| Identification code | mo_B0425_0m |
| Empirical formula | C36H60Fe2N2OSi4 |
| Formula weight | 760.92 |
| Temperature/K | 99.99 |
| Crystal system | triclinic |
| Space group | P-1 |
| a/Å | 9.7419(18) |
| b/Å | 13.252(3) |
| c/Å | 17.228(3) |
| α/° | 98.993(5) |
| β/° | 98.779(5) |
| γ/° | 110.464(5) |
| Volume/Å3 | 2005.8(6) |
| Z | 2 |
| ρcalcg/cm3 | 1.260 |
| μ/mm‑1 | 0.872 |
| F(000) | 812.0 |
| Crystal size/mm3 | 0.294 × 0.26 × 0.07 |
| Radiation | MoKα (λ = 0.71073) |
| 2Θ range for data collection/° | 4.528 to 59.356 |
| Index ranges | -13 ≤ h ≤ 13, -18 ≤ k ≤ 18, -23 ≤ l ≤ 23 |
| Reflections collected | 101034 |
| Independent reflections | 11305 [Rint = 0.0374, Rsigma = 0.0219] |
| Data/restraints/parameters | 11305/0/421 |
| Goodness-of-fit on F2 | 1.132 |
| Final R indexes [I>=2σ (I)] | R1 = 0.0418, wR2 = 0.1106 |
| Final R indexes [all data] | R1 = 0.0512, wR2 = 0.1206 |
| Largest diff. peak/hole / e Å-3 | 2.20/-0.53 |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| Fe1 | 5097.8(3) | 1505.0(2) | 3171.4(2) | 13.24(8) |
| Fe2 | 7834.3(3) | 4151.3(2) | 6548.5(2) | 15.08(8) |
| Si1 | 4253.6(7) | 1766.8(5) | 1182.1(3) | 19.19(12) |
| Si2 | 2468.2(6) | 1524.1(4) | 4342.1(3) | 13.52(11) |
| Si3 | 3923.1(6) | 2710.4(4) | 6124.9(3) | 15.18(11) |
| Si4 | 9841.9(7) | 3996.6(5) | 8391.8(4) | 22.20(13) |
| O1 | 3758.3(16) | 2222.6(12) | 5166.6(8) | 19.3(3) |
| N1 | 740(2) | 678.0(16) | 1572.1(12) | 26.4(4) |
| N2 | 6362(2) | 3661.8(14) | 8791.7(10) | 17.9(3) |
| C1 | 3388(2) | 1933.7(15) | 3505.2(11) | 14.0(3) |
| C2 | 2999(2) | 1414.0(15) | 2659.2(11) | 14.3(3) |
| C3 | 4102(2) | 2028.0(16) | 2256.4(11) | 15.0(3) |
| C4 | 5183(2) | 2955.2(16) | 2873.9(12) | 16.9(4) |
| C5 | 4757(2) | 2894.4(16) | 3626.2(12) | 16.3(4) |
| C6 | 5593(2) | 571.2(19) | 3933.3(13) | 21.7(4) |
| C7 | 5053(3) | -62.5(18) | 3122.6(13) | 22.6(4) |
| C8 | 6045(3) | 482.8(19) | 2654.0(13) | 22.8(4) |
| C9 | 7180(2) | 1457(2) | 3173.6(14) | 23.4(4) |
| C10 | 6903(2) | 1511(2) | 3964.7(13) | 23.3(4) |
| C11 | 3248(3) | 2501(2) | 619.7(14) | 28.7(5) |
| C12 | 6305(3) | 2373(2) | 1164.9(15) | 30.6(5) |
| C13 | 3489(3) | 264(2) | 673.7(14) | 29.4(5) |
| C14 | 1608(2) | 415.2(17) | 2230.9(12) | 18.8(4) |
| C15 | 209(3) | 1520(2) | 1858.5(17) | 36.5(6) |
| C16 | -540(3) | -320(2) | 1119.9(19) | 44.6(7) |
| C17 | 1849(2) | 13.9(17) | 4315.4(14) | 23.2(4) |
| C18 | 813(2) | 1919.9(19) | 4336.6(13) | 22.2(4) |
| C19 | 2541(2) | 1672(2) | 6533.1(14) | 24.4(4) |
| C20 | 3520(3) | 3995.8(19) | 6244.8(14) | 26.3(5) |
| C21 | 5874(2) | 2923.3(15) | 6612.5(11) | 13.7(3) |
| C22 | 6771(2) | 3518.7(15) | 7407.6(11) | 13.2(3) |
| C23 | 8223(2) | 3438.2(16) | 7499.9(11) | 16.0(4) |
| C24 | 8208(2) | 2777.6(17) | 6747.9(12) | 18.5(4) |
| C25 | 6791(2) | 2465.1(16) | 6212.1(11) | 16.3(4) |
| C26 | 7254(3) | 5060.9(18) | 5790.3(13) | 25.3(4) |
| C27 | 7848(3) | 5713.6(17) | 6590.9(13) | 22.9(4) |
| C28 | 9338(3) | 5759.6(18) | 6832.2(14) | 25.1(4) |
