| Identification code | 3091 |
| Empirical formula | C46H52Br2Fe4N2O4Si2Zn2 |
| Formula weight | 1267.03 |
| Temperature/K | 173 |
| Crystal system | orthorhombic |
| Space group | Pbcn |
| a/Å | 15.5968(12) |
| b/Å | 11.1687(9) |
| c/Å | 27.587(2) |
| α/° | 90 |
| β/° | 90 |
| γ/° | 90 |
| Volume/Å3 | 4805.5(7) |
| Z | 4 |
| ρcalcg/cm3 | 1.751 |
| μ/mm‑1 | 3.915 |
| F(000) | 2544.0 |
| Crystal size/mm3 | 0.3 × 0.2 × 0.1 |
| Radiation | MoKα (λ = 0.71073) |
| 2Θ range for data collection/° | 4.486 to 51.992 |
| Index ranges | -12 ≤ h ≤ 19, -13 ≤ k ≤ 12, -27 ≤ l ≤ 34 |
| Reflections collected | 17657 |
| Independent reflections | 4721 [Rint = 0.0611, Rsigma = 0.0644] |
| Data/restraints/parameters | 4721/1/287 |
| Goodness-of-fit on F2 | 1.043 |
| Final R indexes [I>=2σ (I)] | R1 = 0.0532, wR2 = 0.1000 |
| Final R indexes [all data] | R1 = 0.0942, wR2 = 0.1182 |
| Largest diff. peak/hole / e Å-3 | 1.22/-1.18 |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| Br1 | 1207.5(4) | -157.4(7) | 2711.2(3) | 52.0(2) |
| Zn1 | 0 | 3617.7(8) | 2500 | 21.8(2) |
| Zn2 | 0 | 988.5(8) | 2500 | 25.5(2) |
| Fe1 | -1084.7(6) | 4898.9(7) | 876.0(3) | 30.7(2) |
| Fe2 | 1026.5(6) | 252.7(8) | 850.9(4) | 38.5(3) |
| Si1 | -126.8(9) | 2474.0(13) | 1455.7(6) | 23.8(4) |
| O1 | 100(2) | 2306(3) | 2023.4(13) | 24.7(9) |
| O2 | -1030(2) | 1786(4) | 1323.7(15) | 32.6(10) |
| N1 | -1146(3) | 4505(5) | 2485.8(18) | 34.4(12) |
| C1 | -267(3) | 4105(5) | 1359(2) | 23.9(13) |
| C2 | -876(3) | 4876(5) | 1602(2) | 26.6(13) |
| C3 | -766(4) | 6058(5) | 1418(2) | 38.1(16) |
| C4 | -106(4) | 6034(5) | 1069(2) | 36.5(16) |
| C5 | 198(4) | 4848(5) | 1029(2) | 30.5(14) |
| C6 | -1652(4) | 3565(6) | 486(2) | 39.9(16) |
| C7 | -2265(4) | 4166(7) | 759(3) | 50.5(19) |
| C8 | -2268(5) | 5374(7) | 615(3) | 61(2) |
| C9 | -1638(6) | 5487(7) | 250(3) | 61(2) |
| C10 | -1258(4) | 4383(7) | 170(2) | 46.1(18) |
| C11 | -1504(3) | 4488(6) | 1976(2) | 31.4(15) |
| C12 | -1097(5) | 5777(6) | 2648(2) | 53(2) |
| C13 | -1746(4) | 3841(7) | 2814(2) | 49(2) |
| C14 | 778(4) | 1956(5) | 1082(2) | 30.4(14) |
| C15 | 834(5) | 1906(5) | 566(2) | 42.5(17) |
