| Identification code | mo_B0083_0m |
| Empirical formula | C36H58Fe2Li2N2OSi2 |
| Formula weight | 716.60 |
| Temperature/K | 100.0 |
| Crystal system | monoclinic |
| Space group | P21 |
| a/Å | 12.2143(5) |
| b/Å | 12.0951(6) |
| c/Å | 14.2648(7) |
| α/° | 90 |
| β/° | 113.848(2) |
| γ/° | 90 |
| Volume/Å3 | 1927.46(16) |
| Z | 2 |
| ρcalcg/cm3 | 1.235 |
| μ/mm‑1 | 0.843 |
| F(000) | 764.0 |
| Crystal size/mm3 | 0.553 × 0.236 × 0.176 |
| Radiation | MoKα (λ = 0.71073) |
| 2Θ range for data collection/° | 4.592 to 55.998 |
| Index ranges | -15 ≤ h ≤ 16, -15 ≤ k ≤ 15, -18 ≤ l ≤ 18 |
| Reflections collected | 56891 |
| Independent reflections | 9291 [Rint = 0.0213, Rsigma = 0.0152] |
| Data/restraints/parameters | 9291/3/438 |
| Goodness-of-fit on F2 | 1.129 |
| Final R indexes [I>=2σ (I)] | R1 = 0.0180, wR2 = 0.0476 |
| Final R indexes [all data] | R1 = 0.0189, wR2 = 0.0527 |
| Largest diff. peak/hole / e Å-3 | 0.38/-0.23 |
| Flack parameter | -0.004(2) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| Fe2 | 6852.7(2) | 4896.8(2) | 4585.0(2) | 13.58(6) |
| Fe1 | 7365.9(2) | 2799.7(2) | 8472.6(2) | 14.08(6) |
| Si2 | 9302.8(5) | 5312.7(4) | 3986.3(4) | 17.7(1) |
| Si1 | 5535.3(5) | 3143.6(4) | 9793.2(4) | 16.4(1) |
| O1 | 8439.2(15) | 7162.6(13) | 8411.0(12) | 28.5(3) |
| N2 | 9923.6(14) | 5269.5(14) | 7477.1(12) | 18.9(3) |
| N1 | 4951.7(14) | 5087.3(14) | 6632.7(12) | 19.1(3) |
| C17 | 8360.7(17) | 5721.8(15) | 4681.6(14) | 16.6(3) |
| C18 | 8440.6(16) | 5420.1(15) | 5688.4(14) | 14.8(3) |
| C19 | 7488.1(16) | 5901.3(15) | 5916.5(14) | 15.3(3) |
| C20 | 6813.9(17) | 6520.9(16) | 5001.2(14) | 17.0(4) |
| C21 | 7320.0(18) | 6420.4(15) | 4258.5(14) | 18.1(4) |
| C22 | 6653.0(19) | 3598.4(17) | 3604.2(16) | 22.2(4) |
| C23 | 6826.4(17) | 3200.5(17) | 4594.2(15) | 20.2(4) |
| C24 | 5872.9(17) | 3625.8(16) | 4827.2(15) | 18.0(4) |
| C25 | 5129.1(17) | 4295.3(17) | 3983.3(15) | 21.1(4) |
| C26 | 5614.0(19) | 4268.0(17) | 3230.4(15) | 23.1(4) |
| C30 | 9391.3(17) | 4709.0(15) | 6467.5(14) | 18.1(4) |
| C31 | 10552(2) | 6278.4(19) | 7395.1(17) | 28.3(5) |
| C32 | 10768.2(19) | 4518(2) | 8228.1(16) | 26.9(4) |
| C29 | 9920(2) | 3877.0(18) | 4309.6(19) | 32.3(5) |
| C28 | 10595.8(19) | 6282.7(18) | 4323.9(18) | 26.4(4) |
| C27 | 8406(2) | 5422(2) | 2571.2(17) | 34.4(5) |
| C1 | 6573.7(17) | 3698.7(15) | 9251.3(14) | 16.5(3) |
| C2 | 6300.9(16) | 4176.7(15) | 8251.4(14) | 17.0(4) |
| C3 | 7366.1(17) | 4504.5(16) | 8111.1(15) | 18.0(4) |
| C4 | 8313.6(17) | 4204.0(16) | 9081.4(15) | 18.3(4) |
| C5 | 7858.7(17) | 3728.4(15) | 9768.6(14) | 17.5(4) |
| C6 | 6849.5(19) | 1179.8(17) | 8449.5(17) | 23.0(4) |
| C7 | 6425.5(19) | 1609.7(17) | 7434.9(16) | 24.2(4) |
| C8 | 7437(2) | 1952.6(18) | 7251.1(16) | 24.3(4) |
| C9 | 8487.2(18) | 1741.9(17) | 8157.5(17) | 22.6(4) |
| C10 | 8118.9(19) | 1260.8(17) | 8894.8(16) | 22.6(4) |
| C14 | 5026.5(17) | 4303.5(17) | 7447.6(15) | 20.6(4) |
| C15 | 5125(2) | 6228.8(18) | 7031.6(17) | 27.2(5) |
| C16 | 3763.5(18) | 5001(2) | 5775.9(15) | 27.6(4) |
| C13 | 6400(2) | 2221.8(19) | 10902.7(16) | 26.0(4) |
| C12 | 4246.2(18) | 2371.0(18) | 8815.2(15) | 22.3(4) |
| C11 | 4897(2) | 4311.3(19) | 10279.4(18) | 30.0(5) |