| C29 | 9658(3) | 5137(2) | 6184.1(16) | 30.1(5) |
| C30 | 8363(3) | 4702(2) | 5537.6(14) | 29.4(5) |
| C31 | 9601(4) | 2933(2) | 9010.4(16) | 38.5(7) |
| C32 | 10055(3) | 5352.4(18) | 9013.2(13) | 23.3(4) |
| C33 | 11598(3) | 4197(3) | 7998.6(18) | 42.6(7) |
| C34 | 6274(2) | 4108.6(16) | 8066.2(11) | 16.2(4) |
| C35 | 5345(3) | 2506.3(19) | 8634.7(14) | 30.7(5) |
| C36 | 6025(3) | 4321.5(19) | 9442.0(12) | 23.4(4) |
| Atom | U11 | U22 | U33 | U23 | U13 | U12 |
|---|---|---|---|---|---|---|
| Fe1 | 11.21(13) | 14.71(14) | 13.87(13) | 3.75(10) | 2.06(9) | 5.15(10) |
| Fe2 | 16.34(14) | 14.70(14) | 13.20(13) | 3.71(10) | 5.12(10) | 3.75(11) |
| Si1 | 22.8(3) | 20.9(3) | 14.1(2) | 5.5(2) | 4.4(2) | 7.8(2) |
| Si2 | 10.8(2) | 15.8(2) | 14.2(2) | 4.50(18) | 2.60(18) | 5.03(19) |
| Si3 | 15.2(2) | 17.1(2) | 14.0(2) | 4.24(19) | 2.91(18) | 6.9(2) |
| Si4 | 21.1(3) | 25.2(3) | 18.0(3) | -2.5(2) | -2.4(2) | 12.0(2) |
| O1 | 15.4(7) | 24.9(7) | 14.7(6) | 3.0(5) | 1.1(5) | 5.9(6) |
| N1 | 24.2(9) | 24.6(9) | 25.5(9) | 1.8(7) | -5.1(7) | 9.7(8) |
| N2 | 25.1(9) | 17.8(8) | 11.9(7) | 3.6(6) | 6.6(6) | 8.5(7) |
| C1 | 12.9(8) | 13.7(8) | 15.4(8) | 3.1(6) | 2.7(6) | 5.4(7) |
| C2 | 13.4(8) | 13.8(8) | 15.9(8) | 4.0(6) | 2.3(6) | 5.5(7) |
| C3 | 16.7(9) | 14.4(8) | 14.9(8) | 4.6(6) | 3.1(7) | 6.8(7) |
| C4 | 16.5(9) | 13.2(8) | 19.7(9) | 4.5(7) | 3.4(7) | 4.1(7) |
| C5 | 14.9(9) | 14.3(8) | 18.1(9) | 1.9(7) | 2.6(7) | 4.8(7) |
| C6 | 23(1) | 29.4(11) | 21.3(10) | 13.1(8) | 6.6(8) | 16.4(9) |
| C7 | 24.8(10) | 21(1) | 26.6(10) | 8.3(8) | 4.7(8) | 13.4(8) |
| C8 | 26.3(11) | 28.8(11) | 21.6(10) | 7.6(8) | 6.5(8) | 19.4(9) |
| C9 | 15.9(9) | 33.3(12) | 27(1) | 11.9(9) | 6.7(8) | 13.5(9) |
| C10 | 16.3(9) | 32.4(11) | 21.7(10) | 6.1(8) | 0.3(7) | 11.8(9) |
| C11 | 34.8(12) | 32.9(12) | 22.2(10) | 13.5(9) | 5.2(9) | 14.7(10) |
| C12 | 27.7(12) | 40.9(14) | 25.7(11) | 12.7(10) | 12.9(9) | 11.1(10) |
| C13 | 34.9(13) | 28.4(11) | 22.5(10) | -0.8(9) | 0.9(9) | 14.5(10) |
| C14 | 16.6(9) | 16.5(9) | 18.6(9) | 3.9(7) | -0.5(7) | 2.5(7) |
| C15 | 31.2(13) | 42.4(15) | 35.4(13) | -2.0(11) | -5.3(10) | 23.3(12) |
| C16 | 38.0(15) | 33.4(14) | 44.0(16) | 0.0(12) | -18.6(12) | 7.1(12) |
| C17 | 21(1) | 18.5(9) | 29.7(11) | 9.0(8) | 7.1(8) | 4.9(8) |
| C18 | 15.8(9) | 30.3(11) | 26.5(10) | 12.6(8) | 7.8(8) | 12.0(8) |
| C19 | 17.2(10) | 30.3(11) | 24.9(10) | 10.3(9) | 6.8(8) | 5.8(9) |
| C20 | 31.2(12) | 26.5(11) | 27.0(11) | 6.4(9) | 5.6(9) | 18.1(10) |
| C21 | 16.2(8) | 11.2(8) | 13.3(8) | 3.6(6) | 3.8(6) | 4.0(7) |
| C22 | 16.1(8) | 12.1(8) | 12.0(8) | 3.7(6) | 4.2(6) | 5.5(7) |
| C23 | 18.2(9) | 16.0(8) | 13.7(8) | 1.6(7) | 3.1(7) | 7.2(7) |
| C24 | 19.9(9) | 19.9(9) | 16.5(9) | 0.4(7) | 3.7(7) | 10.3(8) |
| C25 | 17.9(9) | 14.8(8) | 14.3(8) | 0.4(6) | 3.3(7) | 5.5(7) |
| C26 | 29.8(11) | 22.6(10) | 21.7(10) | 12.3(8) | 3.8(8) | 5.7(9) |
| C27 | 28.4(11) | 16.0(9) | 25.9(10) | 8.9(8) | 8.6(8) | 7.6(8) |
