| Identification code | 3120_twin1_hklf4 |
| Empirical formula | C48H56Br2Fe4N2O4Si2Zn2 |
| Formula weight | 1295.08 |
| Temperature/K | 173.15 |
| Crystal system | monoclinic |
| Space group | P21/c |
| a/Å | 8.1910(6) |
| b/Å | 30.593(2) |
| c/Å | 9.8539(7) |
| α/° | 90 |
| β/° | 103.762(7) |
| γ/° | 90 |
| Volume/Å3 | 2398.3(3) |
| Z | 2 |
| ρcalcg/cm3 | 1.793 |
| μ/mm‑1 | 3.924 |
| F(000) | 1304.0 |
| Crystal size/mm3 | 0.3 × 0.1 × 0.05 |
| Radiation | MoKα (λ = 0.71073) |
| 2Θ range for data collection/° | 4.46 to 52 |
| Index ranges | -10 ≤ h ≤ 10, -37 ≤ k ≤ 37, -12 ≤ l ≤ 12 |
| Reflections collected | 9157 |
| Independent reflections | 9157 [Rint = ?, Rsigma = 0.0956] |
| Data/restraints/parameters | 9157/0/293 |
| Goodness-of-fit on F2 | 1.122 |
| Final R indexes [I>=2σ (I)] | R1 = 0.0818, wR2 = 0.2449 |
| Final R indexes [all data] | R1 = 0.1253, wR2 = 0.2662 |
| Largest diff. peak/hole / e Å-3 | 1.65/-1.06 |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| Br1 | 12249.0(16) | 5520.8(4) | 2927.2(16) | 65.0(4) |
| Zn1 | 10021.4(15) | 5218.7(4) | 3708.2(13) | 39.5(4) |
| Fe1 | 7261.2(19) | 6703.3(5) | 3765.5(17) | 43.1(4) |
| Fe2 | 11730.5(19) | 6609.1(5) | 8618.4(16) | 41.5(4) |
| Si1 | 9475(4) | 5878.4(9) | 6135(3) | 40.9(7) |
| O1 | 9688(11) | 5391(2) | 5571(8) | 50.6(18) |
| O2 | 7997(10) | 5895(2) | 6996(9) | 50.8(19) |
| N1 | 7677(10) | 5325(2) | 2399(9) | 35.8(17) |
| C1 | 9031(11) | 6228(3) | 4535(11) | 37(2) |
| C2 | 8039(12) | 6112(3) | 3179(9) | 35(2) |
| C3 | 8157(14) | 6428(3) | 2173(14) | 51(3) |
| C4 | 9278(14) | 6771(4) | 2896(13) | 50(3) |
| C5 | 9830(12) | 6636(3) | 4313(13) | 45(3) |
| C6 | 5833(14) | 6836(3) | 5194(13) | 49(3) |
| C7 | 4787(15) | 6646(3) | 3961(16) | 57(3) |
| C8 | 4898(14) | 6918(4) | 2855(14) | 69(4) |
| C9 | 5961(15) | 7272(4) | 3317(14) | 61(4) |
| C10 | 6532(15) | 7224(4) | 4770(13) | 58(3) |
| C14 | 11305(12) | 6043(3) | 7453(10) | 33(2) |
| C15 | 11596(16) | 5965(3) | 8949(12) | 48(3) |
| C16 | 13274(14) | 6109(4) | 9674(12) | 49(3) |
| C17 | 13973(16) | 6302(4) | 8659(14) | 61(3) |
| C18 | 12843(12) | 6264(3) | 7357(13) | 44(2) |
| C23 | 9819(17) | 7027(5) | 7773(13) | 69(4) |