| C33 | 8828(2) | 7058(2) | 9496.8(17) | 31.5(5) |
| C34 | 7824(3) | 6999(3) | 9847(2) | 42.6(6) |
| C35 | 7949(5) | 8270(4) | 8119(6) | 35.5(13) |
| C35B | 7826(14) | 8094(12) | 7713(10) | 49(3) |
| C36 | 8197(5) | 8681(3) | 7263(4) | 34.8(13) |
| C36B | 8793(15) | 8880(9) | 7892(13) | 63(4) |
| Li2 | 6544(3) | 4855(3) | 6501(2) | 20.6(6) |
| Li1 | 8299(3) | 5802(3) | 7602(3) | 21.3(7) |
| Atom | U11 | U22 | U33 | U23 | U13 | U12 |
|---|---|---|---|---|---|---|
| Fe2 | 15.42(12) | 14.22(12) | 11.94(11) | -0.70(9) | 6.38(9) | -1.83(9) |
| Fe1 | 14.75(12) | 14.76(12) | 13.00(11) | 2.43(9) | 5.90(9) | 1.52(9) |
| Si2 | 21.3(2) | 17.9(2) | 18.3(2) | -1.49(19) | 12.6(2) | -3.46(19) |
| Si1 | 18.9(2) | 18.5(2) | 14.2(2) | 0.80(18) | 9.18(19) | 0.62(19) |
| O1 | 39.0(9) | 22.7(8) | 27.4(8) | 3.1(6) | 17.2(7) | 4.9(7) |
| N2 | 17.0(7) | 22.0(8) | 14.8(7) | 0.0(6) | 3.6(6) | -0.9(6) |
| N1 | 20.1(7) | 22.0(9) | 15.0(7) | 5.7(6) | 6.7(6) | 6.7(6) |
| C17 | 19.1(8) | 16.2(8) | 16.2(8) | -1.3(7) | 9.1(7) | -4.4(7) |
| C18 | 16.6(8) | 14.1(8) | 14.4(8) | -1.9(7) | 7.0(7) | -3.1(7) |
| C19 | 17.5(8) | 14.3(8) | 14.7(8) | -1.6(6) | 7.0(7) | -1.1(7) |
| C20 | 19.1(9) | 14.9(8) | 17.6(9) | -0.4(7) | 8.0(7) | -0.4(7) |
| C21 | 24.3(9) | 15.4(8) | 16.4(8) | 1.3(7) | 10.0(7) | -3.3(7) |
| C22 | 26.6(10) | 22.6(9) | 21.1(9) | -10.9(7) | 13.4(8) | -9.8(8) |
| C23 | 22.6(10) | 14.4(8) | 23.6(10) | -3.8(7) | 9.4(8) | -3.0(7) |
| C24 | 20.3(9) | 17.3(9) | 17.8(9) | -1.9(7) | 9.2(7) | -5.1(7) |
| C25 | 17.2(9) | 21.1(10) | 22.6(9) | -0.9(7) | 5.6(7) | -2.7(7) |
| C26 | 26.6(10) | 24.1(10) | 15.1(9) | -2.6(7) | 4.9(8) | -8.4(8) |
| C30 | 18.6(8) | 18.1(10) | 17.9(8) | -1.4(7) | 7.6(7) | 0.7(7) |
| C31 | 24.7(10) | 30.8(12) | 27.2(10) | -4.1(9) | 8.2(9) | -10.1(9) |
| C32 | 21.3(10) | 36.2(11) | 20.2(9) | 4.0(8) | 5.3(8) | 4.7(8) |
| C29 | 50.8(14) | 20.7(10) | 39.0(12) | 0.4(9) | 32.4(11) | 3.0(9) |
| C28 | 24.7(10) | 24.9(10) | 36.2(11) | -4.1(9) | 19.2(9) | -5.6(8) |
| C27 | 32.4(12) | 54.0(15) | 21(1) | -2.8(10) | 15.3(9) | -2.3(11) |
| C1 | 18.4(8) | 17.7(8) | 14.6(8) | 1.4(7) | 8.0(7) | 1.7(7) |
| C2 | 18.4(9) | 16.8(9) | 17.5(8) | 3.9(7) | 8.9(7) | 3.0(7) |
| C3 | 18.2(9) | 16.6(8) | 20.5(9) | 3.7(7) | 9.2(7) | 1.8(7) |
| C4 | 17.2(9) | 17.7(9) | 19.4(9) | 0.5(7) | 6.9(7) | -1.2(7) |
| C5 | 20.2(9) | 16.8(9) | 14.5(8) | 0.3(7) | 6.2(7) | -0.2(7) |
| C6 | 26.6(10) | 15.4(9) | 31.7(11) | -1.3(8) | 16.4(9) | -2.0(8) |
| C7 | 23.2(10) | 22.5(10) | 23(1) | -7.0(8) | 5.3(8) | 0.7(8) |
| C8 | 33.9(11) | 23(1) | 19.5(9) | -0.2(8) | 14.4(9) | 5.8(8) |
| C9 | 22.1(10) | 20.2(9) | 28.9(10) | 1.7(8) | 13.8(8) | 4.7(8) |
| C10 | 26.8(10) | 17.0(9) | 23.7(10) | 5.1(7) | 9.7(8) | 4.4(7) |
| C14 | 17.7(9) | 25.6(10) | 20.3(9) | 9.3(7) | 9.5(7) | 5.4(7) |
| C15 | 34.6(12) | 22.3(10) | 24.9(10) | 5.1(8) | 12.2(9) | 11.8(9) |
| C16 | 20.8(9) | 40.2(12) | 19.8(9) | 6.7(9) | 6.1(8) | 9.1(9) |
| C13 | 27.9(11) | 32.4(11) | 18.4(9) | 7.2(8) | 10.1(8) | 0.8(9) |
| C12 | 20.3(9) | 26.8(10) | 21.0(9) | -0.1(8) | 9.6(8) | -1.7(8) |
| C11 | 33.6(12) | 28.6(11) | 36.0(12) | -6.8(9) | 22.5(10) | 0.0(9) |
| C33 | 31.3(11) | 36.4(12) | 24.5(11) | -12.2(9) | 9.0(9) | -5.4(9) |
