| Identification code | mo_B0613_Cc |
| Empirical formula | C38H44Fe2N2O3Si2 |
| Formula weight | 744.63 |
| Temperature/K | 100.01 |
| Crystal system | monoclinic |
| Space group | Cc |
| a/Å | 24.4022(13) |
| b/Å | 14.0997(7) |
| c/Å | 10.2884(6) |
| α/° | 90 |
| β/° | 90.067(2) |
| γ/° | 90 |
| Volume/Å3 | 3539.9(3) |
| Z | 4 |
| ρcalcg/cm3 | 1.397 |
| μ/mm‑1 | 0.927 |
| F(000) | 1560.0 |
| Crystal size/mm3 | 0.52 × 0.498 × 0.318 |
| Radiation | MoKα (λ = 0.71073) |
| 2Θ range for data collection/° | 5.176 to 62 |
| Index ranges | -35 ≤ h ≤ 35, -20 ≤ k ≤ 20, -14 ≤ l ≤ 14 |
| Reflections collected | 105245 |
| Independent reflections | 11142 [Rint = 0.0347, Rsigma = 0.0207] |
| Data/restraints/parameters | 11142/2/432 |
| Goodness-of-fit on F2 | 1.033 |
| Final R indexes [I>=2σ (I)] | R1 = 0.0201, wR2 = 0.0472 |
| Final R indexes [all data] | R1 = 0.0207, wR2 = 0.0474 |
| Largest diff. peak/hole / e Å-3 | 0.30/-0.28 |
| Flack parameter | 0.000(3) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| Fe1 | 6771.5(2) | 1668.0(2) | 3887.7(2) | 10.81(5) |
| Fe2 | 3243.9(2) | 3490.9(2) | 3961.5(2) | 9.78(5) |
| Si1 | 5623.8(2) | 2726.1(3) | 5171.7(5) | 9.57(9) |
| Si2 | 4378.4(2) | 2279.6(3) | 5010.0(5) | 9.90(9) |
| O1 | 4994.4(6) | 2462.6(11) | 5581.1(13) | 12.8(2) |
| O2 | 5647.0(6) | 3512.1(10) | 4040.5(17) | 18.7(3) |
| O3 | 4387.9(6) | 1725.6(11) | 3642.5(15) | 18.1(3) |
| N1 | 5155.8(7) | 935.7(12) | 2194.5(16) | 15.0(3) |
| N2 | 4889.2(6) | 4410.4(12) | 2640.9(15) | 13.3(3) |
| C1 | 5999.9(7) | 1636.9(12) | 4677.1(18) | 9.7(3) |
| C2 | 6021.5(7) | 1126.8(13) | 3458.8(18) | 12.1(3) |
| C3 | 6414.4(8) | 376.8(14) | 3586(2) | 16.1(4) |
| C4 | 6642.8(8) | 414.1(14) | 4856(2) | 16.0(4) |
| C5 | 6393.1(7) | 1188.1(13) | 5524.6(18) | 12.2(3) |
| C6 | 6940.7(8) | 3061.3(16) | 3499(2) | 19.8(4) |
| C7 | 6991.9(8) | 2508.4(19) | 2352(2) | 24.5(5) |
| C8 | 7399.1(9) | 1796.6(19) | 2579(2) | 24.3(4) |
| C9 | 7598.3(8) | 1922.1(15) | 3865(2) | 18.4(4) |
| C10 | 7315.4(8) | 2701.7(14) | 4438(2) | 16.1(4) |
| C11 | 5713.3(7) | 1349.6(14) | 2233.3(18) | 14.2(3) |
| C12 | 5165.2(9) | -99.9(16) | 2322(3) | 25.3(4) |
| C13 | 4890.5(9) | 1196.1(19) | 962(2) | 25.8(5) |
| C14 | 5962.7(8) | 3157.9(14) | 6692(2) | 15.1(4) |
| C15 | 6334.3(8) | 3913.4(16) | 6672(2) | 22.4(4) |