| C28 | 23.6(11) | 20.1(10) | 26.1(10) | 10.2(8) | 4.7(8) | -0.2(8) |
| C29 | 24.9(11) | 31.4(12) | 39.8(13) | 17.7(10) | 20.5(10) | 8.3(10) |
| C30 | 40.7(13) | 26.7(11) | 21.2(10) | 10.4(9) | 15.8(9) | 7.8(10) |
| C31 | 57.6(17) | 26.9(12) | 27.1(12) | -0.8(9) | -13.7(11) | 24.0(12) |
| C32 | 23.5(10) | 20.9(10) | 18.7(9) | 0.3(8) | 1.4(8) | 3.7(8) |
| C33 | 24.3(12) | 59.6(19) | 37.0(14) | -10.5(13) | -1.1(10) | 20.2(12) |
| C34 | 19.2(9) | 17.5(9) | 13.8(8) | 3.4(7) | 5.1(7) | 8.9(7) |
| C35 | 47.9(15) | 20.6(10) | 18.6(10) | 6.1(8) | 11.5(10) | 4.7(10) |
| C36 | 29.2(11) | 28.4(11) | 14.3(9) | 2.5(8) | 8.1(8) | 12.6(9) |
| Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
|---|---|---|---|---|---|---|
| Fe1 | C1 | 2.0691(19) | Si4 | C23 | 1.867(2) | |
| Fe1 | C2 | 2.0539(19) | Si4 | C31 | 1.868(3) | |
| Fe1 | C3 | 2.0619(19) | Si4 | C32 | 1.867(2) | |
| Fe1 | C4 | 2.042(2) | Si4 | C33 | 1.884(3) | |
| Fe1 | C5 | 2.042(2) | N1 | C14 | 1.470(3) | |
| Fe1 | C6 | 2.054(2) | N1 | C15 | 1.437(3) | |
| Fe1 | C7 | 2.050(2) | N1 | C16 | 1.462(3) | |
| Fe1 | C8 | 2.056(2) | N2 | C34 | 1.468(2) | |
| Fe1 | C9 | 2.051(2) | N2 | C35 | 1.459(3) | |
| Fe1 | C10 | 2.053(2) | N2 | C36 | 1.461(3) | |
| Fe2 | C21 | 2.0624(19) | C1 | C2 | 1.441(3) | |
| Fe2 | C22 | 2.0530(18) | C1 | C5 | 1.445(3) | |
| Fe2 | C23 | 2.066(2) | C2 | C3 | 1.446(3) | |
| Fe2 | C24 | 2.046(2) | C2 | C14 | 1.506(3) | |
| Fe2 | C25 | 2.047(2) | C3 | C4 | 1.448(3) | |
| Fe2 | C26 | 2.055(2) | C4 | C5 | 1.425(3) | |
| Fe2 | C27 | 2.055(2) | C6 | C7 | 1.426(3) | |
| Fe2 | C28 | 2.049(2) | C6 | C10 | 1.424(3) | |
| Fe2 | C29 | 2.057(2) | C7 | C8 | 1.429(3) | |
| Fe2 | C30 | 2.059(2) | C8 | C9 | 1.425(3) | |
| Si1 | C3 | 1.867(2) | C9 | C10 | 1.425(3) | |
| Si1 | C11 | 1.875(2) | C21 | C22 | 1.441(3) | |
| Si1 | C12 | 1.882(3) | C21 | C25 | 1.441(3) | |
| Si1 | C13 | 1.873(2) | C22 | C23 | 1.442(3) | |
| Si2 | O1 | 1.6385(15) | C22 | C34 | 1.513(3) | |
| Si2 | C1 | 1.864(2) | C23 | C24 | 1.441(3) | |
| Si2 | C17 | 1.868(2) | C24 | C25 | 1.422(3) | |
| Si2 | C18 | 1.861(2) | C26 | C27 | 1.421(3) | |
| Si3 | O1 | 1.6376(15) | C26 | C30 | 1.422(4) | |
| Si3 | C19 | 1.870(2) | C27 | C28 | 1.424(3) | |
| Si3 | C20 | 1.865(2) | C28 | C29 | 1.422(3) | |
| Si3 | C21 | 1.861(2) | C29 | C30 | 1.424(4) |
| Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|
| C2 | Fe1 | C1 | 40.92(7) | C18 | Si2 | C17 | 108.55(10) | |
| C2 | Fe1 | C3 | 41.15(7) | O1 | Si3 | C19 | 109.91(9) | |
| C2 | Fe1 | C6 | 126.86(8) | O1 | Si3 | C20 | 109.22(9) | |
| C2 | Fe1 | C8 | 121.78(8) | O1 | Si3 | C21 | 104.67(8) | |
| C3 | Fe1 | C1 | 69.96(8) | C20 | Si3 | C19 | 108.66(11) | |
| C4 | Fe1 | C1 | 69.27(8) | C21 | Si3 | C19 | 110.02(9) | |
| C4 | Fe1 | C2 | 68.55(8) | C21 | Si3 | C20 | 114.28(10) | |
| C4 | Fe1 | C3 | 41.30(7) | C23 | Si4 | C31 | 107.98(11) | |
| C4 | Fe1 | C6 | 154.02(9) | C23 | Si4 | C32 | 113.60(10) | |