| C34 | 46.8(15) | 53.4(16) | 33.0(13) | -4.3(12) | 21.7(12) | 1.9(12) |
| C35 | 49(3) | 22(2) | 45(3) | 11(2) | 29(3) | 12.3(19) |
| C35B | 77(7) | 41(6) | 32(6) | -6(5) | 26(6) | 8(5) |
| C36 | 55(3) | 23.9(19) | 29(2) | 5.5(16) | 20(2) | 4.6(17) |
| C36B | 97(10) | 43(6) | 70(10) | -8(5) | 56(10) | 1(5) |
| Li2 | 20.3(15) | 23.3(16) | 20.0(15) | 2.0(14) | 9.9(12) | -1.5(14) |
| Li1 | 23.0(16) | 23.5(16) | 17.9(15) | -0.1(13) | 8.7(13) | 0.6(13) |
| Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
|---|---|---|---|---|---|---|
| Fe2 | C17 | 2.0499(18) | N2 | C32 | 1.464(3) | |
| Fe2 | C18 | 2.0424(18) | N2 | Li1 | 2.161(4) | |
| Fe2 | C19 | 2.1199(18) | N1 | C14 | 1.474(2) | |
| Fe2 | C20 | 2.0581(19) | N1 | C15 | 1.476(3) | |
| Fe2 | C21 | 2.0381(18) | N1 | C16 | 1.475(2) | |
| Fe2 | C22 | 2.0512(19) | N1 | Li2 | 2.047(4) | |
| Fe2 | C23 | 2.052(2) | C17 | C18 | 1.446(2) | |
| Fe2 | C24 | 2.0613(19) | C17 | C21 | 1.440(3) | |
| Fe2 | C25 | 2.0584(19) | C18 | C19 | 1.451(2) | |
| Fe2 | C26 | 2.0585(19) | C18 | C30 | 1.510(3) | |
| Fe2 | Li2 | 2.907(3) | C19 | C20 | 1.441(3) | |
| Fe1 | C1 | 2.0547(18) | C19 | Li2 | 2.099(4) | |
| Fe1 | C2 | 2.0576(18) | C19 | Li1 | 2.202(4) | |
| Fe1 | C3 | 2.1255(19) | C20 | C21 | 1.431(3) | |
| Fe1 | C4 | 2.041(2) | C22 | C23 | 1.424(3) | |
| Fe1 | C5 | 2.0351(19) | C22 | C26 | 1.415(3) | |
| Fe1 | C6 | 2.054(2) | C23 | C24 | 1.430(3) | |
| Fe1 | C7 | 2.051(2) | C24 | C25 | 1.430(3) | |
| Fe1 | C8 | 2.053(2) | C25 | C26 | 1.421(3) | |
| Fe1 | C9 | 2.052(2) | C1 | C2 | 1.448(2) | |
| Fe1 | C10 | 2.055(2) | C1 | C5 | 1.440(3) | |
| Si2 | C17 | 1.8642(19) | C2 | C3 | 1.449(3) | |
| Si2 | C29 | 1.875(2) | C2 | C14 | 1.522(3) | |
| Si2 | C28 | 1.868(2) | C3 | C4 | 1.446(3) | |
| Si2 | C27 | 1.872(2) | C3 | Li2 | 2.144(4) | |
| Si1 | C1 | 1.8574(19) | C3 | Li1 | 2.227(4) | |
| Si1 | C13 | 1.874(2) | C4 | C5 | 1.429(3) | |
| Si1 | C12 | 1.877(2) | C6 | C7 | 1.424(3) | |
| Si1 | C11 | 1.877(2) | C6 | C10 | 1.421(3) | |
| O1 | C33 | 1.430(3) | C7 | C8 | 1.424(3) | |
| O1 | C35 | 1.458(5) | C8 | C9 | 1.429(3) | |
| O1 | C35B | 1.490(14) | C9 | C10 | 1.425(3) | |
| O1 | Li1 | 1.978(4) | C33 | C34 | 1.501(3) | |
| N2 | C30 | 1.483(2) | C35 | C36 | 1.458(7) | |
| N2 | C31 | 1.471(3) | C35B | C36B | 1.46(2) |
| Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|
| C17 | Fe2 | C19 | 70.57(7) | C35B | O1 | Li1 | 109.8(6) | |
| C17 | Fe2 | C20 | 68.96(7) | C30 | N2 | Li1 | 99.18(14) | |
| C17 | Fe2 | C22 | 105.92(8) | C31 | N2 | C30 | 109.87(15) | |
| C17 | Fe2 | C23 | 120.14(8) | C31 | N2 | Li1 | 106.58(16) | |
| C17 | Fe2 | C24 | 156.71(8) | C32 | N2 | C30 | 109.23(16) | |
| C17 | Fe2 | C25 | 160.01(8) | C32 | N2 | C31 | 109.70(16) | |
| C17 | Fe2 | C26 | 122.84(8) | C32 | N2 | Li1 | 121.56(15) | |
| C17 | Fe2 | Li2 | 113.57(8) | C14 | N1 | C15 | 110.13(16) | |
| C18 | Fe2 | C17 | 41.39(7) | C14 | N1 | C16 | 109.55(16) | |
| C18 | Fe2 | C19 | 40.74(7) | C14 | N1 | Li2 | 103.05(14) | |
| C18 | Fe2 | C20 | 66.88(7) | C15 | N1 | Li2 | 99.81(16) | |
| C18 | Fe2 | C22 | 125.23(8) | C16 | N1 | C15 | 108.95(17) | |
| C18 | Fe2 | C23 | 108.50(8) | C16 | N1 | Li2 | 124.56(15) | |
| C18 | Fe2 | C24 | 122.47(7) | Si2 | C17 | Fe2 | 124.48(10) | |
