| Identification code | 3161 |
| Empirical formula | C46H48Cl2Fe2N2O4Si2Zn2 |
| Formula weight | 1062.38 |
| Temperature/K | 173 |
| Crystal system | monoclinic |
| Space group | P21/c |
| a/Å | 12.1868(6) |
| b/Å | 10.3523(4) |
| c/Å | 18.1265(8) |
| α/° | 90 |
| β/° | 99.579(4) |
| γ/° | 90 |
| Volume/Å3 | 2254.98(18) |
| Z | 2 |
| ρcalcg/cm3 | 1.565 |
| μ/mm‑1 | 1.898 |
| F(000) | 1088.0 |
| Crystal size/mm3 | 0.106 × 0.094 × 0.056 |
| Radiation | MoKα (λ = 0.71073) |
| 2Θ range for data collection/° | 4.546 to 53.996 |
| Index ranges | -15 ≤ h ≤ 15, -13 ≤ k ≤ 13, -23 ≤ l ≤ 22 |
| Reflections collected | 20568 |
| Independent reflections | 4909 [Rint = 0.0476, Rsigma = 0.0446] |
| Data/restraints/parameters | 4909/1/277 |
| Goodness-of-fit on F2 | 1.032 |
| Final R indexes [I>=2σ (I)] | R1 = 0.0373, wR2 = 0.0793 |
| Final R indexes [all data] | R1 = 0.0536, wR2 = 0.0857 |
| Largest diff. peak/hole / e Å-3 | 0.81/-0.34 |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| Zn1 | 9712.6(3) | 153.1(3) | 750.4(2) | 19.86(9) |
| Fe1 | 13418.2(3) | -702.9(4) | 2494.5(2) | 22.81(11) |
| Cl1 | 8863.8(8) | 1856.1(8) | 1139.0(5) | 40.1(2) |
| Si1 | 12322.7(6) | 274.3(7) | 671.7(4) | 19.20(17) |
| O1 | 11031.0(15) | 353.4(17) | 269.4(10) | 20.2(4) |
| O2 | 12881.5(18) | -1057.4(19) | 408.8(12) | 30.1(5) |
| N1 | 9857(2) | -1329(2) | 1523.9(13) | 24.5(5) |
| C1 | 12359(2) | 283(2) | 1691.4(16) | 20.8(6) |
| C2 | 11758(2) | -574(3) | 2121.1(15) | 20.0(6) |
| C3 | 12008(2) | -195(3) | 2889.7(16) | 25.8(6) |
| C4 | 12742(2) | 874(3) | 2942.7(17) | 27.5(7) |
| C5 | 12961(2) | 1164(3) | 2218.2(16) | 25.1(6) |
| C6 | 14110(3) | -2233(3) | 2034.4(18) | 34.0(8) |
| C7 | 13864(3) | -2573(3) | 2738(2) | 40.5(8) |
| C8 | 14471(3) | -1744(4) | 3269.3(19) | 46.3(10) |
| C9 | 15081(3) | -902(4) | 2901(2) | 48.8(10) |
| C10 | 14863(3) | -1199(3) | 2139(2) | 43.2(9) |
| C11 | 11052(2) | -1685(3) | 1805.7(16) | 23.4(6) |
| C12 | 9296(3) | -2492(3) | 1149.8(18) | 37.1(8) |
| C13 | 9304(3) | -978(4) | 2168.3(18) | 38.4(8) |
| C14 | 13090(2) | 1693(3) | 371.1(15) | 21.8(6) |
| C15 | 13997(2) | 1458(3) | 24.9(17) | 29.5(7) |
| C16 | 14554(3) | 2457(3) | -289.0(18) | 36.0(8) |
| C17 | 14177(3) | 3686(3) | -275.5(17) | 34.4(8) |
| C18 | 13254(3) | 4004(3) | 68.7(16) | 27.8(7) |
| C19 | 12827(3) | 5276(3) | 65.7(19) | 39.9(8) |
| C20 | 11927(3) | 5552(3) | 385(2) | 47(1) |
| C21 | 11408(3) | 4580(3) | 743(2) | 40.9(9) |