| C16 | 1652(5) | 1474(6) | 432(3) | 60(2) |
| C17 | 2124(5) | 1246(6) | 859(4) | 66(3) |
| C18 | 1596(4) | 1542(5) | 1261(3) | 40.6(17) |
| C19 | 71(6) | -863(6) | 629(3) | 58(2) |
| C20 | 138(6) | -878(6) | 1125(3) | 61(2) |
| C21 | 959(9) | -1264(8) | 1258(4) | 98(4) |
| C22 | 1393(6) | -1464(7) | 803(6) | 97(5) |
| C23 | 835(8) | -1215(7) | 440(4) | 87(4) |
| Atom | U11 | U22 | U33 | U23 | U13 | U12 |
|---|---|---|---|---|---|---|
| Br1 | 41.1(4) | 65.9(5) | 49.0(5) | -5.9(4) | -2.6(3) | 28.8(4) |
| Zn1 | 20.2(4) | 24.6(5) | 20.6(5) | 0 | 0.2(4) | 0 |
| Zn2 | 24.4(5) | 25.8(5) | 26.3(6) | 0 | -1.5(4) | 0 |
| Fe1 | 45.3(5) | 24.9(5) | 21.7(5) | 4.9(4) | -2.9(4) | 1.7(4) |
| Fe2 | 46.1(6) | 22.4(5) | 47.0(6) | -12.5(4) | 14.6(5) | -5.8(4) |
| Si1 | 27.0(8) | 21.8(8) | 22.5(9) | -1.3(6) | 0.0(7) | -5.4(7) |
| O1 | 28(2) | 23(2) | 23(2) | -2.4(17) | -2.6(17) | 0.0(17) |
| O2 | 29(2) | 33(2) | 35(3) | 7(2) | -5.8(19) | -11.6(19) |
| N1 | 31(3) | 46(3) | 26(3) | 2(2) | 6(2) | 17(2) |
| C1 | 26(3) | 26(3) | 20(3) | -1(2) | -1(2) | -5(2) |
| C2 | 34(3) | 25(3) | 21(3) | 0(3) | -1(2) | 1(3) |
| C3 | 56(4) | 28(3) | 30(4) | -4(3) | -2(3) | 10(3) |
| C4 | 56(4) | 21(3) | 32(4) | 2(3) | 3(3) | -9(3) |
| C5 | 34(3) | 28(3) | 30(3) | -4(3) | 3(3) | -12(3) |
| C6 | 50(4) | 40(4) | 29(4) | -4(3) | -19(3) | 2(3) |
| C7 | 42(4) | 73(5) | 37(4) | 8(4) | -17(3) | -2(4) |
| C8 | 69(5) | 63(5) | 51(5) | -6(4) | -25(4) | 33(4) |
| C9 | 99(6) | 47(5) | 37(5) | 21(4) | -28(5) | -9(4) |
| C10 | 56(4) | 55(5) | 27(4) | 9(3) | -3(3) | 2(4) |
| C11 | 23(3) | 48(4) | 23(4) | 8(3) | 1(3) | 9(3) |
| C12 | 69(5) | 54(5) | 34(4) | -14(3) | -12(4) | 32(4) |
| C13 | 22(3) | 89(6) | 35(4) | 31(4) | 10(3) | 11(3) |
| C14 | 42(4) | 20(3) | 29(4) | -7(3) | 7(3) | -10(3) |
| C15 | 66(5) | 24(3) | 38(4) | -7(3) | 19(4) | -7(3) |
| C16 | 80(6) | 31(4) | 70(6) | -19(4) | 49(5) | -17(4) |
| C17 | 50(5) | 38(4) | 110(8) | -35(5) | 35(5) | -17(4) |
| C18 | 35(4) | 27(3) | 60(5) | -16(3) | 7(3) | -7(3) |
| C19 | 76(6) | 25(4) | 72(6) | 4(4) | -24(5) | -21(4) |
| C20 | 91(6) | 29(4) | 63(6) | -16(4) | 39(5) | -20(4) |