| C4 | Fe1 | C7 | 163.05(9) | C23 | Si4 | C33 | 107.24(11) | |
| C4 | Fe1 | C8 | 124.97(9) | C31 | Si4 | C33 | 108.69(15) | |
| C4 | Fe1 | C9 | 106.13(9) | C32 | Si4 | C31 | 110.97(11) | |
| C4 | Fe1 | C10 | 118.67(9) | C32 | Si4 | C33 | 108.21(12) | |
| C5 | Fe1 | C1 | 41.16(7) | Si3 | O1 | Si2 | 140.66(10) | |
| C5 | Fe1 | C2 | 68.51(8) | C15 | N1 | C14 | 112.37(19) | |
| C5 | Fe1 | C3 | 69.53(8) | C15 | N1 | C16 | 109.4(2) | |
| C5 | Fe1 | C4 | 40.85(8) | C16 | N1 | C14 | 109.85(19) | |
| C5 | Fe1 | C6 | 119.75(8) | C35 | N2 | C34 | 111.67(16) | |
| C5 | Fe1 | C7 | 155.47(9) | C35 | N2 | C36 | 109.97(18) | |
| C5 | Fe1 | C8 | 161.53(9) | C36 | N2 | C34 | 110.21(16) | |
| C5 | Fe1 | C9 | 123.90(9) | Si2 | C1 | Fe1 | 125.52(10) | |
| C5 | Fe1 | C10 | 106.14(9) | C2 | C1 | Fe1 | 68.98(10) | |
| C6 | Fe1 | C1 | 107.55(8) | C2 | C1 | Si2 | 130.93(14) | |
| C6 | Fe1 | C3 | 163.85(9) | C2 | C1 | C5 | 106.02(16) | |
| C6 | Fe1 | C8 | 68.25(9) | C5 | C1 | Fe1 | 68.41(11) | |
| C7 | Fe1 | C1 | 120.91(8) | C5 | C1 | Si2 | 123.02(14) | |
| C7 | Fe1 | C2 | 109.31(8) | C1 | C2 | Fe1 | 70.11(11) | |
| C7 | Fe1 | C3 | 125.98(8) | C1 | C2 | C3 | 110.21(16) | |
| C7 | Fe1 | C6 | 40.66(9) | C1 | C2 | C14 | 125.94(17) | |
| C7 | Fe1 | C8 | 40.71(9) | C3 | C2 | Fe1 | 69.72(11) | |
| C7 | Fe1 | C9 | 68.51(9) | C3 | C2 | C14 | 123.76(17) | |
| C7 | Fe1 | C10 | 68.46(9) | C14 | C2 | Fe1 | 129.53(14) | |
| C8 | Fe1 | C1 | 156.39(9) | Si1 | C3 | Fe1 | 125.91(10) | |
| C8 | Fe1 | C3 | 107.28(8) | C2 | C3 | Fe1 | 69.13(11) | |
| C9 | Fe1 | C1 | 161.52(9) | C2 | C3 | Si1 | 130.87(14) | |
| C9 | Fe1 | C2 | 155.66(8) | C2 | C3 | C4 | 105.72(16) | |
| C9 | Fe1 | C3 | 119.12(8) | C4 | C3 | Fe1 | 68.63(11) | |
| C9 | Fe1 | C6 | 68.31(9) | C4 | C3 | Si1 | 123.41(14) | |
| C9 | Fe1 | C8 | 40.58(9) | C3 | C4 | Fe1 | 70.07(11) | |
| C9 | Fe1 | C10 | 40.64(9) | C5 | C4 | Fe1 | 69.55(11) | |
| C10 | Fe1 | C1 | 124.62(8) | C5 | C4 | C3 | 109.07(17) | |
| C10 | Fe1 | C2 | 163.05(8) | C1 | C5 | Fe1 | 70.43(11) | |
| C10 | Fe1 | C3 | 153.86(9) | C4 | C5 | Fe1 | 69.60(11) | |
| C10 | Fe1 | C6 | 40.58(9) | C4 | C5 | C1 | 108.98(17) | |
| C10 | Fe1 | C8 | 68.28(9) | C7 | C6 | Fe1 | 69.54(12) | |
| C21 | Fe2 | C23 | 69.60(8) | C10 | C6 | Fe1 | 69.67(12) | |
| C22 | Fe2 | C21 | 41.00(7) | C10 | C6 | C7 | 108.18(19) | |
| C22 | Fe2 | C23 | 40.98(7) | C6 | C7 | Fe1 | 69.80(12) | |
| C22 | Fe2 | C26 | 128.32(9) | C6 | C7 | C8 | 107.8(2) | |
| C22 | Fe2 | C27 | 108.64(8) | C8 | C7 | Fe1 | 69.87(12) | |
| C22 | Fe2 | C29 | 152.79(9) | C7 | C8 | Fe1 | 69.42(12) | |
| C22 | Fe2 | C30 | 165.71(10) | C9 | C8 | Fe1 | 69.51(12) | |
| C24 | Fe2 | C21 | 69.04(8) | C9 | C8 | C7 | 108.03(19) | |
| C24 | Fe2 | C22 | 68.46(8) | C8 | C9 | Fe1 | 69.90(12) | |
| C24 | Fe2 | C23 | 41.03(7) | C8 | C9 | C10 | 108.0(2) | |
| C24 | Fe2 | C25 | 40.67(8) | C10 | C9 | Fe1 | 69.74(12) | |
| C24 | Fe2 | C26 | 151.56(9) | C6 | C10 | Fe1 | 69.75(12) | |
