| Identification code | 3094 |
| Empirical formula | C40H52Cl2Fe2N2O4Si2 |
| Formula weight | 863.61 |
| Temperature/K | 150 |
| Crystal system | triclinic |
| Space group | P-1 |
| a/Å | 12.3951(4) |
| b/Å | 12.5719(4) |
| c/Å | 13.6964(5) |
| α/° | 78.754(3) |
| β/° | 85.109(3) |
| γ/° | 77.113(3) |
| Volume/Å3 | 2038.65(12) |
| Z | 2 |
| ρcalcg/cm3 | 1.407 |
| μ/mm‑1 | 0.944 |
| F(000) | 904.0 |
| Crystal size/mm3 | 0.3 × 0.2 × 0.1 |
| Radiation | MoKα (λ = 0.71073) |
| 2Θ range for data collection/° | 4.242 to 51.998 |
| Index ranges | -15 ≤ h ≤ 15, -15 ≤ k ≤ 15, -16 ≤ l ≤ 16 |
| Reflections collected | 48054 |
| Independent reflections | 8022 [Rint = 0.0435, Rsigma = 0.0316] |
| Data/restraints/parameters | 8022/10/492 |
| Goodness-of-fit on F2 | 1.045 |
| Final R indexes [I>=2σ (I)] | R1 = 0.0517, wR2 = 0.1262 |
| Final R indexes [all data] | R1 = 0.0632, wR2 = 0.1337 |
| Largest diff. peak/hole / e Å-3 | 1.30/-0.68 |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| Fe1 | 10567.6(4) | -530.9(4) | 2508.3(3) | 27.48(12) |
| Fe2 | 3482.3(4) | 3954.1(4) | 2989.3(3) | 26.26(12) |
| Si1 | 7761.2(7) | 490.9(7) | 2882.4(6) | 23.76(18) |
| Si2 | 6298.5(7) | 2721.1(7) | 3152.8(6) | 25.36(19) |
| O1 | 7003.4(18) | 1449.3(18) | 3439.8(16) | 28.4(5) |
| O2 | 7360.0(18) | 749.5(18) | 1739.5(17) | 28.9(5) |
| O3 | 6804.9(19) | 3194.2(19) | 2057.9(18) | 33.0(5) |
| N1 | 8981(2) | 2892(2) | 1139(2) | 32.4(6) |
| N2 | 5269(2) | 1792(2) | 941(2) | 36.0(7) |
| C1 | 9218(2) | 579(2) | 2921(2) | 24.4(6) |
| C2 | 9927(3) | 1118(3) | 2186(2) | 25.8(6) |
| C3 | 11001(3) | 918(3) | 2582(3) | 32.1(7) |
| C4 | 10974(3) | 269(3) | 3542(3) | 34.5(8) |
| C5 | 9898(3) | 59(3) | 3757(2) | 30.0(7) |
| C6 | 10069(3) | -1551(3) | 1723(3) | 53.6(11) |
| C7 | 10913(4) | -1053(4) | 1183(3) | 54.2(11) |
| C8 | 11864(3) | -1379(3) | 1759(3) | 44.0(9) |
| C9 | 11605(3) | -2064(3) | 2651(3) | 42.4(9) |
| C10 | 10503(3) | -2167(3) | 2630(3) | 45.3(9) |
| C11 | 9635(3) | 1718(3) | 1160(2) | 29.2(7) |
| C12 | 9537(4) | 3563(3) | 1632(3) | 46.6(10) |
| C13 | 8751(4) | 3444(3) | 87(3) | 45.1(9) |
| C14 | 7542(3) | -876(3) | 3584(3) | 35.3(8) |
| C15 | 6425(3) | -1108(3) | 3461(2) | 33.0(7) |
| C16 | 5468(3) | -488(3) | 3840(3) | 44.6(9) |
| C17 | 4444(4) | -686(5) | 3763(4) | 78.0(18) |
| C18 | 4344(6) | -1514(7) | 3311(5) | 108(3) |
| C19 | 5250(7) | -2138(5) | 2884(4) | 101(2) |
| C20 | 6332(5) | -1949(4) | 2969(3) | 60.5(13) |
| C21 | 4822(3) | 2667(2) | 3127(2) | 26.4(7) |
| C22 | 4176(3) | 2686(3) | 2288(3) | 29.7(7) |
| C23 | 3086(3) | 2592(3) | 2659(3) | 38.2(8) |
| C24 | 3036(3) | 2521(3) | 3704(3) | 37.7(8) |
| C25 | 4086(3) | 2567(3) | 4001(3) | 31.8(7) |
| C26 | 4024(3) | 5413(3) | 2553(3) | 42.8(9) |
| C27 | 3218(3) | 5350(3) | 1912(3) | 44.3(9) |
| C28 | 2227(3) | 5269(3) | 2482(3) | 43.9(9) |
| C29 | 2420(3) | 5266(3) | 3488(3) | 40.0(8) |
| C30 | 3529(3) | 5356(3) | 3534(3) | 40.5(9) |
| C31 | 4549(3) | 2823(3) | 1220(2) | 34.8(8) |
| C32 | 4745(3) | 813(3) | 1198(3) | 49.1(10) |
