| Identification code | 3118 |
| Empirical formula | C46H52Cl2Fe4N2O4Si2Zn2 |
| Formula weight | 1178.11 |
| Temperature/K | 173.15 |
| Crystal system | orthorhombic |
| Space group | Pbcn |
| a/Å | 15.0001(6) |
| b/Å | 11.2793(5) |
| c/Å | 27.6027(12) |
| α/° | 90 |
| β/° | 90 |
| γ/° | 90 |
| Volume/Å3 | 4670.1(3) |
| Z | 4 |
| ρcalcg/cm3 | 1.676 |
| μ/mm‑1 | 2.431 |
| F(000) | 2400.0 |
| Crystal size/mm3 | 0.2 × 0.1 × 0.05 |
| Radiation | MoKα (λ = 0.71073) |
| 2Θ range for data collection/° | 4.518 to 53.998 |
| Index ranges | -19 ≤ h ≤ 19, -13 ≤ k ≤ 14, -35 ≤ l ≤ 34 |
| Reflections collected | 35271 |
| Independent reflections | 5097 [Rint = 0.0431, Rsigma = 0.0282] |
| Data/restraints/parameters | 5097/1/287 |
| Goodness-of-fit on F2 | 1.082 |
| Final R indexes [I>=2σ (I)] | R1 = 0.0449, wR2 = 0.1050 |
| Final R indexes [all data] | R1 = 0.0607, wR2 = 0.1138 |
| Largest diff. peak/hole / e Å-3 | 0.73/-0.61 |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| Zn1 | 5000 | 3675.8(5) | 2500 | 21.20(14) |
| Zn2 | 5000 | 1082.3(5) | 2500 | 24.77(15) |
| Fe1 | 6088.8(4) | 4935.5(5) | 4123.2(2) | 26.12(14) |
| Fe2 | 3988.0(4) | 294.5(5) | 4131.9(2) | 32.05(16) |
| Cl1 | 3815.8(8) | 53.0(12) | 2280.8(4) | 51.7(3) |
| Si1 | 5137.5(6) | 2544.3(8) | 3535.4(4) | 21.1(2) |
| O1 | 4873.8(15) | 2388(2) | 2972.8(9) | 23.8(5) |
| O2 | 6095.5(17) | 1893(2) | 3646.1(10) | 30.7(6) |
| N1 | 6188(2) | 4558(3) | 2522.0(11) | 30.6(7) |
| C1 | 5261(2) | 4163(3) | 3634.2(12) | 21.7(7) |
| C2 | 5893(2) | 4930(3) | 3397.3(12) | 25.4(8) |
| C3 | 5772(3) | 6095(3) | 3583.7(14) | 33.1(9) |
| C4 | 5075(3) | 6066(3) | 3928.2(15) | 34.9(9) |
| C5 | 4761(2) | 4890(3) | 3957.5(13) | 26.4(8) |
| C6 | 6646(3) | 3609(4) | 4517.5(14) | 36.7(10) |
| C7 | 7298(3) | 4183(5) | 4245.7(16) | 45.7(11) |
| C8 | 7314(3) | 5372(5) | 4388.0(18) | 56.6(14) |
| C9 | 6658(4) | 5522(4) | 4747.5(16) | 53.1(13) |
| C10 | 6247(3) | 4426(4) | 4826.3(14) | 40.9(10) |
| C11 | 6554(2) | 4533(4) | 3030.0(13) | 29.8(8) |
| C12 | 6144(3) | 5802(4) | 2348.9(16) | 49.4(13) |
| C13 | 6821(3) | 3892(5) | 2201.3(16) | 50.4(13) |
| C14 | 4226(2) | 2004(3) | 3918.2(14) | 27.0(8) |
| C15 | 4196(3) | 1920(3) | 4430.6(15) | 36.4(10) |
| C16 | 3349(3) | 1472(4) | 4571.6(19) | 50.2(13) |