| C16 | 6585.6(10) | 4227.9(18) | 7824(3) | 33.6(6) |
| C17 | 6467.9(10) | 3794.9(19) | 8991(3) | 35.6(6) |
| C18 | 6103.5(10) | 3041.0(18) | 9036(2) | 29.5(5) |
| C19 | 5855.5(9) | 2725.7(15) | 7890(2) | 20.0(4) |
| C20 | 4008.4(7) | 3425.1(12) | 4802.3(18) | 9.7(3) |
| C21 | 4000.1(7) | 4068.6(12) | 3707.6(17) | 10.7(3) |
| C22 | 3605.1(7) | 4797.9(12) | 3961(2) | 13.7(3) |
| C23 | 3361.4(7) | 4613.3(13) | 5198.4(19) | 13.4(3) |
| C24 | 3607.4(7) | 3775.4(13) | 5706.5(18) | 11.2(3) |
| C25 | 3106.1(8) | 2184.6(15) | 3151(2) | 19.5(4) |
| C26 | 3037.2(9) | 2912.2(18) | 2215(2) | 23.6(4) |
| C27 | 2614.7(8) | 3530.3(16) | 2650(2) | 21.5(4) |
| C28 | 2421.2(8) | 3180.9(14) | 3859(2) | 16.9(3) |
| C29 | 2726.6(8) | 2353.7(14) | 4180(2) | 17.2(4) |
| C30 | 4334.2(7) | 3996.5(13) | 2490.2(17) | 12.8(3) |
| C31 | 4861.3(9) | 5428.5(15) | 2937(2) | 20.2(4) |
| C32 | 5200.9(9) | 4278.0(18) | 1437(2) | 23.0(4) |
| C33 | 3990.0(8) | 1589.8(14) | 6257(2) | 15.8(4) |
| C34 | 3974.4(9) | 1852.8(16) | 7563(2) | 23.1(4) |
| C35 | 3632.0(11) | 1374(2) | 8439(3) | 35.6(6) |
| C36 | 3307.9(10) | 630(2) | 8004(3) | 41.1(7) |
| C37 | 3330.9(10) | 341(2) | 6728(3) | 38.1(7) |
| C38 | 3668.1(9) | 815.5(17) | 5857(2) | 25.0(5) |
| Atom | U11 | U22 | U33 | U23 | U13 | U12 |
|---|---|---|---|---|---|---|
| Fe1 | 6.92(10) | 15.56(11) | 9.96(11) | -0.94(10) | 0.58(9) | 1.45(9) |
| Fe2 | 6.42(10) | 12.06(10) | 10.85(11) | 0.08(10) | -1.42(9) | 0.21(8) |
| Si1 | 6.87(19) | 10.7(2) | 11.1(2) | -0.41(17) | -1.01(16) | 1.56(16) |
| Si2 | 6.82(19) | 11.2(2) | 11.6(2) | -0.42(17) | 0.00(16) | 1.49(16) |
| O1 | 6.6(5) | 18.6(6) | 13.2(5) | 0.0(5) | -0.1(5) | 2.3(4) |
| O2 | 12.0(6) | 19.1(6) | 24.9(8) | 10.3(6) | -0.3(6) | 2.8(5) |
| O3 | 12.1(7) | 22.9(7) | 19.3(7) | -9.7(5) | -1.8(5) | 4.3(5) |
| N1 | 10.4(7) | 19.8(8) | 14.9(7) | -6.4(6) | -1.7(6) | -1.1(6) |
| N2 | 9.3(6) | 17.9(7) | 12.6(7) | 3.9(6) | -0.3(5) | -2.9(5) |
| C1 | 7.5(7) | 11.1(7) | 10.3(8) | 0.6(6) | 0.2(6) | 0.1(6) |
| C2 | 9.0(7) | 13.7(8) | 13.7(8) | -2.2(6) | 0.4(6) | -0.8(6) |
| C3 | 15.0(8) | 14.6(8) | 18.8(9) | -5.9(7) | -1.5(7) | 3.3(6) |
| C4 | 16.3(9) | 13.1(8) | 18.7(9) | 0.4(7) | -1.8(7) | 5.1(7) |
| C5 | 11.6(7) | 12.7(8) | 12.4(8) | 1.1(6) | 0.4(6) | 1.0(6) |
