| Identification code | 3214 |
| Empirical formula | C28H39Fe2NO2Si2 |
| Formula weight | 589.48 |
| Temperature/K | 173.15 |
| Crystal system | triclinic |
| Space group | P-1 |
| a/Å | 6.5034(3) |
| b/Å | 14.1336(6) |
| c/Å | 15.1720(7) |
| α/° | 91.897(4) |
| β/° | 96.259(4) |
| γ/° | 93.728(4) |
| Volume/Å3 | 1382.17(11) |
| Z | 2 |
| ρcalcg/cm3 | 1.416 |
| μ/mm‑1 | 1.162 |
| F(000) | 620.0 |
| Crystal size/mm3 | 0.096 × 0.072 × 0.043 |
| Radiation | MoKα (λ = 0.71073) |
| 2Θ range for data collection/° | 5.406 to 51.996 |
| Index ranges | -8 ≤ h ≤ 8, -17 ≤ k ≤ 17, -18 ≤ l ≤ 18 |
| Reflections collected | 18465 |
| Independent reflections | 5406 [Rint = 0.0357, Rsigma = 0.0370] |
| Data/restraints/parameters | 5406/0/323 |
| Goodness-of-fit on F2 | 1.026 |
| Final R indexes [I>=2σ (I)] | R1 = 0.0343, wR2 = 0.0798 |
| Final R indexes [all data] | R1 = 0.0459, wR2 = 0.0857 |
| Largest diff. peak/hole / e Å-3 | 0.74/-0.48 |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| Fe1 | 2265.4(5) | 1430.8(2) | 7114.0(2) | 20.78(10) |
| Fe2 | 2940.0(7) | 2057.4(3) | 11064.1(2) | 42.24(13) |
| Si1 | 2037.7(9) | 2969.6(5) | 8934.0(4) | 21.32(15) |
| Si2 | 2976.9(10) | 2446.3(5) | 5068.9(4) | 23.81(15) |
| O1 | 3207(2) | 3957.2(11) | 9365.7(10) | 25.3(4) |
| O2 | -476(2) | 3016.4(13) | 8842.8(11) | 33.6(4) |
| N1 | 157(3) | 4325.6(15) | 7019.7(13) | 30.2(5) |
| C1 | 2894(3) | 2694.3(16) | 7835.9(14) | 20.0(5) |
| C2 | 1957(3) | 2844.3(15) | 6950.5(14) | 18.5(4) |
| C3 | 3221(3) | 2485.1(16) | 6310.2(14) | 20.7(5) |
| C4 | 4943(3) | 2108.2(18) | 6816.7(15) | 25.7(5) |
| C5 | 4743(3) | 2232.9(17) | 7733.1(15) | 24.9(5) |
| C6 | -285(4) | 721.3(18) | 7515.8(19) | 37.9(6) |
| C7 | -331(4) | 617.7(19) | 6588.5(19) | 39.3(7) |
| C8 | 1455(5) | 179.5(18) | 6400.7(17) | 41.2(7) |
| C9 | 2623(5) | 4.6(19) | 7209.7(19) | 41.4(7) |
| C10 | 1532(5) | 343.2(18) | 7899.3(17) | 38.9(7) |
| C11 | 4389(5) | 3525(2) | 4695.2(17) | 40.1(7) |
| C12 | 242(4) | 2369(2) | 4542.4(17) | 47.1(8) |
| C13 | 4274(4) | 1383.3(19) | 4694.3(16) | 34.5(6) |
| C14 | -44(4) | 3316.2(17) | 6761.5(15) | 24.3(5) |
| C15 | 1567(5) | 4854(2) | 6509.0(19) | 45.9(7) |
| C16 | -1880(5) | 4699(2) | 6908(2) | 54.4(9) |
| C17 | 3532(4) | 4796.6(18) | 8895.5(16) | 31.8(6) |
| C18 | -1480(5) | 3742(3) | 9236(3) | 64.7(11) |
| C19 | 2771(4) | 2039.2(18) | 9706.9(15) | 31.1(6) |