| C17 | 2848(3) | 1264(4) | 4149(2) | 54.6(15) |
| C18 | 3373(3) | 1583(4) | 3743.3(17) | 38.4(10) |
| C19 | 4965(3) | -782(4) | 3874.2(19) | 46.0(12) |
| C20 | 4939(4) | -838(4) | 4378.2(19) | 49.8(12) |
| C21 | 4100(5) | -1226(5) | 4509(2) | 70.1(19) |
| C22 | 3602(4) | -1405(4) | 4094(4) | 88(3) |
| C23 | 4145(5) | -1138(4) | 3698(2) | 70.3(19) |
| Atom | U11 | U22 | U33 | U23 | U13 | U12 |
|---|---|---|---|---|---|---|
| Zn1 | 20.8(3) | 25.8(3) | 17.1(3) | 0 | 0.3(2) | 0 |
| Zn2 | 27.1(3) | 24.8(3) | 22.4(3) | 0 | -1.8(2) | 0 |
| Fe1 | 36.5(3) | 24.7(3) | 17.2(3) | -2.4(2) | -1.1(2) | -2.4(2) |
| Fe2 | 34.0(3) | 21.6(3) | 40.5(4) | 9.7(2) | 7.6(2) | 2.5(2) |
| Cl1 | 45.8(6) | 66.5(8) | 42.8(6) | 10.1(6) | -5.2(5) | -29.9(6) |
| Si1 | 23.8(5) | 21.3(5) | 18.1(5) | 0.9(4) | 0.4(4) | 2.4(4) |
| O1 | 28.9(13) | 24.5(13) | 18.1(12) | 0.3(10) | -0.9(10) | 0.2(10) |
| O2 | 27.3(13) | 34.1(15) | 30.7(15) | -5.4(12) | -5.1(11) | 7.8(11) |
| N1 | 31.0(16) | 42.6(19) | 18.2(15) | -3.8(14) | 4.9(12) | -14.1(15) |
| C1 | 24.7(17) | 24.9(18) | 15.7(16) | 1.8(14) | -1.5(13) | 1.9(14) |
| C2 | 33.2(19) | 26.3(18) | 16.8(17) | 1.2(14) | -0.9(14) | -4.6(16) |
| C3 | 53(2) | 21.3(18) | 25(2) | 1.9(16) | -1.6(18) | -5.0(17) |
| C4 | 52(3) | 23.2(19) | 29(2) | -1.2(17) | 0.4(18) | 11.5(18) |
| C5 | 31.7(19) | 25.8(19) | 21.7(18) | 1.5(15) | 4.0(15) | 10.0(15) |
| C6 | 44(2) | 39(2) | 27(2) | 2.0(18) | -13.4(18) | 5.9(19) |
| C7 | 32(2) | 72(3) | 32(2) | -6(2) | -9.2(18) | 8(2) |
| C8 | 57(3) | 68(3) | 44(3) | 9(3) | -19(2) | -27(3) |
| C9 | 84(4) | 47(3) | 29(2) | -16(2) | -24(2) | 6(3) |
| C10 | 47(2) | 57(3) | 18(2) | 1(2) | -4.6(17) | 7(2) |
| C11 | 26.1(18) | 42(2) | 21.3(19) | -4.1(17) | 0.8(14) | -10.9(16) |
| C12 | 62(3) | 57(3) | 30(2) | 8(2) | -1(2) | -28(3) |
| C13 | 28(2) | 92(4) | 31(2) | -26(2) | 9.2(18) | -16(2) |
| C14 | 33.0(19) | 18.3(17) | 30(2) | 4.9(15) | 6.5(16) | 5.3(15) |
| C15 | 54(3) | 25(2) | 31(2) | 2.4(17) | 14.0(19) | 5.7(18) |
| C16 | 62(3) | 36(2) | 53(3) | 13(2) | 34(3) | 12(2) |
| C17 | 37(2) | 35(2) | 92(4) | 26(3) | 25(3) | 8(2) |
| C18 | 34(2) | 30(2) | 51(3) | 14(2) | 2.1(19) | 5.0(17) |
| C19 | 59(3) | 23(2) | 56(3) | 7(2) | 20(2) | 13(2) |
| C20 | 66(3) | 33(2) | 50(3) | 0(2) | -10(2) | 19(2) |