| C6 | 12.2(8) | 21.7(10) | 25.5(10) | 10.5(8) | 1.0(7) | -2.4(7) |
| C7 | 13.5(9) | 44.6(13) | 15.3(9) | 11.1(9) | -0.1(7) | -6.1(9) |
| C8 | 12.4(9) | 41.8(13) | 18.7(10) | -6.8(9) | 7.0(8) | -3.5(8) |
| C9 | 7.7(7) | 27.0(9) | 20.6(10) | -1.8(9) | 0.1(7) | 0.5(7) |
| C10 | 11.8(8) | 18.8(9) | 17.7(9) | 0.3(7) | -0.6(7) | -3.7(7) |
| C11 | 10.7(8) | 19.9(8) | 11.9(8) | -2.8(7) | -1.1(6) | -1.2(6) |
| C12 | 21.8(10) | 20.2(10) | 34.1(12) | -8.3(9) | -1.8(9) | -5.4(8) |
| C13 | 18.3(9) | 39.7(13) | 19.4(10) | -6.1(9) | -8.2(8) | -1.9(9) |
| C14 | 11.7(8) | 14.4(8) | 19.1(9) | -7.2(7) | -4.4(7) | 6.0(6) |
| C15 | 15.8(9) | 18.4(9) | 33.0(11) | -9.0(8) | -4.4(8) | 2.1(7) |
| C16 | 21.7(10) | 25.2(11) | 53.8(16) | -22.0(11) | -13.7(10) | 3.2(9) |
| C17 | 31.9(12) | 39.6(13) | 35.3(14) | -23.9(12) | -21.5(11) | 18.8(10) |
| C18 | 31.8(11) | 37.2(12) | 19.5(10) | -9.6(10) | -9.7(9) | 20.4(10) |
| C19 | 18.4(9) | 23.4(10) | 18.2(9) | -5.1(8) | -5.3(7) | 9.3(8) |
| C20 | 7.1(7) | 11.4(8) | 10.4(8) | -0.2(6) | -0.8(6) | -0.7(6) |
| C21 | 8.2(7) | 11.9(7) | 11.9(8) | 1.5(6) | -1.1(6) | -1.2(6) |
| C22 | 11.7(7) | 11.0(7) | 18.4(8) | 2.1(7) | -0.4(7) | 1.0(6) |
| C23 | 11.0(8) | 13.1(8) | 16.1(8) | -1.7(7) | -0.1(6) | 1.9(6) |
| C24 | 9.1(7) | 12.8(8) | 11.8(8) | -2.3(6) | -1.3(6) | 1.0(6) |
| C25 | 12.9(8) | 20.0(9) | 25.5(10) | -10.3(8) | -4.8(7) | -0.7(7) |
| C26 | 15.1(9) | 41.0(13) | 14.7(9) | -6.7(9) | -4.4(7) | -5.8(8) |
| C27 | 12.7(9) | 29.6(11) | 22(1) | 5.5(8) | -9.6(8) | -2.5(7) |
| C28 | 7.4(7) | 18.8(8) | 24.4(10) | -1.6(8) | -2.2(7) | -1.2(6) |
| C29 | 13.1(8) | 14.5(8) | 23.9(10) | -0.9(7) | -2.9(7) | -3.6(6) |
| C30 | 10.6(7) | 16.4(8) | 11.5(8) | 1.8(6) | -0.3(6) | -2.1(6) |
| C31 | 22.2(9) | 17.3(9) | 21.1(10) | 5.7(7) | -3.6(8) | -7.4(8) |
| C32 | 17.6(9) | 33.6(11) | 18.0(9) | 4.2(8) | 5.7(7) | -5.3(8) |
| C33 | 9.9(8) | 14.7(8) | 22.9(10) | 6.8(7) | 0.6(7) | 4.8(6) |
| C34 | 23.8(10) | 22.4(10) | 23.0(11) | 7.1(8) | 6.1(8) | 9.9(8) |
| C35 | 34.3(13) | 40.3(14) | 32.1(13) | 20.5(11) | 15.3(11) | 20.9(11) |
| C36 | 21.5(11) | 43.8(15) | 58.1(18) | 35.6(14) | 11.4(11) | 7.4(10) |
| C37 | 23.2(11) | 31.1(12) | 60.2(18) | 26.0(12) | -3.1(12) | -6.6(9) |
| C38 | 18.3(9) | 21.8(10) | 34.8(12) | 11.0(9) | -3.9(9) | -2.9(8) |
| Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
|---|---|---|---|---|---|---|
| Fe1 | C1 | 2.0520(17) | C1 | C2 | 1.446(3) | |
| Fe1 | C2 | 2.0311(18) | C1 | C5 | 1.442(2) | |
| Fe1 | C3 | 2.042(2) | C2 | C3 | 1.433(3) | |
| Fe1 | C4 | 2.053(2) | C2 | C11 | 1.501(3) | |
| Fe1 | C5 | 2.0373(19) | C3 | C4 | 1.421(3) | |
| Fe1 | C6 | 2.047(2) | C4 | C5 | 1.427(3) | |
| Fe1 | C7 | 2.048(2) | C6 | C7 | 1.421(3) | |
| Fe1 | C8 | 2.049(2) | C6 | C10 | 1.422(3) | |
| Fe1 | C9 | 2.0493(19) | C7 | C8 | 1.431(3) | |
| Fe1 | C10 | 2.0503(19) | C8 | C9 | 1.420(3) | |
| Fe2 | C20 | 2.0574(18) | C9 | C10 | 1.426(3) | |
| Fe2 | C21 | 2.0342(17) | C14 | C15 | 1.399(3) | |
| Fe2 | C22 | 2.0427(18) | C14 | C19 | 1.400(3) | |
| Fe2 | C23 | 2.0507(19) | C15 | C16 | 1.405(3) | |
| Fe2 | C24 | 2.0413(18) | C16 | C17 | 1.377(5) | |
| Fe2 | C25 | 2.049(2) | C17 | C18 | 1.387(4) | |
| Fe2 | C26 | 2.036(2) | C18 | C19 | 1.397(3) | |
| Fe2 | C27 | 2.044(2) | C20 | C21 | 1.446(2) | |
| Fe2 | C28 | 2.0570(19) | C20 | C24 | 1.438(2) | |
| Fe2 | C29 | 2.0532(19) | C21 | C22 | 1.433(2) | |
| Si1 | O1 | 1.6358(15) | C21 | C30 | 1.499(2) | |
| Si1 | O2 | 1.6081(15) | C22 | C23 | 1.430(3) | |
| Si1 | C1 | 1.8602(18) | C23 | C24 | 1.424(3) | |
| Si1 | C14 | 1.870(2) | C25 | C26 | 1.417(3) | |
| Si2 | O1 | 1.6339(14) | C25 | C29 | 1.427(3) | |
| Si2 | O3 | 1.6095(15) | C26 | C27 | 1.422(3) | |
| Si2 | C20 | 1.8626(18) | C27 | C28 | 1.420(3) | |
| Si2 | C33 | 1.869(2) | C28 | C29 | 1.423(3) | |
| N1 | C11 | 1.481(2) | C33 | C34 | 1.395(3) | |
| N1 | C12 | 1.466(3) | C33 | C38 | 1.406(3) | |
| N1 | C13 | 1.470(3) | C34 | C35 | 1.403(3) | |
| N2 | C30 | 1.483(2) | C35 | C36 | 1.389(5) | |
| N2 | C31 | 1.469(3) | C36 | C37 | 1.375(5) | |
| N2 | C32 | 1.467(3) | C37 | C38 | 1.389(3) |
| Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|
| C1 | Fe1 | C4 | 69.44(7) | O3 | Si2 | C33 | 110.80(9) | |
| C2 | Fe1 | C1 | 41.48(7) | C20 | Si2 | C33 | 106.49(8) | |
| C2 | Fe1 | C3 | 41.20(7) | Si2 | O1 | Si1 | 143.81(9) | |
| C2 | Fe1 | C4 | 69.12(8) | C12 | N1 | C11 | 112.07(16) | |
| C2 | Fe1 | C5 | 69.24(7) | C12 | N1 | C13 | 109.43(18) | |
| C2 | Fe1 | C6 | 120.01(8) | C13 | N1 | C11 | 109.18(16) | |
| C2 | Fe1 | C7 | 106.69(8) | C31 | N2 | C30 | 111.34(16) | |
| C2 | Fe1 | C8 | 124.37(8) | C32 | N2 | C30 | 109.64(15) | |