| C20 | 1406(6) | 1316(2) | 10001.9(17) | 51.7(9) |
| C21 | 2595(9) | 712(2) | 10547(2) | 77.6(14) |
| C22 | 4664(8) | 1040(3) | 10598(2) | 74.6(14) |
| C23 | 4813(5) | 1862(2) | 10090.3(17) | 47.6(8) |
| C24 | 2214(6) | 3350(2) | 11504.7(18) | 48.5(8) |
| C25 | 782(6) | 2633(3) | 11748(2) | 63(1) |
| C26 | 1927(7) | 1997(2) | 12277.2(19) | 70.3(12) |
| C27 | 4021(7) | 2328(2) | 12365.8(19) | 63.7(11) |
| C28 | 4186(6) | 3159(2) | 11895.3(18) | 49.6(8) |
| Atom | U11 | U22 | U33 | U23 | U13 | U12 |
|---|---|---|---|---|---|---|
| Fe1 | 26.49(19) | 19.70(18) | 16.71(16) | -0.82(12) | 2.91(13) | 5.70(13) |
| Fe2 | 87.2(4) | 24.7(2) | 16.55(19) | -1.58(15) | 14.13(19) | 3.7(2) |
| Si1 | 22.1(3) | 24.8(4) | 16.9(3) | -4.3(2) | 3.6(2) | 0.9(3) |
| Si2 | 26.6(4) | 29.9(4) | 15.3(3) | -0.9(3) | 3.5(2) | 3.8(3) |
| O1 | 28.6(9) | 27.0(9) | 19.2(8) | -3.9(7) | 1.8(7) | -1.9(7) |
| O2 | 22.3(9) | 44.2(11) | 33.9(10) | -12.2(8) | 6.0(7) | 0.6(8) |
| N1 | 39.5(12) | 26.2(12) | 24.6(10) | -5.7(8) | -2.6(9) | 13.8(9) |
| C1 | 20.9(12) | 20.4(12) | 18.1(11) | -3.2(9) | 2.3(9) | -0.6(9) |
| C2 | 20.3(11) | 15.7(11) | 19.0(11) | -1.8(8) | 2.5(8) | -1.5(9) |
| C3 | 20.7(12) | 22.8(12) | 18.9(11) | 0.0(9) | 4.6(9) | -0.7(9) |
| C4 | 19.4(12) | 37.0(15) | 21.5(12) | -2.4(10) | 4.7(9) | 5.1(10) |
| C5 | 21.3(12) | 33.8(14) | 19.1(11) | -2.4(10) | -1.5(9) | 4.7(10) |
| C6 | 45.1(17) | 20.8(14) | 50.6(17) | 3.4(12) | 20.7(13) | -2.0(12) |
| C7 | 42.6(17) | 25.9(14) | 45.8(16) | 2.2(12) | -5.3(13) | -7.5(12) |
| C8 | 72(2) | 22.6(14) | 28.9(14) | -8.2(11) | 13.8(13) | -6.0(13) |
| C9 | 56.3(19) | 22.4(14) | 48.6(17) | 3.5(12) | 11.2(14) | 16.3(13) |
| C10 | 70(2) | 22.0(14) | 25.5(13) | 3.5(10) | 7.3(13) | 3.9(13) |
| C11 | 58.8(19) | 37.4(16) | 26.5(14) | 5.7(12) | 14.4(13) | 2.4(14) |
| C12 | 36.3(16) | 82(2) | 21.6(13) | -11.9(14) | -2.8(11) | 7.7(15) |
| C13 | 47.7(16) | 34.8(15) | 22.7(12) | -2.0(11) | 10.4(11) | 6.6(12) |
| C14 | 25.7(12) | 27.5(13) | 19.1(11) | -4.9(9) | -0.3(9) | 5.6(10) |
| C15 | 68(2) | 25.8(15) | 43.6(17) | 4.3(12) | 4.1(15) | 4.6(14) |
| C16 | 63(2) | 50(2) | 49.5(18) | -18.7(15) | -9.1(15) | 35.3(17) |
| C17 | 38.9(15) | 28.7(14) | 26.6(13) | -2.4(10) | 3.0(11) | -5.1(11) |
| C18 | 29.9(16) | 78(3) | 86(3) | -41(2) | 14.9(16) | 8.1(16) |
| C19 | 49.8(16) | 28.1(14) | 16.6(11) | -3.4(10) | 8.7(11) | 5.0(12) |