| C21 | 91(4) | 41(3) | 78(4) | 38(3) | 45(4) | 29(3) |
| C22 | 46(3) | 21(2) | 197(9) | 12(4) | -3(4) | -8(2) |
| C23 | 116(5) | 31(3) | 64(4) | -9(3) | -37(4) | 17(3) |
| Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
|---|---|---|---|---|---|---|
| Zn1 | Zn2 | 2.9253(9) | Si1 | O1 | 1.612(3) | |
| Zn1 | O11 | 1.962(2) | Si1 | O2 | 1.643(3) | |
| Zn1 | O1 | 1.962(2) | Si1 | C1 | 1.856(4) | |
| Zn1 | N1 | 2.042(3) | Si1 | C14 | 1.832(4) | |
| Zn1 | N11 | 2.042(3) | N1 | C11 | 1.506(5) | |
| Zn2 | Cl11 | 2.2067(11) | N1 | C12 | 1.483(6) | |
| Zn2 | Cl1 | 2.2067(11) | N1 | C13 | 1.499(5) | |
| Zn2 | O11 | 1.977(2) | C1 | C2 | 1.440(5) | |
| Zn2 | O1 | 1.977(2) | C1 | C5 | 1.425(5) | |
| Fe1 | C1 | 2.030(3) | C2 | C3 | 1.422(5) | |
| Fe1 | C2 | 2.025(3) | C2 | C11 | 1.487(5) | |
| Fe1 | C3 | 2.038(4) | C3 | C4 | 1.414(6) | |
| Fe1 | C4 | 2.057(4) | C4 | C5 | 1.410(5) | |
| Fe1 | C5 | 2.044(4) | C6 | C7 | 1.392(6) | |
| Fe1 | C6 | 2.030(4) | C6 | C10 | 1.390(6) | |
| Fe1 | C7 | 2.031(4) | C7 | C8 | 1.398(7) | |
| Fe1 | C8 | 2.038(5) | C8 | C9 | 1.407(7) | |
| Fe1 | C9 | 2.034(4) | C9 | C10 | 1.399(7) | |
| Fe1 | C10 | 2.038(4) | C14 | C15 | 1.418(6) | |
| Fe2 | C14 | 2.048(4) | C14 | C18 | 1.447(6) | |
| Fe2 | C15 | 2.034(4) | C15 | C16 | 1.421(6) | |
| Fe2 | C16 | 2.039(4) | C16 | C17 | 1.408(8) | |
| Fe2 | C17 | 2.030(4) | C17 | C18 | 1.416(6) | |
| Fe2 | C18 | 2.028(4) | C19 | C20 | 1.393(7) | |
| Fe2 | C19 | 2.032(4) | C19 | C23 | 1.383(8) | |
| Fe2 | C20 | 2.032(4) | C20 | C21 | 1.380(8) | |
| Fe2 | C21 | 2.012(5) | C21 | C22 | 1.381(10) | |
| Fe2 | C22 | 2.005(5) | C22 | C23 | 1.397(9) | |
| Fe2 | C23 | 2.025(5) |
| Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|
| O11 | Zn1 | Zn2 | 42.24(7) | C22 | Fe2 | C18 | 121.8(3) | |
| O1 | Zn1 | Zn2 | 42.24(7) | C22 | Fe2 | C19 | 67.6(2) | |
| O1 | Zn1 | O11 | 84.49(14) | C22 | Fe2 | C20 | 67.6(2) | |
| O11 | Zn1 | N11 | 115.17(12) | C22 | Fe2 | C21 | 40.2(3) | |
| O1 | Zn1 | N11 | 107.24(11) | C22 | Fe2 | C23 | 40.6(3) | |
| O11 | Zn1 | N1 | 107.24(11) | C23 | Fe2 | C14 | 124.1(2) | |
| O1 | Zn1 | N1 | 115.16(12) | C23 | Fe2 | C15 | 160.2(3) | |
| N11 | Zn1 | Zn2 | 119.17(10) | C23 | Fe2 | C16 | 157.9(3) | |
| N1 | Zn1 | Zn2 | 119.17(10) | C23 | Fe2 | C17 | 122.8(3) | |