| C24 | Fe2 | C27 | 166.51(9) | C6 | C10 | C9 | 108.0(2) | |
| C24 | Fe2 | C28 | 128.26(9) | C9 | C10 | Fe1 | 69.62(12) | |
| C24 | Fe2 | C29 | 107.82(10) | N1 | C14 | C2 | 110.40(17) | |
| C24 | Fe2 | C30 | 117.87(9) | Si3 | C21 | Fe2 | 126.91(10) | |
| C25 | Fe2 | C21 | 41.07(7) | C22 | C21 | Fe2 | 69.15(10) | |
| C25 | Fe2 | C22 | 68.50(7) | C22 | C21 | Si3 | 130.74(14) | |
| C25 | Fe2 | C23 | 69.06(8) | C22 | C21 | C25 | 106.35(16) | |
| C25 | Fe2 | C26 | 118.00(9) | C25 | C21 | Fe2 | 68.88(11) | |
| C25 | Fe2 | C27 | 151.88(9) | C25 | C21 | Si3 | 122.92(14) | |
| C25 | Fe2 | C28 | 165.65(9) | C21 | C22 | Fe2 | 69.85(10) | |
| C25 | Fe2 | C29 | 127.27(9) | C21 | C22 | C23 | 109.62(16) | |
| C25 | Fe2 | C30 | 107.26(9) | C21 | C22 | C34 | 126.14(17) | |
| C26 | Fe2 | C21 | 107.39(9) | C23 | C22 | Fe2 | 69.99(11) | |
| C26 | Fe2 | C23 | 166.36(9) | C23 | C22 | C34 | 124.20(16) | |
| C26 | Fe2 | C27 | 40.45(9) | C34 | C22 | Fe2 | 128.27(13) | |
| C26 | Fe2 | C29 | 67.99(10) | Si4 | C23 | Fe2 | 128.36(11) | |
| C26 | Fe2 | C30 | 40.44(10) | C22 | C23 | Fe2 | 69.04(10) | |
| C27 | Fe2 | C21 | 118.05(9) | C22 | C23 | Si4 | 129.90(14) | |
| C27 | Fe2 | C23 | 128.24(8) | C24 | C23 | Fe2 | 68.75(11) | |
| C27 | Fe2 | C29 | 68.35(10) | C24 | C23 | Si4 | 123.85(15) | |
| C27 | Fe2 | C30 | 68.25(9) | C24 | C23 | C22 | 106.22(16) | |
| C28 | Fe2 | C21 | 152.52(9) | C23 | C24 | Fe2 | 70.22(11) | |
| C28 | Fe2 | C22 | 119.35(8) | C25 | C24 | Fe2 | 69.70(11) | |
| C28 | Fe2 | C23 | 108.24(9) | C25 | C24 | C23 | 109.01(17) | |
| C28 | Fe2 | C26 | 67.91(9) | C21 | C25 | Fe2 | 70.05(11) | |
| C28 | Fe2 | C27 | 40.61(9) | C24 | C25 | Fe2 | 69.64(11) | |
| C28 | Fe2 | C29 | 40.53(10) | C24 | C25 | C21 | 108.80(16) | |
| C28 | Fe2 | C30 | 68.06(10) | C27 | C26 | Fe2 | 69.80(12) | |
| C29 | Fe2 | C21 | 165.08(9) | C27 | C26 | C30 | 108.6(2) | |
| C29 | Fe2 | C23 | 118.27(10) | C30 | C26 | Fe2 | 69.94(13) | |
| C29 | Fe2 | C30 | 40.47(10) | C26 | C27 | Fe2 | 69.76(12) | |
| C30 | Fe2 | C21 | 126.98(9) | C26 | C27 | C28 | 107.4(2) | |
| C30 | Fe2 | C23 | 151.79(10) | C28 | C27 | Fe2 | 69.47(12) | |
| C3 | Si1 | C11 | 108.62(10) | C27 | C28 | Fe2 | 69.92(12) | |
| C3 | Si1 | C12 | 107.70(10) | C29 | C28 | Fe2 | 70.02(13) | |
| C3 | Si1 | C13 | 113.59(10) | C29 | C28 | C27 | 108.5(2) | |
| C11 | Si1 | C12 | 108.77(12) | C28 | C29 | Fe2 | 69.45(12) | |
| C13 | Si1 | C11 | 109.93(11) | C28 | C29 | C30 | 107.8(2) | |
| C13 | Si1 | C12 | 108.12(12) | C30 | C29 | Fe2 | 69.85(13) | |
| O1 | Si2 | C1 | 104.75(8) | C26 | C30 | Fe2 | 69.62(12) | |
| O1 | Si2 | C17 | 109.28(9) | C26 | C30 | C29 | 107.8(2) | |
| O1 | Si2 | C18 | 109.68(9) | C29 | C30 | Fe2 | 69.68(13) | |
| C1 | Si2 | C17 | 113.57(9) | N2 | C34 | C22 | 111.66(16) | |
| C18 | Si2 | C1 | 110.92(9) |
| A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|---|---|
| Fe1 | C1 | C2 | C3 | -58.27(13) | C10 | C6 | C7 | C8 | 0.6(2) | |