| C33 | 5597(4) | 1988(4) | -137(3) | 68.0(15) |
| C34 | 6487(3) | 3509(3) | 4119(3) | 33.1(7) |
| C35 | 7642(3) | 3702(3) | 4138(2) | 30.6(7) |
| C36 | 7902(4) | 4717(3) | 3741(3) | 43.5(9) |
| C37 | 8987(4) | 4868(4) | 3766(3) | 57.4(12) |
| C38 | 9803(4) | 4015(4) | 4171(3) | 55.3(11) |
| C39 | 9561(3) | 3014(4) | 4549(3) | 50.5(10) |
| C40 | 8503(3) | 2849(3) | 4535(3) | 38.3(8) |
| Cl1 | 7545.9(8) | -813.0(9) | 324.4(7) | 48.4(2) |
| Cl2 | 6554.9(10) | 5520.7(10) | 1072.4(10) | 77.4(4) |
| O4 | 8346(5) | 6762(5) | 7(6) | 172(3) |
| Atom | U11 | U22 | U33 | U23 | U13 | U12 |
|---|---|---|---|---|---|---|
| Fe1 | 24.9(2) | 30.3(2) | 28.2(2) | -10.34(18) | -4.39(18) | -2.12(18) |
| Fe2 | 23.9(2) | 24.0(2) | 30.5(2) | -7.46(18) | 0.94(18) | -3.02(18) |
| Si1 | 21.1(4) | 21.6(4) | 29.7(4) | -6.5(3) | 0.3(3) | -5.7(3) |
| Si2 | 24.6(4) | 24.5(4) | 28.4(4) | -9.5(3) | -1.0(3) | -4.1(3) |
| O1 | 27.2(11) | 27.6(11) | 29.8(11) | -5.6(9) | 2.3(9) | -5.5(9) |
| O2 | 27.4(11) | 24.0(11) | 36.3(12) | -7.7(9) | -7.0(9) | -3.4(9) |
| O3 | 35.1(13) | 26.1(12) | 36.5(13) | -3.5(10) | -0.3(10) | -6.3(10) |
| N1 | 36.4(16) | 31.1(15) | 27.5(14) | -5.7(11) | 0.2(12) | -2.7(12) |
| N2 | 35.9(16) | 37.3(16) | 32.5(15) | -11.9(12) | -9.0(13) | 4.2(13) |
| C1 | 25.2(15) | 26.3(15) | 25.4(15) | -11.3(12) | -0.2(12) | -7.4(12) |
| C2 | 23.6(15) | 27.4(16) | 28.8(16) | -12.0(12) | 2.4(12) | -5.5(12) |
| C3 | 25.3(16) | 34.2(17) | 41.5(19) | -14.1(14) | -0.1(14) | -10.9(13) |
| C4 | 28.5(17) | 39.3(19) | 39.9(19) | -14.8(15) | -10.6(14) | -6.1(14) |
| C5 | 34.6(17) | 34.8(17) | 22.7(15) | -9.0(13) | -3.0(13) | -7.9(14) |
| C6 | 46(2) | 44(2) | 79(3) | -42(2) | -27(2) | 9.4(18) |
| C7 | 76(3) | 48(2) | 36(2) | -24.7(18) | -9(2) | 8(2) |
| C8 | 40(2) | 44(2) | 46(2) | -19.1(17) | 6.5(17) | 2.4(17) |
| C9 | 36(2) | 32.8(19) | 56(2) | -11.3(17) | -10.0(17) | 4.8(15) |
| C10 | 43(2) | 29.8(18) | 66(3) | -19.8(18) | -0.7(19) | -5.2(16) |
| C11 | 32.2(17) | 30.1(16) | 26.8(16) | -11.4(13) | 3.5(13) | -6.3(13) |
| C12 | 57(2) | 32.8(19) | 53(2) | -12.9(17) | -4.9(19) | -11.6(18) |
| C13 | 56(2) | 41(2) | 29.7(18) | -1.0(16) | -1.3(17) | 2.8(18) |
| C14 | 31.0(17) | 27.9(17) | 44(2) | 0.7(15) | 0.1(15) | -6.0(14) |
| C15 | 40.6(19) | 29.1(17) | 30.7(17) | 2.4(13) | -1.4(15) | -17.1(14) |
| C16 | 34.6(19) | 43(2) | 50(2) | 8.8(17) | 1.6(17) | -11.8(16) |
| C17 | 38(2) | 93(4) | 89(4) | 38(3) | -12(2) | -29(2) |
| C18 | 105(4) | 145(6) | 86(4) | 50(4) | -50(4) | -96(4) |
| C19 | 198(7) | 88(4) | 49(3) | 13(3) | -33(4) | -113(4) |
| C20 | 105(4) | 42(2) | 44(2) | -2.2(18) | -2(2) | -39(2) |
| C21 | 28.8(16) | 18.2(14) | 30.9(16) | -4.0(12) | 1.1(13) | -3.5(12) |
| C22 | 28.4(16) | 21.6(15) | 40.3(18) | -8.6(13) | -4.1(14) | -3.9(13) |
| C23 | 31.4(18) | 24.5(17) | 61(2) | -10.6(16) | -5.4(17) | -6.4(14) |
| C24 | 29.2(17) | 28.1(17) | 53(2) | -5.1(15) | 11.6(16) | -7.8(14) |
| C25 | 33.6(18) | 21.3(15) | 35.7(18) | -0.9(13) | 3.6(14) | -1.1(13) |
| C26 | 43(2) | 21.8(17) | 62(2) | -5.7(16) | 8.6(19) | -10.0(15) |