| C21 | 168(12) | 38(5) | 90(8) | 20(5) | -79(8) | -46(6) |
| C22 | 53(6) | 18(4) | 220(16) | -20(7) | -2(8) | 6(4) |
| C23 | 134(9) | 36(5) | 91(8) | -38(5) | 67(7) | -35(6) |
| Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
|---|---|---|---|---|---|---|
| Br1 | Zn2 | 2.3504(8) | Si1 | O1 | 1.617(4) | |
| Zn1 | Zn2 | 2.9365(13) | Si1 | O2 | 1.646(4) | |
| Zn1 | O11 | 1.975(4) | Si1 | C1 | 1.854(6) | |
| Zn1 | O1 | 1.975(4) | Si1 | C14 | 1.841(6) | |
| Zn1 | N1 | 2.044(4) | N1 | C11 | 1.514(7) | |
| Zn1 | N11 | 2.044(4) | N1 | C12 | 1.492(8) | |
| Zn2 | Br11 | 2.3504(8) | N1 | C13 | 1.499(7) | |
| Zn2 | O11 | 1.979(4) | C1 | C2 | 1.446(7) | |
| Zn2 | O1 | 1.979(4) | C1 | C5 | 1.428(8) | |
| Fe1 | C1 | 2.045(5) | C2 | C3 | 1.424(8) | |
| Fe1 | C2 | 2.028(6) | C2 | C11 | 1.488(8) | |
| Fe1 | C3 | 2.039(6) | C3 | C4 | 1.409(8) | |
| Fe1 | C4 | 2.054(6) | C4 | C5 | 1.412(8) | |
| Fe1 | C5 | 2.045(6) | C6 | C7 | 1.392(9) | |
| Fe1 | C6 | 2.040(6) | C6 | C10 | 1.403(9) | |
| Fe1 | C7 | 2.041(7) | C7 | C8 | 1.407(10) | |
| Fe1 | C8 | 2.051(7) | C8 | C9 | 1.412(10) | |
| Fe1 | C9 | 2.040(7) | C9 | C10 | 1.386(10) | |
| Fe1 | C10 | 2.048(7) | C14 | C15 | 1.426(8) | |
| Fe2 | C14 | 2.044(5) | C14 | C18 | 1.443(8) | |
| Fe2 | C15 | 2.029(6) | C15 | C16 | 1.414(9) | |
| Fe2 | C16 | 2.038(7) | C16 | C17 | 1.414(11) | |
| Fe2 | C17 | 2.040(7) | C17 | C18 | 1.421(9) | |
| Fe2 | C18 | 2.035(6) | C19 | C20 | 1.374(11) | |
| Fe2 | C19 | 2.037(7) | C19 | C23 | 1.358(11) | |
| Fe2 | C20 | 2.021(7) | C20 | C21 | 1.399(13) | |
| Fe2 | C21 | 2.035(8) | C21 | C22 | 1.443(14) | |
| Fe2 | C22 | 2.006(8) | C22 | C23 | 1.355(14) | |
| Fe2 | C23 | 2.015(8) |
| Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|
| O11 | Zn1 | Zn2 | 42.10(10) | C22 | Fe2 | C19 | 66.6(3) | |
| O1 | Zn1 | Zn2 | 42.10(10) | C22 | Fe2 | C20 | 67.8(4) | |
| O1 | Zn1 | O11 | 84.2(2) | C22 | Fe2 | C21 | 41.8(4) | |
| O1 | Zn1 | N1 | 114.58(18) | C22 | Fe2 | C23 | 39.4(4) | |
| O1 | Zn1 | N11 | 107.67(17) | C23 | Fe2 | C14 | 154.8(5) | |
| O11 | Zn1 | N1 | 107.67(17) | C23 | Fe2 | C15 | 120.1(4) | |
| O11 | Zn1 | N11 | 114.58(18) | C23 | Fe2 | C16 | 107.2(3) | |
