| Identification code | 3103_twin1_hklf4 |
| Empirical formula | C23H28ClFe2NO2Si |
| Formula weight | 525.70 |
| Temperature/K | 173 |
| Crystal system | monoclinic |
| Space group | P21/c |
| a/Å | 7.5429(5) |
| b/Å | 10.7933(6) |
| c/Å | 26.917(2) |
| α/° | 90 |
| β/° | 93.719(6) |
| γ/° | 90 |
| Volume/Å3 | 2186.7(2) |
| Z | 4 |
| ρcalcg/cm3 | 1.597 |
| μ/mm‑1 | 1.525 |
| F(000) | 1088.0 |
| Crystal size/mm3 | 0.35 × 0.2 × 0.15 |
| Radiation | MoKα (λ = 0.71073) |
| 2Θ range for data collection/° | 4.842 to 53.998 |
| Index ranges | -9 ≤ h ≤ 9, -13 ≤ k ≤ 13, -34 ≤ l ≤ 34 |
| Reflections collected | 5183 |
| Independent reflections | 5183 [Rint = ?, Rsigma = 0.0494] |
| Data/restraints/parameters | 5183/6/280 |
| Goodness-of-fit on F2 | 1.142 |
| Final R indexes [I>=2σ (I)] | R1 = 0.0869, wR2 = 0.2406 |
| Final R indexes [all data] | R1 = 0.0986, wR2 = 0.2450 |
| Largest diff. peak/hole / e Å-3 | 0.87/-1.16 |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| Fe1 | 652.0(18) | 6460.7(14) | 901.1(6) | 21.3(3) |
| Fe2 | 5108.0(18) | 1394.0(14) | 913.5(6) | 23.8(3) |
| Cl1 | 4681(4) | 1909(3) | 2776.3(11) | 34.4(7) |
| Si1 | 2741(4) | 3819(2) | 1414.6(11) | 22.8(6) |
| O1 | 2215(10) | 3141(8) | 1934(3) | 33.6(19) |
| O2 | 4562(10) | 4629(7) | 1495(3) | 30.4(17) |
| N1 | -1246(12) | 5302(8) | 2357(3) | 23.5(19) |
| C1 | 726(12) | 4726(9) | 1215(4) | 18.6(19) |
| C2 | -284(13) | 5594(9) | 1497(4) | 22(2) |
| C3 | -1729(13) | 6054(9) | 1175(4) | 25(2) |
| C4 | -1645(14) | 5527(10) | 704(4) | 29(2) |
| C5 | -117(13) | 4704(9) | 721(4) | 22(2) |
| C6 | 3161(13) | 7034(11) | 792(5) | 34(3) |
| C7 | 2460(15) | 7791(11) | 1151(5) | 34(3) |
| C8 | 927(17) | 8333(9) | 918(6) | 42(3) |
| C9 | 707(17) | 7934(11) | 417(5) | 40(3) |
| C10 | 2110(20) | 7106(12) | 340(5) | 46(4) |
| C11 | 81(13) | 5879(10) | 2028(4) | 25(2) |
| C12 | -652(19) | 5356(12) | 2878(4) | 41(3) |
| C13 | -1761(16) | 4027(11) | 2222(4) | 33(3) |
| C14 | 3087(13) | 2705(9) | 913(4) | 20(2) |
| C15 | 4232(15) | 2879(10) | 502(4) | 30(2) |
| C16 | 4150(15) | 1798(11) | 205(4) | 32(3) |
| C17 | 3035(14) | 924(11) | 415(4) | 29(2) |
| C18 | 2418(13) | 1473(11) | 854(4) | 30(2) |
| C19 | 6552(14) | 1482(12) | 1585(4) | 33(3) |
| C20 | 7614(14) | 1798(10) | 1192(4) | 30(2) |
| C21 | 7625(15) | 771(10) | 863(4) | 29.8(18) |
| C22 | 6603(16) | -170(11) | 1046(5) | 39(3) |