| N11 | Zn1 | N1 | 121.7(2) | C23 | Fe2 | C18 | 108.2(2) | |
| Cl1 | Zn2 | Zn1 | 121.74(4) | C23 | Fe2 | C19 | 39.9(2) | |
| Cl11 | Zn2 | Zn1 | 121.74(4) | C23 | Fe2 | C20 | 67.3(2) | |
| Cl1 | Zn2 | Cl11 | 116.51(8) | O1 | Si1 | O2 | 110.18(14) | |
| O11 | Zn2 | Zn1 | 41.83(7) | O1 | Si1 | C1 | 105.86(14) | |
| O1 | Zn2 | Zn1 | 41.83(7) | O1 | Si1 | C14 | 109.64(16) | |
| O1 | Zn2 | Cl11 | 106.74(7) | O2 | Si1 | C1 | 109.00(15) | |
| O11 | Zn2 | Cl11 | 119.73(8) | O2 | Si1 | C14 | 113.38(16) | |
| O1 | Zn2 | Cl1 | 119.73(8) | C14 | Si1 | C1 | 108.48(16) | |
| O11 | Zn2 | Cl1 | 106.74(7) | Zn1 | O1 | Zn2 | 95.92(11) | |
| O11 | Zn2 | O1 | 83.67(14) | Si1 | O1 | Zn1 | 122.45(14) | |
| C1 | Fe1 | C3 | 69.31(15) | Si1 | O1 | Zn2 | 133.92(14) | |
| C1 | Fe1 | C4 | 68.88(15) | C11 | N1 | Zn1 | 109.6(2) | |
| C1 | Fe1 | C5 | 40.94(14) | C12 | N1 | Zn1 | 114.3(3) | |
| C1 | Fe1 | C7 | 118.53(17) | C12 | N1 | C11 | 109.5(3) | |
| C1 | Fe1 | C8 | 153.32(19) | C12 | N1 | C13 | 108.2(3) | |
| C1 | Fe1 | C9 | 163.66(19) | C13 | N1 | Zn1 | 106.9(2) | |
| C1 | Fe1 | C10 | 125.70(17) | C13 | N1 | C11 | 108.1(3) | |
| C2 | Fe1 | C1 | 41.60(14) | Si1 | C1 | Fe1 | 125.51(18) | |
| C2 | Fe1 | C3 | 40.98(15) | C2 | C1 | Fe1 | 69.0(2) | |
| C2 | Fe1 | C4 | 68.62(16) | C2 | C1 | Si1 | 126.2(3) | |
| C2 | Fe1 | C5 | 68.72(15) | C5 | C1 | Fe1 | 70.1(2) | |
| C2 | Fe1 | C6 | 126.03(16) | C5 | C1 | Si1 | 127.3(3) | |
| C2 | Fe1 | C7 | 107.06(17) | C5 | C1 | C2 | 106.6(3) | |
| C2 | Fe1 | C8 | 119.11(18) | C1 | C2 | Fe1 | 69.40(19) | |
| C2 | Fe1 | C9 | 154.18(19) | C1 | C2 | C11 | 124.6(3) | |
| C2 | Fe1 | C10 | 163.41(17) | C3 | C2 | Fe1 | 70.0(2) | |
| C3 | Fe1 | C4 | 40.39(16) | C3 | C2 | C1 | 107.8(3) | |
| C3 | Fe1 | C5 | 67.99(16) | C3 | C2 | C11 | 127.6(3) | |
| C5 | Fe1 | C4 | 40.22(15) | C11 | C2 | Fe1 | 125.3(3) | |
| C6 | Fe1 | C1 | 106.97(16) | C2 | C3 | Fe1 | 69.0(2) | |
| C6 | Fe1 | C3 | 163.88(18) | C4 | C3 | Fe1 | 70.5(2) | |
| C6 | Fe1 | C4 | 154.37(18) | C4 | C3 | C2 | 108.5(3) | |
| C6 | Fe1 | C5 | 120.15(17) | C3 | C4 | Fe1 | 69.1(2) | |
| C6 | Fe1 | C7 | 40.11(18) | C5 | C4 | Fe1 | 69.4(2) | |
| C6 | Fe1 | C8 | 67.3(2) | C5 | C4 | C3 | 107.9(3) | |
| C6 | Fe1 | C9 | 67.22(18) | C1 | C5 | Fe1 | 69.0(2) | |