| C22 | 11799(3) | 3336(3) | 758.6(17) | 28.3(7) |
| C23 | 12718(2) | 2999(3) | 414.9(15) | 21.8(6) |
| Atom | U11 | U22 | U33 | U23 | U13 | U12 |
|---|---|---|---|---|---|---|
| Zn1 | 22.77(18) | 20.35(17) | 15.91(17) | 0.49(12) | 1.59(13) | 0.35(13) |
| Fe1 | 25.0(2) | 22.9(2) | 18.5(2) | 0.80(16) | -2.44(16) | 4.38(17) |
| Cl1 | 54.5(5) | 32.2(4) | 34.1(5) | -8.2(3) | 8.4(4) | 12.8(4) |
| Si1 | 20.9(4) | 16.7(4) | 19.1(4) | 1.8(3) | 0.8(3) | 1.4(3) |
| O1 | 21.3(10) | 21.3(10) | 16.8(10) | 1.6(7) | 0.0(8) | -0.8(8) |
| O2 | 36.9(13) | 24.1(11) | 28.4(12) | 0.8(9) | 2.8(10) | 10.7(9) |
| N1 | 25.7(13) | 28.1(13) | 19.2(13) | 5.7(10) | 2.1(10) | -4.9(10) |
| C1 | 20.3(14) | 17.7(13) | 22.7(15) | 2.7(11) | -1.4(11) | 2.3(11) |
| C2 | 21.0(14) | 20.7(14) | 17.1(14) | 2.3(11) | -0.1(11) | 2.8(11) |
| C3 | 27.3(16) | 29.5(15) | 19.4(15) | 2.6(12) | 0.5(12) | 6.3(13) |
| C4 | 31.0(16) | 24.6(15) | 23.1(16) | -6.3(12) | -6.9(13) | 6.0(13) |
| C5 | 25.2(15) | 20.3(14) | 27.3(16) | 0.1(12) | -3.1(13) | -0.9(12) |
| C6 | 37.4(19) | 31.0(17) | 30.3(18) | -5.9(13) | -3.6(14) | 15.6(14) |
| C7 | 45(2) | 25.2(17) | 53(2) | 10.8(15) | 11.4(18) | 13.8(15) |
| C8 | 58(2) | 50(2) | 26.2(19) | 2.2(16) | -8.0(17) | 36.7(19) |
| C9 | 30.0(19) | 41(2) | 68(3) | -11.4(19) | -14.0(18) | 12.0(16) |
| C10 | 34.3(19) | 47(2) | 50(2) | 5.8(17) | 11.5(17) | 15.1(17) |
| C11 | 26.6(15) | 19.7(14) | 23.3(15) | 5.1(11) | 2.4(12) | -2.2(12) |
| C12 | 38.8(19) | 31.5(17) | 36.1(19) | 9.0(14) | -7.6(15) | -16.0(15) |
| C13 | 29.6(18) | 59(2) | 28.2(18) | 13.9(16) | 11.0(14) | 2.8(16) |
| C14 | 19.2(14) | 26.9(15) | 17.0(14) | 3.3(11) | -3.8(11) | -2.7(12) |
| C15 | 21.0(15) | 39.1(18) | 28.2(17) | 3.8(13) | 2.9(13) | 3.9(13) |
| C16 | 23.9(17) | 56(2) | 29.5(18) | 3.3(15) | 8.4(14) | -3.8(15) |
| C17 | 30.7(18) | 46(2) | 25.6(17) | 8.4(14) | 3.1(14) | -16.2(15) |
| C18 | 31.4(17) | 29.3(16) | 21.0(15) | 2.9(12) | -0.2(13) | -10.3(13) |
| C19 | 56(2) | 25.5(16) | 37(2) | 6.1(14) | 5.8(17) | -12.8(16) |
| C20 | 70(3) | 19.4(16) | 54(2) | 4.1(15) | 19(2) | 2.4(17) |
| C21 | 56(2) | 25.7(17) | 46(2) | 0.8(15) | 21.9(18) | 8.7(16) |
| C22 | 34.1(17) | 21.7(15) | 30.3(17) | 0.0(12) | 8.8(14) | -4.5(13) |
| C23 | 23.9(15) | 21.6(14) | 18.6(14) | 2.3(11) | -0.3(12) | -3.1(12) |
| Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
|---|---|---|---|---|---|---|
| Zn1 | Zn11 | 2.9371(6) | C1 | C2 | 1.455(4) | |