| C23 | 5917(15) | 259(11) | 1504(5) | 33(3) |
| Atom | U11 | U22 | U33 | U23 | U13 | U12 |
|---|---|---|---|---|---|---|
| Fe1 | 18.1(7) | 17.1(7) | 28.7(7) | 1.3(6) | 3.0(6) | 0.6(6) |
| Fe2 | 17.8(7) | 19.8(7) | 33.9(8) | -1.4(7) | 3.6(6) | 2.9(6) |
| Cl1 | 24.5(13) | 38.1(15) | 39.9(15) | 12.9(13) | -2.8(11) | -12.6(12) |
| Si1 | 19.7(13) | 14.3(13) | 34.5(15) | 0.7(11) | 3.7(12) | 4.5(11) |
| O1 | 19(4) | 43(5) | 39(5) | 6(4) | 1(3) | 11(3) |
| O2 | 28(4) | 22(4) | 41(5) | -5(3) | 0(3) | 10(3) |
| N1 | 25(5) | 22(4) | 25(4) | -2(4) | 10(4) | -1(4) |
| C1 | 11(4) | 17(4) | 29(5) | 5(4) | 4(4) | -1(4) |
| C2 | 20(5) | 19(5) | 29(5) | 6(4) | 8(4) | 3(4) |
| C3 | 14(5) | 18(5) | 44(6) | 12(5) | 12(4) | 5(4) |
| C4 | 15(5) | 31(6) | 41(6) | 9(5) | -3(4) | -4(4) |
| C5 | 20(5) | 20(5) | 26(5) | 0(4) | -4(4) | -8(4) |
| C6 | 7(5) | 35(6) | 62(8) | 5(6) | 3(5) | -5(4) |
| C7 | 31(6) | 29(6) | 42(7) | 7(5) | -8(5) | -16(5) |
| C8 | 40(7) | 9(5) | 76(9) | 8(5) | 8(7) | -2(5) |
| C9 | 34(7) | 34(7) | 50(7) | 21(6) | -4(6) | -6(6) |
| C10 | 74(10) | 35(7) | 31(6) | -1(5) | 16(7) | -23(7) |
| C11 | 15(5) | 21(5) | 40(6) | 3(4) | 4(4) | -6(4) |
| C12 | 51(8) | 36(7) | 34(6) | 2(5) | -4(6) | -2(6) |
| C13 | 28(6) | 34(6) | 36(6) | -4(5) | 5(5) | -15(5) |
| C14 | 16(5) | 27(5) | 17(4) | -3(4) | -1(4) | 4(4) |
| C15 | 27(6) | 23(5) | 40(6) | 0(5) | 4(5) | 8(5) |
| C16 | 31(6) | 33(6) | 31(6) | -4(5) | 0(5) | 1(5) |
| C17 | 21(5) | 28(6) | 39(6) | -6(5) | -2(4) | 0(4) |
| C18 | 15(5) | 38(6) | 36(6) | 4(5) | 3(4) | 6(5) |
| C19 | 23(5) | 40(6) | 36(6) | 0(5) | 1(5) | 8(5) |
| C20 | 20(5) | 27(6) | 43(7) | -1(5) | 6(5) | -3(4) |
| C21 | 29.8(18) | 29.8(18) | 29.8(18) | 0.00(11) | 1.94(16) | 0.01(11) |
| C22 | 32(6) | 20(5) | 61(8) | -3(5) | -19(6) | 10(5) |
| C23 | 25(6) | 33(6) | 42(7) | 11(5) | -1(5) | 2(5) |
| Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
|---|---|---|---|---|---|---|
| Fe1 | C1 | 2.053(9) | N1 | C11 | 1.514(12) | |
| Fe1 | C2 | 2.024(10) | N1 | C12 | 1.445(14) | |
| Fe1 | C3 | 2.033(10) | N1 | C13 | 1.468(13) | |
| Fe1 | C4 | 2.044(11) | C1 | C2 | 1.453(14) | |
| Fe1 | C5 | 2.032(10) | C1 | C5 | 1.436(13) | |
| Fe1 | C6 | 2.030(10) | C2 | C3 | 1.436(14) | |
| Fe1 | C7 | 2.062(11) | C2 | C11 | 1.468(14) | |
| Fe1 | C8 | 2.032(10) | C3 | C4 | 1.394(16) | |
| Fe1 | C9 | 2.058(12) | C4 | C5 | 1.454(15) | |