| C2 | Fe1 | C9 | 161.83(8) | C32 | N2 | C31 | 108.87(17) | |
| C2 | Fe1 | C10 | 155.49(8) | Si1 | C1 | Fe1 | 122.94(9) | |
| C3 | Fe1 | C1 | 69.48(7) | C2 | C1 | Fe1 | 68.48(10) | |
| C3 | Fe1 | C4 | 40.59(8) | C2 | C1 | Si1 | 131.77(13) | |
| C3 | Fe1 | C6 | 155.80(8) | C5 | C1 | Fe1 | 68.81(10) | |
| C3 | Fe1 | C7 | 120.73(9) | C5 | C1 | Si1 | 121.66(14) | |
| C3 | Fe1 | C8 | 107.34(9) | C5 | C1 | C2 | 106.32(15) | |
| C3 | Fe1 | C9 | 125.03(8) | C1 | C2 | Fe1 | 70.03(10) | |
| C3 | Fe1 | C10 | 162.12(8) | C1 | C2 | C11 | 127.26(16) | |
| C5 | Fe1 | C1 | 41.29(7) | C3 | C2 | Fe1 | 69.81(11) | |
| C5 | Fe1 | C3 | 68.64(8) | C3 | C2 | C1 | 108.24(16) | |
| C5 | Fe1 | C4 | 40.84(7) | C3 | C2 | C11 | 124.44(17) | |
| C5 | Fe1 | C6 | 124.88(8) | C11 | C2 | Fe1 | 123.67(13) | |
| C5 | Fe1 | C7 | 161.79(9) | C2 | C3 | Fe1 | 68.99(11) | |
| C5 | Fe1 | C8 | 155.89(9) | C4 | C3 | Fe1 | 70.13(11) | |
| C5 | Fe1 | C9 | 120.99(9) | C4 | C3 | C2 | 108.56(16) | |
| C5 | Fe1 | C10 | 107.57(8) | C3 | C4 | Fe1 | 69.27(11) | |
| C6 | Fe1 | C1 | 106.45(8) | C3 | C4 | C5 | 107.73(16) | |
| C6 | Fe1 | C4 | 162.17(9) | C5 | C4 | Fe1 | 68.97(11) | |
| C6 | Fe1 | C7 | 40.60(10) | C1 | C5 | Fe1 | 69.90(10) | |
| C6 | Fe1 | C8 | 68.64(9) | C4 | C5 | Fe1 | 70.19(11) | |
| C6 | Fe1 | C9 | 68.36(8) | C4 | C5 | C1 | 109.15(16) | |
| C6 | Fe1 | C10 | 40.63(8) | C7 | C6 | Fe1 | 69.73(13) | |
| C7 | Fe1 | C1 | 124.05(8) | C7 | C6 | C10 | 108.14(19) | |
| C7 | Fe1 | C4 | 155.91(10) | C10 | C6 | Fe1 | 69.82(11) | |
| C7 | Fe1 | C8 | 40.90(10) | C6 | C7 | Fe1 | 69.67(12) | |
| C7 | Fe1 | C9 | 68.31(9) | C6 | C7 | C8 | 108.12(19) | |
| C7 | Fe1 | C10 | 68.35(9) | C8 | C7 | Fe1 | 69.59(13) | |
| C8 | Fe1 | C1 | 161.64(8) | C7 | C8 | Fe1 | 69.51(12) | |
| C8 | Fe1 | C4 | 120.65(9) | C9 | C8 | Fe1 | 69.75(12) | |
| C8 | Fe1 | C9 | 40.55(9) | C9 | C8 | C7 | 107.5(2) | |
| C8 | Fe1 | C10 | 68.56(9) | C8 | C9 | Fe1 | 69.70(11) | |
| C9 | Fe1 | C1 | 155.82(8) | C8 | C9 | C10 | 108.42(19) | |
| C9 | Fe1 | C4 | 107.89(8) | C10 | C9 | Fe1 | 69.68(11) | |
| C9 | Fe1 | C10 | 40.71(8) | C6 | C10 | Fe1 | 69.56(12) | |
| C10 | Fe1 | C1 | 120.00(8) | C6 | C10 | C9 | 107.78(19) | |
| C10 | Fe1 | C4 | 125.27(8) | C9 | C10 | Fe1 | 69.60(11) | |