| C18 | Fe2 | C25 | 157.43(8) | C18 | C17 | Fe2 | 69.02(10) | |
| C18 | Fe2 | C26 | 161.16(8) | C18 | C17 | Si2 | 130.76(14) | |
| C18 | Fe2 | Li2 | 74.01(8) | C21 | C17 | Fe2 | 68.93(10) | |
| C19 | Fe2 | Li2 | 46.14(8) | C21 | C17 | Si2 | 124.26(14) | |
| C20 | Fe2 | C19 | 40.31(7) | C21 | C17 | C18 | 104.95(15) | |
| C20 | Fe2 | C24 | 125.51(7) | C17 | C18 | Fe2 | 69.58(10) | |
| C20 | Fe2 | C25 | 108.59(8) | C17 | C18 | C19 | 112.54(16) | |
| C20 | Fe2 | C26 | 121.97(8) | C17 | C18 | C30 | 126.71(16) | |
| C20 | Fe2 | Li2 | 73.64(9) | C19 | C18 | Fe2 | 72.50(10) | |
| C21 | Fe2 | C17 | 41.25(8) | C19 | C18 | C30 | 120.74(16) | |
| C21 | Fe2 | C18 | 68.25(7) | C30 | C18 | Fe2 | 126.78(13) | |
| C21 | Fe2 | C19 | 69.61(7) | Fe2 | C19 | Li1 | 141.90(13) | |
| C21 | Fe2 | C20 | 40.90(7) | C18 | C19 | Fe2 | 66.76(10) | |
| C21 | Fe2 | C22 | 120.22(8) | C18 | C19 | Li2 | 117.83(16) | |
| C21 | Fe2 | C23 | 155.79(8) | C18 | C19 | Li1 | 100.10(15) | |
| C21 | Fe2 | C24 | 161.41(8) | C20 | C19 | Fe2 | 67.54(10) | |
| C21 | Fe2 | C25 | 123.92(8) | C20 | C19 | C18 | 102.81(15) | |
| C21 | Fe2 | C26 | 106.68(8) | C20 | C19 | Li2 | 117.98(16) | |
| C21 | Fe2 | Li2 | 112.66(9) | C20 | C19 | Li1 | 149.09(16) | |
| C22 | Fe2 | C19 | 161.70(8) | Li2 | C19 | Fe2 | 87.12(11) | |
| C22 | Fe2 | C20 | 156.52(8) | Li2 | C19 | Li1 | 67.05(14) | |
| C22 | Fe2 | C23 | 40.63(8) | C19 | C20 | Fe2 | 72.15(10) | |
| C22 | Fe2 | C24 | 68.06(8) | C21 | C20 | Fe2 | 68.80(10) | |
| C22 | Fe2 | C25 | 68.00(8) | C21 | C20 | C19 | 111.53(16) | |
| C22 | Fe2 | C26 | 40.29(9) | C17 | C21 | Fe2 | 69.82(11) | |
| C22 | Fe2 | Li2 | 127.11(9) | C20 | C21 | Fe2 | 70.30(10) | |
| C23 | Fe2 | C19 | 124.63(7) | C20 | C21 | C17 | 108.17(16) | |
| C23 | Fe2 | C20 | 161.84(8) | C23 | C22 | Fe2 | 69.72(11) | |
| C23 | Fe2 | C24 | 40.68(8) | C26 | C22 | Fe2 | 70.13(11) | |
| C23 | Fe2 | C25 | 68.49(8) | C26 | C22 | C23 | 108.55(17) | |
| C23 | Fe2 | C26 | 68.23(8) | C22 | C23 | Fe2 | 69.65(12) | |
| C23 | Fe2 | Li2 | 88.19(9) | C22 | C23 | C24 | 107.48(18) | |
| C24 | Fe2 | C19 | 107.72(7) | C24 | C23 | Fe2 | 70.01(11) | |
| C24 | Fe2 | Li2 | 61.62(9) | C23 | C24 | Fe2 | 69.31(11) | |
| C25 | Fe2 | C19 | 121.23(8) | C23 | C24 | C25 | 107.93(17) | |
| C25 | Fe2 | C24 | 40.63(8) | C25 | C24 | Fe2 | 69.57(11) | |
| C25 | Fe2 | C26 | 40.39(8) | C24 | C25 | Fe2 | 69.79(11) | |
| C25 | Fe2 | Li2 | 83.48(9) | C26 | C25 | Fe2 | 69.81(11) | |
| C26 | Fe2 | C19 | 156.45(8) | C26 | C25 | C24 | 107.81(17) | |
| C26 | Fe2 | C24 | 68.01(8) | C22 | C26 | Fe2 | 69.58(11) | |
| C26 | Fe2 | Li2 | 123.42(9) | C22 | C26 | C25 | 108.23(18) | |
| C1 | Fe1 | C2 | 41.22(7) | C25 | C26 | Fe2 | 69.80(11) | |
| C1 | Fe1 | C3 | 70.37(7) | N2 | C30 | C18 | 111.05(15) | |
| C1 | Fe1 | C10 | 125.00(8) | Si1 | C1 | Fe1 | 125.72(10) | |
| C2 | Fe1 | C3 | 40.50(7) | C2 | C1 | Fe1 | 69.50(10) | |
| C4 | Fe1 | C1 | 68.88(8) | C2 | C1 | Si1 | 129.10(14) | |
| C4 | Fe1 | C2 | 66.81(8) | C5 | C1 | Fe1 | 68.66(10) | |
| C4 | Fe1 | C3 | 40.56(7) | C5 | C1 | Si1 | 125.60(14) | |
| C4 | Fe1 | C6 | 156.64(8) | C5 | C1 | C2 | 105.30(16) | |
| C4 | Fe1 | C7 | 161.22(8) | C1 | C2 | Fe1 | 69.28(10) | |