| Fe1 | C10 | 2.045(12) | C6 | C7 | 1.394(18) | |
| Fe2 | C14 | 2.080(10) | C6 | C10 | 1.411(18) | |
| Fe2 | C15 | 2.034(11) | C7 | C8 | 1.406(17) | |
| Fe2 | C16 | 2.042(11) | C8 | C9 | 1.417(19) | |
| Fe2 | C17 | 2.057(11) | C9 | C10 | 1.408(19) | |
| Fe2 | C18 | 2.027(10) | C14 | C15 | 1.458(14) | |
| Fe2 | C19 | 2.051(11) | C14 | C18 | 1.427(15) | |
| Fe2 | C20 | 2.035(11) | C15 | C16 | 1.414(15) | |
| Fe2 | C21 | 2.027(11) | C16 | C17 | 1.406(16) | |
| Fe2 | C22 | 2.049(11) | C17 | C18 | 1.427(15) | |
| Fe2 | C23 | 2.068(11) | C19 | C20 | 1.410(15) | |
| Si1 | O1 | 1.649(8) | C19 | C23 | 1.417(17) | |
| Si1 | O2 | 1.631(8) | C20 | C21 | 1.420(15) | |
| Si1 | C1 | 1.858(10) | C21 | C22 | 1.386(16) | |
| Si1 | C14 | 1.840(10) | C22 | C23 | 1.444(17) |
| Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|
| C1 | Fe1 | C7 | 120.1(4) | C22 | Fe2 | C14 | 162.9(5) | |
| C1 | Fe1 | C9 | 164.5(5) | C22 | Fe2 | C17 | 107.3(5) | |
| C2 | Fe1 | C1 | 41.8(4) | C22 | Fe2 | C19 | 68.3(5) | |
| C2 | Fe1 | C3 | 41.5(4) | C22 | Fe2 | C23 | 41.0(5) | |
| C2 | Fe1 | C4 | 69.1(4) | C23 | Fe2 | C14 | 125.7(4) | |
| C2 | Fe1 | C5 | 69.5(4) | O1 | Si1 | C1 | 104.0(4) | |
| C2 | Fe1 | C6 | 129.2(5) | O1 | Si1 | C14 | 112.7(5) | |
| C2 | Fe1 | C7 | 108.7(5) | O2 | Si1 | O1 | 111.9(4) | |
| C2 | Fe1 | C8 | 118.8(5) | O2 | Si1 | C1 | 115.0(4) | |
| C2 | Fe1 | C9 | 151.9(5) | O2 | Si1 | C14 | 106.9(4) | |
| C2 | Fe1 | C10 | 166.9(5) | C14 | Si1 | C1 | 106.5(4) | |
| C3 | Fe1 | C1 | 69.8(4) | C12 | N1 | C11 | 112.1(9) | |
| C3 | Fe1 | C4 | 40.0(5) | C12 | N1 | C13 | 109.8(9) | |
| C3 | Fe1 | C7 | 127.8(5) | C13 | N1 | C11 | 114.5(8) | |
| C3 | Fe1 | C9 | 116.8(5) | Si1 | C1 | Fe1 | 126.8(5) | |
| C3 | Fe1 | C10 | 150.5(5) | C2 | C1 | Fe1 | 68.1(5) | |
| C4 | Fe1 | C1 | 69.9(4) | C2 | C1 | Si1 | 129.4(8) | |
| C4 | Fe1 | C7 | 163.5(5) | C5 | C1 | Fe1 | 68.6(5) | |
| C4 | Fe1 | C9 | 105.6(5) | C5 | C1 | Si1 | 124.3(8) | |
| C4 | Fe1 | C10 | 117.6(5) | C5 | C1 | C2 | 106.2(8) | |
| C5 | Fe1 | C1 | 41.2(4) | C1 | C2 | Fe1 | 70.2(5) | |
| C5 | Fe1 | C3 | 68.9(4) | C1 | C2 | C11 | 124.9(9) | |
| C5 | Fe1 | C4 | 41.8(4) | C3 | C2 | Fe1 | 69.6(5) | |
| C5 | Fe1 | C7 | 154.1(5) | C3 | C2 | C1 | 108.1(9) | |
| C5 | Fe1 | C9 | 125.9(5) | C3 | C2 | C11 | 127.0(9) | |
| C5 | Fe1 | C10 | 107.5(5) | C11 | C2 | Fe1 | 128.4(7) | |