| C6 | Fe1 | C10 | 39.97(17) | C4 | C5 | Fe1 | 70.4(2) | |
| C7 | Fe1 | C3 | 126.76(19) | C4 | C5 | C1 | 109.2(3) | |
| C7 | Fe1 | C4 | 164.43(19) | C7 | C6 | Fe1 | 70.0(3) | |
| C7 | Fe1 | C5 | 153.75(18) | C10 | C6 | Fe1 | 70.3(2) | |
| C7 | Fe1 | C8 | 40.2(2) | C10 | C6 | C7 | 108.9(4) | |
| C7 | Fe1 | C9 | 67.7(2) | C6 | C7 | Fe1 | 69.9(2) | |
| C7 | Fe1 | C10 | 67.63(18) | C6 | C7 | C8 | 107.9(4) | |
| C8 | Fe1 | C3 | 108.52(19) | C8 | C7 | Fe1 | 70.2(3) | |
| C8 | Fe1 | C4 | 127.7(2) | C7 | C8 | Fe1 | 69.6(3) | |
| C8 | Fe1 | C5 | 164.8(2) | C7 | C8 | C9 | 107.6(4) | |
| C9 | Fe1 | C3 | 120.55(18) | C9 | C8 | Fe1 | 69.6(3) | |
| C9 | Fe1 | C4 | 109.30(19) | C8 | C9 | Fe1 | 69.9(3) | |
| C9 | Fe1 | C5 | 127.36(19) | C10 | C9 | Fe1 | 70.1(2) | |
| C9 | Fe1 | C8 | 40.4(2) | C10 | C9 | C8 | 108.1(4) | |
| C9 | Fe1 | C10 | 40.17(19) | C6 | C10 | Fe1 | 69.7(2) | |
| C10 | Fe1 | C3 | 154.68(18) | C6 | C10 | C9 | 107.5(4) | |
| C10 | Fe1 | C4 | 120.68(17) | C9 | C10 | Fe1 | 69.8(2) | |
| C10 | Fe1 | C5 | 108.64(17) | C2 | C11 | N1 | 112.7(3) | |
| C10 | Fe1 | C8 | 67.75(19) | Si1 | C14 | Fe2 | 127.54(19) | |
| C15 | Fe2 | C14 | 40.67(15) | C15 | C14 | Fe2 | 69.1(2) | |
| C15 | Fe2 | C16 | 40.83(18) | C15 | C14 | Si1 | 128.4(3) | |
| C16 | Fe2 | C14 | 68.89(16) | C15 | C14 | C18 | 106.4(3) | |
| C17 | Fe2 | C14 | 69.29(16) | C18 | C14 | Fe2 | 68.5(2) | |
| C17 | Fe2 | C15 | 68.5(2) | C18 | C14 | Si1 | 125.2(3) | |
| C17 | Fe2 | C16 | 40.5(2) | C14 | C15 | Fe2 | 70.2(2) | |
| C17 | Fe2 | C19 | 159.6(2) | C14 | C15 | C16 | 109.0(4) | |
| C17 | Fe2 | C20 | 157.2(2) | C16 | C15 | Fe2 | 69.8(3) | |
| C18 | Fe2 | C14 | 41.58(16) | C15 | C16 | Fe2 | 69.4(2) | |
| C18 | Fe2 | C15 | 68.78(18) | C17 | C16 | Fe2 | 69.4(3) | |
| C18 | Fe2 | C16 | 68.5(2) | C17 | C16 | C15 | 108.0(4) | |
| C18 | Fe2 | C17 | 40.84(18) | C16 | C17 | Fe2 | 70.1(3) | |
| C18 | Fe2 | C19 | 124.81(19) | C16 | C17 | C18 | 108.4(4) | |
| C18 | Fe2 | C20 | 161.2(2) | C18 | C17 | Fe2 | 69.5(2) | |
| C19 | Fe2 | C14 | 109.63(16) | C14 | C18 | Fe2 | 69.9(2) | |
| C19 | Fe2 | C15 | 124.74(19) | C17 | C18 | Fe2 | 69.7(2) | |
| C19 | Fe2 | C16 | 159.5(2) | C17 | C18 | C14 | 108.2(4) | |
| C20 | Fe2 | C14 | 124.49(19) | C20 | C19 | Fe2 | 69.9(3) | |
| C20 | Fe2 | C15 | 108.9(2) | C23 | C19 | Fe2 | 69.8(3) | |
