| Identification code | 3148 |
| Empirical formula | C44H60Fe2N2O3Si4 |
| Formula weight | 889.00 |
| Temperature/K | 173.15 |
| Crystal system | triclinic |
| Space group | P-1 |
| a/Å | 11.2756(3) |
| b/Å | 12.7949(4) |
| c/Å | 16.9084(4) |
| α/° | 75.308(2) |
| β/° | 87.164(2) |
| γ/° | 74.135(2) |
| Volume/Å3 | 2269.22(11) |
| Z | 2 |
| ρcalcg/cm3 | 1.301 |
| μ/mm‑1 | 0.784 |
| F(000) | 940.0 |
| Crystal size/mm3 | 0.15 × 0.05 × 0.05 |
| Radiation | MoKα (λ = 0.71073) |
| 2Θ range for data collection/° | 4.342 to 53.998 |
| Index ranges | -14 ≤ h ≤ 14, -16 ≤ k ≤ 16, -21 ≤ l ≤ 21 |
| Reflections collected | 47916 |
| Independent reflections | 9895 [Rint = 0.0301, Rsigma = 0.0224] |
| Data/restraints/parameters | 9895/0/506 |
| Goodness-of-fit on F2 | 1.016 |
| Final R indexes [I>=2σ (I)] | R1 = 0.0285, wR2 = 0.0689 |
| Final R indexes [all data] | R1 = 0.0348, wR2 = 0.0722 |
| Largest diff. peak/hole / e Å-3 | 0.39/-0.21 |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| Fe1 | 8852.4(2) | 3388.1(2) | 1193.2(2) | 21.31(6) |
| Fe2 | 7355.1(2) | -1353.3(2) | 4537.9(2) | 25.05(6) |
| Si1 | 6871.7(4) | 2123.7(3) | 2549.9(2) | 18.82(9) |
| Si2 | 8430.5(4) | -329.1(3) | 2582.7(2) | 19.60(9) |
| Si3 | 4240.5(4) | 2282.2(4) | 1932.5(3) | 24.84(10) |
| Si4 | 7646.7(5) | -927.0(4) | 1029.1(3) | 32.84(11) |
| O1 | 7920.8(9) | 929.6(8) | 2713.6(6) | 22.1(2) |
| O2 | 5537(1) | 1910.5(9) | 2467.2(7) | 25.1(2) |
| O3 | 8067.2(11) | -302.9(9) | 1660.2(6) | 27.1(2) |
| N1 | 5352.8(12) | 5285.0(11) | 2044.9(9) | 29.4(3) |
| N2 | 9796.2(16) | -3567.2(12) | 3171.2(10) | 40.5(4) |
| C1 | 7217.8(13) | 3041.0(12) | 1584.3(9) | 21.2(3) |
| C2 | 7073.4(14) | 4237.5(13) | 1352.1(10) | 24.3(3) |
| C3 | 7396.3(14) | 4534.4(14) | 517.4(10) | 30.1(4) |
| C4 | 7747.6(15) | 3555.7(15) | 221.6(10) | 31.4(4) |
| C5 | 7643.2(14) | 2638.9(14) | 873.1(9) | 26.2(3) |
| C6 | 9990.5(15) | 3402.5(14) | 2093.6(10) | 28.7(3) |
| C7 | 10154.6(15) | 4158.2(15) | 1351.4(11) | 31.7(4) |
| C8 | 10534.3(15) | 3541.4(16) | 757.9(11) | 35.0(4) |
| C9 | 10597.7(15) | 2403.5(16) | 1131.8(12) | 35.8(4) |
| C10 | 10260.6(15) | 2318.6(14) | 1958.3(11) | 30.4(4) |
| C11 | 6677.0(14) | 5032.1(13) | 1890.2(10) | 27.4(3) |
| C12 | 4632.6(17) | 5899.6(16) | 1297.3(12) | 41.2(4) |
| C13 | 5061.1(19) | 5927.5(16) | 2657.9(12) | 42.2(5) |
| C14 | 6851.6(14) | 2691.6(12) | 3465.5(9) | 22.5(3) |
| C15 | 5741.7(16) | 3113.3(14) | 3826(1) | 30.9(4) |
| C16 | 5719.0(19) | 3546.3(15) | 4505.0(11) | 39.4(4) |
| C17 | 6799(2) | 3566.4(15) | 4834.6(11) | 41.0(5) |
| C18 | 7916.7(19) | 3153.7(15) | 4489.2(11) | 38.2(4) |
| C19 | 7934.3(16) | 2715.9(14) | 3815.9(10) | 29.2(3) |
| C20 | 7675.8(14) | -1267.7(13) | 3322.0(9) | 22.9(3) |
| C21 | 8157.3(15) | -2395.9(13) | 3818.5(9) | 25.2(3) |
| C22 | 7154.7(17) | -2749.5(15) | 4247.9(10) | 33.3(4) |
| C23 | 6062.7(17) | -1864.8(16) | 4037.8(11) | 34.4(4) |
| C24 | 6373.3(15) | -955.5(14) | 3473.8(9) | 27.7(3) |
| C25 | 8694.4(17) | -1226.9(16) | 5251.4(10) | 34.5(4) |
| C26 | 7895(2) | -1783.5(18) | 5738.6(11) | 43.4(5) |
| C27 | 6689.1(19) | -1048(2) | 5621.9(11) | 47.9(5) |
| C28 | 6752.3(18) | -44.4(17) | 5065.5(12) | 42.6(5) |