| N11 | Zn1 | Zn2 | 119.00(15) | C23 | Fe2 | C17 | 125.0(4) | |
| N1 | Zn1 | Zn2 | 119.00(15) | C23 | Fe2 | C18 | 162.3(4) | |
| N1 | Zn1 | N11 | 122.0(3) | C23 | Fe2 | C19 | 39.2(3) | |
| Br11 | Zn2 | Br1 | 114.02(5) | C23 | Fe2 | C20 | 66.5(3) | |
| Br1 | Zn2 | Zn1 | 122.99(3) | C23 | Fe2 | C21 | 68.0(4) | |
| Br11 | Zn2 | Zn1 | 122.99(3) | O1 | Si1 | O2 | 110.3(2) | |
| O1 | Zn2 | Br11 | 107.65(10) | O1 | Si1 | C1 | 106.3(2) | |
| O11 | Zn2 | Br1 | 107.65(10) | O1 | Si1 | C14 | 109.8(2) | |
| O11 | Zn2 | Br11 | 120.42(10) | O2 | Si1 | C1 | 109.0(2) | |
| O1 | Zn2 | Br1 | 120.42(10) | O2 | Si1 | C14 | 112.7(2) | |
| O11 | Zn2 | Zn1 | 41.99(10) | C14 | Si1 | C1 | 108.6(3) | |
| O1 | Zn2 | Zn1 | 41.99(10) | Zn1 | O1 | Zn2 | 95.92(16) | |
| O1 | Zn2 | O11 | 84.0(2) | Si1 | O1 | Zn1 | 122.8(2) | |
| C1 | Fe1 | C4 | 68.7(2) | Si1 | O1 | Zn2 | 135.5(2) | |
| C1 | Fe1 | C8 | 154.4(3) | C11 | N1 | Zn1 | 109.5(3) | |
| C1 | Fe1 | C10 | 125.4(3) | C12 | N1 | Zn1 | 114.3(4) | |
| C2 | Fe1 | C1 | 41.6(2) | C12 | N1 | C11 | 108.1(5) | |
| C2 | Fe1 | C3 | 41.0(2) | C12 | N1 | C13 | 108.7(5) | |
| C2 | Fe1 | C4 | 68.5(2) | C13 | N1 | Zn1 | 107.2(4) | |
| C2 | Fe1 | C5 | 68.8(2) | C13 | N1 | C11 | 108.9(5) | |
| C2 | Fe1 | C6 | 125.6(2) | Si1 | C1 | Fe1 | 126.4(3) | |
| C2 | Fe1 | C7 | 107.2(3) | C2 | C1 | Fe1 | 68.6(3) | |
| C2 | Fe1 | C8 | 119.7(3) | C2 | C1 | Si1 | 126.6(4) | |
| C2 | Fe1 | C9 | 155.2(3) | C5 | C1 | Fe1 | 69.5(3) | |
| C2 | Fe1 | C10 | 162.9(3) | C5 | C1 | Si1 | 127.0(4) | |
| C3 | Fe1 | C1 | 69.3(2) | C5 | C1 | C2 | 106.4(5) | |
| C3 | Fe1 | C4 | 40.3(2) | C1 | C2 | Fe1 | 69.8(3) | |
| C3 | Fe1 | C5 | 68.2(2) | C1 | C2 | C11 | 125.5(5) | |
| C3 | Fe1 | C6 | 163.0(3) | C3 | C2 | Fe1 | 69.9(3) | |
| C3 | Fe1 | C7 | 126.2(3) | C3 | C2 | C1 | 107.9(5) | |
| C3 | Fe1 | C8 | 108.2(3) | C3 | C2 | C11 | 126.6(5) | |
| C3 | Fe1 | C9 | 121.3(3) | C11 | C2 | Fe1 | 125.6(4) | |
| C3 | Fe1 | C10 | 155.2(3) | C2 | C3 | Fe1 | 69.1(3) | |
| C5 | Fe1 | C1 | 40.9(2) | C4 | C3 | Fe1 | 70.5(4) | |
| C5 | Fe1 | C4 | 40.3(2) | C4 | C3 | C2 | 108.3(5) | |
| C5 | Fe1 | C8 | 163.7(3) | C3 | C4 | Fe1 | 69.3(4) | |