| C27 | 60(2) | 25.2(18) | 40(2) | -1.8(15) | -0.4(18) | 3.7(17) |
| C28 | 40(2) | 27.0(18) | 59(2) | -8.8(17) | -12.4(18) | 8.8(15) |
| C29 | 36.0(19) | 28.7(18) | 53(2) | -14.9(16) | 6.0(17) | 1.3(15) |
| C30 | 44(2) | 25.9(17) | 54(2) | -16.9(16) | -4.4(17) | -0.9(15) |
| C31 | 32.5(18) | 37.9(19) | 32.1(17) | -10.7(14) | -10.0(14) | 3.2(15) |
| C32 | 43(2) | 44(2) | 68(3) | -32(2) | -7.8(19) | -4.7(17) |
| C33 | 77(3) | 79(3) | 26(2) | -7(2) | -1(2) | 28(3) |
| C34 | 33.3(18) | 33.2(18) | 36.1(18) | -17.2(14) | -2.2(14) | -4.3(14) |
| C35 | 38.2(18) | 33.1(17) | 25.8(16) | -12.1(13) | -5.0(14) | -11.5(14) |
| C36 | 57(2) | 31.8(19) | 45(2) | -9.7(16) | -10.6(18) | -11.6(17) |
| C37 | 77(3) | 49(2) | 60(3) | -17(2) | 9(2) | -40(2) |
| C38 | 43(2) | 71(3) | 63(3) | -30(2) | -6(2) | -21(2) |
| C39 | 41(2) | 61(3) | 54(2) | -18(2) | -14.6(19) | -9.3(19) |
| C40 | 44(2) | 37.5(19) | 34.3(18) | -4.9(15) | -9.7(16) | -8.7(16) |
| Cl1 | 44.8(5) | 57.2(6) | 42.2(5) | -20.3(4) | -11.8(4) | 5.0(4) |
| Cl2 | 63.5(7) | 49.3(6) | 85.8(9) | 31.2(6) | 24.6(6) | 9.8(5) |
| O4 | 97(4) | 99(3) | 342(9) | -115(5) | 119(5) | -47(3) |
| Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
|---|---|---|---|---|---|---|
| Fe1 | C1 | 2.042(3) | C1 | C5 | 1.440(4) | |
| Fe1 | C2 | 2.023(3) | C2 | C3 | 1.432(4) | |
| Fe1 | C3 | 2.034(3) | C2 | C11 | 1.492(4) | |
| Fe1 | C4 | 2.043(3) | C3 | C4 | 1.408(5) | |
| Fe1 | C5 | 2.036(3) | C4 | C5 | 1.412(5) | |
| Fe1 | C6 | 2.047(4) | C6 | C7 | 1.418(7) | |
| Fe1 | C7 | 2.030(4) | C6 | C10 | 1.409(6) | |
| Fe1 | C8 | 2.038(4) | C7 | C8 | 1.413(6) | |
| Fe1 | C9 | 2.049(4) | C8 | C9 | 1.408(6) | |
| Fe1 | C10 | 2.050(4) | C9 | C10 | 1.404(5) | |
| Fe2 | C21 | 2.036(3) | C14 | C15 | 1.507(5) | |
| Fe2 | C22 | 2.013(3) | C15 | C16 | 1.387(5) | |
| Fe2 | C23 | 2.023(3) | C15 | C20 | 1.389(5) | |
| Fe2 | C24 | 2.043(3) | C16 | C17 | 1.364(6) | |
| Fe2 | C25 | 2.043(3) | C17 | C18 | 1.343(10) | |
| Fe2 | C26 | 2.056(3) | C18 | C19 | 1.375(10) | |
| Fe2 | C27 | 2.044(4) | C19 | C20 | 1.431(8) | |
| Fe2 | C28 | 2.056(3) | C21 | C22 | 1.448(5) | |
| Fe2 | C29 | 2.059(3) | C21 | C25 | 1.445(5) | |
| Fe2 | C30 | 2.057(4) | C22 | C23 | 1.425(5) | |
| Si1 | O1 | 1.627(2) | C22 | C31 | 1.485(5) | |
| Si1 | O2 | 1.633(2) | C23 | C24 | 1.413(5) | |
| Si1 | C1 | 1.840(3) | C24 | C25 | 1.413(5) | |
| Si1 | C14 | 1.862(3) | C26 | C27 | 1.411(6) | |
| Si2 | O1 | 1.632(2) | C26 | C30 | 1.425(6) | |
| Si2 | O3 | 1.629(2) | C27 | C28 | 1.410(6) | |
| Si2 | C21 | 1.850(3) | C28 | C29 | 1.417(6) | |
| Si2 | C34 | 1.858(3) | C29 | C30 | 1.411(5) | |
| N1 | C11 | 1.513(4) | C34 | C35 | 1.507(5) | |
| N1 | C12 | 1.484(5) | C35 | C36 | 1.382(5) | |
| N1 | C13 | 1.494(4) | C35 | C40 | 1.395(5) | |
| N2 | C31 | 1.497(4) | C36 | C37 | 1.404(6) | |
| N2 | C32 | 1.486(5) | C37 | C38 | 1.364(7) | |
| N2 | C33 | 1.484(5) | C38 | C39 | 1.354(6) | |
| C1 | C2 | 1.447(4) | C39 | C40 | 1.374(5) |
| Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|