| C21 | Fe2 | C20 | 41.40(7) | N1 | C11 | C2 | 113.55(16) | |
| C21 | Fe2 | C22 | 41.17(7) | C15 | C14 | Si1 | 121.46(17) | |
| C21 | Fe2 | C23 | 69.17(7) | C15 | C14 | C19 | 117.76(19) | |
| C21 | Fe2 | C24 | 68.96(7) | C19 | C14 | Si1 | 120.78(16) | |
| C21 | Fe2 | C25 | 117.14(8) | C14 | C15 | C16 | 120.7(2) | |
| C21 | Fe2 | C26 | 105.72(8) | C17 | C16 | C15 | 120.3(2) | |
| C21 | Fe2 | C27 | 125.81(8) | C16 | C17 | C18 | 120.2(2) | |
| C21 | Fe2 | C28 | 164.55(8) | C17 | C18 | C19 | 119.5(3) | |
| C21 | Fe2 | C29 | 152.21(8) | C18 | C19 | C14 | 121.6(2) | |
| C22 | Fe2 | C20 | 69.50(7) | Si2 | C20 | Fe2 | 121.77(9) | |
| C22 | Fe2 | C23 | 40.89(8) | C21 | C20 | Fe2 | 68.44(10) | |
| C22 | Fe2 | C25 | 151.79(9) | C21 | C20 | Si2 | 129.77(14) | |
| C22 | Fe2 | C27 | 107.40(8) | C24 | C20 | Fe2 | 68.86(10) | |
| C22 | Fe2 | C28 | 127.79(7) | C24 | C20 | Si2 | 123.61(14) | |
| C22 | Fe2 | C29 | 165.90(8) | C24 | C20 | C21 | 106.22(15) | |
| C23 | Fe2 | C20 | 69.38(7) | C20 | C21 | Fe2 | 70.16(10) | |
| C23 | Fe2 | C28 | 109.35(8) | C20 | C21 | C30 | 126.94(16) | |
| C23 | Fe2 | C29 | 128.33(8) | C22 | C21 | Fe2 | 69.74(10) | |
| C24 | Fe2 | C20 | 41.09(7) | C22 | C21 | C20 | 108.49(15) | |
| C24 | Fe2 | C22 | 68.65(8) | C22 | C21 | C30 | 124.55(16) | |
| C24 | Fe2 | C23 | 40.74(7) | C30 | C21 | Fe2 | 125.07(12) | |
| C24 | Fe2 | C25 | 127.25(8) | C21 | C22 | Fe2 | 69.10(10) | |
| C24 | Fe2 | C27 | 154.26(9) | C23 | C22 | Fe2 | 69.86(11) | |
| C24 | Fe2 | C28 | 120.64(8) | C23 | C22 | C21 | 108.17(16) | |
| C24 | Fe2 | C29 | 108.88(8) | C22 | C23 | Fe2 | 69.26(10) | |
| C25 | Fe2 | C20 | 106.18(7) | C24 | C23 | Fe2 | 69.28(10) | |
| C25 | Fe2 | C23 | 165.64(9) | C24 | C23 | C22 | 107.59(16) | |
| C25 | Fe2 | C28 | 68.20(8) | C20 | C24 | Fe2 | 70.06(10) | |
| C25 | Fe2 | C29 | 40.72(9) | C23 | C24 | Fe2 | 69.98(10) | |
| C26 | Fe2 | C20 | 125.20(8) | C23 | C24 | C20 | 109.52(16) | |
| C26 | Fe2 | C22 | 117.88(9) | C26 | C25 | Fe2 | 69.21(12) | |
| C26 | Fe2 | C23 | 153.01(9) | C26 | C25 | C29 | 107.86(18) | |
| C26 | Fe2 | C24 | 164.09(8) | C29 | C25 | Fe2 | 69.79(11) | |
| C26 | Fe2 | C25 | 40.59(10) | C25 | C26 | Fe2 | 70.20(12) | |
| C26 | Fe2 | C27 | 40.81(9) | C25 | C26 | C27 | 108.38(19) | |
| C26 | Fe2 | C28 | 68.23(9) | C27 | C26 | Fe2 | 69.88(12) | |