| C5 | Fe1 | C10 | 108.5(3) | C3 | C4 | C5 | 108.4(5) | |
| C6 | Fe1 | C1 | 107.3(2) | C5 | C4 | Fe1 | 69.5(3) | |
| C6 | Fe1 | C4 | 155.4(3) | C1 | C5 | Fe1 | 69.6(3) | |
| C6 | Fe1 | C5 | 120.8(3) | C4 | C5 | Fe1 | 70.2(4) | |
| C6 | Fe1 | C7 | 39.9(3) | C4 | C5 | C1 | 109.0(5) | |
| C6 | Fe1 | C8 | 67.3(3) | C7 | C6 | Fe1 | 70.1(4) | |
| C6 | Fe1 | C10 | 40.1(3) | C7 | C6 | C10 | 108.9(6) | |
| C7 | Fe1 | C1 | 119.4(3) | C10 | C6 | Fe1 | 70.3(4) | |
| C7 | Fe1 | C4 | 163.5(3) | C6 | C7 | Fe1 | 70.0(4) | |
| C7 | Fe1 | C5 | 154.7(3) | C6 | C7 | C8 | 108.1(7) | |
| C7 | Fe1 | C8 | 40.2(3) | C8 | C7 | Fe1 | 70.3(4) | |
| C7 | Fe1 | C10 | 67.6(3) | C7 | C8 | Fe1 | 69.5(4) | |
| C8 | Fe1 | C4 | 126.8(3) | C7 | C8 | C9 | 106.6(7) | |
| C9 | Fe1 | C1 | 162.7(3) | C9 | C8 | Fe1 | 69.4(4) | |
| C9 | Fe1 | C4 | 109.6(3) | C8 | C9 | Fe1 | 70.2(4) | |
| C9 | Fe1 | C5 | 126.7(3) | C10 | C9 | Fe1 | 70.5(4) | |
| C9 | Fe1 | C6 | 66.7(3) | C10 | C9 | C8 | 109.4(6) | |
| C9 | Fe1 | C7 | 67.3(3) | C6 | C10 | Fe1 | 69.6(4) | |
| C9 | Fe1 | C8 | 40.4(3) | C9 | C10 | Fe1 | 69.8(4) | |
| C9 | Fe1 | C10 | 39.6(3) | C9 | C10 | C6 | 107.0(6) | |
| C10 | Fe1 | C4 | 121.2(3) | C2 | C11 | N1 | 113.4(5) | |
| C10 | Fe1 | C8 | 67.7(3) | Si1 | C14 | Fe2 | 127.7(3) | |
| C15 | Fe2 | C14 | 41.0(2) | C15 | C14 | Fe2 | 68.9(3) | |
| C15 | Fe2 | C16 | 40.7(3) | C15 | C14 | Si1 | 128.1(5) | |
| C15 | Fe2 | C17 | 68.5(3) | C15 | C14 | C18 | 106.0(6) | |
| C15 | Fe2 | C18 | 68.6(3) | C18 | C14 | Fe2 | 69.0(3) | |
| C15 | Fe2 | C19 | 109.4(3) | C18 | C14 | Si1 | 125.9(5) | |
| C15 | Fe2 | C21 | 164.4(5) | C14 | C15 | Fe2 | 70.1(4) | |
| C16 | Fe2 | C14 | 69.2(2) | C16 | C15 | Fe2 | 70.0(4) | |
| C16 | Fe2 | C17 | 40.6(3) | C16 | C15 | C14 | 109.3(7) | |
| C17 | Fe2 | C14 | 69.5(3) | C15 | C16 | Fe2 | 69.3(4) | |
| C18 | Fe2 | C14 | 41.4(2) | C17 | C16 | Fe2 | 69.8(4) | |
| C18 | Fe2 | C16 | 68.5(3) | C17 | C16 | C15 | 108.2(7) | |
| C18 | Fe2 | C17 | 40.8(3) | C16 | C17 | Fe2 | 69.6(4) | |
| C18 | Fe2 | C19 | 156.8(3) | C16 | C17 | C18 | 107.9(7) | |
| C19 | Fe2 | C14 | 121.7(3) | C18 | C17 | Fe2 | 69.4(4) | |
| C19 | Fe2 | C16 | 126.1(4) | C14 | C18 | Fe2 | 69.6(3) | |