| C1 | Fe1 | C4 | 69.48(13) | C21 | Si2 | C34 | 110.12(15) | |
| C1 | Fe1 | C6 | 109.40(14) | Si1 | O1 | Si2 | 138.76(15) | |
| C1 | Fe1 | C9 | 153.24(15) | C12 | N1 | C11 | 113.2(3) | |
| C1 | Fe1 | C10 | 120.24(14) | C12 | N1 | C13 | 110.5(3) | |
| C2 | Fe1 | C1 | 41.71(12) | C13 | N1 | C11 | 109.7(3) | |
| C2 | Fe1 | C3 | 41.34(12) | C32 | N2 | C31 | 113.1(3) | |
| C2 | Fe1 | C4 | 68.93(13) | C33 | N2 | C31 | 110.3(3) | |
| C2 | Fe1 | C5 | 69.08(13) | C33 | N2 | C32 | 110.4(3) | |
| C2 | Fe1 | C6 | 118.55(15) | Si1 | C1 | Fe1 | 126.02(15) | |
| C2 | Fe1 | C7 | 106.36(15) | C2 | C1 | Fe1 | 68.44(17) | |
| C2 | Fe1 | C8 | 125.88(15) | C2 | C1 | Si1 | 130.7(2) | |
| C2 | Fe1 | C9 | 164.03(14) | C5 | C1 | Fe1 | 69.08(18) | |
| C2 | Fe1 | C10 | 153.47(14) | C5 | C1 | Si1 | 123.6(2) | |
| C3 | Fe1 | C1 | 69.88(12) | C5 | C1 | C2 | 105.7(3) | |
| C3 | Fe1 | C4 | 40.41(14) | C1 | C2 | Fe1 | 69.85(17) | |
| C3 | Fe1 | C5 | 68.39(14) | C1 | C2 | C11 | 126.8(3) | |
| C3 | Fe1 | C6 | 151.08(17) | C3 | C2 | Fe1 | 69.74(18) | |
| C3 | Fe1 | C8 | 105.07(15) | C3 | C2 | C1 | 108.3(3) | |
| C3 | Fe1 | C9 | 126.17(14) | C3 | C2 | C11 | 124.7(3) | |
| C3 | Fe1 | C10 | 165.03(15) | C11 | C2 | Fe1 | 123.1(2) | |
| C4 | Fe1 | C6 | 168.24(18) | C2 | C3 | Fe1 | 68.92(18) | |
| C4 | Fe1 | C9 | 107.71(15) | C4 | C3 | Fe1 | 70.16(19) | |
| C4 | Fe1 | C10 | 129.45(16) | C4 | C3 | C2 | 108.2(3) | |
| C5 | Fe1 | C1 | 41.37(12) | C3 | C4 | Fe1 | 69.43(19) | |
| C5 | Fe1 | C4 | 40.51(13) | C3 | C4 | C5 | 108.4(3) | |
| C5 | Fe1 | C6 | 131.15(17) | C5 | C4 | Fe1 | 69.45(18) | |
| C5 | Fe1 | C8 | 150.60(15) | C1 | C5 | Fe1 | 69.55(17) | |
| C5 | Fe1 | C9 | 119.21(15) | C4 | C5 | Fe1 | 70.04(19) | |
| C5 | Fe1 | C10 | 110.98(16) | C4 | C5 | C1 | 109.4(3) | |
| C6 | Fe1 | C9 | 67.70(15) | C7 | C6 | Fe1 | 69.0(2) | |
| C6 | Fe1 | C10 | 40.24(17) | C10 | C6 | Fe1 | 70.0(2) | |
| C7 | Fe1 | C1 | 128.30(15) | C10 | C6 | C7 | 107.7(4) | |
| C7 | Fe1 | C3 | 115.74(17) | C6 | C7 | Fe1 | 70.3(2) | |
| C7 | Fe1 | C4 | 149.10(18) | C8 | C7 | Fe1 | 70.0(2) | |
| C7 | Fe1 | C5 | 168.42(16) | C8 | C7 | C6 | 107.8(4) | |
| C7 | Fe1 | C6 | 40.72(19) | C7 | C8 | Fe1 | 69.4(2) | |
| C7 | Fe1 | C8 | 40.67(17) | C9 | C8 | Fe1 | 70.3(2) | |
| C7 | Fe1 | C9 | 68.04(17) | C9 | C8 | C7 | 107.9(4) | |
| C7 | Fe1 | C10 | 68.04(18) | C8 | C9 | Fe1 | 69.4(2) | |
| C8 | Fe1 | C1 | 165.62(14) | C10 | C9 | Fe1 | 70.0(2) | |
| C8 | Fe1 | C4 | 115.95(15) | C10 | C9 | C8 | 108.2(4) | |
| C8 | Fe1 | C6 | 68.14(17) | C6 | C10 | Fe1 | 69.7(2) | |
| C8 | Fe1 | C9 | 40.31(16) | C9 | C10 | Fe1 | 69.9(2) | |
| C8 | Fe1 | C10 | 67.74(17) | C9 | C10 | C6 | 108.4(4) | |
| C9 | Fe1 | C10 | 40.06(15) | C2 | C11 | N1 | 113.0(3) | |
| C21 | Fe2 | C24 | 69.33(13) | C15 | C14 | Si1 | 114.3(2) | |
| C21 | Fe2 | C25 | 41.51(13) | C16 | C15 | C14 | 120.6(3) | |
| C21 | Fe2 | C26 | 108.75(14) | C16 | C15 | C20 | 118.7(4) | |
| C21 | Fe2 | C27 | 128.25(14) | C20 | C15 | C14 | 120.8(4) | |
| C21 | Fe2 | C28 | 165.85(15) | C17 | C16 | C15 | 122.5(5) | |