| C4 | Fe1 | C8 | 124.41(9) | C1 | C2 | C3 | 112.55(16) | |
| C4 | Fe1 | C9 | 107.34(8) | C1 | C2 | C14 | 122.69(16) | |
| C4 | Fe1 | C10 | 121.28(8) | C3 | C2 | Fe1 | 72.27(11) | |
| C5 | Fe1 | C1 | 41.22(7) | C3 | C2 | C14 | 124.76(16) | |
| C5 | Fe1 | C2 | 68.22(7) | C14 | C2 | Fe1 | 125.98(14) | |
| C5 | Fe1 | C3 | 69.87(8) | Fe1 | C3 | Li2 | 113.95(14) | |
| C5 | Fe1 | C4 | 41.03(8) | Fe1 | C3 | Li1 | 144.39(13) | |
| C5 | Fe1 | C6 | 121.14(8) | C2 | C3 | Fe1 | 67.23(10) | |
| C5 | Fe1 | C7 | 156.42(8) | C2 | C3 | Li2 | 98.28(15) | |
| C5 | Fe1 | C8 | 161.42(8) | C2 | C3 | Li1 | 147.59(17) | |
| C5 | Fe1 | C9 | 124.37(8) | C4 | C3 | Fe1 | 66.59(11) | |
| C5 | Fe1 | C10 | 107.50(8) | C4 | C3 | C2 | 102.41(16) | |
| C6 | Fe1 | C1 | 107.74(8) | C4 | C3 | Li2 | 157.19(17) | |
| C6 | Fe1 | C2 | 126.77(8) | C4 | C3 | Li1 | 99.91(15) | |
| C6 | Fe1 | C3 | 162.07(8) | Li2 | C3 | Li1 | 65.86(14) | |
| C6 | Fe1 | C10 | 40.47(9) | C3 | C4 | Fe1 | 72.86(11) | |
| C7 | Fe1 | C1 | 120.85(8) | C5 | C4 | Fe1 | 69.26(11) | |
| C7 | Fe1 | C2 | 108.81(8) | C5 | C4 | C3 | 112.03(17) | |
| C7 | Fe1 | C3 | 124.10(8) | C1 | C5 | Fe1 | 70.12(10) | |
| C7 | Fe1 | C6 | 40.58(9) | C4 | C5 | Fe1 | 69.71(11) | |
| C7 | Fe1 | C8 | 40.61(9) | C4 | C5 | C1 | 107.71(16) | |
| C7 | Fe1 | C9 | 68.47(8) | C7 | C6 | Fe1 | 69.59(12) | |
| C7 | Fe1 | C10 | 68.27(8) | C10 | C6 | Fe1 | 69.81(12) | |
| C8 | Fe1 | C1 | 156.00(8) | C10 | C6 | C7 | 108.17(18) | |
| C8 | Fe1 | C2 | 120.98(8) | C6 | C7 | Fe1 | 69.83(12) | |
| C8 | Fe1 | C3 | 105.90(8) | C6 | C7 | C8 | 107.91(18) | |
| C8 | Fe1 | C6 | 68.19(9) | C8 | C7 | Fe1 | 69.77(12) | |
| C8 | Fe1 | C10 | 68.25(8) | C7 | C8 | Fe1 | 69.62(11) | |
| C9 | Fe1 | C1 | 161.83(8) | C7 | C8 | C9 | 108.04(18) | |
| C9 | Fe1 | C2 | 155.15(8) | C9 | C8 | Fe1 | 69.60(11) | |
| C9 | Fe1 | C3 | 119.08(8) | C8 | C9 | Fe1 | 69.66(11) | |
| C9 | Fe1 | C6 | 68.27(8) | C10 | C9 | Fe1 | 69.82(11) | |
| C9 | Fe1 | C8 | 40.73(9) | C10 | C9 | C8 | 107.75(18) | |
| C9 | Fe1 | C10 | 40.59(8) | C6 | C10 | Fe1 | 69.73(11) | |
| C10 | Fe1 | C2 | 163.37(8) | C6 | C10 | C9 | 108.13(18) | |
| C10 | Fe1 | C3 | 154.91(8) | C9 | C10 | Fe1 | 69.59(11) | |
| C17 | Si2 | C29 | 112.86(9) | N1 | C14 | C2 | 112.16(15) | |
| C17 | Si2 | C28 | 109.61(9) | O1 | C33 | C34 | 114.0(2) | |
| C17 | Si2 | C27 | 109.70(10) | C36 | C35 | O1 | 110.6(4) | |
| C28 | Si2 | C29 | 107.71(11) | C36B | C35B | O1 | 102.9(12) | |
| C28 | Si2 | C27 | 107.36(11) | N1 | Li2 | Fe2 | 124.96(14) | |
| C27 | Si2 | C29 | 109.43(12) | N1 | Li2 | C19 | 130.46(19) | |
| C1 | Si1 | C13 | 108.67(9) | N1 | Li2 | C3 | 88.86(14) | |
| C1 | Si1 | C12 | 112.30(9) | C19 | Li2 | Fe2 | 46.74(8) | |
| C1 | Si1 | C11 | 109.73(10) | C19 | Li2 | C3 | 116.76(16) | |
| C13 | Si1 | C12 | 110.40(10) | C3 | Li2 | Fe2 | 145.87(15) | |
| C13 | Si1 | C11 | 108.19(11) | O1 | Li1 | N2 | 115.50(17) | |
| C11 | Si1 | C12 | 107.47(10) | O1 | Li1 | C19 | 119.09(18) | |
| C33 | O1 | C35 | 108.0(3) | O1 | Li1 | C3 | 109.33(17) | |
| C33 | O1 | C35B | 130.4(6) | N2 | Li1 | C19 | 87.08(14) | |
| C33 | O1 | Li1 | 118.10(17) | N2 | Li1 | C3 | 115.16(17) | |
| C35 | O1 | Li1 | 132.0(3) | C19 | Li1 | C3 | 109.32(16) |
