| Identification code | 3193_twin1_hklf4 |
| Empirical formula | C16H26ClFeNSi |
| Formula weight | 351.77 |
| Temperature/K | 173.15 |
| Crystal system | triclinic |
| Space group | P-1 |
| a/Å | 10.4038(9) |
| b/Å | 11.5162(11) |
| c/Å | 16.0747(16) |
| α/° | 71.308(9) |
| β/° | 81.097(8) |
| γ/° | 89.850(7) |
| Volume/Å3 | 1800.1(3) |
| Z | 4 |
| ρcalcg/cm3 | 1.298 |
| μ/mm‑1 | 1.044 |
| F(000) | 744.0 |
| Crystal size/mm3 | 0.107 × 0.105 × 0.01 |
| Radiation | MoKα (λ = 0.71073) |
| 2Θ range for data collection/° | 4.426 to 52 |
| Index ranges | -12 ≤ h ≤ 12, -14 ≤ k ≤ 14, -19 ≤ l ≤ 19 |
| Reflections collected | 8830 |
| Independent reflections | 8830 [Rint = N/A, Rsigma = 0.1178] |
| Data/restraints/parameters | 8830/60/372 |
| Goodness-of-fit on F2 | 0.990 |
| Final R indexes [I>=2σ (I)] | R1 = 0.0621, wR2 = 0.1572 |
| Final R indexes [all data] | R1 = 0.1101, wR2 = 0.1843 |
| Largest diff. peak/hole / e Å-3 | 0.78/-0.56 |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| Fe1 | 1824.6(10) | 4660.0(9) | 1662.3(7) | 30.8(3) |
| Si1 | -1335(2) | 5716.3(17) | 2051.8(13) | 25.6(5) |
| N1 | 428(5) | 2805(5) | 4418(4) | 24.2(13) |
| C1 | -173(6) | 4462(6) | 2097(4) | 22.7(15) |
| C2 | 526(6) | 3810(6) | 2795(4) | 23.5(16) |
| C3 | 1291(7) | 2937(6) | 2497(4) | 26.3(16) |
| C4 | 1098(7) | 3037(6) | 1623(4) | 28.6(17) |
| C5 | 202(7) | 3972(5) | 1384(4) | 24.9(16) |
| C6 | 2406(9) | 6477(7) | 1145(6) | 55(3) |
| C7 | 2918(13) | 5909(11) | 1904(8) | 84(4) |
| C8 | 3695(10) | 4987(12) | 1745(10) | 99(5) |
| C9 | 3616(10) | 4964(9) | 883(8) | 74(3) |
| C10 | 2819(9) | 5877(8) | 532(6) | 56(3) |
| C11 | 523(7) | 3988(5) | 3680(4) | 26.5(16) |
| C12 | -773(7) | 2030(6) | 4508(5) | 35.0(19) |
| C13 | 502(6) | 3025(6) | 5269(4) | 26.4(16) |
| C14 | -1576(8) | 6391(7) | 875(5) | 42(2) |
| C15 | -716(8) | 6934(7) | 2441(5) | 47(2) |
| C16 | -2917(7) | 5057(6) | 2786(5) | 41(2) |
| Fe2 | -5248.3(10) | 9660.4(10) | 1799.9(7) | 32.1(3) |
| Si2 | -2201(2) | 10617.5(17) | 2124.4(13) | 27.7(5) |
| N2 | -5159(5) | 7754(5) | 4540(3) | 20.8(12) |
| C17 | -3453(7) | 9400(5) | 2206(4) | 23.6(15) |
| C18 | -4490(7) | 8764(6) | 2912(5) | 28.6(17) |
| C19 | -5154(7) | 7918(6) | 2623(4) | 30.1(17) |
| C20 | -4557(7) | 8018(6) | 1759(4) | 26.9(16) |
| C21 | -3529(7) | 8923(6) | 1486(4) | 25.5(16) |
| C22 | -5481(11) | 11510(9) | 1200(8) | 72(3) |
| C23 | -6189(12) | 11159(10) | 1997(8) | 79(3) |
| C24 | -7045(10) | 10263(10) | 2105(7) | 71(3) |
| C25 | -6893(11) | 9936(9) | 1260(11) | 115(6) |
| C26 | -5868(11) | 10842(9) | 718(6) | 67(3) |
| C27 | -4813(7) | 8947(6) | 3796(4) | 27.3(16) |
| C28 | -4056(8) | 6938(7) | 4642(5) | 40(2) |