| C20 | Fe2 | C16 | 122.7(2) | C23 | C19 | C20 | 108.2(5) | |
| C20 | Fe2 | C19 | 40.1(2) | C19 | C20 | Fe2 | 70.0(3) | |
| C21 | Fe2 | C14 | 159.5(3) | C21 | C20 | Fe2 | 69.3(3) | |
| C21 | Fe2 | C15 | 123.1(2) | C21 | C20 | C19 | 107.6(5) | |
| C21 | Fe2 | C16 | 106.7(2) | C20 | C21 | Fe2 | 70.8(3) | |
| C21 | Fe2 | C17 | 121.1(2) | C20 | C21 | C22 | 108.8(5) | |
| C21 | Fe2 | C18 | 157.2(2) | C22 | C21 | Fe2 | 69.6(3) | |
| C21 | Fe2 | C19 | 67.2(2) | C21 | C22 | Fe2 | 70.2(3) | |
| C21 | Fe2 | C20 | 39.9(2) | C21 | C22 | C23 | 107.6(5) | |
| C21 | Fe2 | C23 | 67.4(3) | C23 | C22 | Fe2 | 70.5(3) | |
| C22 | Fe2 | C14 | 159.3(3) | C19 | C23 | Fe2 | 70.4(3) | |
| C22 | Fe2 | C15 | 157.9(3) | C19 | C23 | C22 | 107.9(5) | |
| C22 | Fe2 | C16 | 121.2(3) | C22 | C23 | Fe2 | 69.0(3) | |
| C22 | Fe2 | C17 | 105.8(2) |
| A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|---|---|
| Zn1 | N1 | C11 | C2 | -51.2(4) | C1 | C2 | C3 | C4 | -0.4(4) | |
| Fe1 | C1 | C2 | C3 | -59.7(3) | C1 | C2 | C11 | N1 | 88.1(4) | |
| Fe1 | C1 | C2 | C11 | 119.4(4) | C2 | C1 | C5 | Fe1 | -59.6(2) | |
| Fe1 | C1 | C5 | C4 | 59.0(3) | C2 | C1 | C5 | C4 | -0.6(4) | |
| Fe1 | C2 | C3 | C4 | -59.7(3) | C2 | C3 | C4 | Fe1 | 58.8(3) | |
| Fe1 | C2 | C11 | N1 | 176.1(2) | C2 | C3 | C4 | C5 | 0.0(5) | |
| Fe1 | C3 | C4 | C5 | -58.8(3) | C3 | C2 | C11 | N1 | -92.9(5) | |
| Fe1 | C4 | C5 | C1 | -58.2(3) | C3 | C4 | C5 | Fe1 | 58.6(3) | |
| Fe1 | C6 | C7 | C8 | 60.2(3) | C3 | C4 | C5 | C1 | 0.4(4) | |
| Fe1 | C6 | C10 | C9 | -59.8(3) | C5 | C1 | C2 | Fe1 | 60.3(2) | |
| Fe1 | C7 | C8 | C9 | 59.5(3) | C5 | C1 | C2 | C3 | 0.6(4) | |
| Fe1 | C8 | C9 | C10 | 59.9(3) | C5 | C1 | C2 | C11 | 179.7(3) | |
| Fe1 | C9 | C10 | C6 | 59.7(3) | C6 | C7 | C8 | Fe1 | -60.0(3) | |
| Fe2 | C14 | C15 | C16 | -59.2(3) | C6 | C7 | C8 | C9 | -0.5(5) | |
| Fe2 | C14 | C18 | C17 | 59.4(3) | C7 | C6 | C10 | Fe1 | 59.6(3) | |
| Fe2 | C15 | C16 | C17 | -58.9(3) | C7 | C6 | C10 | C9 | -0.2(5) | |
| Fe2 | C16 | C17 | C18 | -59.1(3) | C7 | C8 | C9 | Fe1 | -59.5(3) | |
| Fe2 | C17 | C18 | C14 | -59.6(3) | C7 | C8 | C9 | C10 | 0.4(5) | |
| Fe2 | C19 | C20 | C21 | 59.3(3) | C8 | C9 | C10 | Fe1 | -59.8(3) | |
| Fe2 | C19 | C23 | C22 | -59.0(4) | C8 | C9 | C10 | C6 | -0.1(5) | |