| A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|---|---|
| Fe2 | C17 | C18 | C19 | -59.88(13) | C32 | N2 | C30 | C18 | 175.46(15) | |
| Fe2 | C17 | C18 | C30 | 121.30(18) | C29 | Si2 | C17 | Fe2 | -58.84(15) | |
| Fe2 | C17 | C21 | C20 | 60.09(13) | C29 | Si2 | C17 | C18 | 32.2(2) | |
| Fe2 | C18 | C19 | C20 | -58.40(12) | C29 | Si2 | C17 | C21 | -145.41(17) | |
| Fe2 | C18 | C19 | Li2 | 73.22(14) | C28 | Si2 | C17 | Fe2 | -178.89(11) | |
| Fe2 | C18 | C19 | Li1 | 142.50(13) | C28 | Si2 | C17 | C18 | -87.81(19) | |
| Fe2 | C18 | C30 | N2 | -141.12(14) | C28 | Si2 | C17 | C21 | 94.54(18) | |
| Fe2 | C19 | C20 | C21 | -57.62(13) | C27 | Si2 | C17 | Fe2 | 63.46(15) | |
| Fe2 | C20 | C21 | C17 | -59.79(13) | C27 | Si2 | C17 | C18 | 154.54(18) | |
| Fe2 | C22 | C23 | C24 | 60.06(13) | C27 | Si2 | C17 | C21 | -23.1(2) | |
| Fe2 | C22 | C26 | C25 | -59.30(14) | C1 | C2 | C3 | Fe1 | 57.66(14) | |
| Fe2 | C23 | C24 | C25 | 59.05(13) | C1 | C2 | C3 | C4 | -0.1(2) | |
| Fe2 | C24 | C25 | C26 | 59.70(14) | C1 | C2 | C3 | Li2 | 170.23(17) | |
| Fe2 | C25 | C26 | C22 | 59.16(13) | C1 | C2 | C3 | Li1 | -132.6(3) | |
| Fe1 | C1 | C2 | C3 | -59.36(14) | C1 | C2 | C14 | N1 | 163.28(17) | |
| Fe1 | C1 | C2 | C14 | 120.24(18) | C2 | C1 | C5 | Fe1 | -60.22(12) | |
| Fe1 | C1 | C5 | C4 | 59.83(13) | C2 | C1 | C5 | C4 | -0.4(2) | |
| Fe1 | C2 | C3 | C4 | -57.75(13) | C2 | C3 | C4 | Fe1 | 58.19(13) | |
| Fe1 | C2 | C3 | Li2 | 112.57(13) | C2 | C3 | C4 | C5 | -0.2(2) | |
| Fe1 | C2 | C3 | Li1 | 169.8(3) | C3 | C2 | C14 | N1 | -17.2(3) | |
| Fe1 | C2 | C14 | N1 | -109.79(17) | C3 | C4 | C5 | Fe1 | 60.44(14) | |
| Fe1 | C3 | C4 | C5 | -58.36(14) | C3 | C4 | C5 | C1 | 0.4(2) | |
| Fe1 | C4 | C5 | C1 | -60.09(13) | C5 | C1 | C2 | Fe1 | 59.66(12) | |
| Fe1 | C6 | C7 | C8 | 59.62(14) | C5 | C1 | C2 | C3 | 0.3(2) | |
| Fe1 | C6 | C10 | C9 | -59.20(14) | C5 | C1 | C2 | C14 | 179.90(17) | |
| Fe1 | C7 | C8 | C9 | 59.20(14) | C6 | C7 | C8 | Fe1 | -59.66(14) | |
| Fe1 | C8 | C9 | C10 | 59.68(14) | C6 | C7 | C8 | C9 | -0.5(2) | |
| Fe1 | C9 | C10 | C6 | 59.28(14) | C7 | C6 | C10 | Fe1 | 59.21(14) | |
| Si2 | C17 | C18 | Fe2 | -118.04(16) | C7 | C6 | C10 | C9 | 0.0(2) | |
| Si2 | C17 | C18 | C19 | -177.92(14) | C7 | C8 | C9 | Fe1 | -59.21(14) | |
| Si2 | C17 | C18 | C30 | 3.3(3) | C7 | C8 | C9 | C10 | 0.5(2) | |
| Si2 | C17 | C21 | Fe2 | 118.15(14) | C8 | C9 | C10 | Fe1 | -59.57(14) | |
| Si2 | C17 | C21 | C20 | 178.24(13) | C8 | C9 | C10 | C6 | -0.3(2) | |
| Si1 | C1 | C2 | Fe1 | -119.95(16) | C10 | C6 | C7 | Fe1 | -59.35(14) | |
| Si1 | C1 | C2 | C3 | -179.31(15) | C10 | C6 | C7 | C8 | 0.3(2) | |
| Si1 | C1 | C2 | C14 | 0.3(3) | C14 | C2 | C3 | Fe1 | -121.93(19) | |
| Si1 | C1 | C5 | Fe1 | 119.41(15) | C14 | C2 | C3 | C4 | -179.68(18) | |
| Si1 | C1 | C5 | C4 | 179.24(14) | C14 | C2 | C3 | Li2 | -9.4(2) | |
| C17 | C18 | C19 | Fe2 | 58.21(13) | C14 | C2 | C3 | Li1 | 47.8(4) | |
| C17 | C18 | C19 | C20 | -0.2(2) | C15 | N1 | C14 | C2 | -72.0(2) | |
| C17 | C18 | C19 | Li2 | 131.43(17) | C16 | N1 | C14 | C2 | 168.22(16) | |
| C17 | C18 | C19 | Li1 | -159.29(16) | C13 | Si1 | C1 | Fe1 | 69.22(14) | |
| C17 | C18 | C30 | N2 | 128.07(19) | C13 | Si1 | C1 | C2 | 160.85(18) | |