| C21 | Fe2 | C29 | 152.55(15) | C18 | C17 | C16 | 119.5(6) | |
| C21 | Fe2 | C30 | 119.27(14) | C17 | C18 | C19 | 121.3(5) | |
| C22 | Fe2 | C21 | 41.91(13) | C18 | C19 | C20 | 119.8(5) | |
| C22 | Fe2 | C23 | 41.34(14) | C15 | C20 | C19 | 118.2(5) | |
| C22 | Fe2 | C24 | 69.22(14) | Si2 | C21 | Fe2 | 128.12(16) | |
| C22 | Fe2 | C25 | 69.68(14) | C22 | C21 | Fe2 | 68.18(17) | |
| C22 | Fe2 | C26 | 117.58(15) | C22 | C21 | Si2 | 129.5(2) | |
| C22 | Fe2 | C27 | 106.38(15) | C25 | C21 | Fe2 | 69.49(18) | |
| C22 | Fe2 | C28 | 126.38(15) | C25 | C21 | Si2 | 124.1(2) | |
| C22 | Fe2 | C29 | 164.79(14) | C25 | C21 | C22 | 106.4(3) | |
| C22 | Fe2 | C30 | 152.49(14) | C21 | C22 | Fe2 | 69.91(18) | |
| C23 | Fe2 | C21 | 69.82(13) | C21 | C22 | C31 | 127.0(3) | |
| C23 | Fe2 | C24 | 40.67(15) | C23 | C22 | Fe2 | 69.72(19) | |
| C23 | Fe2 | C25 | 68.73(15) | C23 | C22 | C21 | 107.9(3) | |
| C23 | Fe2 | C26 | 150.52(17) | C23 | C22 | C31 | 125.0(3) | |
| C23 | Fe2 | C27 | 116.25(16) | C31 | C22 | Fe2 | 124.1(2) | |
| C23 | Fe2 | C28 | 106.24(15) | C22 | C23 | Fe2 | 68.94(18) | |
| C23 | Fe2 | C29 | 127.17(15) | C24 | C23 | Fe2 | 70.4(2) | |
| C23 | Fe2 | C30 | 165.92(15) | C24 | C23 | C22 | 108.5(3) | |
| C24 | Fe2 | C25 | 40.46(14) | C23 | C24 | Fe2 | 68.93(19) | |
| C24 | Fe2 | C26 | 168.31(16) | C25 | C24 | Fe2 | 69.77(18) | |
| C24 | Fe2 | C27 | 149.88(17) | C25 | C24 | C23 | 108.6(3) | |
| C24 | Fe2 | C28 | 117.11(16) | C21 | C25 | Fe2 | 69.01(17) | |
| C24 | Fe2 | C29 | 108.26(15) | C24 | C25 | Fe2 | 69.77(19) | |
| C24 | Fe2 | C30 | 129.51(16) | C24 | C25 | C21 | 108.5(3) | |
| C25 | Fe2 | C26 | 130.69(15) | C27 | C26 | Fe2 | 69.4(2) | |
| C25 | Fe2 | C27 | 168.09(15) | C27 | C26 | C30 | 107.7(3) | |
| C25 | Fe2 | C28 | 151.02(15) | C30 | C26 | Fe2 | 69.8(2) | |
| C25 | Fe2 | C29 | 118.79(15) | C26 | C27 | Fe2 | 70.3(2) | |
| C25 | Fe2 | C30 | 110.13(15) | C28 | C27 | Fe2 | 70.3(2) | |
| C26 | Fe2 | C29 | 67.79(15) | C28 | C27 | C26 | 108.3(4) | |
| C26 | Fe2 | C30 | 40.54(16) | C27 | C28 | Fe2 | 69.4(2) | |
| C27 | Fe2 | C26 | 40.25(16) | C27 | C28 | C29 | 108.1(4) | |
| C27 | Fe2 | C28 | 40.24(16) | C29 | C28 | Fe2 | 70.0(2) | |
| C27 | Fe2 | C29 | 67.83(16) | C28 | C29 | Fe2 | 69.7(2) | |
| C27 | Fe2 | C30 | 67.86(16) | C30 | C29 | Fe2 | 69.9(2) | |
| C28 | Fe2 | C26 | 67.59(16) | C30 | C29 | C28 | 107.9(3) | |
| C28 | Fe2 | C29 | 40.31(16) | C26 | C30 | Fe2 | 69.7(2) | |
| C28 | Fe2 | C30 | 67.56(16) | C29 | C30 | Fe2 | 70.0(2) | |
| C30 | Fe2 | C29 | 40.10(15) | C29 | C30 | C26 | 108.0(4) | |
| O1 | Si1 | O2 | 106.72(12) | C22 | C31 | N2 | 113.3(3) | |
| O1 | Si1 | C1 | 107.86(13) | C35 | C34 | Si2 | 114.7(2) | |
| O1 | Si1 | C14 | 107.64(14) | C36 | C35 | C34 | 121.8(3) | |
| O2 | Si1 | C1 | 111.50(13) | C36 | C35 | C40 | 117.1(3) | |
| O2 | Si1 | C14 | 112.76(15) | C40 | C35 | C34 | 121.1(3) | |
| C1 | Si1 | C14 | 110.10(15) | C35 | C36 | C37 | 120.4(4) | |
| O1 | Si2 | C21 | 107.80(13) | C38 | C37 | C36 | 120.7(4) | |
| O1 | Si2 | C34 | 108.84(14) | C39 | C38 | C37 | 119.4(4) | |