| C20 | 97(3) | 34.2(17) | 23.6(14) | -9.5(12) | 20.9(15) | -15.6(16) |
| C21 | 185(5) | 26.2(18) | 24.3(16) | -4.0(13) | 26(2) | 4(2) |
| C22 | 150(4) | 54(2) | 25.2(16) | 3.6(15) | 5(2) | 59(3) |
| C23 | 73(2) | 51.7(19) | 22.0(13) | 0.3(12) | 6.9(13) | 31.7(17) |
| C24 | 86(2) | 32.0(16) | 30.2(15) | -9.0(12) | 18.2(15) | 7.6(16) |
| C25 | 82(3) | 68(3) | 40.7(18) | -23.3(17) | 29.7(17) | -5(2) |
| C26 | 146(4) | 43(2) | 23.2(15) | -8.9(14) | 36(2) | -20(2) |
| C27 | 134(4) | 33.0(18) | 22.4(15) | -3.4(12) | 5.1(18) | 4(2) |
| C28 | 90(3) | 30.8(16) | 26.7(14) | -5.4(12) | 6.0(15) | -0.1(16) |
| Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
|---|---|---|---|---|---|---|
| Fe1 | C1 | 2.058(2) | Si2 | C13 | 1.872(3) | |
| Fe1 | C2 | 2.041(2) | O1 | C17 | 1.420(3) | |
| Fe1 | C3 | 2.064(2) | O2 | C18 | 1.402(3) | |
| Fe1 | C4 | 2.033(2) | N1 | C14 | 1.461(3) | |
| Fe1 | C5 | 2.031(2) | N1 | C15 | 1.450(4) | |
| Fe1 | C6 | 2.043(3) | N1 | C16 | 1.453(3) | |
| Fe1 | C7 | 2.050(3) | C1 | C2 | 1.441(3) | |
| Fe1 | C8 | 2.050(3) | C1 | C5 | 1.426(3) | |
| Fe1 | C9 | 2.052(3) | C2 | C3 | 1.440(3) | |
| Fe1 | C10 | 2.040(3) | C2 | C14 | 1.505(3) | |
| Fe2 | C19 | 2.049(2) | C3 | C4 | 1.430(3) | |
| Fe2 | C20 | 2.023(3) | C4 | C5 | 1.417(3) | |
| Fe2 | C21 | 2.023(3) | C6 | C7 | 1.407(4) | |
| Fe2 | C22 | 2.034(3) | C6 | C10 | 1.404(4) | |
| Fe2 | C23 | 2.037(3) | C7 | C8 | 1.403(4) | |
| Fe2 | C24 | 2.026(3) | C8 | C9 | 1.409(4) | |
| Fe2 | C25 | 2.030(3) | C9 | C10 | 1.414(4) | |
| Fe2 | C26 | 2.024(3) | C19 | C20 | 1.426(4) | |
| Fe2 | C27 | 2.038(3) | C19 | C23 | 1.431(4) | |
| Fe2 | C28 | 2.039(3) | C20 | C21 | 1.415(5) | |
| Si1 | O1 | 1.6274(17) | C21 | C22 | 1.388(6) | |
| Si1 | O2 | 1.6316(17) | C22 | C23 | 1.420(5) | |
| Si1 | C1 | 1.851(2) | C24 | C25 | 1.416(5) | |
| Si1 | C19 | 1.842(3) | C24 | C28 | 1.399(5) | |
| Si2 | C3 | 1.871(2) | C25 | C26 | 1.419(5) | |
| Si2 | C11 | 1.865(3) | C26 | C27 | 1.402(6) | |
| Si2 | C12 | 1.863(3) | C27 | C28 | 1.399(4) |
| Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|
| C1 | Fe1 | C3 | 69.81(9) | O1 | Si1 | O2 | 111.26(9) | |
| C2 | Fe1 | C1 | 41.17(8) | O1 | Si1 | C1 | 110.58(9) | |
| C2 | Fe1 | C3 | 41.06(9) | O1 | Si1 | C19 | 106.27(10) | |
| C2 | Fe1 | C6 | 114.06(10) | O2 | Si1 | C1 | 110.07(9) | |
| C2 | Fe1 | C7 | 112.11(10) | O2 | Si1 | C19 | 108.69(11) | |