| Fe1 | C1 | C2 | C14 | 125.01(19) | C11 | Si1 | C3 | Fe1 | -176.19(12) | |
| Fe1 | C1 | C5 | C4 | 59.10(14) | C11 | Si1 | C3 | C2 | 91.2(2) | |
| Fe1 | C2 | C3 | Si1 | 120.01(17) | C11 | Si1 | C3 | C4 | -89.71(18) | |
| Fe1 | C2 | C3 | C4 | -59.18(13) | C12 | Si1 | C3 | Fe1 | -58.56(15) | |
| Fe1 | C2 | C14 | N1 | -145.14(16) | C12 | Si1 | C3 | C2 | -151.13(19) | |
| Fe1 | C3 | C4 | C5 | -58.77(14) | C12 | Si1 | C3 | C4 | 27.9(2) | |
| Fe1 | C4 | C5 | C1 | -59.61(14) | C13 | Si1 | C3 | Fe1 | 61.15(16) | |
| Fe1 | C6 | C7 | C8 | 59.80(14) | C13 | Si1 | C3 | C2 | -31.4(2) | |
| Fe1 | C6 | C10 | C9 | -59.34(15) | C13 | Si1 | C3 | C4 | 147.64(17) | |
| Fe1 | C7 | C8 | C9 | 58.98(15) | C14 | C2 | C3 | Fe1 | -124.70(18) | |
| Fe1 | C8 | C9 | C10 | 59.54(15) | C14 | C2 | C3 | Si1 | -4.7(3) | |
| Fe1 | C9 | C10 | C6 | 59.42(15) | C14 | C2 | C3 | C4 | 176.13(18) | |
| Fe2 | C21 | C22 | C23 | -58.81(13) | C15 | N1 | C14 | C2 | -62.6(3) | |
| Fe2 | C21 | C22 | C34 | 123.30(18) | C16 | N1 | C14 | C2 | 175.4(2) | |
| Fe2 | C21 | C25 | C24 | 59.03(14) | C17 | Si2 | O1 | Si3 | -82.54(17) | |
| Fe2 | C22 | C23 | Si4 | 123.08(17) | C17 | Si2 | C1 | Fe1 | -49.38(15) | |
| Fe2 | C22 | C23 | C24 | -58.95(14) | C17 | Si2 | C1 | C2 | 42.7(2) | |
| Fe2 | C22 | C34 | N2 | -147.67(14) | C17 | Si2 | C1 | C5 | -135.07(16) | |
| Fe2 | C23 | C24 | C25 | -59.08(14) | C18 | Si2 | O1 | Si3 | 36.35(18) | |
| Fe2 | C24 | C25 | C21 | -59.28(13) | C18 | Si2 | C1 | Fe1 | -171.95(11) | |
| Fe2 | C26 | C27 | C28 | 59.54(14) | C18 | Si2 | C1 | C2 | -79.9(2) | |
| Fe2 | C26 | C30 | C29 | -59.45(16) | C18 | Si2 | C1 | C5 | 102.36(17) | |
| Fe2 | C27 | C28 | C29 | 59.62(15) | C19 | Si3 | O1 | Si2 | 41.26(19) | |
| Fe2 | C28 | C29 | C30 | 59.57(16) | C19 | Si3 | C21 | Fe2 | -168.59(12) | |
| Fe2 | C29 | C30 | C26 | 59.41(15) | C19 | Si3 | C21 | C22 | -75.2(2) | |
| Si1 | C3 | C4 | Fe1 | -119.76(14) | C19 | Si3 | C21 | C25 | 104.31(17) | |
| Si1 | C3 | C4 | C5 | -178.53(14) | C20 | Si3 | O1 | Si2 | -77.86(18) | |
| Si2 | C1 | C2 | Fe1 | -119.38(17) | C20 | Si3 | C21 | Fe2 | -46.05(15) | |
| Si2 | C1 | C2 | C3 | -177.65(15) | C20 | Si3 | C21 | C22 | 47.4(2) | |
| Si2 | C1 | C2 | C14 | 5.6(3) | C20 | Si3 | C21 | C25 | -133.15(16) | |
| Si2 | C1 | C5 | Fe1 | 119.21(14) | C21 | Si3 | O1 | Si2 | 159.37(15) | |
| Si2 | C1 | C5 | C4 | 178.31(14) | C21 | C22 | C23 | Fe2 | 58.73(13) | |
| Si3 | C21 | C22 | Fe2 | -121.34(16) | C21 | C22 | C23 | Si4 | -178.18(15) | |
| Si3 | C21 | C22 | C23 | 179.85(15) | C21 | C22 | C23 | C24 | -0.2(2) | |
| Si3 | C21 | C22 | C34 | 2.0(3) | C21 | C22 | C34 | N2 | 120.5(2) | |
| Si3 | C21 | C25 | Fe2 | 121.12(14) | C22 | C21 | C25 | Fe2 | -59.28(12) | |
| Si3 | C21 | C25 | C24 | -179.85(14) | C22 | C21 | C25 | C24 | -0.2(2) | |
| Si4 | C23 | C24 | Fe2 | -122.74(15) | C22 | C23 | C24 | Fe2 | 59.14(13) | |
| Si4 | C23 | C24 | C25 | 178.18(15) | C22 | C23 | C24 | C25 | 0.1(2) | |
| O1 | Si2 | C1 | Fe1 | 69.79(13) | C23 | C22 | C34 | N2 | -57.1(2) | |