| Fe2 | C20 | C21 | C22 | 59.4(4) | C10 | C6 | C7 | Fe1 | -59.8(3) | |
| Fe2 | C21 | C22 | C23 | 60.9(4) | C10 | C6 | C7 | C8 | 0.4(5) | |
| Fe2 | C22 | C23 | C19 | 59.9(3) | C11 | C2 | C3 | Fe1 | -119.8(4) | |
| Si1 | C1 | C2 | Fe1 | -119.3(3) | C11 | C2 | C3 | C4 | -179.5(4) | |
| Si1 | C1 | C2 | C3 | -179.0(3) | C12 | N1 | C11 | C2 | 75.0(4) | |
| Si1 | C1 | C2 | C11 | 0.1(5) | C13 | N1 | C11 | C2 | -167.3(3) | |
| Si1 | C1 | C5 | Fe1 | 120.0(3) | C14 | Si1 | O1 | Zn1 | 131.01(17) | |
| Si1 | C1 | C5 | C4 | 179.0(3) | C14 | Si1 | O1 | Zn2 | -87.6(2) | |
| Si1 | C14 | C15 | Fe2 | -122.0(3) | C14 | Si1 | C1 | Fe1 | 92.4(2) | |
| Si1 | C14 | C15 | C16 | 178.8(3) | C14 | Si1 | C1 | C2 | -179.0(3) | |
| Si1 | C14 | C18 | Fe2 | 121.6(3) | C14 | Si1 | C1 | C5 | 1.4(4) | |
| Si1 | C14 | C18 | C17 | -179.1(3) | C14 | C15 | C16 | Fe2 | 59.4(3) | |
| O1 | Si1 | C1 | Fe1 | -150.04(19) | C14 | C15 | C16 | C17 | 0.6(5) | |
| O1 | Si1 | C1 | C2 | -61.4(3) | C15 | C14 | C18 | Fe2 | -59.0(3) | |
| O1 | Si1 | C1 | C5 | 119.0(3) | C15 | C14 | C18 | C17 | 0.4(4) | |
| O1 | Si1 | C14 | Fe2 | 84.4(3) | C15 | C16 | C17 | Fe2 | 58.8(3) | |
| O1 | Si1 | C14 | C15 | 176.5(3) | C15 | C16 | C17 | C18 | -0.3(5) | |
| O1 | Si1 | C14 | C18 | -4.2(4) | C16 | C17 | C18 | Fe2 | 59.5(3) | |
| O2 | Si1 | O1 | Zn1 | -103.54(17) | C16 | C17 | C18 | C14 | -0.1(5) | |
| O2 | Si1 | O1 | Zn2 | 37.9(2) | C18 | C14 | C15 | Fe2 | 58.6(3) | |
| O2 | Si1 | C1 | Fe1 | -31.5(3) | C18 | C14 | C15 | C16 | -0.6(4) | |
| O2 | Si1 | C1 | C2 | 57.1(3) | C19 | C20 | C21 | Fe2 | -59.8(3) | |
| O2 | Si1 | C1 | C5 | -122.5(3) | C19 | C20 | C21 | C22 | -0.3(6) | |
| O2 | Si1 | C14 | Fe2 | -39.2(3) | C20 | C19 | C23 | Fe2 | 59.6(3) | |
| O2 | Si1 | C14 | C15 | 52.9(4) | C20 | C19 | C23 | C22 | 0.6(5) | |
| O2 | Si1 | C14 | C18 | -127.8(3) | C20 | C21 | C22 | Fe2 | -60.2(4) | |
| C1 | Si1 | O1 | Zn1 | 14.2(2) | C20 | C21 | C22 | C23 | 0.7(6) | |
| C1 | Si1 | O1 | Zn2 | 155.61(19) | C21 | C22 | C23 | Fe2 | -60.7(4) | |
| C1 | Si1 | C14 | Fe2 | -160.4(2) | C21 | C22 | C23 | C19 | -0.8(6) | |
| C1 | Si1 | C14 | C15 | -68.4(4) | C23 | C19 | C20 | Fe2 | -59.5(3) | |
| C1 | Si1 | C14 | C18 | 111.0(3) | C23 | C19 | C20 | C21 | -0.2(5) | |