| Zn1 | Cl1 | 2.2174(8) | C1 | C5 | 1.431(4) | |
| Zn1 | O11 | 1.9888(19) | C2 | C3 | 1.431(4) | |
| Zn1 | O1 | 1.9624(19) | C2 | C11 | 1.492(4) | |
| Zn1 | N1 | 2.066(2) | C3 | C4 | 1.417(4) | |
| Fe1 | C1 | 2.050(3) | C4 | C5 | 1.415(4) | |
| Fe1 | C2 | 2.028(3) | C6 | C7 | 1.403(5) | |
| Fe1 | C3 | 2.038(3) | C6 | C10 | 1.402(5) | |
| Fe1 | C4 | 2.056(3) | C7 | C8 | 1.405(5) | |
| Fe1 | C5 | 2.050(3) | C8 | C9 | 1.387(5) | |
| Fe1 | C6 | 2.037(3) | C9 | C10 | 1.397(5) | |
| Fe1 | C7 | 2.039(3) | C14 | C15 | 1.380(4) | |
| Fe1 | C8 | 2.045(3) | C14 | C23 | 1.433(4) | |
| Fe1 | C9 | 2.048(3) | C15 | C16 | 1.408(4) | |
| Fe1 | C10 | 2.039(3) | C16 | C17 | 1.355(5) | |
| Si1 | O1 | 1.623(2) | C17 | C18 | 1.413(4) | |
| Si1 | O2 | 1.643(2) | C18 | C19 | 1.415(4) | |
| Si1 | C1 | 1.841(3) | C18 | C23 | 1.429(4) | |
| Si1 | C14 | 1.870(3) | C19 | C20 | 1.353(5) | |
| O1 | Zn11 | 1.9889(19) | C20 | C21 | 1.404(5) | |
| N1 | C11 | 1.507(4) | C21 | C22 | 1.371(4) | |
| N1 | C12 | 1.490(4) | C22 | C23 | 1.413(4) | |
| N1 | C13 | 1.487(4) |
| Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|
| Cl1 | Zn1 | Zn11 | 125.16(3) | Si1 | O1 | Zn1 | 126.84(11) | |
| O1 | Zn1 | Zn11 | 42.33(5) | Si1 | O1 | Zn11 | 131.46(11) | |
| O11 | Zn1 | Zn11 | 41.64(5) | C11 | N1 | Zn1 | 112.30(16) | |
| O1 | Zn1 | Cl1 | 121.12(6) | C12 | N1 | Zn1 | 108.08(17) | |
| O11 | Zn1 | Cl1 | 109.90(6) | C12 | N1 | C11 | 107.5(2) | |
| O1 | Zn1 | O11 | 83.97(8) | C13 | N1 | Zn1 | 110.66(19) | |
| O11 | Zn1 | N1 | 114.14(8) | C13 | N1 | C11 | 109.4(2) | |
| O1 | Zn1 | N1 | 113.36(8) | C13 | N1 | C12 | 108.8(2) | |
| N1 | Zn1 | Zn11 | 122.81(7) | Si1 | C1 | Fe1 | 128.13(15) | |
| N1 | Zn1 | Cl1 | 111.49(7) | C2 | C1 | Fe1 | 68.28(15) | |
| C1 | Fe1 | C4 | 68.83(11) | C2 | C1 | Si1 | 127.2(2) | |
| C2 | Fe1 | C1 | 41.82(11) | C5 | C1 | Fe1 | 69.57(16) | |
| C2 | Fe1 | C3 | 41.20(11) | C5 | C1 | Si1 | 126.6(2) | |
| C2 | Fe1 | C4 | 68.70(11) | C5 | C1 | C2 | 106.2(2) | |
| C2 | Fe1 | C5 | 68.95(11) | C1 | C2 | Fe1 | 69.90(15) | |
| C2 | Fe1 | C6 | 111.85(12) | C1 | C2 | C11 | 125.0(2) | |
| C2 | Fe1 | C7 | 110.46(13) | C3 | C2 | Fe1 | 69.78(16) | |
| C2 | Fe1 | C8 | 137.83(15) | C3 | C2 | C1 | 108.0(2) | |
| C2 | Fe1 | C9 | 177.43(14) | C3 | C2 | C11 | 126.9(2) | |
| C2 | Fe1 | C10 | 140.99(14) | C11 | C2 | Fe1 | 123.84(19) | |
| C3 | Fe1 | C1 | 69.69(11) | C2 | C3 | Fe1 | 69.02(16) | |
| C3 | Fe1 | C4 | 40.49(11) | C4 | C3 | Fe1 | 70.45(17) | |