| C29 | 7991.1(17) | -150.6(15) | 4833.7(10) | 33.8(4) |
| C30 | 9464.6(16) | -3098.8(13) | 3878.2(10) | 28.7(3) |
| C31 | 9069(3) | -4332(2) | 3125.6(17) | 72.3(8) |
| C32 | 11108(2) | -4115(2) | 3196.9(16) | 66.1(7) |
| C33 | 10140.1(14) | -741.7(12) | 2686.7(9) | 22.1(3) |
| C34 | 10737.6(15) | -677.3(14) | 3370.2(10) | 28.0(3) |
| C35 | 12008.6(16) | -1021.4(14) | 3460.0(11) | 32.7(4) |
| C36 | 12718.7(16) | -1426.8(14) | 2857.6(11) | 33.9(4) |
| C37 | 12160.5(17) | -1481.8(16) | 2170.1(12) | 37.8(4) |
| C38 | 10885.4(16) | -1144.9(15) | 2085.7(10) | 32.1(4) |
| C39 | 3227.5(16) | 3552.8(15) | 2191.2(13) | 40.1(4) |
| C40 | 4559.4(18) | 2582.6(18) | 822.6(11) | 40.8(4) |
| C41 | 3554.0(16) | 1085.4(14) | 2212.6(11) | 31.1(4) |
| C42 | 7554(2) | 25.1(18) | -4.7(11) | 53.3(6) |
| C43 | 6120(3) | -1168(3) | 1314.8(17) | 71.2(8) |
| C44 | 8795(2) | -2286.3(18) | 1067.1(14) | 58.6(6) |
| Atom | U11 | U22 | U33 | U23 | U13 | U12 |
|---|---|---|---|---|---|---|
| Fe1 | 16.17(11) | 22.95(11) | 23.63(11) | -4.51(8) | 1.28(8) | -4.68(8) |
| Fe2 | 25.11(12) | 28.97(13) | 18.28(11) | -4.78(9) | 2.74(9) | -4.17(9) |
| Si1 | 16.11(19) | 18.61(19) | 21.02(19) | -5.18(15) | 0.51(15) | -3.31(15) |
| Si2 | 22.2(2) | 18.63(19) | 17.05(18) | -5.24(15) | 1.12(15) | -3.38(16) |
| Si3 | 18.0(2) | 26.9(2) | 27.2(2) | -2.02(17) | -0.81(16) | -6.22(17) |
| Si4 | 46.1(3) | 33.1(3) | 22.7(2) | -12.28(19) | -0.2(2) | -11.1(2) |
| O1 | 20.8(5) | 20.0(5) | 24.5(5) | -6.8(4) | -1.5(4) | -2.6(4) |
| O2 | 19.2(5) | 27.2(6) | 27.7(5) | -2.4(4) | -0.7(4) | -8.1(4) |
| O3 | 36.2(6) | 26.8(6) | 18.3(5) | -6.1(4) | -0.8(4) | -8.2(5) |
| N1 | 21.7(7) | 25.1(7) | 35.1(7) | -3.3(6) | 3.8(6) | -0.7(5) |
| N2 | 52.9(10) | 27.5(8) | 41.4(9) | -16.3(7) | 14.4(7) | -6.5(7) |
| C1 | 15.4(7) | 22.5(7) | 24.2(7) | -4.0(6) | -1.5(6) | -4.2(6) |
| C2 | 15.8(7) | 23.1(8) | 30.5(8) | -2.2(6) | -1.5(6) | -3.4(6) |
| C3 | 19.6(8) | 30.7(9) | 32.0(8) | 5.2(7) | -2.7(6) | -5.1(7) |
| C4 | 24.4(8) | 43.8(10) | 23.7(8) | -2.8(7) | -1.0(6) | -10.5(7) |
| C5 | 22.0(8) | 32.8(9) | 26.3(8) | -9.1(6) | -0.1(6) | -9.6(7) |
| C6 | 21.5(8) | 35.5(9) | 30.5(8) | -11.0(7) | -1.0(6) | -7.2(7) |
| C7 | 24.8(8) | 30.5(9) | 41.7(10) | -7.0(7) | -1.9(7) | -11.8(7) |
| C8 | 20.7(8) | 50.7(11) | 32.4(9) | -6.9(8) | 5.0(7) | -11.9(8) |
| C9 | 19.9(8) | 41.9(10) | 46.1(10) | -22.1(8) | -0.2(7) | 1.1(7) |
| C10 | 20.3(8) | 27.9(8) | 38.0(9) | -2.2(7) | -6.1(7) | -3.0(6) |
| C11 | 22.2(8) | 18.2(7) | 38.6(9) | -3.4(6) | 0.3(7) | -3.4(6) |
| C12 | 25.6(9) | 39.2(10) | 45.3(11) | 1.7(8) | -0.7(8) | 2.3(8) |
| C13 | 42.7(11) | 29.4(9) | 48.6(11) | -9.6(8) | 11.9(9) | -2.1(8) |
| C14 | 27.1(8) | 16.9(7) | 21.8(7) | -4.1(6) | 1.6(6) | -3.8(6) |
| C15 | 30.9(9) | 27.5(8) | 33.6(9) | -9.4(7) | 7.1(7) | -6.1(7) |
| C16 | 49.3(12) | 31.5(9) | 34.3(9) | -12.3(8) | 16.0(8) | -4.4(8) |
| C17 | 65.1(14) | 31.8(9) | 26.2(8) | -12.8(7) | 3.2(8) | -8.5(9) |
| C18 | 48.7(11) | 34.8(10) | 31.9(9) | -10.3(7) | -8.2(8) | -9.3(8) |
| C19 | 31.0(9) | 28.3(8) | 27.4(8) | -7.9(7) | 0.2(7) | -5.6(7) |
| C20 | 26.7(8) | 24.2(8) | 19.2(7) | -7.3(6) | 0.4(6) | -7.6(6) |
| C21 | 31.1(9) | 23.6(8) | 22.2(7) | -6.9(6) | 1.6(6) | -8.4(6) |