| C18 | C17 | C21 | Fe2 | -60.01(12) | C13 | Si1 | C1 | C5 | -18.69(19) | |
| C18 | C17 | C21 | C20 | 0.1(2) | C12 | Si1 | C1 | Fe1 | -53.21(14) | |
| C18 | C19 | C20 | Fe2 | 57.86(11) | C12 | Si1 | C1 | C2 | 38.4(2) | |
| C18 | C19 | C20 | C21 | 0.2(2) | C12 | Si1 | C1 | C5 | -141.12(16) | |
| C19 | C18 | C30 | N2 | -50.7(2) | C11 | Si1 | C1 | Fe1 | -172.67(12) | |
| C19 | C20 | C21 | Fe2 | 59.57(13) | C11 | Si1 | C1 | C2 | -81.04(19) | |
| C19 | C20 | C21 | C17 | -0.2(2) | C11 | Si1 | C1 | C5 | 99.42(18) | |
| C21 | C17 | C18 | Fe2 | 59.95(12) | C33 | O1 | C35 | C36 | 145.9(5) | |
| C21 | C17 | C18 | C19 | 0.1(2) | C33 | O1 | C35B | C36B | 77.0(12) | |
| C21 | C17 | C18 | C30 | -178.76(17) | C35 | O1 | C33 | C34 | 71.0(3) | |
| C22 | C23 | C24 | Fe2 | -59.84(13) | C35B | O1 | C33 | C34 | 67.8(8) | |
| C22 | C23 | C24 | C25 | -0.8(2) | Li2 | N1 | C14 | C2 | 33.8(2) | |
| C23 | C22 | C26 | Fe2 | 59.34(13) | Li2 | C19 | C20 | Fe2 | -73.66(15) | |
| C23 | C22 | C26 | C25 | 0.0(2) | Li2 | C19 | C20 | C21 | -131.29(18) | |
| C23 | C24 | C25 | Fe2 | -58.89(13) | Li2 | C3 | C4 | Fe1 | -96.4(5) | |
| C23 | C24 | C25 | C26 | 0.8(2) | Li2 | C3 | C4 | C5 | -154.8(4) | |
| C24 | C25 | C26 | Fe2 | -59.69(13) | Li1 | O1 | C33 | C34 | -95.2(3) | |
| C24 | C25 | C26 | C22 | -0.5(2) | Li1 | O1 | C35 | C36 | -50.5(7) | |
| C26 | C22 | C23 | Fe2 | -59.60(13) | Li1 | O1 | C35B | C36B | -118.8(9) | |
| C26 | C22 | C23 | C24 | 0.5(2) | Li1 | N2 | C30 | C18 | 47.29(18) | |
| C30 | C18 | C19 | Fe2 | -122.89(17) | Li1 | C19 | C20 | Fe2 | -165.3(3) | |
| C30 | C18 | C19 | C20 | 178.72(16) | Li1 | C19 | C20 | C21 | 137.1(3) | |
| C30 | C18 | C19 | Li2 | -49.7(2) | Li1 | C3 | C4 | Fe1 | -145.46(13) | |
| C30 | C18 | C19 | Li1 | 19.6(2) | Li1 | C3 | C4 | C5 | 156.18(16) | |
| C31 | N2 | C30 | C18 | -64.2(2) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| H20 | 6120 | 6943 | 4903 | 20 |
| H21 | 7021 | 6756 | 3600 | 22 |
| H22 | 7151 | 3441 | 3254 | 27 |
| H23 | 7460 | 2737 | 5021 | 24 |
| H24 | 5754 | 3488 | 5435 | 22 |
| H25 | 4435 | 4688 | 3935 | 25 |
| H26 | 5296 | 4636 | 2587 | 28 |
| H30A | 9034 | 3998 | 6542 | 22 |
| H30B | 10027 | 4548 | 6224 | 22 |
| H31A | 11219 | 6079 | 7213 | 42 |
| H31B | 10861 | 6668 | 8054 | 42 |
| H31C | 9995 | 6761 | 6864 | 42 |
| H32A | 11389 | 4298 | 7995 | 40 |
| H32B | 10341 | 3860 | 8300 | 40 |
| H32C | 11140 | 4893 | 8892 | 40 |
| H29A | 10599 | 3881 | 4980 | 48 |
| H29B | 10188 | 3618 | 3786 | 48 |
| H29C | 9297 | 3382 | 4332 | 48 |
| H28A | 10300 | 7027 | 4081 | 40 |
| H28B | 11122 | 6034 | 3998 | 40 |
| H28C | 11045 | 6295 | 5069 | 40 |
| H27A | 7730 | 4908 | 2365 | 52 |
| H27B | 8914 | 5238 | 2209 | 52 |
| H27C | 8106 | 6179 | 2399 | 52 |
| H4 | 9141 | 4310 | 9243 | 22 |
| H5 | 8321 | 3477 | 10445 | 21 |
| H6 | 6368 | 889 | 8773 | 28 |
| H7 | 5612 | 1659 | 6964 | 29 |
| H8 | 7416 | 2266 | 6634 | 29 |
| H9 | 9288 | 1895 | 8252 | 27 |
| H10 | 8632 | 1034 | 9567 | 27 |
| H14A | 4725 | 3573 | 7138 | 25 |
| H14B | 4506 | 4566 | 7784 | 25 |
| H15A | 4485 | 6418 | 7252 | 41 |
| H15B | 5103 | 6740 | 6492 | 41 |
| H15C | 5901 | 6287 | 7616 | 41 |
| H16A | 3648 | 4249 | 5497 | 41 |
| H16B | 3712 | 5529 | 5238 | 41 |