| C19 | Fe2 | C17 | 161.8(4) | C17 | C18 | Fe2 | 69.8(4) | |
| C20 | Fe2 | C14 | 109.6(3) | C17 | C18 | C14 | 108.7(7) | |
| C20 | Fe2 | C15 | 127.7(3) | C20 | C19 | Fe2 | 69.6(4) | |
| C20 | Fe2 | C16 | 163.5(4) | C23 | C19 | Fe2 | 69.5(5) | |
| C20 | Fe2 | C17 | 155.6(4) | C23 | C19 | C20 | 108.1(8) | |
| C20 | Fe2 | C18 | 122.2(3) | C19 | C20 | Fe2 | 70.8(4) | |
| C20 | Fe2 | C19 | 39.6(3) | C19 | C20 | C21 | 109.5(8) | |
| C20 | Fe2 | C21 | 40.4(4) | C21 | C20 | Fe2 | 70.4(5) | |
| C21 | Fe2 | C14 | 126.4(4) | C20 | C21 | Fe2 | 69.3(5) | |
| C21 | Fe2 | C16 | 153.6(5) | C20 | C21 | C22 | 104.4(8) | |
| C21 | Fe2 | C17 | 119.4(4) | C22 | C21 | Fe2 | 68.0(5) | |
| C21 | Fe2 | C18 | 107.8(3) | C21 | C22 | Fe2 | 70.2(5) | |
| C21 | Fe2 | C19 | 67.6(3) | C23 | C22 | Fe2 | 70.7(5) | |
| C22 | Fe2 | C14 | 164.7(5) | C23 | C22 | C21 | 108.0(9) | |
| C22 | Fe2 | C15 | 152.5(5) | C19 | C23 | Fe2 | 71.3(4) | |
| C22 | Fe2 | C16 | 117.8(4) | C22 | C23 | Fe2 | 69.9(5) | |
| C22 | Fe2 | C17 | 106.4(3) | C22 | C23 | C19 | 109.9(9) | |
| C22 | Fe2 | C18 | 126.1(4) |
| A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|---|---|
| Zn1 | N1 | C11 | C2 | -50.1(6) | C1 | C2 | C3 | C4 | -0.1(7) | |
| Fe1 | C1 | C2 | C3 | -59.8(4) | C1 | C2 | C11 | N1 | 87.4(7) | |
| Fe1 | C1 | C2 | C11 | 120.0(6) | C2 | C1 | C5 | Fe1 | -58.9(4) | |
| Fe1 | C1 | C5 | C4 | 59.3(4) | C2 | C1 | C5 | C4 | 0.4(6) | |
| Fe1 | C2 | C3 | C4 | -59.8(4) | C2 | C3 | C4 | Fe1 | 58.9(4) | |
| Fe1 | C2 | C11 | N1 | 176.8(4) | C2 | C3 | C4 | C5 | 0.3(7) | |
| Fe1 | C3 | C4 | C5 | -58.6(4) | C3 | C2 | C11 | N1 | -92.9(7) | |
| Fe1 | C4 | C5 | C1 | -59.0(4) | C3 | C4 | C5 | Fe1 | 58.5(4) | |
| Fe1 | C6 | C7 | C8 | 60.2(5) | C3 | C4 | C5 | C1 | -0.5(7) | |
| Fe1 | C6 | C10 | C9 | -60.1(5) | C5 | C1 | C2 | Fe1 | 59.5(4) | |
| Fe1 | C7 | C8 | C9 | 59.7(5) | C5 | C1 | C2 | C3 | -0.2(6) | |
| Fe1 | C8 | C9 | C10 | 59.9(5) | C5 | C1 | C2 | C11 | 179.5(5) | |
| Fe1 | C9 | C10 | C6 | 59.9(5) | C6 | C7 | C8 | Fe1 | -60.1(4) | |
| Fe2 | C14 | C15 | C16 | -59.2(4) | C6 | C7 | C8 | C9 | -0.3(8) | |
| Fe2 | C14 | C18 | C17 | 59.0(4) | C7 | C6 | C10 | Fe1 | 59.7(4) | |