| C22 | 40.7(10) | 30.8(9) | 29.8(8) | -3.6(7) | 5.0(7) | -16.2(8) |
| C23 | 29.4(9) | 42.6(10) | 33.6(9) | -7.3(8) | 4.5(7) | -16.2(8) |
| C24 | 26.0(8) | 33.1(9) | 23.1(7) | -6.0(6) | -0.6(6) | -7.4(7) |
| C25 | 30.4(9) | 44.9(10) | 26.8(8) | -14.6(7) | -2.6(7) | -2.0(8) |
| C26 | 54.0(12) | 51.0(12) | 20.0(8) | -3.4(8) | -3.2(8) | -10.2(10) |
| C27 | 40.2(11) | 81.9(16) | 26.6(9) | -23.4(10) | 11.9(8) | -17.7(11) |
| C28 | 37.8(11) | 50.9(12) | 36.4(10) | -26.4(9) | -5.2(8) | 7.7(9) |
| C29 | 41.3(10) | 35.2(9) | 27.5(8) | -15.1(7) | -0.8(7) | -7.7(8) |
| C30 | 35.5(9) | 19.3(7) | 27.7(8) | -3.3(6) | 2.3(7) | -4.1(7) |
| C31 | 112(2) | 54.6(15) | 75.3(17) | -44.7(13) | 27.5(16) | -41.0(15) |
| C32 | 67.3(16) | 44.8(13) | 67.0(15) | -14.6(11) | 24.4(13) | 13.0(11) |
| C33 | 24.2(8) | 15.7(7) | 23.8(7) | -3.0(6) | 3.0(6) | -3.3(6) |
| C34 | 28.2(8) | 28.8(8) | 28.9(8) | -11.2(7) | 5.0(7) | -7.8(7) |
| C35 | 29.2(9) | 32.5(9) | 38.3(9) | -11.3(7) | -2.7(7) | -8.8(7) |
| C36 | 23.6(8) | 27.7(9) | 47.3(10) | -7.6(7) | 4.1(7) | -4.3(7) |
| C37 | 30.6(9) | 39(1) | 39.3(10) | -14.0(8) | 11.5(8) | 0.0(8) |
| C38 | 31.8(9) | 35.4(9) | 26.2(8) | -10.7(7) | 2.7(7) | -1.6(7) |
| C39 | 22.4(9) | 34.5(10) | 61.0(12) | -12.3(9) | -2.2(8) | -3.1(7) |
| C40 | 33.9(10) | 52.0(12) | 28.7(9) | 3.7(8) | -3.7(7) | -10.7(9) |
| C41 | 24.8(8) | 34.8(9) | 35.0(9) | -6.0(7) | -3.0(7) | -12.3(7) |
| C42 | 80.9(17) | 51.0(13) | 23.6(9) | -10.9(8) | -7.6(10) | -7.6(11) |
| C43 | 75.3(18) | 94(2) | 76.6(17) | -51.8(16) | 17.4(14) | -51.2(16) |
| C44 | 88.8(18) | 39.5(12) | 44.8(12) | -22.5(10) | -10.4(12) | 0.2(11) |
| Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
|---|---|---|---|---|---|---|
| Fe1 | C1 | 2.0517(15) | N1 | C13 | 1.452(2) | |
| Fe1 | C2 | 2.0444(15) | N2 | C30 | 1.458(2) | |
| Fe1 | C3 | 2.0424(16) | N2 | C31 | 1.456(3) | |
| Fe1 | C4 | 2.0432(16) | N2 | C32 | 1.451(3) | |
| Fe1 | C5 | 2.0301(16) | C1 | C2 | 1.446(2) | |
| Fe1 | C6 | 2.0458(16) | C1 | C5 | 1.436(2) | |
| Fe1 | C7 | 2.0401(17) | C2 | C3 | 1.422(2) | |
| Fe1 | C8 | 2.0418(17) | C2 | C11 | 1.497(2) | |
| Fe1 | C9 | 2.0400(17) | C3 | C4 | 1.415(3) | |
| Fe1 | C10 | 2.0457(16) | C4 | C5 | 1.418(2) | |
| Fe2 | C20 | 2.0502(15) | C6 | C7 | 1.415(2) | |
| Fe2 | C21 | 2.0327(15) | C6 | C10 | 1.411(2) | |
| Fe2 | C22 | 2.0393(18) | C7 | C8 | 1.410(3) | |
| Fe2 | C23 | 2.0471(18) | C8 | C9 | 1.416(3) | |
| Fe2 | C24 | 2.0363(16) | C9 | C10 | 1.415(3) | |
| Fe2 | C25 | 2.0434(18) | C14 | C15 | 1.397(2) | |
| Fe2 | C26 | 2.0417(18) | C14 | C19 | 1.394(2) | |
| Fe2 | C27 | 2.0354(18) | C15 | C16 | 1.392(2) | |
| Fe2 | C28 | 2.0342(18) | C16 | C17 | 1.373(3) | |
| Fe2 | C29 | 2.0401(18) | C17 | C18 | 1.389(3) | |
| Si1 | O1 | 1.6249(10) | C18 | C19 | 1.388(2) | |
| Si1 | O2 | 1.6197(11) | C20 | C21 | 1.444(2) | |
| Si1 | C1 | 1.8468(15) | C20 | C24 | 1.441(2) | |
| Si1 | C14 | 1.8664(15) | C21 | C22 | 1.429(2) | |
| Si2 | O1 | 1.6232(10) | C21 | C30 | 1.495(2) | |
| Si2 | O3 | 1.6221(11) | C22 | C23 | 1.415(3) | |
| Si2 | C20 | 1.8496(16) | C23 | C24 | 1.419(2) | |
| Si2 | C33 | 1.8589(16) | C25 | C26 | 1.406(3) | |
| Si3 | O2 | 1.6472(11) | C25 | C29 | 1.410(3) | |