| C19 | 9716(16) | 6896(4) | 9066(13) | 54(3) |
| C20 | 11115(17) | 7024(3) | 10064(13) | 55(3) |
| C21 | 12186(14) | 7244(3) | 9287(15) | 55(3) |
| C22 | 11390(20) | 7215(4) | 7888(14) | 69(4) |
| C24 | 6391(16) | 5711(4) | 6590(14) | 57(3) |
| C11 | 6850(13) | 5713(3) | 2897(12) | 43(2) |
| C12 | 7843(19) | 5401(5) | 958(13) | 70(4) |
| C13 | 6585(14) | 4949(4) | 2404(14) | 56(3) |
| Atom | U11 | U22 | U33 | U23 | U13 | U12 |
|---|---|---|---|---|---|---|
| Br1 | 50.8(8) | 65.8(8) | 83.3(11) | 7.1(7) | 25.9(7) | -5.3(6) |
| Zn1 | 41.6(7) | 38.3(6) | 39.5(7) | 0.9(5) | 11.2(5) | 0.7(5) |
| Fe1 | 44.7(8) | 39.7(8) | 42.6(9) | -0.7(6) | 5.9(7) | 1.5(6) |
| Fe2 | 46.4(9) | 41.5(8) | 35.6(8) | -1.7(6) | 7.7(6) | 4.5(6) |
| Si1 | 45.5(16) | 39.8(14) | 39.8(16) | -5.5(12) | 14.7(12) | -1.3(12) |
| O1 | 66(5) | 43(4) | 43(5) | -3(3) | 13(4) | -2(3) |
| O2 | 55(5) | 47(4) | 52(5) | 4(3) | 16(4) | 2(3) |
| N1 | 34(4) | 39(4) | 35(5) | 0(3) | 10(3) | -8(3) |
| C1 | 31(5) | 32(4) | 50(6) | 7(4) | 11(4) | 12(4) |
| C2 | 40(5) | 49(5) | 19(4) | -10(4) | 14(4) | 2(4) |
| C3 | 48(6) | 46(6) | 60(8) | 6(5) | 16(5) | -18(5) |
| C4 | 48(6) | 44(6) | 63(8) | 9(5) | 19(5) | -1(5) |
| C5 | 31(5) | 31(4) | 69(8) | 0(5) | 7(5) | -14(4) |
| C6 | 53(7) | 34(5) | 63(8) | 28(5) | 22(6) | -1(5) |
| C7 | 43(6) | 36(5) | 101(11) | 1(6) | 38(7) | 17(5) |
| C8 | 34(6) | 76(8) | 68(9) | -12(7) | -44(6) | 12(5) |
| C9 | 46(6) | 46(6) | 70(9) | 13(6) | -26(6) | 20(5) |
| C10 | 55(7) | 69(7) | 42(7) | -16(6) | -1(6) | 13(6) |
| C14 | 41(5) | 27(4) | 33(5) | 3(4) | 16(4) | 17(4) |
| C15 | 81(8) | 41(5) | 34(6) | -10(4) | 34(6) | -1(5) |
| C16 | 44(6) | 58(6) | 37(6) | -6(5) | -5(5) | -4(5) |
| C17 | 49(7) | 74(8) | 51(7) | -8(6) | -8(6) | -4(6) |
| C18 | 32(5) | 35(5) | 59(7) | 9(5) | 1(5) | -8(4) |
| C23 | 56(8) | 99(10) | 39(7) | 0(7) | -11(6) | 22(7) |
| C19 | 57(7) | 52(6) | 55(8) | -20(6) | 17(6) | -6(5) |
| C20 | 85(9) | 41(6) | 40(6) | -8(5) | 19(6) | 14(6) |
| C21 | 45(6) | 20(4) | 90(10) | -19(5) | -6(6) | 5(4) |
| C22 | 113(13) | 48(7) | 42(7) | -19(6) | 10(7) | 23(7) |
| C24 | 67(8) | 59(7) | 49(7) | -8(6) | 25(6) | 0(6) |
| C11 | 36(5) | 45(6) | 49(7) | -14(5) | 9(4) | -4(4) |