| Fe2 | C15 | C16 | C17 | -59.2(5) | C7 | C6 | C10 | C9 | -0.4(8) | |
| Fe2 | C16 | C17 | C18 | -59.1(5) | C7 | C8 | C9 | Fe1 | -59.8(5) | |
| Fe2 | C17 | C18 | C14 | -58.9(4) | C7 | C8 | C9 | C10 | 0.1(8) | |
| Fe2 | C19 | C20 | C21 | -60.0(5) | C8 | C9 | C10 | Fe1 | -59.7(5) | |
| Fe2 | C19 | C23 | C22 | 59.5(6) | C8 | C9 | C10 | C6 | 0.2(8) | |
| Fe2 | C20 | C21 | C22 | -59.2(5) | C10 | C6 | C7 | Fe1 | -59.8(4) | |
| Fe2 | C21 | C22 | C23 | -60.9(6) | C10 | C6 | C7 | C8 | 0.5(7) | |
| Fe2 | C22 | C23 | C19 | -60.3(6) | C11 | C2 | C3 | Fe1 | -120.0(6) | |
| Si1 | C1 | C2 | Fe1 | -120.2(4) | C11 | C2 | C3 | C4 | -179.8(6) | |
| Si1 | C1 | C2 | C3 | -179.9(4) | C12 | N1 | C11 | C2 | 75.0(6) | |
| Si1 | C1 | C2 | C11 | -0.2(8) | C13 | N1 | C11 | C2 | -167.0(5) | |
| Si1 | C1 | C5 | Fe1 | 120.8(4) | C14 | Si1 | O1 | Zn1 | 127.6(3) | |
| Si1 | C1 | C5 | C4 | -179.9(4) | C14 | Si1 | O1 | Zn2 | -86.3(3) | |
| Si1 | C14 | C15 | Fe2 | -122.1(5) | C14 | Si1 | C1 | Fe1 | 94.6(4) | |
| Si1 | C14 | C15 | C16 | 178.7(4) | C14 | Si1 | C1 | C2 | -176.5(5) | |
| Si1 | C14 | C18 | Fe2 | 122.1(4) | C14 | Si1 | C1 | C5 | 3.9(6) | |
| Si1 | C14 | C18 | C17 | -178.9(4) | C14 | C15 | C16 | Fe2 | 59.2(4) | |
| O1 | Si1 | C1 | Fe1 | -147.4(3) | C14 | C15 | C16 | C17 | 0.0(7) | |
| O1 | Si1 | C1 | C2 | -58.5(5) | C15 | C14 | C18 | Fe2 | -59.3(4) | |
| O1 | Si1 | C1 | C5 | 121.9(5) | C15 | C14 | C18 | C17 | -0.3(7) | |
| O1 | Si1 | C14 | Fe2 | 85.8(4) | C15 | C16 | C17 | Fe2 | 58.9(5) | |
| O1 | Si1 | C14 | C15 | 177.5(5) | C15 | C16 | C17 | C18 | -0.2(8) | |
| O1 | Si1 | C14 | C18 | -4.2(5) | C16 | C17 | C18 | Fe2 | 59.2(5) | |
| O2 | Si1 | O1 | Zn1 | -107.6(3) | C16 | C17 | C18 | C14 | 0.3(7) | |
| O2 | Si1 | O1 | Zn2 | 38.5(4) | C18 | C14 | C15 | Fe2 | 59.3(4) | |
| O2 | Si1 | C1 | Fe1 | -28.6(4) | C18 | C14 | C15 | C16 | 0.2(7) | |
| O2 | Si1 | C1 | C2 | 60.4(5) | C19 | C20 | C21 | Fe2 | 60.2(5) | |
| O2 | Si1 | C1 | C5 | -119.3(5) | C19 | C20 | C21 | C22 | 1.0(9) | |
| O2 | Si1 | C14 | Fe2 | -37.6(5) | C20 | C19 | C23 | Fe2 | -59.1(5) | |
| O2 | Si1 | C14 | C15 | 54.1(6) | C20 | C19 | C23 | C22 | 0.4(9) | |
