
| C17 | C18 | C30 | N2 | -167.4(5) | Li2 | C3 | C2 | C1 | -136.8(5) | |
| C6 | C7 | C8 | Fe1 | 59.6(4) | Li2 | C3 | C2 | C14 | 47.2(7) | |
| C6 | C7 | C8 | C9 | 0.1(7) | Li2 | C3 | C4 | Fe1 | 78.6(5) | |
| C6 | C10 | C9 | Fe1 | -59.4(4) | Li2 | C3 | C4 | C5 | 137.6(5) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| H7 | 1705 | 6225 | 8362 | 40 |
| H14A | 3150(60) | 3570(60) | 7660(30) | 30 |
| H14B | 2600(60) | 2440(50) | 8160(30) | 30 |
| H16A | 3545 | 2726 | 6787 | 55 |
| H16B | 2873 | 1458 | 7133 | 55 |
| H16C | 4500 | 1094 | 6693 | 55 |
| H15A | 3967 | -110 | 7935 | 51 |
| H15B | 5329 | 100 | 8207 | 51 |
| H15C | 5661 | -484 | 7548 | 51 |
| H20 | 5711 | 3296 | 6111 | 33 |
| H30A | 7050(60) | 7320(60) | 6950(30) | 37 |
| H30B | 8800(60) | 6310(60) | 6630(30) | 37 |
| H12A | 376 | 2791 | 8853 | 59 |
| H12B | 256 | 4093 | 9215 | 59 |
| H12C | -532 | 2892 | 9546 | 59 |
| H6 | 1324 | 5618 | 9524 | 41 |
| H21 | 6277 | 5046 | 5183 | 31 |
| H13A | 2120 | 3258 | 10413 | 74 |
| H13B | 2904 | 1577 | 10589 | 74 |
| H13C | 1078 | 2217 | 10647 | 74 |
| H8 | 4254 | 6773 | 8037 | 45 |
| H26 | 2874 | 7228 | 5445 | 45 |
| H23 | 3852 | 8238 | 6995 | 48 |
| H5 | 5156 | 2429 | 9828 | 32 |
| H29A | 7077 | 9105 | 6007 | 78 |
| H29B | 5894 | 9637 | 5520 | 78 |
| H29C | 7555 | 9852 | 5330 | 78 |
| H32A | 7307 | 7146 | 7928 | 64 |
| H32B | 9117 | 6599 | 7701 | 64 |
| H32C | 8347 | 5722 | 8277 | 64 |
| H10 | 3595 | 5788 | 9924 | 45 |
| H25 | 2275 | 5488 | 6342 | 46 |
| H31A | 10248 | 4465 | 7279 | 57 |
| H31B | 9259 | 3664 | 7050 | 57 |
| H31C | 9350 | 3529 | 7773 | 57 |
| H4 | 7112 | 3073 | 8981 | 38 |
| H22 | 3844 | 8944 | 5857 | 51 |
| H24 | 2882 | 6062 | 7318 | 41 |
| H27A | 10367 | 6064 | 4975 | 77 |
| H27B | 10195 | 6747 | 5599 | 77 |
| H27C | 10225 | 7723 | 4943 | 77 |
| H33A | 8899 | -1097 | 7994 | 57 |
| H33B | 7882 | 314 | 8310 | 57 |
| H9 | 5402 | 6479 | 9015 | 46 |
| H34A | 9990 | 1053 | 8249 | 116 |
| H34B | 11037 | -187 | 7835 | 116 |
| H34C | 10422 | -588 | 8549 | 116 |
| H28A | 6094 | 7657 | 4550 | 74 |
| H28B | 7771 | 6654 | 4308 | 74 |
| H28C | 7417 | 8359 | 4231 | 74 |
| H36A | 9813 | 1502 | 6309 | 111 |
| H36B | 8308 | 1122 | 6260 | 111 |
| H36C | 9966 | 101 | 6008 | 111 |
| H11A | 3283 | -554 | 9728 | 89 |
| H11B | 2492 | -116 | 9116 | 89 |
| H11C | 1463 | -164 | 9785 | 89 |
| H35A | 9155 | -962 | 6914 | 114 |
| H35B | 10512 | -403 | 7004 | 114 |
Experimental
Single crystals of C36H58Fe2Li2N2OSi2 [3207_twin1_hklf4] were []. A suitable crystal was selected and [] on a Xcalibur, Sapphire3 diffractometer. The crystal was kept at 173.15 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 [3207_twin1_hklf4]
Crystal Data for C36H58Fe2Li2N2OSi2 (M =716.60 g/mol): triclinic, space group P-1 (no. 2), a = 9.3542(8) Å, b = 9.9397(8) Å, c = 22.1527(17) Å, α = 79.942(7)°, β = 78.411(7)°, γ = 70.771(7)°, V = 1892.0(3) Å3, Z = 2, T = 173.15 K, μ(MoKα) = 0.859 mm-1, Dcalc = 1.258 g/cm3, 8461 reflections measured (4.37° ≤ 2Θ ≤ 51.998°), 8461 unique (Rint = 0.1294, Rsigma = 0.1020) which were used in all calculations. The final R1 was 0.0506 (I > 2σ(I)) and wR2 was 0.1391 (all data).
Refinement model description
Number of restraints - 6, number of constraints - unknown.
Details:
1. Twinned data refinement
Scales: 0.6675(10) 0.3325(10)
2. 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
3. Uiso/Uaniso restraints and constraints
Uanis(C5) ≈ Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
C33(H33A,H33B), C35(H35A,H35B)
4.b Aromatic/amide H refined with riding coordinates:
C7(H7), C20(H20), C6(H6), C21(H21), C8(H8), C26(H26), C23(H23), C5(H5),
C10(H10), C25(H25), C4(H4), C22(H22), C24(H24), C9(H9)
4.c Idealised Me refined as rotating group:
C16(H16A,H16B,H16C), C15(H15A,H15B,H15C), C12(H12A,H12B,H12C), C13(H13A,H13B,
H13C), C29(H29A,H29B,H29C), C32(H32A,H32B,H32C), C31(H31A,H31B,H31C), C27(H27A,
H27B,H27C), C34(H34A,H34B,H34C), C28(H28A,H28B,H28C), C36(H36A,H36B,H36C),
C11(H11A,H11B,H11C)
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.