| Si3 | C39 | 1.8534(18) | C26 | C27 | 1.417(3) | |
| Si3 | C40 | 1.8553(18) | C27 | C28 | 1.403(3) | |
| Si3 | C41 | 1.8472(17) | C28 | C29 | 1.411(3) | |
| Si4 | O3 | 1.6402(11) | C33 | C34 | 1.397(2) | |
| Si4 | C42 | 1.849(2) | C33 | C38 | 1.396(2) | |
| Si4 | C43 | 1.850(3) | C34 | C35 | 1.383(2) | |
| Si4 | C44 | 1.851(2) | C35 | C36 | 1.381(2) | |
| N1 | C11 | 1.464(2) | C36 | C37 | 1.375(3) | |
| N1 | C12 | 1.457(2) | C37 | C38 | 1.387(2) |
| Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|
| C2 | Fe1 | C1 | 41.33(6) | C41 | Si3 | C40 | 109.29(9) | |
| C2 | Fe1 | C6 | 110.83(6) | O3 | Si4 | C42 | 106.83(8) | |
| C2 | Fe1 | C10 | 134.80(7) | O3 | Si4 | C43 | 109.79(9) | |
| C3 | Fe1 | C1 | 68.96(6) | O3 | Si4 | C44 | 109.99(9) | |
| C3 | Fe1 | C2 | 40.72(6) | C42 | Si4 | C43 | 110.02(13) | |
| C3 | Fe1 | C4 | 40.52(7) | C42 | Si4 | C44 | 110.65(10) | |
| C3 | Fe1 | C6 | 134.89(7) | C43 | Si4 | C44 | 109.53(13) | |
| C3 | Fe1 | C10 | 174.45(7) | Si2 | O1 | Si1 | 150.08(7) | |
| C4 | Fe1 | C1 | 69.21(6) | Si1 | O2 | Si3 | 146.83(7) | |
| C4 | Fe1 | C2 | 68.79(7) | Si2 | O3 | Si4 | 149.06(8) | |
| C4 | Fe1 | C6 | 173.12(7) | C12 | N1 | C11 | 111.29(13) | |
| C4 | Fe1 | C10 | 144.58(7) | C13 | N1 | C11 | 109.86(14) | |
| C5 | Fe1 | C1 | 41.20(6) | C13 | N1 | C12 | 110.11(14) | |
| C5 | Fe1 | C2 | 68.97(6) | C31 | N2 | C30 | 111.04(16) | |
| C5 | Fe1 | C3 | 68.32(7) | C32 | N2 | C30 | 110.09(17) | |
| C5 | Fe1 | C4 | 40.74(7) | C32 | N2 | C31 | 111.47(19) | |
| C5 | Fe1 | C6 | 146.02(7) | Si1 | C1 | Fe1 | 129.62(8) | |
| C5 | Fe1 | C7 | 171.95(7) | C2 | C1 | Fe1 | 69.07(8) | |
| C5 | Fe1 | C8 | 132.39(7) | C2 | C1 | Si1 | 130.68(12) | |
| C5 | Fe1 | C9 | 108.48(7) | C5 | C1 | Fe1 | 68.60(9) | |
| C5 | Fe1 | C10 | 114.40(7) | C5 | C1 | Si1 | 122.85(11) | |
| C6 | Fe1 | C1 | 115.35(6) | C5 | C1 | C2 | 106.37(13) | |
| C7 | Fe1 | C1 | 146.32(7) | C1 | C2 | Fe1 | 69.61(8) | |
| C7 | Fe1 | C2 | 115.16(7) | C1 | C2 | C11 | 126.68(14) | |
| C7 | Fe1 | C3 | 109.86(7) | C3 | C2 | Fe1 | 69.57(9) | |
| C7 | Fe1 | C4 | 132.92(7) | C3 | C2 | C1 | 107.86(14) | |
| C7 | Fe1 | C6 | 40.54(7) | C3 | C2 | C11 | 125.45(15) | |
| C7 | Fe1 | C8 | 40.41(7) | C11 | C2 | Fe1 | 125.54(11) | |
| C7 | Fe1 | C10 | 68.15(7) | C2 | C3 | Fe1 | 69.72(9) | |
| C8 | Fe1 | C1 | 172.50(7) | C4 | C3 | Fe1 | 69.77(9) | |
| C8 | Fe1 | C2 | 145.11(7) | C4 | C3 | C2 | 108.98(14) | |
| C8 | Fe1 | C3 | 113.91(7) | C3 | C4 | Fe1 | 69.71(9) | |
| C8 | Fe1 | C4 | 108.12(7) | C3 | C4 | C5 | 107.64(15) | |
| C8 | Fe1 | C6 | 68.02(7) | C5 | C4 | Fe1 | 69.13(9) | |
| C8 | Fe1 | C10 | 68.22(7) | C1 | C5 | Fe1 | 70.21(9) | |
| C9 | Fe1 | C1 | 133.22(7) | C4 | C5 | Fe1 | 70.12(9) | |
| C9 | Fe1 | C2 | 173.92(7) | C4 | C5 | C1 | 109.14(14) | |
| C9 | Fe1 | C3 | 144.26(7) | C7 | C6 | Fe1 | 69.52(9) | |
| C9 | Fe1 | C4 | 113.18(7) | C10 | C6 | Fe1 | 69.82(9) | |
| C9 | Fe1 | C6 | 67.95(7) | C10 | C6 | C7 | 108.17(15) | |
| C9 | Fe1 | C7 | 68.10(7) | C6 | C7 | Fe1 | 69.95(9) | |
| C9 | Fe1 | C8 | 40.60(8) | C8 | C7 | Fe1 | 69.86(10) | |
| C9 | Fe1 | C10 | 40.53(7) | C8 | C7 | C6 | 108.05(15) | |
| C10 | Fe1 | C1 | 109.60(6) | C7 | C8 | Fe1 | 69.73(10) | |
| C10 | Fe1 | C6 | 40.35(7) | C7 | C8 | C9 | 107.89(16) | |