| O2 | Si1 | C14 | C18 | -127.6(5) | C20 | C21 | C22 | Fe2 | 60.1(5) | |
| C1 | Si1 | O1 | Zn1 | 10.4(3) | C20 | C21 | C22 | C23 | -0.8(9) | |
| C1 | Si1 | O1 | Zn2 | 156.5(3) | C21 | C22 | C23 | Fe2 | 60.6(6) | |
| C1 | Si1 | C14 | Fe2 | -158.4(4) | C21 | C22 | C23 | C19 | 0.2(10) | |
| C1 | Si1 | C14 | C15 | -66.7(6) | C23 | C19 | C20 | Fe2 | 59.0(5) | |
| C1 | Si1 | C14 | C18 | 111.5(5) | C23 | C19 | C20 | C21 | -0.9(9) | |
| C1 | C2 | C3 | Fe1 | 59.7(4) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| H2 | -1370(40) | 1310(60) | 1550(20) | 100(30) |
| H3 | -1083 | 6744 | 1514 | 46 |
| H4 | 99 | 6704 | 891 | 44 |
| H5 | 640 | 4585 | 817 | 37 |
| H6 | -1521 | 2737 | 509 | 48 |
| H7 | -2621 | 3821 | 1002 | 61 |
| H8 | -2624 | 5993 | 738 | 73 |
| H9 | -1497 | 6207 | 85 | 73 |
| H10 | -814 | 4212 | -55 | 55 |
| H11A | -1699 | 3665 | 1899 | 38 |
| H11B | -2011 | 5020 | 1962 | 38 |
| H12A | -851 | 5811 | 2975 | 79 |
| H12B | -1674 | 6124 | 2653 | 79 |
| H12C | -734 | 6232 | 2424 | 79 |
| H13A | -1791 | 3007 | 2707 | 73 |
| H13B | -2314 | 4217 | 2803 | 73 |
| H13C | -1527 | 3867 | 3147 | 73 |
| H15 | 391 | 2128 | 348 | 51 |
| H16 | 1850 | 1358 | 109 | 73 |
| H17 | 2694 | 947 | 875 | 79 |
| H18 | 1754 | 1479 | 1592 | 49 |
| H19 | -424 | -645 | 448 | 69 |
| H20 | -304 | -659 | 1345 | 73 |
| H21 | 1180 | -1371 | 1576 | 118 |
| H22 | 1969 | -1725 | 765 | 116 |
| H23 | 960 | -1277 | 104 | 104 |
Experimental
Single crystals of C46H52Br2Fe4N2O4Si2Zn2 [3091] were []. A suitable crystal was selected and [] on a Xcalibur, Sapphire3 diffractometer. The crystal was kept at 173 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 [3091]
Crystal Data for C46H52Br2Fe4N2O4Si2Zn2 (M =1267.03 g/mol): orthorhombic, space group Pbcn (no. 60), a = 15.5968(12) Å, b = 11.1687(9) Å, c = 27.587(2) Å, V = 4805.5(7) Å3, Z = 4, T = 173 K, μ(MoKα) = 3.915 mm-1, Dcalc = 1.751 g/cm3, 17657 reflections measured (4.486° ≤ 2Θ ≤ 51.992°), 4721 unique (Rint = 0.0611, Rsigma = 0.0644) which were used in all calculations. The final R1 was 0.0532 (I > 2σ(I)) and wR2 was 0.1182 (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.