| C3 | Fe1 | C5 | 68.39(12) | C4 | C3 | C2 | 108.1(3) | |
| C3 | Fe1 | C7 | 112.24(13) | C3 | C4 | Fe1 | 69.06(16) | |
| C3 | Fe1 | C8 | 111.36(14) | C5 | C4 | Fe1 | 69.62(16) | |
| C3 | Fe1 | C9 | 137.84(14) | C5 | C4 | C3 | 108.5(3) | |
| C3 | Fe1 | C10 | 177.81(14) | C1 | C5 | Fe1 | 69.56(15) | |
| C5 | Fe1 | C1 | 40.86(11) | C4 | C5 | Fe1 | 70.08(16) | |
| C5 | Fe1 | C4 | 40.31(11) | C4 | C5 | C1 | 109.3(3) | |
| C6 | Fe1 | C1 | 110.54(12) | C7 | C6 | Fe1 | 69.95(18) | |
| C6 | Fe1 | C3 | 140.82(13) | C10 | C6 | Fe1 | 69.97(18) | |
| C6 | Fe1 | C4 | 178.46(13) | C10 | C6 | C7 | 107.6(3) | |
| C6 | Fe1 | C5 | 138.34(13) | C6 | C7 | Fe1 | 69.77(17) | |
| C6 | Fe1 | C7 | 40.27(13) | C6 | C7 | C8 | 107.6(3) | |
| C6 | Fe1 | C8 | 67.42(13) | C8 | C7 | Fe1 | 70.10(18) | |
| C6 | Fe1 | C9 | 67.49(14) | C7 | C8 | Fe1 | 69.66(18) | |
| C6 | Fe1 | C10 | 40.24(14) | C9 | C8 | Fe1 | 70.3(2) | |
| C7 | Fe1 | C1 | 137.72(13) | C9 | C8 | C7 | 108.5(3) | |
| C7 | Fe1 | C4 | 141.09(13) | C8 | C9 | Fe1 | 70.1(2) | |
| C7 | Fe1 | C5 | 178.38(13) | C8 | C9 | C10 | 108.0(3) | |
| C7 | Fe1 | C8 | 40.24(14) | C10 | C9 | Fe1 | 69.7(2) | |
| C7 | Fe1 | C9 | 67.35(15) | C6 | C10 | Fe1 | 69.79(19) | |
| C7 | Fe1 | C10 | 67.45(14) | C9 | C10 | Fe1 | 70.4(2) | |
| C8 | Fe1 | C1 | 177.85(13) | C9 | C10 | C6 | 108.3(3) | |
| C8 | Fe1 | C4 | 113.22(13) | C2 | C11 | N1 | 113.9(2) | |
| C8 | Fe1 | C5 | 141.16(14) | C15 | C14 | Si1 | 118.1(2) | |
| C8 | Fe1 | C9 | 39.62(15) | C15 | C14 | C23 | 118.4(3) | |
| C9 | Fe1 | C1 | 140.72(15) | C23 | C14 | Si1 | 123.2(2) | |
| C9 | Fe1 | C4 | 112.03(13) | C14 | C15 | C16 | 122.1(3) | |
| C9 | Fe1 | C5 | 113.28(14) | C17 | C16 | C15 | 119.7(3) | |
| C10 | Fe1 | C1 | 112.08(13) | C16 | C17 | C18 | 121.6(3) | |
| C10 | Fe1 | C4 | 138.49(14) | C17 | C18 | C19 | 122.3(3) | |
| C10 | Fe1 | C5 | 111.98(13) | C17 | C18 | C23 | 118.7(3) | |
| C10 | Fe1 | C8 | 66.91(15) | C19 | C18 | C23 | 119.0(3) | |
| C10 | Fe1 | C9 | 39.97(15) | C20 | C19 | C18 | 121.3(3) | |
| O1 | Si1 | O2 | 109.25(11) | C19 | C20 | C21 | 120.4(3) | |
| O1 | Si1 | C1 | 108.07(11) | C22 | C21 | C20 | 120.0(3) | |
| O1 | Si1 | C14 | 108.90(11) | C21 | C22 | C23 | 121.4(3) | |
| O2 | Si1 | C1 | 110.69(12) | C18 | C23 | C14 | 119.4(3) | |
| O2 | Si1 | C14 | 108.84(12) | C22 | C23 | C14 | 122.6(2) | |
| C1 | Si1 | C14 | 111.05(12) | C22 | C23 | C18 | 117.9(3) | |
| Zn1 | O1 | Zn11 | 96.03(8) |