| C21 | Fe2 | C20 | 41.42(6) | C9 | C8 | Fe1 | 69.63(10) | |
| C21 | Fe2 | C22 | 41.08(7) | C8 | C9 | Fe1 | 69.77(10) | |
| C21 | Fe2 | C23 | 69.01(7) | C10 | C9 | Fe1 | 69.95(9) | |
| C21 | Fe2 | C24 | 69.12(6) | C10 | C9 | C8 | 108.12(15) | |
| C21 | Fe2 | C25 | 108.57(7) | C6 | C10 | Fe1 | 69.83(9) | |
| C21 | Fe2 | C26 | 118.89(7) | C6 | C10 | C9 | 107.78(15) | |
| C21 | Fe2 | C27 | 152.59(8) | C9 | C10 | Fe1 | 69.52(10) | |
| C21 | Fe2 | C28 | 165.86(8) | N1 | C11 | C2 | 112.79(13) | |
| C21 | Fe2 | C29 | 128.09(7) | C15 | C14 | Si1 | 120.93(13) | |
| C22 | Fe2 | C20 | 69.27(6) | C19 | C14 | Si1 | 121.73(12) | |
| C22 | Fe2 | C23 | 40.50(7) | C19 | C14 | C15 | 117.34(15) | |
| C22 | Fe2 | C25 | 128.36(7) | C16 | C15 | C14 | 121.24(17) | |
| C22 | Fe2 | C26 | 108.22(8) | C17 | C16 | C15 | 120.20(17) | |
| C22 | Fe2 | C29 | 166.34(7) | C16 | C17 | C18 | 119.88(16) | |
| C23 | Fe2 | C20 | 69.32(7) | C19 | C18 | C17 | 119.66(18) | |
| C24 | Fe2 | C20 | 41.29(6) | C18 | C19 | C14 | 121.66(16) | |
| C24 | Fe2 | C22 | 68.36(7) | Si2 | C20 | Fe2 | 128.94(8) | |
| C24 | Fe2 | C23 | 40.66(7) | C21 | C20 | Fe2 | 68.64(8) | |
| C24 | Fe2 | C25 | 153.32(7) | C21 | C20 | Si2 | 131.32(12) | |
| C24 | Fe2 | C26 | 164.62(8) | C24 | C20 | Fe2 | 68.83(8) | |
| C24 | Fe2 | C29 | 118.87(7) | C24 | C20 | Si2 | 122.37(12) | |
| C25 | Fe2 | C20 | 119.12(7) | C24 | C20 | C21 | 106.27(14) | |
| C25 | Fe2 | C23 | 165.31(7) | C20 | C21 | Fe2 | 69.94(8) | |
| C26 | Fe2 | C20 | 153.09(8) | C20 | C21 | C30 | 127.14(14) | |
| C26 | Fe2 | C23 | 127.16(8) | C22 | C21 | Fe2 | 69.71(9) | |
| C26 | Fe2 | C25 | 40.27(8) | C22 | C21 | C20 | 108.02(14) | |
| C27 | Fe2 | C20 | 164.68(8) | C22 | C21 | C30 | 124.84(15) | |
| C27 | Fe2 | C22 | 118.27(8) | C30 | C21 | Fe2 | 126.54(11) | |
| C27 | Fe2 | C23 | 107.04(8) | C21 | C22 | Fe2 | 69.21(9) | |
| C27 | Fe2 | C24 | 126.51(8) | C23 | C22 | Fe2 | 70.04(10) | |
| C27 | Fe2 | C25 | 68.03(8) | C23 | C22 | C21 | 108.74(15) | |
| C27 | Fe2 | C26 | 40.67(8) | C22 | C23 | Fe2 | 69.45(10) | |
| C27 | Fe2 | C29 | 68.06(8) | C22 | C23 | C24 | 107.84(15) | |
| C28 | Fe2 | C20 | 127.08(7) | C24 | C23 | Fe2 | 69.26(10) | |
| C28 | Fe2 | C22 | 151.72(8) | C20 | C24 | Fe2 | 69.87(9) | |
| C28 | Fe2 | C23 | 117.90(8) | C23 | C24 | Fe2 | 70.08(10) | |
| C28 | Fe2 | C24 | 107.41(7) | C23 | C24 | C20 | 109.14(15) | |
| C28 | Fe2 | C25 | 68.00(7) | C26 | C25 | Fe2 | 69.80(11) | |
| C28 | Fe2 | C26 | 68.04(8) | C26 | C25 | C29 | 108.17(17) | |
| C28 | Fe2 | C27 | 40.35(9) | C29 | C25 | Fe2 | 69.67(10) | |
| C28 | Fe2 | C29 | 40.54(8) | C25 | C26 | Fe2 | 69.93(10) | |
| C29 | Fe2 | C20 | 107.82(7) | C25 | C26 | C27 | 107.87(18) | |
| C29 | Fe2 | C23 | 152.24(7) | C27 | C26 | Fe2 | 69.43(10) | |
| C29 | Fe2 | C25 | 40.41(7) | C26 | C27 | Fe2 | 69.91(10) | |
| C29 | Fe2 | C26 | 67.95(8) | C28 | C27 | Fe2 | 69.78(10) | |
| O1 | Si1 | C1 | 108.30(6) | C28 | C27 | C26 | 107.93(18) | |
| O1 | Si1 | C14 | 107.71(6) | C27 | C28 | Fe2 | 69.87(11) | |
| O2 | Si1 | O1 | 108.97(6) | C27 | C28 | C29 | 108.23(17) | |
| O2 | Si1 | C1 | 109.55(6) | C29 | C28 | Fe2 | 69.95(10) | |
| O2 | Si1 | C14 | 107.83(7) | C25 | C29 | Fe2 | 69.92(10) | |