| C2 | Fe1 | C8 | 137.67(10) | C19 | Si1 | C1 | 109.88(11) | |
| C2 | Fe1 | C9 | 176.87(10) | C3 | Si2 | C13 | 107.86(11) | |
| C4 | Fe1 | C1 | 68.93(9) | C11 | Si2 | C3 | 108.89(11) | |
| C4 | Fe1 | C2 | 68.27(9) | C11 | Si2 | C13 | 107.98(13) | |
| C4 | Fe1 | C3 | 40.84(9) | C12 | Si2 | C3 | 113.65(11) | |
| C4 | Fe1 | C6 | 174.96(10) | C12 | Si2 | C11 | 109.44(14) | |
| C4 | Fe1 | C7 | 143.93(11) | C12 | Si2 | C13 | 108.86(14) | |
| C4 | Fe1 | C8 | 114.10(11) | C17 | O1 | Si1 | 124.91(14) | |
| C4 | Fe1 | C9 | 110.00(11) | C18 | O2 | Si1 | 123.56(18) | |
| C4 | Fe1 | C10 | 135.27(11) | C15 | N1 | C14 | 111.9(2) | |
| C5 | Fe1 | C1 | 40.81(9) | C15 | N1 | C16 | 110.4(2) | |
| C5 | Fe1 | C2 | 68.41(9) | C16 | N1 | C14 | 109.0(2) | |
| C5 | Fe1 | C3 | 69.12(9) | Si1 | C1 | Fe1 | 125.77(12) | |
| C5 | Fe1 | C4 | 40.79(9) | C2 | C1 | Fe1 | 68.81(12) | |
| C5 | Fe1 | C6 | 135.09(10) | C2 | C1 | Si1 | 131.25(17) | |
| C5 | Fe1 | C7 | 175.27(11) | C5 | C1 | Fe1 | 68.61(13) | |
| C5 | Fe1 | C8 | 142.56(11) | C5 | C1 | Si1 | 122.75(16) | |
| C5 | Fe1 | C9 | 112.15(11) | C5 | C1 | C2 | 105.99(19) | |
| C5 | Fe1 | C10 | 109.07(11) | C1 | C2 | Fe1 | 70.02(12) | |
| C6 | Fe1 | C1 | 109.61(10) | C1 | C2 | C14 | 123.14(19) | |
| C6 | Fe1 | C3 | 143.76(10) | C3 | C2 | Fe1 | 70.31(13) | |
| C6 | Fe1 | C7 | 40.21(11) | C3 | C2 | C1 | 109.86(19) | |
| C6 | Fe1 | C8 | 67.51(12) | C3 | C2 | C14 | 127.00(19) | |
| C6 | Fe1 | C9 | 67.88(12) | C14 | C2 | Fe1 | 126.45(16) | |
| C7 | Fe1 | C1 | 136.58(11) | Si2 | C3 | Fe1 | 127.13(12) | |
| C7 | Fe1 | C3 | 114.55(10) | C2 | C3 | Fe1 | 68.63(12) | |
| C7 | Fe1 | C8 | 40.01(12) | C2 | C3 | Si2 | 133.15(17) | |
| C7 | Fe1 | C9 | 67.60(12) | C4 | C3 | Fe1 | 68.44(13) | |
| C8 | Fe1 | C1 | 176.58(11) | C4 | C3 | Si2 | 121.21(17) | |
| C8 | Fe1 | C3 | 111.27(10) | C4 | C3 | C2 | 105.64(18) | |
| C8 | Fe1 | C9 | 40.18(11) | C3 | C4 | Fe1 | 70.73(13) | |
| C9 | Fe1 | C1 | 141.16(10) | C5 | C4 | Fe1 | 69.53(13) | |
| C9 | Fe1 | C3 | 135.95(10) | C5 | C4 | C3 | 109.4(2) | |
| C10 | Fe1 | C1 | 111.67(10) | C1 | C5 | Fe1 | 70.58(13) | |
| C10 | Fe1 | C2 | 142.60(10) | C4 | C5 | Fe1 | 69.68(13) | |
| C10 | Fe1 | C3 | 175.57(11) | C4 | C5 | C1 | 109.09(19) | |
| C10 | Fe1 | C6 | 40.25(11) | C7 | C6 | Fe1 | 70.17(15) | |
| C10 | Fe1 | C7 | 67.49(11) | C10 | C6 | Fe1 | 69.76(16) | |
| C10 | Fe1 | C8 | 67.51(11) | C10 | C6 | C7 | 107.8(2) | |