| O3 | Si2 | O1 | 104.75(12) | C38 | C39 | C40 | 120.8(4) | |
| O3 | Si2 | C21 | 112.21(14) | C39 | C40 | C35 | 121.6(4) | |
| O3 | Si2 | C34 | 112.82(15) |
| D | H | A | d(D-H)/Å | d(H-A)/Å | d(D-A)/Å | D-H-A/° |
|---|---|---|---|---|---|---|
| O2 | H2 | Cl1 | 0.962(19) | 2.02(2) | 2.979(2) | 171(4) |
| O3 | H3 | Cl2 | 0.961(19) | 2.18(3) | 2.933(2) | 134(3) |
| N1 | H1 | O3 | 0.985(18) | 1.89(2) | 2.856(4) | 167(3) |
| N2 | H2A | O2 | 0.991(18) | 1.87(2) | 2.836(4) | 163(3) |
| C11 | H11A | O2 | 0.99 | 2.65 | 3.292(4) | 123.0 |
| O4 | H4A | Cl2 | 0.87 | 2.29 | 3.099(5) | 153.8 |
| A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|---|---|
| Fe1 | C1 | C2 | C3 | -59.3(2) | C5 | C1 | C2 | C3 | 0.0(3) | |
| Fe1 | C1 | C2 | C11 | 116.8(3) | C5 | C1 | C2 | C11 | 176.2(3) | |
| Fe1 | C1 | C5 | C4 | 58.8(2) | C6 | C7 | C8 | Fe1 | -60.4(3) | |
| Fe1 | C2 | C3 | C4 | -59.3(2) | C6 | C7 | C8 | C9 | -0.5(4) | |
| Fe1 | C2 | C11 | N1 | 169.5(2) | C7 | C6 | C10 | Fe1 | 58.9(3) | |
| Fe1 | C3 | C4 | C5 | -58.7(2) | C7 | C6 | C10 | C9 | -0.5(4) | |
| Fe1 | C4 | C5 | C1 | -58.5(2) | C7 | C8 | C9 | Fe1 | -59.3(3) | |
| Fe1 | C6 | C7 | C8 | 60.2(3) | C7 | C8 | C9 | C10 | 0.2(4) | |
| Fe1 | C6 | C10 | C9 | -59.5(3) | C8 | C9 | C10 | Fe1 | -59.1(3) | |
| Fe1 | C7 | C8 | C9 | 59.9(3) | C8 | C9 | C10 | C6 | 0.2(4) | |
| Fe1 | C8 | C9 | C10 | 59.5(3) | C10 | C6 | C7 | Fe1 | -59.6(3) | |
| Fe1 | C9 | C10 | C6 | 59.4(3) | C10 | C6 | C7 | C8 | 0.6(4) | |
| Fe2 | C21 | C22 | C23 | -59.6(2) | C11 | C2 | C3 | Fe1 | -116.9(3) | |
| Fe2 | C21 | C22 | C31 | 118.1(3) | C11 | C2 | C3 | C4 | -176.2(3) | |
| Fe2 | C21 | C25 | C24 | 58.7(2) | C12 | N1 | C11 | C2 | 54.5(4) | |
| Fe2 | C22 | C23 | C24 | -59.5(2) | C13 | N1 | C11 | C2 | 178.4(3) | |
| Fe2 | C22 | C31 | N2 | 166.5(2) | C14 | Si1 | O1 | Si2 | -146.2(2) | |
| Fe2 | C23 | C24 | C25 | -58.6(2) | C14 | Si1 | C1 | Fe1 | 54.2(2) | |
| Fe2 | C24 | C25 | C21 | -58.3(2) | C14 | Si1 | C1 | C2 | 145.7(3) | |
| Fe2 | C26 | C27 | C28 | 60.3(2) | C14 | Si1 | C1 | C5 | -33.1(3) | |
| Fe2 | C26 | C30 | C29 | -59.8(2) | C14 | C15 | C16 | C17 | -178.6(4) | |
| Fe2 | C27 | C28 | C29 | 59.5(2) | C14 | C15 | C20 | C19 | 179.4(4) | |
| Fe2 | C28 | C29 | C30 | 59.7(2) | C15 | C16 | C17 | C18 | 0.4(7) | |
| Fe2 | C29 | C30 | C26 | 59.6(2) | C16 | C15 | C20 | C19 | -0.3(5) | |
| Si1 | C1 | C2 | Fe1 | -119.6(3) | C16 | C17 | C18 | C19 | -2.9(8) | |
| Si1 | C1 | C2 | C3 | -178.9(2) | C17 | C18 | C19 | C20 | 3.6(9) | |
| Si1 | C1 | C2 | C11 | -2.8(5) | C18 | C19 | C20 | C15 | -2.0(7) | |
| Si1 | C1 | C5 | Fe1 | 120.1(2) | C20 | C15 | C16 | C17 | 1.1(6) | |
| Si1 | C1 | C5 | C4 | 179.0(2) | C21 | Si2 | O1 | Si1 | 99.3(2) | |
| Si1 | C14 | C15 | C16 | -67.1(4) | C21 | Si2 | C34 | C35 | -174.3(2) | |
| Si1 | C14 | C15 | C20 | 113.2(3) | C21 | C22 | C23 | Fe2 | 59.7(2) | |
| Si2 | C21 | C22 | Fe2 | -122.1(3) | C21 | C22 | C23 | C24 | 0.3(4) | |
| Si2 | C21 | C22 | C23 | 178.3(2) | C21 | C22 | C31 | N2 | 77.0(4) | |
| Si2 | C21 | C22 | C31 | -4.0(5) | C22 | C21 | C25 | Fe2 | -58.4(2) | |