| O1 | Si2 | C1 | C2 | 161.83(17) | C23 | C24 | C25 | Fe2 | 59.40(14) | |
| O1 | Si2 | C1 | C5 | -15.90(18) | C23 | C24 | C25 | C21 | 0.1(2) | |
| O1 | Si3 | C21 | Fe2 | 73.38(13) | C25 | C21 | C22 | Fe2 | 59.10(13) | |
| O1 | Si3 | C21 | C22 | 166.78(17) | C25 | C21 | C22 | C23 | 0.3(2) | |
| O1 | Si3 | C21 | C25 | -13.72(18) | C25 | C21 | C22 | C34 | -177.60(17) | |
| C1 | Si2 | O1 | Si3 | 155.45(15) | C26 | C27 | C28 | Fe2 | -59.72(14) | |
| C1 | C2 | C3 | Fe1 | 58.49(13) | C26 | C27 | C28 | C29 | -0.1(2) | |
| C1 | C2 | C3 | Si1 | 178.51(15) | C27 | C26 | C30 | Fe2 | 59.29(15) | |
| C1 | C2 | C3 | C4 | -0.7(2) | C27 | C26 | C30 | C29 | -0.2(2) | |
| C1 | C2 | C14 | N1 | 121.8(2) | C27 | C28 | C29 | Fe2 | -59.56(15) | |
| C2 | C1 | C5 | Fe1 | -59.00(13) | C27 | C28 | C29 | C30 | 0.0(3) | |
| C2 | C1 | C5 | C4 | 0.1(2) | C28 | C29 | C30 | Fe2 | -59.32(16) | |
| C2 | C3 | C4 | Fe1 | 59.50(13) | C28 | C29 | C30 | C26 | 0.1(3) | |
| C2 | C3 | C4 | C5 | 0.7(2) | C30 | C26 | C27 | Fe2 | -59.38(15) | |
| C3 | C2 | C14 | N1 | -54.5(3) | C30 | C26 | C27 | C28 | 0.2(2) | |
| C3 | C4 | C5 | Fe1 | 59.08(14) | C31 | Si4 | C23 | Fe2 | -177.00(14) | |
| C3 | C4 | C5 | C1 | -0.5(2) | C31 | Si4 | C23 | C22 | 89.2(2) | |
| C5 | C1 | C2 | Fe1 | 58.64(13) | C31 | Si4 | C23 | C24 | -88.5(2) | |
| C5 | C1 | C2 | C3 | 0.4(2) | C32 | Si4 | C23 | Fe2 | 59.48(16) | |
| C5 | C1 | C2 | C14 | -176.35(18) | C32 | Si4 | C23 | C22 | -34.4(2) | |
| C6 | C7 | C8 | Fe1 | -59.76(14) | C32 | Si4 | C23 | C24 | 148.00(17) | |
| C6 | C7 | C8 | C9 | -0.8(2) | C33 | Si4 | C23 | Fe2 | -60.03(17) | |
| C7 | C6 | C10 | Fe1 | 59.07(14) | C33 | Si4 | C23 | C22 | -153.9(2) | |
| C7 | C6 | C10 | C9 | -0.3(2) | C33 | Si4 | C23 | C24 | 28.5(2) | |
| C7 | C8 | C9 | Fe1 | -58.92(15) | C34 | C22 | C23 | Fe2 | -123.33(18) | |
| C7 | C8 | C9 | C10 | 0.6(2) | C34 | C22 | C23 | Si4 | -0.2(3) | |
| C8 | C9 | C10 | Fe1 | -59.64(15) | C34 | C22 | C23 | C24 | 177.72(18) | |
| C8 | C9 | C10 | C6 | -0.2(2) | C35 | N2 | C34 | C22 | -63.3(2) | |
| C10 | C6 | C7 | Fe1 | -59.15(15) | C36 | N2 | C34 | C22 | 174.18(17) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| H4 | 6040 | 3514 | 2791 | 20 |
| H5 | 5288 | 3403 | 4126 | 20 |
| H6 | 5154 | 397 | 4376 | 26 |
| H7 | 4187 | -728 | 2929 | 27 |
| H8 | 5963 | 239 | 2094 | 27 |
| H9 | 7982 | 1980 | 3020 | 28 |
| H10 | 7489 | 2074 | 4431 | 28 |
| H11A | 2181 | 2201 | 633 | 43 |
| H11B | 3350 | 2392 | 59 | 43 |
| H11C | 3688 | 3292 | 873 | 43 |
| H12A | 6706 | 3173 | 1385 | 46 |
| H12B | 6421 | 2225 | 608 | 46 |
| H12C | 6855 | 2035 | 1492 | 46 |
| H13A | 3970 | -124 | 991 | 44 |
| H13B | 3696 | 181 | 133 | 44 |
| H13C | 2401 | -52 | 630 | 44 |
| H14A | 1898 | -197 | 2010 | 23 |
| H14B | 979 | 170 | 2618 | 23 |
| H15A | -489 | 1251 | 2203 | 55 |
| H15B | -311 | 1698 | 1398 | 55 |
| H15C | 1064 | 2185 | 2170 | 55 |
| H16A | -1177 | -620 | 1484 | 67 |
| H16B | -174 | -872 | 884 | 67 |