| C26 | Fe2 | C29 | 68.41(9) | C26 | C27 | Fe2 | 69.31(11) | |
| C27 | Fe2 | C20 | 163.52(8) | C28 | C27 | Fe2 | 70.24(11) | |
| C27 | Fe2 | C23 | 119.55(9) | C28 | C27 | C26 | 107.75(19) | |
| C27 | Fe2 | C25 | 68.47(9) | C27 | C28 | Fe2 | 69.25(11) | |
| C27 | Fe2 | C28 | 40.52(9) | C27 | C28 | C29 | 108.25(19) | |
| C27 | Fe2 | C29 | 68.42(9) | C29 | C28 | Fe2 | 69.60(11) | |
| C28 | Fe2 | C20 | 153.66(8) | C25 | C29 | Fe2 | 69.50(11) | |
| C29 | Fe2 | C20 | 118.42(7) | C28 | C29 | Fe2 | 69.89(11) | |
| C29 | Fe2 | C28 | 40.50(8) | C28 | C29 | C25 | 107.76(19) | |
| O1 | Si1 | C1 | 110.28(8) | N2 | C30 | C21 | 112.56(15) | |
| O1 | Si1 | C14 | 105.84(8) | C34 | C33 | Si2 | 122.50(16) | |
| O2 | Si1 | O1 | 112.13(8) | C34 | C33 | C38 | 118.2(2) | |
| O2 | Si1 | C1 | 110.68(8) | C38 | C33 | Si2 | 119.17(17) | |
| O2 | Si1 | C14 | 111.41(9) | C33 | C34 | C35 | 120.6(3) | |
| C1 | Si1 | C14 | 106.25(8) | C36 | C35 | C34 | 119.7(3) | |
| O1 | Si2 | C20 | 110.49(8) | C37 | C36 | C35 | 120.5(2) | |
| O1 | Si2 | C33 | 107.61(8) | C36 | C37 | C38 | 119.9(3) | |
| O3 | Si2 | O1 | 112.14(8) | C37 | C38 | C33 | 121.1(3) | |
| O3 | Si2 | C20 | 109.15(8) |
| D | H | A | d(D-H)/Å | d(H-A)/Å | d(D-A)/Å | D-H-A/° |
|---|---|---|---|---|---|---|
| O2 | H2 | N2 | 0.84 | 1.95 | 2.663(2) | 142.3 |
| O3 | H3 | N1 | 0.84 | 1.92 | 2.642(2) | 143.3 |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| H2 | 5332 | 3734 | 3916 | 28 |
| H3 | 4709 | 1548 | 3480 | 27 |
| H3A | 6507 | -70 | 2931 | 19 |
| H4 | 6913 | -1 | 5198 | 19 |
| H5 | 6473 | 1378 | 6390 | 15 |
| H6 | 6698 | 3581 | 3619 | 24 |
| H7 | 6791 | 2596 | 1569 | 29 |
| H8 | 7515 | 1326 | 1978 | 29 |
| H9 | 7873 | 1550 | 4274 | 22 |
| H10 | 7368 | 2939 | 5293 | 19 |
| H11A | 5684 | 2047 | 2142 | 17 |
| H11B | 5925 | 1109 | 1482 | 17 |
| H12A | 5378 | -373 | 1607 | 38 |
| H12B | 4790 | -345 | 2290 | 38 |
| H12C | 5334 | -274 | 3153 | 38 |
| H13A | 4881 | 1888 | 880 | 39 |
| H13B | 4516 | 947 | 948 | 39 |
| H13C | 5098 | 926 | 236 | 39 |
| H15 | 6418 | 4217 | 5872 | 27 |
| H16 | 6837 | 4741 | 7798 | 40 |
| H17 | 6637 | 4013 | 9767 | 43 |
| H18 | 6023 | 2741 | 9840 | 35 |
| H19 | 5608 | 2206 | 7925 | 24 |
| H22 | 3520 | 5314 | 3403 | 16 |
| H23 | 3085 | 4983 | 5608 | 16 |
| H24 | 3520 | 3492 | 6518 | 13 |