| D | H | A | d(D-H)/Å | d(H-A)/Å | d(D-A)/Å | D-H-A/° |
|---|---|---|---|---|---|---|
| O2 | H2 | Cl11 | 0.970(19) | 2.44(3) | 3.331(2) | 153(4) |
| A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|---|---|
| Zn1 | N1 | C11 | C2 | 54.8(3) | C3 | C2 | C11 | N1 | 94.5(3) | |
| Fe1 | C1 | C2 | C3 | 59.58(19) | C3 | C4 | C5 | Fe1 | -58.3(2) | |
| Fe1 | C1 | C2 | C11 | -117.9(3) | C3 | C4 | C5 | C1 | 0.4(3) | |
| Fe1 | C1 | C5 | C4 | -59.0(2) | C5 | C1 | C2 | Fe1 | -59.55(18) | |
| Fe1 | C2 | C3 | C4 | 59.9(2) | C5 | C1 | C2 | C3 | 0.0(3) | |
| Fe1 | C2 | C11 | N1 | -176.53(17) | C5 | C1 | C2 | C11 | -177.4(3) | |
| Fe1 | C3 | C4 | C5 | 58.6(2) | C6 | C7 | C8 | Fe1 | 60.0(2) | |
| Fe1 | C4 | C5 | C1 | 58.66(19) | C6 | C7 | C8 | C9 | 0.2(4) | |
| Fe1 | C6 | C7 | C8 | -60.2(2) | C7 | C6 | C10 | Fe1 | -60.1(2) | |
| Fe1 | C6 | C10 | C9 | 60.0(2) | C7 | C6 | C10 | C9 | 0.0(4) | |
| Fe1 | C7 | C8 | C9 | -59.8(2) | C7 | C8 | C9 | Fe1 | 59.4(2) | |
| Fe1 | C8 | C9 | C10 | -59.6(2) | C7 | C8 | C9 | C10 | -0.2(4) | |
| Fe1 | C9 | C10 | C6 | -59.7(2) | C8 | C9 | C10 | Fe1 | 59.9(2) | |
| Si1 | C1 | C2 | Fe1 | 122.1(2) | C8 | C9 | C10 | C6 | 0.2(4) | |
| Si1 | C1 | C2 | C3 | -178.3(2) | C10 | C6 | C7 | Fe1 | 60.1(2) | |
| Si1 | C1 | C2 | C11 | 4.3(4) | C10 | C6 | C7 | C8 | -0.1(3) | |
| Si1 | C1 | C5 | Fe1 | -123.0(2) | C11 | C2 | C3 | Fe1 | 117.8(3) | |
| Si1 | C1 | C5 | C4 | 178.1(2) | C11 | C2 | C3 | C4 | 177.6(3) | |
| Si1 | C14 | C15 | C16 | 173.3(2) | C12 | N1 | C11 | C2 | 173.5(2) | |
| Si1 | C14 | C23 | C18 | -170.4(2) | C13 | N1 | C11 | C2 | -68.5(3) | |
| Si1 | C14 | C23 | C22 | 6.5(4) | C14 | Si1 | O1 | Zn11 | 81.42(16) | |
| O1 | Si1 | C1 | Fe1 | 143.60(16) | C14 | Si1 | O1 | Zn1 | -131.75(14) | |
| O1 | Si1 | C1 | C2 | 53.3(3) | C14 | Si1 | C1 | Fe1 | -97.02(19) | |
| O1 | Si1 | C1 | C5 | -124.6(2) | C14 | Si1 | C1 | C2 | 172.7(2) | |
| O1 | Si1 | C14 | C15 | -122.0(2) | C14 | Si1 | C1 | C5 | -5.3(3) | |
| O1 | Si1 | C14 | C23 | 51.6(3) | C14 | C15 | C16 | C17 | -2.1(5) | |
| O2 | Si1 | O1 | Zn1 | 109.49(14) | C15 | C14 | C23 | C18 | 3.2(4) | |
| O2 | Si1 | O1 | Zn11 | -37.35(17) | C15 | C14 | C23 | C22 | -179.9(3) | |
| O2 | Si1 | C1 | Fe1 | 24.0(2) | C15 | C16 | C17 | C18 | 2.1(5) | |
| O2 | Si1 | C1 | C2 | -66.3(3) | C16 | C17 | C18 | C19 | -177.8(3) | |
| O2 | Si1 | C1 | C5 | 115.8(2) | C16 | C17 | C18 | C23 | 0.5(5) | |
| O2 | Si1 | C14 | C15 | -3.0(3) | C17 | C18 | C19 | C20 | 178.5(3) | |