| C29 | -5653(7) | 7975(6) | 5379(4) | 30.2(17) |
| C30 | -1306(8) | 11109(7) | 956(5) | 44(2) |
| C31 | -1052(8) | 10008(6) | 2892(5) | 39(2) |
| C32 | -2934(8) | 11966(6) | 2389(5) | 44(2) |
| Cl1 | 2496.4(17) | 898.3(15) | 4466.1(12) | 29.0(4) |
| Cl2 | -7267.3(17) | 5903.6(15) | 4522.9(12) | 31.0(4) |
| Atom | U11 | U22 | U33 | U23 | U13 | U12 |
|---|---|---|---|---|---|---|
| Fe1 | 26.9(6) | 27.8(6) | 35.3(6) | -8.7(5) | -0.7(5) | -4.0(5) |
| Si1 | 33.6(12) | 19(1) | 24.7(11) | -6.9(9) | -6.4(9) | 7.7(9) |
| N1 | 20(3) | 24(3) | 34(3) | -14(3) | -10(3) | 0(3) |
| C1 | 19(4) | 20(3) | 29(4) | -9(3) | 1(3) | -1(3) |
| C2 | 27(4) | 20(3) | 29(4) | -10(3) | -17(3) | -2(3) |
| C3 | 32(4) | 20(4) | 29(4) | -7(3) | -14(3) | 9(3) |
| C4 | 35(4) | 21(4) | 32(4) | -13(3) | 0(3) | 1(3) |
| C5 | 34(4) | 18(3) | 26(4) | -11(3) | -7(3) | 1(3) |
| C6 | 63(7) | 30(5) | 62(6) | -9(5) | 9(5) | -23(5) |
| C7 | 90(9) | 94(9) | 71(8) | -39(7) | 3(7) | -68(8) |
| C8 | 30(6) | 107(11) | 112(11) | 40(9) | -28(7) | -35(6) |
| C9 | 40(6) | 62(7) | 90(9) | -4(7) | 31(6) | -8(5) |
| C10 | 63(7) | 51(6) | 43(5) | -15(5) | 28(5) | -29(5) |
| C11 | 38(4) | 16(3) | 24(4) | -3(3) | -9(3) | 3(3) |
| C12 | 33(5) | 31(4) | 41(5) | -18(4) | 7(4) | -5(4) |
| C13 | 20(4) | 29(4) | 31(4) | -10(3) | -4(3) | 7(3) |
| C14 | 49(5) | 40(4) | 34(5) | -7(4) | -10(4) | 28(4) |
| C15 | 67(6) | 40(5) | 42(5) | -20(4) | -20(5) | 8(5) |
| C16 | 37(5) | 24(4) | 53(5) | -7(4) | 0(4) | 8(4) |
| Fe2 | 29.8(6) | 38.8(6) | 30.5(6) | -13.6(5) | -8.0(5) | 11.1(5) |
| Si2 | 34.9(13) | 20.7(10) | 27.2(11) | -9.0(9) | -0.8(9) | -4.3(9) |
| N2 | 20(3) | 21(3) | 24(3) | -12(2) | -2(2) | -3(2) |
| C17 | 30(4) | 16(3) | 26(4) | -10(3) | -3(3) | 8(3) |
| C18 | 30(4) | 21(4) | 41(4) | -16(3) | -11(3) | 2(3) |
| C19 | 37(5) | 19(4) | 30(4) | -5(3) | 2(3) | -5(3) |
| C20 | 27(4) | 25(4) | 31(4) | -11(3) | -8(3) | -3(3) |
| C21 | 27(4) | 23(4) | 27(4) | -11(3) | 0(3) | 7(3) |
| C22 | 72(8) | 53(6) | 88(8) | -12(6) | -27(7) | 32(6) |
| C23 | 83(9) | 66(7) | 99(9) | -39(7) | -27(7) | 48(7) |
| C24 | 51(5) | 73(5) | 70(5) | -1(4) | -4(4) | 19(4) |
| C25 | 73(8) | 56(7) | 268(18) | -81(9) | -129(10) | 39(6) |
| C26 | 100(9) | 76(7) | 52(6) | -38(6) | -61(6) | 52(7) |
| C27 | 24(4) | 24(4) | 35(4) | -9(3) | -8(3) | 3(3) |
| C28 | 52(5) | 38(5) | 44(5) | -22(4) | -28(4) | 18(4) |
| C29 | 35(5) | 23(4) | 32(4) | -6(3) | -7(3) | -4(3) |
| C30 | 58(6) | 35(4) | 34(5) | -7(4) | 2(4) | -21(4) |
| C31 | 46(5) | 28(4) | 47(5) | -16(4) | -14(4) | -5(4) |
| C32 | 60(6) | 24(4) | 57(5) | -23(4) | -11(5) | 1(4) |
| Cl1 | 26.5(10) | 24.6(9) | 37.2(10) | -11.7(8) | -5.7(8) | 5.1(8) |