| C1 | Si1 | C14 | 114.36(7) | C25 | C29 | C28 | 107.81(17) | |
| O1 | Si2 | C20 | 108.57(6) | C28 | C29 | Fe2 | 69.51(11) | |
| O1 | Si2 | C33 | 107.94(6) | N2 | C30 | C21 | 111.76(14) | |
| O3 | Si2 | O1 | 108.53(6) | C34 | C33 | Si2 | 121.82(11) | |
| O3 | Si2 | C20 | 109.24(6) | C38 | C33 | Si2 | 121.19(12) | |
| O3 | Si2 | C33 | 108.30(6) | C38 | C33 | C34 | 116.98(15) | |
| C20 | Si2 | C33 | 114.13(7) | C35 | C34 | C33 | 121.75(15) | |
| O2 | Si3 | C39 | 108.11(8) | C36 | C35 | C34 | 119.80(16) | |
| O2 | Si3 | C40 | 110.14(7) | C37 | C36 | C35 | 119.91(16) | |
| O2 | Si3 | C41 | 107.11(7) | C36 | C37 | C38 | 120.11(16) | |
| C39 | Si3 | C40 | 110.15(10) | C37 | C38 | C33 | 121.44(16) | |
| C41 | Si3 | C39 | 112.00(9) |
| A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|---|---|
| Fe1 | C1 | C2 | C3 | 59.26(11) | C5 | C1 | C2 | Fe1 | -58.69(10) | |
| Fe1 | C1 | C2 | C11 | -119.76(15) | C5 | C1 | C2 | C3 | 0.57(17) | |
| Fe1 | C1 | C5 | C4 | -59.51(11) | C5 | C1 | C2 | C11 | -178.45(14) | |
| Fe1 | C2 | C3 | C4 | 58.87(11) | C6 | C7 | C8 | Fe1 | 59.76(11) | |
| Fe1 | C2 | C11 | N1 | -165.19(11) | C6 | C7 | C8 | C9 | 0.36(19) | |
| Fe1 | C3 | C4 | C5 | 58.93(11) | C7 | C6 | C10 | Fe1 | -59.14(11) | |
| Fe1 | C4 | C5 | C1 | 59.56(11) | C7 | C6 | C10 | C9 | 0.25(19) | |
| Fe1 | C6 | C7 | C8 | -59.71(12) | C7 | C8 | C9 | Fe1 | 59.46(12) | |
| Fe1 | C6 | C10 | C9 | 59.39(11) | C7 | C8 | C9 | C10 | -0.21(19) | |
| Fe1 | C7 | C8 | C9 | -59.40(12) | C8 | C9 | C10 | Fe1 | 59.55(12) | |
| Fe1 | C8 | C9 | C10 | -59.67(12) | C8 | C9 | C10 | C6 | -0.03(19) | |
| Fe1 | C9 | C10 | C6 | -59.58(11) | C10 | C6 | C7 | Fe1 | 59.32(11) | |
| Fe2 | C20 | C21 | C22 | 59.54(11) | C10 | C6 | C7 | C8 | -0.38(19) | |
| Fe2 | C20 | C21 | C30 | -121.23(16) | C11 | C2 | C3 | Fe1 | 119.75(15) | |
| Fe2 | C20 | C24 | C23 | -59.25(12) | C11 | C2 | C3 | C4 | 178.62(14) | |
| Fe2 | C21 | C22 | C23 | 59.05(12) | C12 | N1 | C11 | C2 | -65.76(18) | |
| Fe2 | C21 | C30 | N2 | -168.50(11) | C13 | N1 | C11 | C2 | 172.02(14) | |
| Fe2 | C22 | C23 | C24 | 58.81(12) | C14 | Si1 | O1 | Si2 | 148.81(14) | |
| Fe2 | C23 | C24 | C20 | 59.13(11) | C14 | Si1 | O2 | Si3 | 112.67(14) | |
| Fe2 | C25 | C26 | C27 | -59.28(13) | C14 | Si1 | C1 | Fe1 | 72.18(12) | |
| Fe2 | C25 | C29 | C28 | 59.41(12) | C14 | Si1 | C1 | C2 | -23.56(16) | |
| Fe2 | C26 | C27 | C28 | -59.66(13) | C14 | Si1 | C1 | C5 | 160.50(12) | |
| Fe2 | C27 | C28 | C29 | -59.66(12) | C14 | C15 | C16 | C17 | 0.0(3) | |
| Fe2 | C28 | C29 | C25 | -59.67(12) | C15 | C14 | C19 | C18 | -0.8(2) | |
| Si1 | C1 | C2 | Fe1 | 124.86(13) | C15 | C16 | C17 | C18 | 0.0(3) | |
| Si1 | C1 | C2 | C3 | -175.88(12) | C16 | C17 | C18 | C19 | -0.5(3) | |
| Si1 | C1 | C2 | C11 | 5.1(2) | C17 | C18 | C19 | C14 | 0.9(3) | |
| Si1 | C1 | C5 | Fe1 | -124.21(11) | C19 | C14 | C15 | C16 | 0.4(2) | |
| Si1 | C1 | C5 | C4 | 176.28(11) | C20 | Si2 | O1 | Si1 | -82.09(15) | |
| Si1 | C14 | C15 | C16 | -179.48(13) | C20 | Si2 | O3 | Si4 | -26.75(18) | |
| Si1 | C14 | C19 | C18 | 179.02(13) | C20 | Si2 | C33 | C34 | -67.83(14) | |
| Si2 | C20 | C21 | Fe2 | 123.69(13) | C20 | Si2 | C33 | C38 | 111.35(13) | |