| C6 | Fe1 | C1 | 109.7(4) | C2 | C3 | Fe1 | 68.9(5) | |
| C6 | Fe1 | C3 | 166.3(5) | C4 | C3 | Fe1 | 70.4(6) | |
| C6 | Fe1 | C4 | 153.6(5) | C4 | C3 | C2 | 109.3(9) | |
| C6 | Fe1 | C5 | 120.3(5) | C3 | C4 | Fe1 | 69.6(6) | |
| C6 | Fe1 | C7 | 39.8(5) | C3 | C4 | C5 | 107.7(9) | |
| C6 | Fe1 | C8 | 66.7(5) | C5 | C4 | Fe1 | 68.7(6) | |
| C6 | Fe1 | C9 | 67.4(5) | C1 | C5 | Fe1 | 70.2(5) | |
| C6 | Fe1 | C10 | 40.5(5) | C1 | C5 | C4 | 108.7(9) | |
| C8 | Fe1 | C1 | 153.9(5) | C4 | C5 | Fe1 | 69.5(6) | |
| C8 | Fe1 | C3 | 107.3(5) | C7 | C6 | Fe1 | 71.3(6) | |
| C8 | Fe1 | C4 | 125.4(5) | C7 | C6 | C10 | 110.3(11) | |
| C8 | Fe1 | C5 | 163.9(5) | C10 | C6 | Fe1 | 70.3(7) | |
| C8 | Fe1 | C7 | 40.1(5) | C6 | C7 | Fe1 | 68.9(6) | |
| C8 | Fe1 | C9 | 40.5(5) | C6 | C7 | C8 | 105.9(11) | |
| C8 | Fe1 | C10 | 67.6(5) | C8 | C7 | Fe1 | 68.8(6) | |
| C9 | Fe1 | C7 | 68.2(5) | C7 | C8 | Fe1 | 71.1(6) | |
| C10 | Fe1 | C1 | 127.8(5) | C7 | C8 | C9 | 109.8(11) | |
| C10 | Fe1 | C7 | 68.1(5) | C9 | C8 | Fe1 | 70.7(7) | |
| C10 | Fe1 | C9 | 40.1(5) | C8 | C9 | Fe1 | 68.8(6) | |
| C15 | Fe2 | C14 | 41.5(4) | C10 | C9 | Fe1 | 69.4(7) | |
| C15 | Fe2 | C16 | 40.6(4) | C10 | C9 | C8 | 106.8(11) | |
| C15 | Fe2 | C17 | 68.4(5) | C6 | C10 | Fe1 | 69.2(6) | |
| C15 | Fe2 | C19 | 125.3(5) | C9 | C10 | Fe1 | 70.4(7) | |
| C15 | Fe2 | C20 | 107.0(5) | C9 | C10 | C6 | 107.1(11) | |
| C15 | Fe2 | C22 | 154.2(5) | C2 | C11 | N1 | 113.2(8) | |
| C15 | Fe2 | C23 | 162.7(5) | Si1 | C14 | Fe2 | 125.6(5) | |
| C16 | Fe2 | C14 | 68.9(4) | C15 | C14 | Fe2 | 67.6(6) | |
| C16 | Fe2 | C17 | 40.1(5) | C15 | C14 | Si1 | 126.3(8) | |
| C16 | Fe2 | C19 | 161.5(5) | C18 | C14 | Fe2 | 67.7(5) | |
| C16 | Fe2 | C22 | 119.7(5) | C18 | C14 | Si1 | 128.6(8) | |
| C16 | Fe2 | C23 | 156.0(5) | C18 | C14 | C15 | 105.0(9) | |
| C17 | Fe2 | C14 | 68.9(4) | C14 | C15 | Fe2 | 70.9(6) | |
| C17 | Fe2 | C23 | 122.0(5) | C16 | C15 | Fe2 | 70.0(6) | |
| C18 | Fe2 | C14 | 40.7(4) | C16 | C15 | C14 | 108.4(10) | |
| C18 | Fe2 | C15 | 68.6(5) | C15 | C16 | Fe2 | 69.4(6) | |
| C18 | Fe2 | C16 | 68.0(5) | C17 | C16 | Fe2 | 70.5(7) | |
| C18 | Fe2 | C17 | 40.9(4) | C17 | C16 | C15 | 109.3(10) | |
| C18 | Fe2 | C19 | 122.6(4) | C16 | C17 | Fe2 | 69.4(6) | |
| C18 | Fe2 | C20 | 157.1(5) | C16 | C17 | C18 | 106.9(10) | |
| C18 | Fe2 | C22 | 125.8(5) | C18 | C17 | Fe2 | 68.4(6) | |