| C12 | 87(10) | 75(8) | 32(6) | -10(6) | -15(6) | 22(7) |
| C13 | 32(5) | 50(6) | 72(9) | 2(6) | -14(5) | 19(5) |
| Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
|---|---|---|---|---|---|---|
| Br1 | Zn1 | 2.3332(16) | Si1 | C14 | 1.806(11) | |
| Zn1 | Zn11 | 2.884(2) | O1 | Zn11 | 1.988(7) | |
| Zn1 | O11 | 1.988(7) | O2 | C24 | 1.399(15) | |
| Zn1 | O1 | 1.990(8) | N1 | C11 | 1.507(12) | |
| Zn1 | N1 | 2.069(8) | N1 | C12 | 1.477(15) | |
| Fe1 | C1 | 2.066(9) | N1 | C13 | 1.458(14) | |
| Fe1 | C2 | 2.046(9) | C1 | C2 | 1.433(13) | |
| Fe1 | C3 | 2.064(12) | C1 | C5 | 1.451(13) | |
| Fe1 | C4 | 2.044(11) | C2 | C3 | 1.404(15) | |
| Fe1 | C5 | 2.054(10) | C2 | C11 | 1.545(14) | |
| Fe1 | C6 | 2.073(11) | C3 | C4 | 1.463(16) | |
| Fe1 | C7 | 2.088(11) | C4 | C5 | 1.423(17) | |
| Fe1 | C8 | 2.039(10) | C6 | C7 | 1.433(19) | |
| Fe1 | C9 | 2.032(10) | C6 | C10 | 1.422(16) | |
| Fe1 | C10 | 2.037(11) | C7 | C8 | 1.390(18) | |
| Fe2 | C14 | 2.062(9) | C8 | C9 | 1.397(17) | |
| Fe2 | C15 | 2.006(10) | C9 | C10 | 1.404(17) | |
| Fe2 | C16 | 2.097(12) | C14 | C15 | 1.456(14) | |
| Fe2 | C17 | 2.054(13) | C14 | C18 | 1.453(13) | |
| Fe2 | C18 | 2.007(12) | C15 | C16 | 1.458(16) | |
| Fe2 | C23 | 2.039(13) | C16 | C17 | 1.397(18) | |
| Fe2 | C19 | 2.009(12) | C17 | C18 | 1.397(16) | |
| Fe2 | C20 | 2.058(10) | C23 | C19 | 1.357(18) | |
| Fe2 | C21 | 2.056(9) | C23 | C22 | 1.39(2) | |
| Fe2 | C22 | 1.983(13) | C19 | C20 | 1.377(18) | |
| Si1 | O1 | 1.616(8) | C20 | C21 | 1.458(17) | |
| Si1 | O2 | 1.637(8) | C21 | C22 | 1.381(18) | |
| Si1 | C1 | 1.868(11) |
| Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|
| Br1 | Zn1 | Zn11 | 130.52(8) | C22 | Fe2 | C16 | 151.5(6) | |
| O11 | Zn1 | Br1 | 116.9(2) | C22 | Fe2 | C17 | 118.9(6) | |
| O1 | Zn1 | Br1 | 119.3(2) | C22 | Fe2 | C18 | 108.2(5) | |
| O11 | Zn1 | Zn11 | 43.6(2) | C22 | Fe2 | C23 | 40.3(6) | |
| O1 | Zn1 | Zn11 | 43.5(2) | C22 | Fe2 | C19 | 67.6(6) | |
| O11 | Zn1 | O1 | 87.1(3) | C22 | Fe2 | C20 | 68.8(5) | |
| O11 | Zn1 | N1 | 112.6(3) | C22 | Fe2 | C21 | 39.9(5) | |
| O1 | Zn1 | N1 | 102.9(3) | O1 | Si1 | O2 | 111.1(4) | |