| C10 | Fe1 | C9 | 40.44(11) | C6 | C7 | Fe1 | 69.62(15) | |
| C20 | Fe2 | C19 | 40.99(11) | C8 | C7 | Fe1 | 70.03(16) | |
| C20 | Fe2 | C22 | 68.19(16) | C8 | C7 | C6 | 108.1(2) | |
| C20 | Fe2 | C23 | 68.55(13) | C7 | C8 | Fe1 | 69.96(15) | |
| C20 | Fe2 | C24 | 124.54(14) | C7 | C8 | C9 | 108.5(2) | |
| C20 | Fe2 | C25 | 107.32(15) | C9 | C8 | Fe1 | 69.98(15) | |
| C20 | Fe2 | C26 | 121.29(15) | C8 | C9 | Fe1 | 69.84(15) | |
| C20 | Fe2 | C27 | 156.65(13) | C8 | C9 | C10 | 107.2(3) | |
| C20 | Fe2 | C28 | 161.49(13) | C10 | C9 | Fe1 | 69.30(15) | |
| C21 | Fe2 | C19 | 68.99(11) | C6 | C10 | Fe1 | 69.99(15) | |
| C21 | Fe2 | C20 | 40.95(15) | C6 | C10 | C9 | 108.4(2) | |
| C21 | Fe2 | C22 | 40.00(17) | C9 | C10 | Fe1 | 70.26(15) | |
| C21 | Fe2 | C23 | 68.27(16) | N1 | C14 | C2 | 112.69(19) | |
| C21 | Fe2 | C24 | 160.31(19) | Si1 | C19 | Fe2 | 129.66(13) | |
| C21 | Fe2 | C25 | 122.70(19) | C20 | C19 | Fe2 | 68.52(14) | |
| C21 | Fe2 | C26 | 105.82(14) | C20 | C19 | Si1 | 126.2(2) | |
| C21 | Fe2 | C27 | 120.64(14) | C20 | C19 | C23 | 106.3(3) | |
| C21 | Fe2 | C28 | 156.84(17) | C23 | C19 | Fe2 | 69.06(14) | |
| C22 | Fe2 | C19 | 68.85(11) | C23 | C19 | Si1 | 127.4(2) | |
| C22 | Fe2 | C23 | 40.81(14) | C19 | C20 | Fe2 | 70.49(16) | |
| C22 | Fe2 | C27 | 106.87(15) | C21 | C20 | Fe2 | 69.51(19) | |
| C22 | Fe2 | C28 | 122.93(18) | C21 | C20 | C19 | 108.5(3) | |
| C23 | Fe2 | C19 | 41.00(11) | C20 | C21 | Fe2 | 69.54(18) | |
| C23 | Fe2 | C27 | 123.58(16) | C22 | C21 | Fe2 | 70.4(2) | |
| C23 | Fe2 | C28 | 109.17(14) | C22 | C21 | C20 | 108.5(3) | |
| C24 | Fe2 | C19 | 108.71(11) | C21 | C22 | Fe2 | 69.6(2) | |
| C24 | Fe2 | C22 | 159.00(19) | C21 | C22 | C23 | 108.5(3) | |
| C24 | Fe2 | C23 | 123.67(13) | C23 | C22 | Fe2 | 69.72(18) | |
| C24 | Fe2 | C25 | 40.88(13) | C19 | C23 | Fe2 | 69.95(16) | |
| C24 | Fe2 | C27 | 68.14(13) | C22 | C23 | Fe2 | 69.5(2) | |
| C24 | Fe2 | C28 | 40.27(13) | C22 | C23 | C19 | 108.1(3) | |
| C25 | Fe2 | C19 | 122.68(13) | C25 | C24 | Fe2 | 69.70(18) | |
| C25 | Fe2 | C22 | 158.22(18) | C28 | C24 | Fe2 | 70.34(17) | |
| C25 | Fe2 | C23 | 159.41(14) | C28 | C24 | C25 | 107.7(3) | |
| C25 | Fe2 | C27 | 68.33(16) | C24 | C25 | Fe2 | 69.43(18) | |
| C25 | Fe2 | C28 | 67.97(15) | C24 | C25 | C26 | 107.3(3) | |
| C26 | Fe2 | C19 | 158.06(16) | C26 | C25 | Fe2 | 69.3(2) | |