| C18 | Fe2 | C23 | 109.2(5) | C14 | C18 | Fe2 | 71.7(6) | |
| C19 | Fe2 | C14 | 108.5(4) | C17 | C18 | Fe2 | 70.7(6) | |
| C19 | Fe2 | C17 | 157.5(5) | C17 | C18 | C14 | 110.2(10) | |
| C19 | Fe2 | C23 | 40.2(5) | C20 | C19 | Fe2 | 69.2(6) | |
| C20 | Fe2 | C14 | 121.2(4) | C20 | C19 | C23 | 108.3(10) | |
| C20 | Fe2 | C16 | 124.2(5) | C23 | C19 | Fe2 | 70.5(7) | |
| C20 | Fe2 | C17 | 160.4(5) | C19 | C20 | Fe2 | 70.4(6) | |
| C20 | Fe2 | C19 | 40.4(4) | C19 | C20 | C21 | 107.8(10) | |
| C20 | Fe2 | C22 | 68.0(5) | C21 | C20 | Fe2 | 69.2(6) | |
| C20 | Fe2 | C23 | 67.9(5) | C20 | C21 | Fe2 | 69.9(6) | |
| C21 | Fe2 | C14 | 156.2(4) | C22 | C21 | Fe2 | 71.0(7) | |
| C21 | Fe2 | C15 | 119.8(4) | C22 | C21 | C20 | 108.9(10) | |
| C21 | Fe2 | C16 | 106.5(5) | C21 | C22 | Fe2 | 69.3(6) | |
| C21 | Fe2 | C17 | 123.4(5) | C21 | C22 | C23 | 107.9(10) | |
| C21 | Fe2 | C18 | 161.1(5) | C23 | C22 | Fe2 | 70.2(6) | |
| C21 | Fe2 | C19 | 68.2(4) | C19 | C23 | Fe2 | 69.2(6) | |
| C21 | Fe2 | C20 | 40.9(4) | C19 | C23 | C22 | 107.1(10) | |
| C21 | Fe2 | C22 | 39.7(5) | C22 | C23 | Fe2 | 68.8(6) | |
| C21 | Fe2 | C23 | 67.9(5) |
| D | H | A | d(D-H)/Å | d(H-A)/Å | d(D-A)/Å | D-H-A/° |
|---|---|---|---|---|---|---|
| O1 | H1 | Cl1 | 0.84 | 2.38 | 3.134(8) | 150.3 |
| O2 | H2 | Cl11 | 0.84 | 2.41 | 3.175(8) | 152.2 |
| N1 | H1A | Cl12 | 1.03(9) | 2.10(10) | 3.120(9) | 173(8) |
| A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|---|---|
| Fe1 | C1 | C2 | C3 | 59.5(7) | C1 | C2 | C11 | N1 | -105.8(11) | |
| Fe1 | C1 | C2 | C11 | -123.6(10) | C2 | C1 | C5 | Fe1 | 57.9(6) | |
| Fe1 | C1 | C5 | C4 | -59.1(7) | C2 | C1 | C5 | C4 | -1.2(11) | |
| Fe1 | C2 | C3 | C4 | 59.0(7) | C2 | C3 | C4 | Fe1 | -58.1(7) | |
| Fe1 | C2 | C11 | N1 | 162.7(7) | C2 | C3 | C4 | C5 | 0.1(12) | |
| Fe1 | C3 | C4 | C5 | 58.2(7) | C3 | C2 | C11 | N1 | 70.5(13) | |
| Fe1 | C4 | C5 | C1 | 59.5(7) | C3 | C4 | C5 | Fe1 | -58.8(7) | |
| Fe1 | C6 | C7 | C8 | -59.1(8) | C3 | C4 | C5 | C1 | 0.7(11) | |
| Fe1 | C6 | C10 | C9 | 60.5(8) | C5 | C1 | C2 | Fe1 | -58.2(6) | |
| Fe1 | C7 | C8 | C9 | -60.4(8) | C5 | C1 | C2 | C3 | 1.3(11) | |
| Fe1 | C8 | C9 | C10 | -59.3(8) | C5 | C1 | C2 | C11 | 178.2(9) | |
| Fe1 | C9 | C10 | C6 | -59.7(8) | C6 | C7 | C8 | Fe1 | 59.1(8) | |
| Fe2 | C14 | C15 | C16 | 60.2(8) | C6 | C7 | C8 | C9 | -1.2(13) | |