| N1 | Zn1 | Br1 | 114.5(2) | O1 | Si1 | C1 | 104.7(4) | |
| N1 | Zn1 | Zn11 | 114.8(2) | O1 | Si1 | C14 | 111.4(4) | |
| C1 | Fe1 | C6 | 110.4(4) | O2 | Si1 | C1 | 113.6(4) | |
| C1 | Fe1 | C7 | 121.3(4) | O2 | Si1 | C14 | 102.0(4) | |
| C2 | Fe1 | C1 | 40.8(4) | C14 | Si1 | C1 | 114.2(4) | |
| C2 | Fe1 | C3 | 39.9(4) | Zn11 | O1 | Zn1 | 92.9(3) | |
| C2 | Fe1 | C5 | 67.5(4) | Si1 | O1 | Zn1 | 127.6(4) | |
| C2 | Fe1 | C6 | 129.0(4) | Si1 | O1 | Zn11 | 139.1(5) | |
| C2 | Fe1 | C7 | 109.0(4) | C24 | O2 | Si1 | 126.9(8) | |
| C3 | Fe1 | C1 | 69.3(5) | C11 | N1 | Zn1 | 110.1(6) | |
| C3 | Fe1 | C6 | 163.0(4) | C12 | N1 | Zn1 | 109.9(7) | |
| C3 | Fe1 | C7 | 124.4(5) | C12 | N1 | C11 | 109.8(9) | |
| C4 | Fe1 | C1 | 70.1(4) | C13 | N1 | Zn1 | 110.7(6) | |
| C4 | Fe1 | C2 | 68.6(4) | C13 | N1 | C11 | 107.3(8) | |
| C4 | Fe1 | C3 | 41.7(4) | C13 | N1 | C12 | 109.0(10) | |
| C4 | Fe1 | C5 | 40.6(5) | Si1 | C1 | Fe1 | 133.8(5) | |
| C4 | Fe1 | C6 | 155.1(5) | C2 | C1 | Fe1 | 68.8(5) | |
| C4 | Fe1 | C7 | 161.0(6) | C2 | C1 | Si1 | 126.8(7) | |
| C5 | Fe1 | C1 | 41.2(4) | C2 | C1 | C5 | 104.4(9) | |
| C5 | Fe1 | C3 | 68.4(5) | C5 | C1 | Fe1 | 69.0(5) | |
| C5 | Fe1 | C6 | 123.3(5) | C5 | C1 | Si1 | 128.0(8) | |
| C5 | Fe1 | C7 | 157.4(5) | C1 | C2 | Fe1 | 70.4(5) | |
| C6 | Fe1 | C7 | 40.3(5) | C1 | C2 | C11 | 123.8(9) | |
| C8 | Fe1 | C1 | 153.9(5) | C3 | C2 | Fe1 | 70.7(6) | |
| C8 | Fe1 | C2 | 119.1(5) | C3 | C2 | C1 | 111.7(9) | |
| C8 | Fe1 | C3 | 105.6(6) | C3 | C2 | C11 | 124.3(9) | |
| C8 | Fe1 | C4 | 124.1(6) | C11 | C2 | Fe1 | 121.6(6) | |
| C8 | Fe1 | C5 | 162.5(5) | C2 | C3 | Fe1 | 69.3(6) | |
| C8 | Fe1 | C6 | 66.8(5) | C2 | C3 | C4 | 106.9(11) | |
| C8 | Fe1 | C7 | 39.3(5) | C4 | C3 | Fe1 | 68.4(7) | |
| C9 | Fe1 | C1 | 165.4(5) | C3 | C4 | Fe1 | 69.9(6) | |
| C9 | Fe1 | C2 | 151.3(5) | C5 | C4 | Fe1 | 70.1(6) | |
| C9 | Fe1 | C3 | 116.5(5) | C5 | C4 | C3 | 106.6(9) | |
| C9 | Fe1 | C4 | 104.8(5) | C1 | C5 | Fe1 | 69.8(5) | |
| C9 | Fe1 | C5 | 126.4(4) | C4 | C5 | Fe1 | 69.3(6) | |
| C9 | Fe1 | C6 | 68.2(5) | C4 | C5 | C1 | 110.4(9) | |
| C9 | Fe1 | C7 | 67.8(5) | C7 | C6 | Fe1 | 70.4(6) | |
| C9 | Fe1 | C8 | 40.1(5) | C10 | C6 | Fe1 | 68.4(6) | |