| Si2 | C20 | C21 | C22 | -176.77(12) | C20 | C21 | C22 | Fe2 | -59.68(10) | |
| Si2 | C20 | C21 | C30 | 2.5(2) | C20 | C21 | C22 | C23 | -0.63(19) | |
| Si2 | C20 | C24 | Fe2 | -123.54(11) | C20 | C21 | C30 | N2 | -77.0(2) | |
| Si2 | C20 | C24 | C23 | 177.21(12) | C21 | C20 | C24 | Fe2 | 58.68(10) | |
| Si2 | C33 | C34 | C35 | 177.70(13) | C21 | C20 | C24 | C23 | -0.58(17) | |
| Si2 | C33 | C38 | C37 | -178.27(14) | C21 | C22 | C23 | Fe2 | -58.54(12) | |
| O1 | Si1 | O2 | Si3 | -130.68(13) | C21 | C22 | C23 | C24 | 0.3(2) | |
| O1 | Si1 | C1 | Fe1 | -47.92(11) | C22 | C21 | C30 | N2 | 102.08(18) | |
| O1 | Si1 | C1 | C2 | -143.66(13) | C22 | C23 | C24 | Fe2 | -58.93(12) | |
| O1 | Si1 | C1 | C5 | 40.40(14) | C22 | C23 | C24 | C20 | 0.20(19) | |
| O1 | Si1 | C14 | C15 | -132.96(13) | C24 | C20 | C21 | Fe2 | -58.80(10) | |
| O1 | Si1 | C14 | C19 | 47.19(14) | C24 | C20 | C21 | C22 | 0.73(17) | |
| O1 | Si2 | O3 | Si4 | -144.96(15) | C24 | C20 | C21 | C30 | 179.97(15) | |
| O1 | Si2 | C20 | Fe2 | -43.44(12) | C25 | C26 | C27 | Fe2 | 59.60(13) | |
| O1 | Si2 | C20 | C21 | -138.42(14) | C25 | C26 | C27 | C28 | -0.1(2) | |
| O1 | Si2 | C20 | C24 | 44.42(14) | C26 | C25 | C29 | Fe2 | -59.39(13) | |
| O1 | Si2 | C33 | C34 | 52.96(14) | C26 | C25 | C29 | C28 | 0.02(19) | |
| O1 | Si2 | C33 | C38 | -127.86(13) | C26 | C27 | C28 | Fe2 | 59.74(13) | |
| O2 | Si1 | O1 | Si2 | 32.09(16) | C26 | C27 | C28 | C29 | 0.1(2) | |
| O2 | Si1 | C1 | Fe1 | -166.65(9) | C27 | C28 | C29 | Fe2 | 59.61(13) | |
| O2 | Si1 | C1 | C2 | 97.61(15) | C27 | C28 | C29 | C25 | -0.1(2) | |
| O2 | Si1 | C1 | C5 | -78.34(13) | C29 | C25 | C26 | Fe2 | 59.31(12) | |
| O2 | Si1 | C14 | C15 | -15.49(15) | C29 | C25 | C26 | C27 | 0.0(2) | |
| O2 | Si1 | C14 | C19 | 164.66(12) | C30 | C21 | C22 | Fe2 | 121.06(15) | |
| O3 | Si2 | O1 | Si1 | 36.54(16) | C30 | C21 | C22 | C23 | -179.89(15) | |
| O3 | Si2 | C20 | Fe2 | -161.62(9) | C31 | N2 | C30 | C21 | -63.7(2) | |
| O3 | Si2 | C20 | C21 | 103.40(15) | C32 | N2 | C30 | C21 | 172.36(16) | |
| O3 | Si2 | C20 | C24 | -73.77(13) | C33 | Si2 | O1 | Si1 | 153.70(14) | |
| O3 | Si2 | C33 | C34 | 170.27(12) | C33 | Si2 | O3 | Si4 | 98.11(16) | |
| O3 | Si2 | C33 | C38 | -10.55(15) | C33 | Si2 | C20 | Fe2 | 76.99(11) | |
| C1 | Si1 | O1 | Si2 | -87.02(15) | C33 | Si2 | C20 | C21 | -17.99(17) | |
| C1 | Si1 | O2 | Si3 | -12.36(16) | C33 | Si2 | C20 | C24 | 164.85(12) | |
| C1 | Si1 | C14 | C15 | 106.62(13) | C33 | C34 | C35 | C36 | 0.9(3) | |
| C1 | Si1 | C14 | C19 | -73.23(14) | C34 | C33 | C38 | C37 | 0.9(2) | |
| C1 | C2 | C3 | Fe1 | -59.28(10) | C34 | C35 | C36 | C37 | 0.3(3) | |
| C1 | C2 | C3 | C4 | -0.41(18) | C35 | C36 | C37 | C38 | -0.9(3) | |
| C1 | C2 | C11 | N1 | -75.30(19) | C36 | C37 | C38 | C33 | 0.2(3) | |
| C2 | C1 | C5 | Fe1 | 58.99(10) | C38 | C33 | C34 | C35 | -1.5(2) | |
| C2 | C1 | C5 | C4 | -0.52(17) | C39 | Si3 | O2 | Si1 | -80.31(16) | |
| C2 | C3 | C4 | Fe1 | -58.84(11) | C40 | Si3 | O2 | Si1 | 40.08(17) | |
| C2 | C3 | C4 | C5 | 0.09(18) | C41 | Si3 | O2 | Si1 | 158.83(14) | |
| C3 | C2 | C11 | N1 | 105.85(18) | C42 | Si4 | O3 | Si2 | -177.87(16) | |
| C3 | C4 | C5 | Fe1 | -59.29(11) | C43 | Si4 | O3 | Si2 | 62.86(19) | |