| C26 | Fe2 | C22 | 121.67(15) | C25 | C26 | Fe2 | 69.73(17) | |
| C26 | Fe2 | C23 | 158.67(16) | C27 | C26 | Fe2 | 70.36(18) | |
| C26 | Fe2 | C24 | 68.62(13) | C27 | C26 | C25 | 108.2(3) | |
| C26 | Fe2 | C25 | 40.97(15) | C26 | C27 | Fe2 | 69.27(18) | |
| C26 | Fe2 | C27 | 40.37(15) | C28 | C27 | Fe2 | 69.95(17) | |
| C26 | Fe2 | C28 | 67.74(14) | C28 | C27 | C26 | 107.9(3) | |
| C27 | Fe2 | C19 | 160.65(15) | C24 | C28 | Fe2 | 69.39(17) | |
| C27 | Fe2 | C28 | 40.14(12) | C27 | C28 | Fe2 | 69.91(18) | |
| C28 | Fe2 | C19 | 125.22(11) | C27 | C28 | C24 | 108.9(3) |
| A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|---|---|
| Fe1 | C1 | C2 | C3 | -59.17(15) | C2 | C1 | C5 | C4 | 0.3(3) | |
| Fe1 | C1 | C2 | C14 | 121.2(2) | C2 | C3 | C4 | Fe1 | 58.83(15) | |
| Fe1 | C1 | C5 | C4 | 59.23(17) | C2 | C3 | C4 | C5 | -0.1(3) | |
| Fe1 | C2 | C3 | Si2 | 121.4(2) | C3 | C2 | C14 | N1 | -110.8(2) | |
| Fe1 | C2 | C3 | C4 | -58.71(16) | C3 | C4 | C5 | Fe1 | 59.65(17) | |
| Fe1 | C2 | C14 | N1 | 157.39(16) | C3 | C4 | C5 | C1 | -0.1(3) | |
| Fe1 | C3 | C4 | C5 | -58.93(17) | C5 | C1 | C2 | Fe1 | 58.81(16) | |
| Fe1 | C4 | C5 | C1 | -59.78(17) | C5 | C1 | C2 | C3 | -0.4(3) | |
| Fe1 | C6 | C7 | C8 | 59.68(19) | C5 | C1 | C2 | C14 | 180.0(2) | |
| Fe1 | C6 | C10 | C9 | -60.00(19) | C6 | C7 | C8 | Fe1 | -59.43(18) | |
| Fe1 | C7 | C8 | C9 | 59.60(19) | C6 | C7 | C8 | C9 | 0.2(3) | |
| Fe1 | C8 | C9 | C10 | 59.49(19) | C7 | C6 | C10 | Fe1 | 60.11(18) | |
| Fe1 | C9 | C10 | C6 | 59.83(19) | C7 | C6 | C10 | C9 | 0.1(3) | |
| Fe2 | C19 | C20 | C21 | -59.3(2) | C7 | C8 | C9 | Fe1 | -59.59(19) | |
| Fe2 | C19 | C23 | C22 | 59.2(2) | C7 | C8 | C9 | C10 | -0.1(3) | |
| Fe2 | C20 | C21 | C22 | -59.9(2) | C8 | C9 | C10 | Fe1 | -59.84(19) | |
| Fe2 | C21 | C22 | C23 | -59.0(2) | C8 | C9 | C10 | C6 | 0.0(3) | |
| Fe2 | C22 | C23 | C19 | -59.47(19) | C10 | C6 | C7 | Fe1 | -59.85(18) | |
| Fe2 | C24 | C25 | C26 | 59.2(2) | C10 | C6 | C7 | C8 | -0.2(3) | |
| Fe2 | C24 | C28 | C27 | -58.9(2) | C11 | Si2 | C3 | Fe1 | -172.95(15) | |
| Fe2 | C25 | C26 | C27 | 60.1(2) | C11 | Si2 | C3 | C2 | 92.3(2) | |
| Fe2 | C26 | C27 | C28 | 59.5(2) | C11 | Si2 | C3 | C4 | -87.6(2) | |
| Fe2 | C27 | C28 | C24 | 58.6(2) | C12 | Si2 | C3 | Fe1 | 64.78(19) | |
| Si1 | C1 | C2 | Fe1 | -119.6(2) | C12 | Si2 | C3 | C2 | -30.0(3) | |
| Si1 | C1 | C2 | C3 | -178.76(17) | C12 | Si2 | C3 | C4 | 150.2(2) | |