| C9 | Fe1 | C10 | 40.4(5) | C10 | C6 | C7 | 106.9(10) | |
| C10 | Fe1 | C1 | 129.3(5) | C6 | C7 | Fe1 | 69.3(6) | |
| C10 | Fe1 | C2 | 167.1(5) | C8 | C7 | Fe1 | 68.4(6) | |
| C10 | Fe1 | C3 | 152.4(5) | C8 | C7 | C6 | 106.6(10) | |
| C10 | Fe1 | C4 | 118.9(5) | C7 | C8 | Fe1 | 72.3(6) | |
| C10 | Fe1 | C5 | 110.5(5) | C7 | C8 | C9 | 111.1(11) | |
| C10 | Fe1 | C6 | 40.5(5) | C9 | C8 | Fe1 | 69.7(6) | |
| C10 | Fe1 | C7 | 67.5(5) | C8 | C9 | Fe1 | 70.2(6) | |
| C10 | Fe1 | C8 | 66.8(5) | C8 | C9 | C10 | 106.4(11) | |
| C14 | Fe2 | C16 | 70.4(4) | C10 | C9 | Fe1 | 70.0(6) | |
| C15 | Fe2 | C14 | 41.9(4) | C6 | C10 | Fe1 | 71.1(7) | |
| C15 | Fe2 | C16 | 41.6(5) | C9 | C10 | Fe1 | 69.6(7) | |
| C15 | Fe2 | C17 | 68.4(5) | C9 | C10 | C6 | 109.1(11) | |
| C15 | Fe2 | C18 | 68.5(4) | Si1 | C14 | Fe2 | 129.5(4) | |
| C15 | Fe2 | C23 | 128.0(6) | C15 | C14 | Fe2 | 67.0(5) | |
| C15 | Fe2 | C19 | 108.3(5) | C15 | C14 | Si1 | 126.2(8) | |
| C15 | Fe2 | C20 | 117.5(4) | C18 | C14 | Fe2 | 67.1(6) | |
| C15 | Fe2 | C21 | 152.8(5) | C18 | C14 | Si1 | 131.9(8) | |
| C17 | Fe2 | C14 | 70.1(4) | C18 | C14 | C15 | 101.9(9) | |
| C17 | Fe2 | C16 | 39.3(5) | C14 | C15 | Fe2 | 71.1(5) | |
| C17 | Fe2 | C20 | 129.3(5) | C14 | C15 | C16 | 110.8(9) | |
| C17 | Fe2 | C21 | 109.4(5) | C16 | C15 | Fe2 | 72.6(6) | |
| C18 | Fe2 | C14 | 41.8(4) | C15 | C16 | Fe2 | 65.9(6) | |
| C18 | Fe2 | C16 | 67.3(4) | C17 | C16 | Fe2 | 68.7(7) | |
| C18 | Fe2 | C17 | 40.2(5) | C17 | C16 | C15 | 106.1(10) | |
| C18 | Fe2 | C23 | 119.6(5) | C16 | C17 | Fe2 | 72.0(7) | |
| C18 | Fe2 | C19 | 152.1(5) | C16 | C17 | C18 | 109.1(11) | |
| C18 | Fe2 | C20 | 167.2(5) | C18 | C17 | Fe2 | 68.1(7) | |
| C18 | Fe2 | C21 | 128.4(5) | C14 | C18 | Fe2 | 71.1(6) | |
| C23 | Fe2 | C14 | 106.7(5) | C17 | C18 | Fe2 | 71.7(8) | |
| C23 | Fe2 | C16 | 166.9(6) | C17 | C18 | C14 | 112.0(11) | |
| C23 | Fe2 | C17 | 152.9(6) | C19 | C23 | Fe2 | 69.2(7) | |
| C23 | Fe2 | C20 | 66.8(5) | C19 | C23 | C22 | 108.0(12) | |
| C23 | Fe2 | C21 | 66.5(5) | C22 | C23 | Fe2 | 67.7(7) | |
| C19 | Fe2 | C14 | 116.8(4) | C23 | C19 | Fe2 | 71.6(7) | |
| C19 | Fe2 | C16 | 129.8(5) | C23 | C19 | C20 | 111.1(12) | |