| C3 | C4 | C5 | C1 | 0.27(18) | C44 | Si4 | O3 | Si2 | -57.73(19) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| H3 | 7379 | 5271 | 208 | 36 |
| H4 | 8007 | 3519 | -316 | 38 |
| H5 | 7826 | 1880 | 844 | 31 |
| H6 | 9742 | 3592 | 2596 | 34 |
| H7 | 10031 | 4944 | 1268 | 38 |
| H8 | 10715 | 3837 | 205 | 42 |
| H9 | 10827 | 1802 | 873 | 43 |
| H10 | 10223 | 1651 | 2352 | 36 |
| H11A | 7137 | 4702 | 2419 | 33 |
| H11B | 6892 | 5740 | 1629 | 33 |
| H12A | 3752 | 6043 | 1417 | 62 |
| H12B | 4826 | 5454 | 891 | 62 |
| H12C | 4836 | 6615 | 1081 | 62 |
| H13A | 5542 | 5503 | 3160 | 63 |
| H13B | 4179 | 6069 | 2774 | 63 |
| H13C | 5265 | 6644 | 2453 | 63 |
| H15 | 4988 | 3104 | 3604 | 37 |
| H16 | 4954 | 3829 | 4741 | 47 |
| H17 | 6781 | 3862 | 5298 | 49 |
| H18 | 8666 | 3171 | 4713 | 46 |
| H19 | 8704 | 2425 | 3588 | 35 |
| H22 | 7212 | -3461 | 4614 | 40 |
| H23 | 5264 | -1877 | 4239 | 41 |
| H24 | 5812 | -253 | 3234 | 33 |
| H25 | 9558 | -1524 | 5211 | 41 |
| H26 | 8124 | -2522 | 6085 | 52 |
| H27 | 5965 | -1206 | 5875 | 57 |
| H28 | 6078 | 596 | 4877 | 51 |
| H29 | 8297 | 404 | 4463 | 41 |
| H30A | 10020 | -2634 | 3920 | 34 |
| H30B | 9581 | -3718 | 4381 | 34 |
| H31A | 9249 | -4969 | 3609 | 108 |
| H31B | 9278 | -4606 | 2631 | 108 |
| H31C | 8189 | -3937 | 3106 | 108 |
| H32A | 11571 | -3582 | 3234 | 99 |
| H32B | 11333 | -4376 | 2699 | 99 |
| H32C | 11307 | -4757 | 3676 | 99 |
| H34 | 10258 | -389 | 3784 | 34 |
| H35 | 12392 | -979 | 3934 | 39 |
| H36 | 13592 | -1667 | 2918 | 41 |
| H37 | 12649 | -1751 | 1752 | 45 |
| H38 | 10511 | -1189 | 1609 | 39 |
| H39A | 2954 | 3355 | 2756 | 60 |
| H39B | 2508 | 3858 | 1819 | 60 |
| H39C | 3685 | 4117 | 2136 | 60 |
| H40A | 4853 | 3259 | 662 | 61 |
| H40B | 3802 | 2701 | 513 | 61 |
| H40C | 5192 | 1946 | 706 | 61 |
| H41A | 4159 | 408 | 2134 | 47 |
| H41B | 2823 | 1245 | 1865 | 47 |
| H41C | 3315 | 968 | 2787 | 47 |
| H42A | 6960 | 747 | -9 | 80 |
| H42B | 7285 | -310 | -401 | 80 |
| H42C | 8367 | 143 | -153 | 80 |
| H43A | 6156 | -1606 | 1884 | 107 |
| H43B | 5895 | -1580 | 956 | 107 |
| H43C | 5501 | -444 | 1256 | 107 |
| H44A | 9535 | -2152 | 778 | 88 |
| H44B | 8443 | -2738 | 805 | 88 |
| H44C | 9013 | -2688 | 1638 | 88 |
Experimental
Single crystals of C44H60Fe2N2O3Si4 [3148] 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 [3148]
Crystal Data for C44H60Fe2N2O3Si4 (M =889.00 g/mol): triclinic, space group P-1 (no. 2), a = 11.2756(3) Å, b = 12.7949(4) Å, c = 16.9084(4) Å, α = 75.308(2)°, β = 87.164(2)°, γ = 74.135(2)°, V = 2269.22(11) Å3, Z = 2, T = 173.15 K, μ(MoKα) = 0.784 mm-1, Dcalc = 1.301 g/cm3, 47916 reflections measured (4.342° ≤ 2Θ ≤ 53.998°), 9895 unique (Rint = 0.0301, Rsigma = 0.0224) which were used in all calculations. The final R1 was 0.0285 (I > 2σ(I)) and wR2 was 0.0722 (all data).
Refinement model description
Number of restraints - 0, number of constraints - unknown.
Details:
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
C11(H11A,H11B), C30(H30A,H30B)
2.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)
2.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), C44(H44A,H44B,H44C)
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.