| Fe2 | C14 | C18 | C17 | -60.4(7) | C7 | C6 | C10 | Fe1 | -60.4(8) | |
| Fe2 | C15 | C16 | C17 | 59.3(8) | C7 | C6 | C10 | C9 | 0.1(13) | |
| Fe2 | C16 | C17 | C18 | 58.3(7) | C7 | C8 | C9 | Fe1 | 60.6(8) | |
| Fe2 | C17 | C18 | C14 | 61.0(7) | C7 | C8 | C9 | C10 | 1.3(13) | |
| Fe2 | C19 | C20 | C21 | -59.4(8) | C8 | C9 | C10 | Fe1 | 58.8(8) | |
| Fe2 | C19 | C23 | C22 | 58.6(8) | C8 | C9 | C10 | C6 | -0.9(13) | |
| Fe2 | C20 | C21 | C22 | -60.5(8) | C10 | C6 | C7 | Fe1 | 59.7(8) | |
| Fe2 | C21 | C22 | C23 | -59.8(8) | C10 | C6 | C7 | C8 | 0.7(13) | |
| Fe2 | C22 | C23 | C19 | -58.9(8) | C11 | C2 | C3 | Fe1 | 123.3(10) | |
| Si1 | C1 | C2 | Fe1 | 120.4(8) | C11 | C2 | C3 | C4 | -177.7(10) | |
| Si1 | C1 | C2 | C3 | 179.9(7) | C12 | N1 | C11 | C2 | 167.1(9) | |
| Si1 | C1 | C2 | C11 | -3.2(15) | C13 | N1 | C11 | C2 | 41.2(13) | |
| Si1 | C1 | C5 | Fe1 | -120.8(7) | C14 | Si1 | C1 | Fe1 | -99.4(7) | |
| Si1 | C1 | C5 | C4 | -179.9(7) | C14 | Si1 | C1 | C2 | 170.0(9) | |
| Si1 | C14 | C15 | Fe2 | 118.6(8) | C14 | Si1 | C1 | C5 | -11.7(9) | |
| Si1 | C14 | C15 | C16 | 178.9(8) | C14 | C15 | C16 | Fe2 | -60.8(7) | |
| Si1 | C14 | C18 | Fe2 | -118.6(8) | C14 | C15 | C16 | C17 | -1.5(13) | |
| Si1 | C14 | C18 | C17 | -179.0(8) | C15 | C14 | C18 | Fe2 | 57.5(7) | |
| O1 | Si1 | C1 | Fe1 | 141.4(6) | C15 | C14 | C18 | C17 | -2.9(11) | |
| O1 | Si1 | C1 | C2 | 50.7(10) | C15 | C16 | C17 | Fe2 | -58.7(8) | |
| O1 | Si1 | C1 | C5 | -130.9(8) | C15 | C16 | C17 | C18 | -0.3(13) | |
| O1 | Si1 | C14 | Fe2 | -65.5(7) | C16 | C17 | C18 | Fe2 | -58.9(8) | |
| O1 | Si1 | C14 | C15 | -152.3(8) | C16 | C17 | C18 | C14 | 2.1(12) | |
| O1 | Si1 | C14 | C18 | 23.0(10) | C18 | C14 | C15 | Fe2 | -57.6(7) | |
| O2 | Si1 | C1 | Fe1 | 18.7(8) | C18 | C14 | C15 | C16 | 2.7(12) | |
| O2 | Si1 | C1 | C2 | -71.9(10) | C19 | C20 | C21 | Fe2 | 60.1(8) | |
| O2 | Si1 | C1 | C5 | 106.5(8) | C19 | C20 | C21 | C22 | -0.4(13) | |
| O2 | Si1 | C14 | Fe2 | 57.7(7) | C20 | C19 | C23 | Fe2 | -59.1(8) | |
| O2 | Si1 | C14 | C15 | -29.0(10) | C20 | C19 | C23 | C22 | -0.6(12) | |
| O2 | Si1 | C14 | C18 | 146.3(9) | C20 | C21 | C22 | Fe2 | 59.8(8) | |
| C1 | Si1 | C14 | Fe2 | -178.9(6) | C20 | C21 | C22 | C23 | 0.0(13) | |
| C1 | Si1 | C14 | C15 | 94.3(9) | C21 | C22 | C23 | Fe2 | 59.2(8) | |
| C1 | Si1 | C14 | C18 | -90.4(10) | C21 | C22 | C23 | C19 | 0.3(13) | |