| C19 | Fe2 | C17 | 166.6(5) | C20 | C19 | Fe2 | 72.1(7) | |
| C19 | Fe2 | C23 | 39.2(5) | C19 | C20 | Fe2 | 68.3(7) | |
| C19 | Fe2 | C20 | 39.6(5) | C19 | C20 | C21 | 105.0(11) | |
| C19 | Fe2 | C21 | 67.2(5) | C21 | C20 | Fe2 | 69.2(6) | |
| C20 | Fe2 | C14 | 150.1(4) | C20 | C21 | Fe2 | 69.3(5) | |
| C20 | Fe2 | C16 | 109.0(5) | C22 | C21 | Fe2 | 67.2(6) | |
| C21 | Fe2 | C14 | 165.0(5) | C22 | C21 | C20 | 107.0(12) | |
| C21 | Fe2 | C16 | 119.2(5) | C23 | C22 | Fe2 | 72.0(8) | |
| C21 | Fe2 | C20 | 41.5(5) | C21 | C22 | Fe2 | 72.9(7) | |
| C22 | Fe2 | C14 | 126.3(4) | C21 | C22 | C23 | 108.6(13) | |
| C22 | Fe2 | C15 | 165.6(6) | N1 | C11 | C2 | 111.6(8) |
| A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|---|---|
| Zn1 | N1 | C11 | C2 | 49.5(10) | C1 | C2 | C3 | Fe1 | -58.5(6) | |
| Fe1 | C1 | C2 | C3 | 58.7(7) | C1 | C2 | C3 | C4 | -0.2(12) | |
| Fe1 | C1 | C2 | C11 | -115.5(9) | C1 | C2 | C11 | N1 | -97.0(11) | |
| Fe1 | C1 | C5 | C4 | -57.4(8) | C2 | C1 | C5 | Fe1 | 60.2(6) | |
| Fe1 | C2 | C3 | C4 | 58.3(8) | C2 | C1 | C5 | C4 | 2.7(11) | |
| Fe1 | C2 | C11 | N1 | 176.6(6) | C2 | C3 | C4 | Fe1 | -58.9(7) | |
| Fe1 | C3 | C4 | C5 | 60.8(7) | C2 | C3 | C4 | C5 | 1.9(12) | |
| Fe1 | C4 | C5 | C1 | 57.7(7) | C3 | C2 | C11 | N1 | 89.5(12) | |
| Fe1 | C6 | C7 | C8 | -58.5(7) | C3 | C4 | C5 | Fe1 | -60.6(7) | |
| Fe1 | C6 | C10 | C9 | 59.5(8) | C3 | C4 | C5 | C1 | -2.9(12) | |
| Fe1 | C7 | C8 | C9 | -59.1(9) | C5 | C1 | C2 | Fe1 | -60.2(6) | |
| Fe1 | C8 | C9 | C10 | -61.0(8) | C5 | C1 | C2 | C3 | -1.5(10) | |
| Fe1 | C9 | C10 | C6 | -60.4(8) | C5 | C1 | C2 | C11 | -175.7(9) | |
| Fe2 | C14 | C15 | C16 | -62.1(7) | C6 | C7 | C8 | Fe1 | 59.0(7) | |
| Fe2 | C14 | C18 | C17 | 60.3(9) | C6 | C7 | C8 | C9 | -0.1(13) | |
| Fe2 | C15 | C16 | C17 | -57.1(8) | C7 | C6 | C10 | Fe1 | -60.2(7) | |
| Fe2 | C16 | C17 | C18 | -58.1(9) | C7 | C6 | C10 | C9 | -0.7(13) | |
| Fe2 | C17 | C18 | C14 | -59.9(7) | C7 | C8 | C9 | Fe1 | 60.6(8) | |
| Fe2 | C23 | C19 | C20 | 61.7(9) | C7 | C8 | C9 | C10 | -0.4(14) | |
| Fe2 | C23 | C22 | C21 | -64.2(8) | C8 | C9 | C10 | Fe1 | 61.1(8) | |
| Fe2 | C19 | C20 | C21 | 59.8(7) | C8 | C9 | C10 | C6 | 0.7(14) | |