| O2 | Si1 | C14 | C23 | 170.6(2) | C17 | C18 | C23 | C14 | -3.2(4) | |
| C1 | Si1 | O1 | Zn11 | -157.85(14) | C17 | C18 | C23 | C22 | 179.8(3) | |
| C1 | Si1 | O1 | Zn1 | -11.01(16) | C18 | C19 | C20 | C21 | 1.3(6) | |
| C1 | Si1 | C14 | C15 | 119.1(2) | C19 | C18 | C23 | C14 | 175.2(3) | |
| C1 | Si1 | C14 | C23 | -67.3(3) | C19 | C18 | C23 | C22 | -1.8(4) | |
| C1 | C2 | C3 | Fe1 | -59.66(19) | C19 | C20 | C21 | C22 | -1.2(6) | |
| C1 | C2 | C3 | C4 | 0.2(3) | C20 | C21 | C22 | C23 | -0.5(5) | |
| C1 | C2 | C11 | N1 | -88.5(3) | C21 | C22 | C23 | C14 | -174.9(3) | |
| C2 | C1 | C5 | Fe1 | 58.71(18) | C21 | C22 | C23 | C18 | 2.0(5) | |
| C2 | C1 | C5 | C4 | -0.3(3) | C23 | C14 | C15 | C16 | -0.6(4) | |
| C2 | C3 | C4 | Fe1 | -58.98(19) | C23 | C18 | C19 | C20 | 0.2(5) | |
| C2 | C3 | C4 | C5 | -0.4(3) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| H2 | 12610(40) | -1300(40) | -107(13) | 87(16) |
| H3 | 11730 | -591 | 3294 | 31 |
| H4 | 13038 | 1322 | 3389 | 33 |
| H5 | 13432 | 1836 | 2100 | 30 |
| H6 | 13819 | -2631 | 1571 | 41 |
| H7 | 13375 | -3242 | 2838 | 49 |
| H8 | 14466 | -1759 | 3793 | 56 |
| H9 | 15562 | -239 | 3127 | 59 |
| H10 | 15173 | -774 | 1757 | 52 |
| H11A | 11073 | -2356 | 2197 | 28 |
| H11B | 11374 | -2065 | 1388 | 28 |
| H12A | 8502 | -2313 | 995 | 56 |
| H12B | 9389 | -3222 | 1499 | 56 |
| H12C | 9630 | -2707 | 709 | 56 |
| H13A | 9665 | -213 | 2419 | 58 |
| H13B | 9365 | -1700 | 2523 | 58 |
| H13C | 8517 | -790 | 1988 | 58 |
| H15 | 14253 | 596 | -2 | 35 |
| H16 | 15191 | 2269 | -509 | 43 |
| H17 | 14543 | 4351 | -503 | 41 |
| H19 | 13179 | 5948 | -165 | 48 |
| H20 | 11645 | 6409 | 367 | 56 |
| H21 | 10785 | 4783 | 974 | 49 |
| H22 | 11445 | 2688 | 1006 | 34 |
Experimental
Single crystals of C46H48Cl2Fe2N2O4Si2Zn2 [3161] 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 [3161]
Crystal Data for C46H48Cl2Fe2N2O4Si2Zn2 (M =1062.38 g/mol): monoclinic, space group P21/c (no. 14), a = 12.1868(6) Å, b = 10.3523(4) Å, c = 18.1265(8) Å, β = 99.579(4)°, V = 2254.98(18) Å3, Z = 2, T = 173 K, μ(MoKα) = 1.898 mm-1, Dcalc = 1.565 g/cm3, 20568 reflections measured (4.546° ≤ 2Θ ≤ 53.996°), 4909 unique (Rint = 0.0476, Rsigma = 0.0446) which were used in all calculations. The final R1 was 0.0373 (I > 2σ(I)) and wR2 was 0.0857 (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), C19(H19), C20(H20), C21(H21), C22(H22)
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.