| C1 | C2 | C3 | Fe1 | -59.9(7) | C23 | C19 | C20 | Fe2 | 60.0(8) | |
| C1 | C2 | C3 | C4 | -0.9(11) | C23 | C19 | C20 | C21 | 0.6(13) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| H1 | 3141 | 3011 | 2117 | 50 |
| H2 | 4500 | 5089 | 1745 | 46 |
| H1A | -2340(130) | 5860(90) | 2280(30) | 10(20) |
| H3 | -2603 | 6628 | 1268 | 30 |
| H4 | -2444 | 5679 | 423 | 35 |
| H5 | 262 | 4230 | 450 | 27 |
| H6 | 4199 | 6541 | 845 | 41 |
| H7 | 2923 | 7915 | 1483 | 41 |
| H8 | 155 | 8885 | 1074 | 50 |
| H9 | -209 | 8177 | 178 | 48 |
| H10 | 2306 | 6677 | 41 | 55 |
| H11A | 69 | 6789 | 2073 | 30 |
| H11B | 1286 | 5578 | 2134 | 30 |
| H12A | 433 | 4863 | 2935 | 61 |
| H12B | -1579 | 5024 | 3079 | 61 |
| H12C | -406 | 6219 | 2973 | 61 |
| H13A | -2389 | 4023 | 1892 | 49 |
| H13B | -2542 | 3699 | 2468 | 49 |
| H13C | -694 | 3510 | 2217 | 49 |
| H15 | 4917 | 3597 | 444 | 36 |
| H16 | 4754 | 1679 | -90 | 38 |
| H17 | 2747 | 122 | 289 | 35 |
| H18 | 1669 | 1075 | 1076 | 36 |
| H19 | 6304 | 2001 | 1857 | 40 |
| H20 | 8215 | 2563 | 1154 | 36 |
| H21 | 8233 | 735 | 565 | 36 |
| H22 | 6392 | -959 | 897 | 47 |
| H23 | 5179 | -194 | 1712 | 40 |
Experimental
Single crystals of C23H28ClFe2NO2Si [3103_twin1_hklf4] 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 [3103_twin1_hklf4]
Crystal Data for C23H28ClFe2NO2Si (M =525.70 g/mol): monoclinic, space group P21/c (no. 14), a = 7.5429(5) Å, b = 10.7933(6) Å, c = 26.917(2) Å, β = 93.719(6)°, V = 2186.7(2) Å3, Z = 4, T = 173 K, μ(MoKα) = 1.525 mm-1, Dcalc = 1.597 g/cm3, 5183 reflections measured (4.842° ≤ 2Θ ≤ 53.998°), 5183 unique (Rint = ?, Rsigma = 0.0494) which were used in all calculations. The final R1 was 0.0869 (I > 2σ(I)) and wR2 was 0.2450 (all data).
Refinement model description
Number of restraints - 6, number of constraints - unknown.
Details:
1. Twinned data refinement
Scales: 0.733(2) 0.267(2)
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, All O(H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C21) ≈ Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
4.a Secondary CH2 refined with riding coordinates:
C11(H11A,H11B)
4.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)
4.c Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)
4.d Idealised tetrahedral OH refined as rotating group:
O1(H1), O2(H2)
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.