| Fe2 | C20 | C21 | C22 | 56.7(7) | C10 | C6 | C7 | Fe1 | 58.9(7) | |
| Fe2 | C21 | C22 | C23 | 63.7(9) | C10 | C6 | C7 | C8 | 0.5(12) | |
| Si1 | C1 | C2 | Fe1 | 129.5(7) | C14 | Si1 | O1 | Zn11 | 62.6(9) | |
| Si1 | C1 | C2 | C3 | -171.7(8) | C14 | Si1 | O1 | Zn1 | -109.1(6) | |
| Si1 | C1 | C2 | C11 | 14.1(13) | C14 | Si1 | O2 | C24 | -165.1(9) | |
| Si1 | C1 | C5 | Fe1 | -129.8(8) | C14 | Si1 | C1 | Fe1 | -105.4(7) | |
| Si1 | C1 | C5 | C4 | 172.8(7) | C14 | Si1 | C1 | C2 | 159.4(7) | |
| Si1 | C14 | C15 | Fe2 | -123.1(6) | C14 | Si1 | C1 | C5 | -8.6(10) | |
| Si1 | C14 | C15 | C16 | 174.9(7) | C14 | C15 | C16 | Fe2 | 61.2(7) | |
| Si1 | C14 | C18 | Fe2 | 123.3(7) | C14 | C15 | C16 | C17 | 4.1(12) | |
| Si1 | C14 | C18 | C17 | -176.5(8) | C15 | C14 | C18 | Fe2 | -58.5(6) | |
| O1 | Si1 | O2 | C24 | -46.2(10) | C15 | C14 | C18 | C17 | 1.8(11) | |
| O1 | Si1 | C1 | Fe1 | 132.5(7) | C15 | C16 | C17 | Fe2 | 55.3(8) | |
| O1 | Si1 | C1 | C2 | 37.2(9) | C15 | C16 | C17 | C18 | -2.8(14) | |
| O1 | Si1 | C1 | C5 | -130.8(9) | C16 | C17 | C18 | Fe2 | 60.5(9) | |
| O1 | Si1 | C14 | Fe2 | -176.7(5) | C16 | C17 | C18 | C14 | 0.6(14) | |
| O1 | Si1 | C14 | C15 | -88.1(8) | C18 | C14 | C15 | Fe2 | 58.5(6) | |
| O1 | Si1 | C14 | C18 | 89.8(9) | C18 | C14 | C15 | C16 | -3.5(10) | |
| O2 | Si1 | O1 | Zn1 | 137.8(6) | C23 | C19 | C20 | Fe2 | -61.4(9) | |
| O2 | Si1 | O1 | Zn11 | -50.5(9) | C23 | C19 | C20 | C21 | -1.6(13) | |
| O2 | Si1 | C1 | Fe1 | 11.1(9) | C19 | C23 | C22 | Fe2 | 57.5(9) | |
| O2 | Si1 | C1 | C2 | -84.2(9) | C19 | C23 | C22 | C21 | -6.7(15) | |
| O2 | Si1 | C1 | C5 | 107.8(9) | C19 | C20 | C21 | Fe2 | -59.2(7) | |
| O2 | Si1 | C14 | Fe2 | -58.0(7) | C19 | C20 | C21 | C22 | -2.5(11) | |
| O2 | Si1 | C14 | C15 | 30.6(8) | C20 | C21 | C22 | Fe2 | -58.0(7) | |
| O2 | Si1 | C14 | C18 | -151.5(8) | C20 | C21 | C22 | C23 | 5.6(12) | |
| C1 | Si1 | O1 | Zn11 | -173.5(7) | C22 | C23 | C19 | Fe2 | -56.6(9) | |
| C1 | Si1 | O1 | Zn1 | 14.8(7) | C22 | C23 | C19 | C20 | 5.1(15) | |
| C1 | Si1 | O2 | C24 | 71.5(10) | C11 | C2 | C3 | Fe1 | 115.7(9) | |
| C1 | Si1 | C14 | Fe2 | 64.9(7) | C11 | C2 | C3 | C4 | 174.0(9) | |