| C1 | C2 | C3 | Fe1 | 59.3(2) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| H2 | 6230(30) | 1470(40) | 3350(11) | 55(15) |
| H3 | 6103 | 6777 | 3492 | 40 |
| H4 | 4856 | 6723 | 4108 | 42 |
| H5 | 4290 | 4624 | 4161 | 32 |
| H6 | 6497 | 2792 | 4496 | 44 |
| H7 | 7667 | 3829 | 4006 | 55 |
| H8 | 7698 | 5970 | 4264 | 68 |
| H9 | 6519 | 6243 | 4909 | 64 |
| H10 | 5781 | 4269 | 5050 | 49 |
| H11A | 6746 | 3715 | 3108 | 36 |
| H11B | 7085 | 5052 | 3047 | 36 |
| H12A | 5748 | 6260 | 2561 | 74 |
| H12B | 5912 | 5817 | 2017 | 74 |
| H12C | 6742 | 6151 | 2355 | 74 |
| H13A | 7423 | 4218 | 2238 | 76 |
| H13B | 6631 | 3970 | 1863 | 76 |
| H13C | 6822 | 3053 | 2293 | 76 |
| H15 | 4666 | 2128 | 4645 | 44 |
| H16 | 3155 | 1338 | 4895 | 60 |
| H17 | 2258 | 960 | 4138 | 65 |
| H18 | 3197 | 1531 | 3413 | 46 |
| H19 | 5462 | -540 | 3684 | 55 |
| H20 | 5412 | -645 | 4593 | 60 |
| H21 | 3897 | -1349 | 4831 | 84 |
| H22 | 2999 | -1663 | 4081 | 106 |
| H23 | 3980 | -1191 | 3366 | 84 |
Experimental
Single crystals of C46H52Cl2Fe4N2O4Si2Zn2 [3118] were []. A suitable crystal was selected and [] on a Xcalibur, Sapphire3 diffractometer. The crystal was kept at 173.15 K during data collection. Using Olex2 [1], the structure was solved with the ShelXS [2] structure solution program using Direct Methods and refined with the XL [3] refinement package using Least Squares minimisation.
Crystal structure determination of [3118]
Crystal Data for C46H52Cl2Fe4N2O4Si2Zn2 (M =1178.11 g/mol): orthorhombic, space group Pbcn (no. 60), a = 15.0001(6) Å, b = 11.2793(5) Å, c = 27.6027(12) Å, V = 4670.1(3) Å3, Z = 4, T = 173.15 K, μ(MoKα) = 2.431 mm-1, Dcalc = 1.676 g/cm3, 35271 reflections measured (4.518° ≤ 2Θ ≤ 53.998°), 5097 unique (Rint = 0.0431, Rsigma = 0.0282) which were used in all calculations. The final R1 was 0.0449 (I > 2σ(I)) and wR2 was 0.1138 (all data).
Refinement model description
Number of restraints - 1, 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. Restrained distances
O2-H2
1 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
C11(H11A,H11B)
3.b Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C15(H15),
C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23)
3.c Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)
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.