| Si1 | C1 | C2 | C14 | 1.6(3) | C13 | Si2 | C3 | Fe1 | -56.01(17) | |
| Si1 | C1 | C5 | Fe1 | 119.64(17) | C13 | Si2 | C3 | C2 | -150.8(2) | |
| Si1 | C1 | C5 | C4 | 178.87(17) | C13 | Si2 | C3 | C4 | 29.4(2) | |
| Si1 | C19 | C20 | Fe2 | -124.2(2) | C14 | C2 | C3 | Fe1 | -121.4(2) | |
| Si1 | C19 | C20 | C21 | 176.5(2) | C14 | C2 | C3 | Si2 | 0.1(4) | |
| Si1 | C19 | C23 | Fe2 | 124.6(2) | C14 | C2 | C3 | C4 | 179.9(2) | |
| Si1 | C19 | C23 | C22 | -176.2(2) | C15 | N1 | C14 | C2 | 64.0(3) | |
| Si2 | C3 | C4 | Fe1 | -121.29(16) | C16 | N1 | C14 | C2 | -173.7(2) | |
| Si2 | C3 | C4 | C5 | 179.78(17) | C19 | Si1 | O1 | C17 | 162.29(19) | |
| O1 | Si1 | O2 | C18 | -11.0(3) | C19 | Si1 | O2 | C18 | 105.7(3) | |
| O1 | Si1 | C1 | Fe1 | 169.17(12) | C19 | Si1 | C1 | Fe1 | 52.17(17) | |
| O1 | Si1 | C1 | C2 | -98.6(2) | C19 | Si1 | C1 | C2 | 144.4(2) | |
| O1 | Si1 | C1 | C5 | 83.2(2) | C19 | Si1 | C1 | C5 | -33.8(2) | |
| O1 | Si1 | C19 | Fe2 | 43.8(2) | C19 | C20 | C21 | Fe2 | 59.9(2) | |
| O1 | Si1 | C19 | C20 | 134.8(2) | C19 | C20 | C21 | C22 | 0.0(3) | |
| O1 | Si1 | C19 | C23 | -49.0(2) | C20 | C19 | C23 | Fe2 | -58.62(17) | |
| O2 | Si1 | O1 | C17 | -79.6(2) | C20 | C19 | C23 | C22 | 0.6(3) | |
| O2 | Si1 | C1 | Fe1 | -67.49(16) | C20 | C21 | C22 | Fe2 | 59.3(2) | |
| O2 | Si1 | C1 | C2 | 24.8(2) | C20 | C21 | C22 | C23 | 0.3(4) | |
| O2 | Si1 | C1 | C5 | -153.42(19) | C21 | C22 | C23 | Fe2 | 58.9(2) | |
| O2 | Si1 | C19 | Fe2 | -76.05(19) | C21 | C22 | C23 | C19 | -0.6(3) | |
| O2 | Si1 | C19 | C20 | 14.9(2) | C23 | C19 | C20 | Fe2 | 58.96(18) | |
| O2 | Si1 | C19 | C23 | -168.9(2) | C23 | C19 | C20 | C21 | -0.4(3) | |
| C1 | Si1 | O1 | C17 | 43.1(2) | C24 | C25 | C26 | Fe2 | -59.3(2) | |
| C1 | Si1 | O2 | C18 | -133.9(3) | C24 | C25 | C26 | C27 | 0.8(3) | |
| C1 | Si1 | C19 | Fe2 | 163.45(16) | C25 | C24 | C28 | Fe2 | 59.9(2) | |
| C1 | Si1 | C19 | C20 | -105.5(2) | C25 | C24 | C28 | C27 | 1.0(3) | |
| C1 | Si1 | C19 | C23 | 70.6(2) | C25 | C26 | C27 | Fe2 | -59.7(2) | |
| C1 | C2 | C3 | Fe1 | 58.99(15) | C25 | C26 | C27 | C28 | -0.2(3) | |
| C1 | C2 | C3 | Si2 | -179.58(18) | C26 | C27 | C28 | Fe2 | -59.1(2) | |
| C1 | C2 | C3 | C4 | 0.3(3) | C26 | C27 | C28 | C24 | -0.5(3) | |
| C1 | C2 | C14 | N1 | 68.8(3) | C28 | C24 | C25 | Fe2 | -60.3(2) | |