| H16C | -1125 | -137 | 689 | 67 |
| H17A | 2701 | -213 | 4295 | 35 |
| H17B | 1042 | -404 | 3836 | 35 |
| H17C | 1480 | -133 | 4801 | 35 |
| H18A | 425 | 1783 | 4819 | 33 |
| H18B | 27 | 1479 | 3854 | 33 |
| H18C | 1115 | 2707 | 4334 | 33 |
| H19A | 1518 | 1523 | 6244 | 37 |
| H19B | 2658 | 1963 | 7109 | 37 |
| H19C | 2723 | 984 | 6460 | 37 |
| H20A | 4217 | 4539 | 6017 | 39 |
| H20B | 3648 | 4303 | 6819 | 39 |
| H20C | 2485 | 3821 | 5962 | 39 |
| H24 | 9016 | 2582 | 6629 | 22 |
| H25 | 6496 | 2026 | 5678 | 20 |
| H26 | 6278 | 4892 | 5476 | 30 |
| H27 | 7345 | 6056 | 6907 | 27 |
| H28 | 10005 | 6142 | 7340 | 30 |
| H29 | 10573 | 5030 | 6183 | 36 |
| H30 | 8259 | 4253 | 5028 | 35 |
| H31A | 10519 | 3149 | 9429 | 58 |
| H31B | 9407 | 2216 | 8663 | 58 |
| H31C | 8751 | 2877 | 9264 | 58 |
| H32A | 10113 | 5882 | 8669 | 35 |
| H32B | 10977 | 5634 | 9438 | 35 |
| H32C | 9187 | 5253 | 9259 | 35 |
| H33A | 11726 | 4742 | 7664 | 64 |
| H33B | 11512 | 3491 | 7674 | 64 |
| H33C | 12470 | 4460 | 8453 | 64 |
| H34A | 6919 | 4906 | 8206 | 19 |
| H34B | 5226 | 4031 | 7865 | 19 |
| H35A | 4304 | 2448 | 8483 | 46 |
| H35B | 5476 | 2223 | 9122 | 46 |
| H35C | 5571 | 2071 | 8194 | 46 |
| H36A | 4999 | 4289 | 9278 | 35 |
| H36B | 6737 | 5091 | 9558 | 35 |
| H36C | 6112 | 4027 | 9927 | 35 |
Experimental
Single crystals of C36H60Fe2N2OSi4 [mo_B0425_0m] were []. A suitable crystal was selected and [] on a Bruker D8 Venture diffractometer. The crystal was kept at 99.99 K during data collection. Using Olex2 [1], the structure was solved with the ShelXT [2] structure solution program using Direct Methods and refined with the XL [3] refinement package using Least Squares minimisation.
Crystal structure determination of [mo_B0425_0m]
Crystal Data for C36H60Fe2N2OSi4 (M =760.92 g/mol): triclinic, space group P-1 (no. 2), a = 9.7419(18) Å, b = 13.252(3) Å, c = 17.228(3) Å, α = 98.993(5)°, β = 98.779(5)°, γ = 110.464(5)°, V = 2005.8(6) Å3, Z = 2, T = 99.99 K, μ(MoKα) = 0.872 mm-1, Dcalc = 1.260 g/cm3, 101034 reflections measured (4.528° ≤ 2Θ ≤ 59.356°), 11305 unique (Rint = 0.0374, Rsigma = 0.0219) which were used in all calculations. The final R1 was 0.0418 (I > 2σ(I)) and wR2 was 0.1206 (all data).
Refinement model description
Number of restraints - 0, number of constraints - unknown.
Details:
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
C14(H14A,H14B), C34(H34A,H34B)
2.b Aromatic/amide H refined with riding coordinates:
C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C24(H24), C25(H25),
C26(H26), C27(H27), C28(H28), C29(H29), C30(H30)
2.c Idealised Me refined as rotating group:
C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,
H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,
H19B,H19C), C20(H20A,H20B,H20C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C),
C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C)
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.