| H16C | 3141 | 5169 | 6023 | 41 |
| H13A | 6782 | 1631 | 10673 | 39 |
| H13B | 5855 | 1897 | 11177 | 39 |
| H13C | 7015 | 2655 | 11439 | 39 |
| H12A | 3664 | 2899 | 8362 | 33 |
| H12B | 3862 | 1914 | 9164 | 33 |
| H12C | 4540 | 1896 | 8410 | 33 |
| H11A | 5550 | 4752 | 10771 | 45 |
| H11B | 4404 | 4012 | 10618 | 45 |
| H11C | 4401 | 4780 | 9703 | 45 |
| H33A | 9343 | 7698 | 9832 | 38 |
| H33B | 9322 | 6382 | 9726 | 38 |
| H34A | 7290 | 6386 | 9498 | 64 |
| H34B | 7374 | 7694 | 9682 | 64 |
| H34C | 8154 | 6878 | 10589 | 64 |
| H35A | 7073 | 8254 | 7920 | 43 |
| H35B | 8308 | 8776 | 8711 | 43 |
| H35C | 7469 | 7850 | 6989 | 59 |
| H35D | 7191 | 8418 | 7893 | 59 |
| H36A | 7815 | 8196 | 6669 | 52 |
| H36B | 9064 | 8690 | 7458 | 52 |
| H36C | 7879 | 9432 | 7089 | 52 |
| H36D | 8524 | 9457 | 7364 | 95 |
| H36E | 9484 | 8494 | 7863 | 95 |
| H36F | 9022 | 9219 | 8569 | 95 |
| Atom | Occupancy | Atom | Occupancy | Atom | Occupancy | ||
|---|---|---|---|---|---|---|---|
| C35 | 0.672(12) | H35A | 0.672(12) | H35B | 0.672(12) | ||
| C35B | 0.328(12) | H35C | 0.328(12) | H35D | 0.328(12) | ||
| C36 | 0.672(12) | H36A | 0.672(12) | H36B | 0.672(12) | ||
| H36C | 0.672(12) | C36B | 0.328(12) | H36D | 0.328(12) | ||
| H36E | 0.328(12) | H36F | 0.328(12) |
Experimental
Single crystals of C36H58Fe2Li2N2OSi2 [mo_B0083_0m] were []. A suitable crystal was selected and [] on a 'Bruker APEX-II CCD' diffractometer. The crystal was kept at 100.0 K during data collection. Using Olex2 [1], the structure was solved with the XT [2] structure solution program using Direct Methods and refined with the XL [3] refinement package using Least Squares minimisation.
Crystal structure determination of [mo_B0083_0m]
Crystal Data for C36H58Fe2Li2N2OSi2 (M =716.60 g/mol): monoclinic, space group P21 (no. 4), a = 12.2143(5) Å, b = 12.0951(6) Å, c = 14.2648(7) Å, β = 113.848(2)°, V = 1927.46(16) Å3, Z = 2, T = 100.0 K, μ(MoKα) = 0.843 mm-1, Dcalc = 1.235 g/cm3, 56891 reflections measured (4.592° ≤ 2Θ ≤ 55.998°), 9291 unique (Rint = 0.0213, Rsigma = 0.0152) which were used in all calculations. The final R1 was 0.0180 (I > 2σ(I)) and wR2 was 0.0527 (all data).
Refinement model description
Number of restraints - 3, 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. Rigid bond restraints
C35B, C36B
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
C35, C36
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Others
Sof(C35B)=Sof(H35C)=Sof(H35D)=Sof(C36B)=Sof(H36D)=Sof(H36E)=Sof(H36F)=1-FVAR(1)
Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
C30(H30A,H30B), C14(H14A,H14B), C33(H33A,H33B), C35(H35A,H35B), C35B(H35C,H35D)
4.b Aromatic/amide H refined with riding coordinates:
C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C4(H4),
C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10)
4.c Idealised Me refined as rotating group:
C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C29(H29A,H29B,H29C), C28(H28A,H28B,
H28C), C27(H27A,H27B,H27C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C13(H13A,
H13B,H13C), C12(H12A,H12B,H12C), C11(H11A,H11B,H11C), C34(H34A,H34B,H34C),
C36(H36A,H36B,H36C), C36B(H36D,H36E,H36F)
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.