| H25 | 3360 | 1675 | 3103 | 23 |
| H26 | 3239 | 2976 | 1431 | 28 |
| H27 | 2485 | 4079 | 2209 | 26 |
| H28 | 2137 | 3453 | 4367 | 20 |
| H29 | 2685 | 1981 | 4943 | 21 |
| H30A | 4369 | 3321 | 2243 | 15 |
| H30B | 4140 | 4329 | 1777 | 15 |
| H31A | 4692 | 5765 | 2205 | 30 |
| H31B | 5232 | 5674 | 3080 | 30 |
| H31C | 4641 | 5526 | 3721 | 30 |
| H32A | 5036 | 4658 | 742 | 35 |
| H32B | 5195 | 3607 | 1190 | 35 |
| H32C | 5581 | 4481 | 1573 | 35 |
| H34 | 4198 | 2360 | 7861 | 28 |
| H35 | 3622 | 1559 | 9327 | 43 |
| H36 | 3068 | 317 | 8592 | 49 |
| H37 | 3117 | -181 | 6443 | 46 |
| H38 | 3682 | 613 | 4977 | 30 |
Experimental
Single crystals of C38H44Fe2N2O3Si2 [mo_B0613_Cc] were [The material was recrystallised from acetone by slow evaporation]. A suitable crystal was selected and [The crystal was mounted on a MITIGEN holder oil] on a Bruker D8 VENTURE area detector diffractometer. The crystal was kept at 100.01 K during data collection. Using Olex2 [1], the structure was solved with the ShelXT [2] structure solution program using Intrinsic Phasing and refined with the XL [3] refinement package using Least Squares minimisation.
Crystal structure determination of [mo_B0613_Cc]
Crystal Data for C38H44Fe2N2O3Si2 (M =744.63 g/mol): monoclinic, space group Cc (no. 9), a = 24.4022(13) Å, b = 14.0997(7) Å, c = 10.2884(6) Å, β = 90.067(2)°, V = 3539.9(3) Å3, Z = 4, T = 100.01 K, μ(MoKα) = 0.927 mm-1, Dcalc = 1.397 g/cm3, 105245 reflections measured (5.176° ≤ 2Θ ≤ 62°), 11142 unique (Rint = 0.0347, Rsigma = 0.0207) which were used in all calculations. The final R1 was 0.0201 (I > 2σ(I)) and wR2 was 0.0474 (all data).
Refinement model description
Number of restraints - 2, number of constraints - unknown.
Details:
1. Twinned data refinement
Scales: 0.8520(7) 0.1480(7)
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, All O(H) groups
3.a Secondary CH2 refined with riding coordinates:
C11(H11A,H11B), C30(H30A,H30B)
3.b Aromatic/amide H refined with riding coordinates:
C3(H3A), 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)
3.c Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C31(H31A,H31B,H31C), C32(H32A,H32B,
H32C)
3.d Idealised tetrahedral OH refined as rotating group:
O2(H2), O3(H3)
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.