| C1 | Si1 | C14 | C15 | 153.5(7) | C12 | N1 | C11 | C2 | -71.6(11) | |
| C1 | Si1 | C14 | C18 | -28.6(10) | C13 | N1 | C11 | C2 | 170.0(9) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| H3 | 7614 | 6420 | 1207 | 61 |
| H4 | 9578 | 7033 | 2497 | 61 |
| H5 | 10611 | 6792 | 5014 | 54 |
| H6 | 6023 | 6724 | 6118 | 58 |
| H7 | 4143 | 6386 | 3909 | 68 |
| H8 | 4326 | 6869 | 1909 | 82 |
| H9 | 6241 | 7500 | 2759 | 73 |
| H10 | 7268 | 7419 | 5373 | 69 |
| H15 | 10801 | 5837 | 9392 | 58 |
| H16 | 13787 | 6078 | 10640 | 59 |
| H17 | 15045 | 6438 | 8827 | 74 |
| H18 | 13055 | 6370 | 6509 | 52 |
| H23 | 8967 | 6996 | 6936 | 82 |
| H19 | 8800 | 6737 | 9258 | 65 |
| H20 | 11335 | 6979 | 11044 | 66 |
| H21 | 13234 | 7381 | 9671 | 66 |
| H22 | 11837 | 7307 | 7132 | 83 |
| H24A | 5923 | 5675 | 7411 | 85 |
| H24B | 6464 | 5425 | 6161 | 85 |
| H24C | 5660 | 5903 | 5912 | 85 |
| H11A | 6511 | 5635 | 3766 | 52 |
| H11B | 5822 | 5791 | 2182 | 52 |
| H12A | 8514 | 5665 | 934 | 104 |
| H12B | 6724 | 5440 | 336 | 104 |
| H12C | 8399 | 5150 | 646 | 104 |
| H13A | 7078 | 4690 | 2071 | 84 |
| H13B | 5477 | 5007 | 1789 | 84 |
| H13C | 6464 | 4897 | 3357 | 84 |
Experimental
Single crystals of C48H56Br2Fe4N2O4Si2Zn2 [3120_twin1_hklf4] 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 [3120_twin1_hklf4]
Crystal Data for C48H56Br2Fe4N2O4Si2Zn2 (M =1295.08 g/mol): monoclinic, space group P21/c (no. 14), a = 8.1910(6) Å, b = 30.593(2) Å, c = 9.8539(7) Å, β = 103.762(7)°, V = 2398.3(3) Å3, Z = 2, T = 173.15 K, μ(MoKα) = 3.924 mm-1, Dcalc = 1.793 g/cm3, 9157 reflections measured (4.46° ≤ 2Θ ≤ 52°), 9157 unique (Rint = ?, Rsigma = 0.0956) which were used in all calculations. The final R1 was 0.0818 (I > 2σ(I)) and wR2 was 0.2662 (all data).
Refinement model description
Number of restraints - 0, number of constraints - unknown.
Details:
1. Twinned data refinement
Scales: 0.8412(14) 0.1588(14)
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
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), C23(H23), C19(H19), C20(H20), C21(H21), C22(H22)
3.c Idealised Me refined as rotating group:
C24(H24A,H24B,H24C), 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.