| Si2 | C21 | C25 | Fe2 | 122.9(2) | C22 | C21 | C25 | C24 | 0.3(3) | |
| Si2 | C21 | C25 | C24 | -178.4(2) | C22 | C23 | C24 | Fe2 | 58.5(2) | |
| Si2 | C34 | C35 | C36 | 102.9(3) | C22 | C23 | C24 | C25 | -0.1(4) | |
| Si2 | C34 | C35 | C40 | -75.3(4) | C23 | C22 | C31 | N2 | -105.7(4) | |
| O1 | Si1 | C1 | Fe1 | 171.40(17) | C23 | C24 | C25 | Fe2 | 58.1(2) | |
| O1 | Si1 | C1 | C2 | -97.1(3) | C23 | C24 | C25 | C21 | -0.2(4) | |
| O1 | Si1 | C1 | C5 | 84.1(3) | C25 | C21 | C22 | Fe2 | 59.2(2) | |
| O1 | Si1 | C14 | C15 | 72.1(3) | C25 | C21 | C22 | C23 | -0.3(3) | |
| O1 | Si2 | C21 | Fe2 | 171.75(18) | C25 | C21 | C22 | C31 | 177.4(3) | |
| O1 | Si2 | C21 | C22 | -96.3(3) | C26 | C27 | C28 | Fe2 | -60.3(2) | |
| O1 | Si2 | C21 | C25 | 82.1(3) | C26 | C27 | C28 | C29 | -0.8(4) | |
| O1 | Si2 | C34 | C35 | 67.8(3) | C27 | C26 | C30 | Fe2 | 59.3(2) | |
| O2 | Si1 | O1 | Si2 | -24.9(2) | C27 | C26 | C30 | C29 | -0.4(4) | |
| O2 | Si1 | C1 | Fe1 | -71.7(2) | C27 | C28 | C29 | Fe2 | -59.2(2) | |
| O2 | Si1 | C1 | C2 | 19.8(3) | C27 | C28 | C29 | C30 | 0.5(4) | |
| O2 | Si1 | C1 | C5 | -159.1(2) | C28 | C29 | C30 | Fe2 | -59.6(2) | |
| O2 | Si1 | C14 | C15 | -45.4(3) | C28 | C29 | C30 | C26 | 0.0(4) | |
| O3 | Si2 | O1 | Si1 | -20.4(3) | C30 | C26 | C27 | Fe2 | -59.5(2) | |
| O3 | Si2 | C21 | Fe2 | -73.4(2) | C30 | C26 | C27 | C28 | 0.8(4) | |
| O3 | Si2 | C21 | C22 | 18.5(3) | C31 | C22 | C23 | Fe2 | -118.0(3) | |
| O3 | Si2 | C21 | C25 | -163.1(2) | C31 | C22 | C23 | C24 | -177.5(3) | |
| O3 | Si2 | C34 | C35 | -48.0(3) | C32 | N2 | C31 | C22 | 55.2(4) | |
| C1 | Si1 | O1 | Si2 | 95.0(2) | C33 | N2 | C31 | C22 | 179.3(3) | |
| C1 | Si1 | C14 | C15 | -170.6(2) | C34 | Si2 | O1 | Si1 | -141.3(2) | |
| C1 | C2 | C3 | Fe1 | 59.4(2) | C34 | Si2 | C21 | Fe2 | 53.2(2) | |
| C1 | C2 | C3 | C4 | 0.1(4) | C34 | Si2 | C21 | C22 | 145.1(3) | |
| C1 | C2 | C11 | N1 | 81.0(4) | C34 | Si2 | C21 | C25 | -36.5(3) | |
| C2 | C1 | C5 | Fe1 | -58.9(2) | C34 | C35 | C36 | C37 | -179.7(3) | |
| C2 | C1 | C5 | C4 | -0.1(4) | C34 | C35 | C40 | C39 | 179.5(3) | |
| C2 | C3 | C4 | Fe1 | 58.6(2) | C35 | C36 | C37 | C38 | 0.7(6) | |
| C2 | C3 | C4 | C5 | -0.1(4) | C36 | C35 | C40 | C39 | 1.2(5) | |
| C3 | C2 | C11 | N1 | -103.5(4) | C36 | C37 | C38 | C39 | 0.3(7) | |
| C3 | C4 | C5 | Fe1 | 58.7(2) | C37 | C38 | C39 | C40 | -0.5(7) | |
| C3 | C4 | C5 | C1 | 0.2(4) | C38 | C39 | C40 | C35 | -0.2(6) | |
| C5 | C1 | C2 | Fe1 | 59.4(2) | C40 | C35 | C36 | C37 | -1.4(5) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| H2 | 7480(40) | 190(30) | 1330(30) | 57(13) |
| H3 | 7150(30) | 3820(30) | 1840(30) | 63(13) |
| H1 | 8267(19) | 2880(30) | 1510(20) | 31(9) |
| H2A | 5970(20) | 1540(30) | 1300(30) | 45(11) |
| H3A | 11624 | 1179 | 2254 | 38 |
| H4 | 11577 | 16 | 3972 | 41 |
| H5 | 9660 | -359 | 4359 | 36 |
| H6 | 9342 | -1481 | 1511 | 64 |
| H7 | 10850 | -585 | 547 | 65 |
| H8 | 12555 | -1173 | 1577 | 53 |
| H9 | 12092 | -2399 | 3177 | 51 |
| H10 | 10115 | -2582 | 3140 | 54 |