| C2 | C1 | C5 | Fe1 | -58.93(15) | C28 | C24 | C25 | C26 | -1.1(3) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| H4 | 6048 | 1819 | 6576 | 31 |
| H5 | 5691 | 2040 | 8204 | 30 |
| H6 | -1301 | 998 | 7827 | 45 |
| H7 | -1388 | 811 | 6163 | 47 |
| H8 | 1816 | 27 | 5825 | 49 |
| H9 | 3904 | -286 | 7279 | 50 |
| H10 | 1956 | 319 | 8517 | 47 |
| H11A | 3759 | 4093 | 4898 | 60 |
| H11B | 4304 | 3502 | 4046 | 60 |
| H11C | 5847 | 3547 | 4946 | 60 |
| H12A | -559 | 1866 | 4812 | 71 |
| H12B | 211 | 2222 | 3905 | 71 |
| H12C | -364 | 2976 | 4633 | 71 |
| H13A | 5756 | 1456 | 4908 | 52 |
| H13B | 4098 | 1326 | 4045 | 52 |
| H13C | 3649 | 812 | 4935 | 52 |
| H14A | -519 | 3240 | 6119 | 29 |
| H14B | -1114 | 2995 | 7086 | 29 |
| H15A | 1011 | 4816 | 5881 | 69 |
| H15B | 2923 | 4583 | 6578 | 69 |
| H15C | 1722 | 5519 | 6723 | 69 |
| H16A | -1764 | 5371 | 7100 | 82 |
| H16B | -2806 | 4345 | 7267 | 82 |
| H16C | -2445 | 4632 | 6282 | 82 |
| H17A | 4285 | 4655 | 8387 | 48 |
| H17B | 4345 | 5279 | 9290 | 48 |
| H17C | 2190 | 5034 | 8685 | 48 |
| H18A | -1035 | 4353 | 9007 | 97 |
| H18B | -1123 | 3756 | 9881 | 97 |
| H18C | -2984 | 3625 | 9095 | 97 |
| H20 | -56 | 1250 | 9857 | 62 |
| H21 | 2066 | 172 | 10829 | 93 |
| H22 | 5791 | 762 | 10920 | 89 |
| H23 | 6052 | 2231 | 10017 | 57 |
| H24 | 1893 | 3867 | 11141 | 58 |
| H25 | -676 | 2587 | 11587 | 76 |
| H26 | 1371 | 1443 | 12528 | 84 |
| H27 | 5132 | 2039 | 12688 | 76 |
| H28 | 5434 | 3534 | 11849 | 60 |
Experimental
Single crystals of C28H39Fe2NO2Si2 [3214] 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 [3214]
Crystal Data for C28H39Fe2NO2Si2 (M =589.48 g/mol): triclinic, space group P-1 (no. 2), a = 6.5034(3) Å, b = 14.1336(6) Å, c = 15.1720(7) Å, α = 91.897(4)°, β = 96.259(4)°, γ = 93.728(4)°, V = 1382.17(11) Å3, Z = 2, T = 173.15 K, μ(MoKα) = 1.162 mm-1, Dcalc = 1.416 g/cm3, 18465 reflections measured (5.406° ≤ 2Θ ≤ 51.996°), 5406 unique (Rint = 0.0357, Rsigma = 0.0370) which were used in all calculations. The final R1 was 0.0343 (I > 2σ(I)) and wR2 was 0.0857 (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:
C14(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21),
C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28)
2.c Idealised Me refined as rotating group:
C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,
H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
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.