| H11A | 9195 | 1302 | 867 | 35 |
| H11B | 10324 | 1739 | 742 | 35 |
| H12A | 9639 | 3215 | 2333 | 70 |
| H12B | 9079 | 4313 | 1593 | 70 |
| H12C | 10261 | 3605 | 1297 | 70 |
| H13A | 9445 | 3560 | -273 | 68 |
| H13B | 8238 | 4162 | 81 | 68 |
| H13C | 8418 | 2973 | -237 | 68 |
| H14A | 8124 | -1469 | 3362 | 42 |
| H14B | 7633 | -907 | 4301 | 42 |
| H16 | 5529 | 96 | 4166 | 53 |
| H17 | 3805 | -242 | 4027 | 94 |
| H18 | 3634 | -1672 | 3285 | 129 |
| H19 | 5158 | -2691 | 2534 | 121 |
| H20 | 6970 | -2387 | 2697 | 73 |
| H23 | 2492 | 2580 | 2270 | 46 |
| H24 | 2403 | 2454 | 4134 | 45 |
| H25 | 4276 | 2538 | 4665 | 38 |
| H26 | 4765 | 5481 | 2364 | 51 |
| H27 | 3323 | 5359 | 1215 | 53 |
| H28 | 1548 | 5224 | 2235 | 53 |
| H29 | 1897 | 5214 | 4034 | 48 |
| H30 | 3883 | 5374 | 4117 | 49 |
| H31A | 4964 | 3427 | 1068 | 42 |
| H31B | 3891 | 3048 | 807 | 42 |
| H32A | 4554 | 680 | 1914 | 74 |
| H32B | 5263 | 160 | 1023 | 74 |
| H32C | 4071 | 955 | 825 | 74 |
| H33A | 4939 | 2129 | -530 | 102 |
| H33B | 6123 | 1332 | -297 | 102 |
| H33C | 5946 | 2632 | -294 | 102 |
| H34A | 5963 | 4237 | 4007 | 40 |
| H34B | 6291 | 3100 | 4780 | 40 |
| H36 | 7344 | 5315 | 3449 | 52 |
| H37 | 9154 | 5572 | 3498 | 69 |
| H38 | 10535 | 4124 | 4189 | 66 |
| H39 | 10129 | 2417 | 4826 | 61 |
| H40 | 8354 | 2138 | 4802 | 46 |
| H4A | 7779 | 6447 | 104 | 258 |
| H4B | 8566 | 6817 | 578 | 258 |
Experimental
Single crystals of C40H52Cl2Fe2N2O4Si2 [3094] were []. A suitable crystal was selected and [] on a Xcalibur, Sapphire3 diffractometer. The crystal was kept at 150 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 [3094]
Crystal Data for C40H52Cl2Fe2N2O4Si2 (M =863.61 g/mol): triclinic, space group P-1 (no. 2), a = 12.3951(4) Å, b = 12.5719(4) Å, c = 13.6964(5) Å, α = 78.754(3)°, β = 85.109(3)°, γ = 77.113(3)°, V = 2038.65(12) Å3, Z = 2, T = 150 K, μ(MoKα) = 0.944 mm-1, Dcalc = 1.407 g/cm3, 48054 reflections measured (4.242° ≤ 2Θ ≤ 51.998°), 8022 unique (Rint = 0.0435, Rsigma = 0.0316) which were used in all calculations. The final R1 was 0.0517 (I > 2σ(I)) and wR2 was 0.1337 (all data).
Refinement model description
Number of restraints - 10, 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, All O(H,H) groups
2. Restrained distances
N2-H2A = N1-H1
1 with sigma of 0.02
O2-H2 = O3-H3
1 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O4) ≈ Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4.a Free rotating group:
O4(H4A,H4B)
4.b Secondary CH2 refined with riding coordinates:
C11(H11A,H11B), C14(H14A,H14B), C31(H31A,H31B), C34(H34A,H34B)
4.c Aromatic/amide H refined with riding coordinates:
C3(H3A), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C16(H16),
C17(H17), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C25(H25), C26(H26),
C27(H27), C28(H28), C29(H29), C30(H30), C36(H36), C37(H37), C38(H38),
C39(H39), C40(H40)
4.d Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C32(H32A,H32B,H32C), C33(H33A,H33B,
H33C)
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.