| Cl2 | 23.9(10) | 21.2(9) | 47.8(11) | -11.6(8) | -4.7(8) | -1.3(8) |
| Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
|---|---|---|---|---|---|---|
| Fe1 | C1 | 2.076(7) | Fe2 | C17 | 2.062(7) | |
| Fe1 | C2 | 2.050(7) | Fe2 | C18 | 2.033(7) | |
| Fe1 | C3 | 2.028(6) | Fe2 | C19 | 2.031(7) | |
| Fe1 | C4 | 2.041(6) | Fe2 | C20 | 2.040(7) | |
| Fe1 | C5 | 2.036(6) | Fe2 | C21 | 2.041(7) | |
| Fe1 | C6 | 2.042(7) | Fe2 | C22 | 2.068(9) | |
| Fe1 | C7 | 2.005(8) | Fe2 | C23 | 2.070(9) | |
| Fe1 | C8 | 2.015(9) | Fe2 | C24 | 2.036(10) | |
| Fe1 | C9 | 2.040(9) | Fe2 | C25 | 2.016(9) | |
| Fe1 | C10 | 2.032(8) | Fe2 | C26 | 2.029(8) | |
| Si1 | C1 | 1.872(7) | Si2 | C17 | 1.875(7) | |
| Si1 | C14 | 1.858(7) | Si2 | C30 | 1.870(7) | |
| Si1 | C15 | 1.862(7) | Si2 | C31 | 1.828(8) | |
| Si1 | C16 | 1.874(7) | Si2 | C32 | 1.868(7) | |
| N1 | C11 | 1.484(8) | N2 | C27 | 1.504(8) | |
| N1 | C12 | 1.499(8) | N2 | C28 | 1.476(8) | |
| N1 | C13 | 1.482(7) | N2 | C29 | 1.467(7) | |
| C1 | C2 | 1.436(9) | C17 | C18 | 1.442(9) | |
| C1 | C5 | 1.435(8) | C17 | C21 | 1.444(8) | |
| C2 | C3 | 1.435(9) | C18 | C19 | 1.427(8) | |
| C2 | C11 | 1.500(8) | C18 | C27 | 1.491(9) | |
| C3 | C4 | 1.417(9) | C19 | C20 | 1.400(9) | |
| C4 | C5 | 1.420(9) | C20 | C21 | 1.411(9) | |
| C6 | C7 | 1.374(14) | C22 | C23 | 1.313(13) | |
| C6 | C10 | 1.392(10) | C22 | C26 | 1.355(12) | |
| C7 | C8 | 1.396(15) | C23 | C24 | 1.315(14) | |
| C8 | C9 | 1.410(15) | C24 | C25 | 1.509(15) | |
| C9 | C10 | 1.368(13) | C25 | C26 | 1.456(16) |
| Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|
| C2 | Fe1 | C1 | 40.7(2) | C17 | Fe2 | C22 | 110.2(4) | |
| C3 | Fe1 | C1 | 68.8(3) | C17 | Fe2 | C23 | 115.0(4) | |
| C3 | Fe1 | C2 | 41.2(2) | C18 | Fe2 | C17 | 41.2(3) | |
| C3 | Fe1 | C4 | 40.8(2) | C18 | Fe2 | C20 | 68.4(3) | |
| C3 | Fe1 | C5 | 67.9(3) | C18 | Fe2 | C21 | 68.9(3) | |
| C3 | Fe1 | C6 | 164.1(3) | C18 | Fe2 | C22 | 130.9(4) | |
| C3 | Fe1 | C9 | 118.6(4) | C18 | Fe2 | C23 | 108.4(4) | |
| C3 | Fe1 | C10 | 153.0(3) | C18 | Fe2 | C24 | 111.7(4) | |
| C4 | Fe1 | C1 | 69.4(3) | C19 | Fe2 | C17 | 69.3(3) | |
| C4 | Fe1 | C2 | 69.4(2) | C19 | Fe2 | C18 | 41.1(2) | |
| C4 | Fe1 | C6 | 154.9(3) | C19 | Fe2 | C20 | 40.2(2) | |
| C5 | Fe1 | C1 | 40.8(2) | C19 | Fe2 | C21 | 68.4(3) | |
| C5 | Fe1 | C2 | 68.3(2) | C19 | Fe2 | C22 | 168.3(4) | |
| C5 | Fe1 | C4 | 40.8(3) | C19 | Fe2 | C23 | 131.8(4) | |
| C5 | Fe1 | C6 | 122.4(4) | C19 | Fe2 | C24 | 108.5(4) | |
| C5 | Fe1 | C9 | 125.3(4) | C20 | Fe2 | C17 | 68.8(2) | |
| C6 | Fe1 | C1 | 110.2(3) | C20 | Fe2 | C21 | 40.5(2) | |
| C6 | Fe1 | C2 | 127.7(3) | C20 | Fe2 | C22 | 151.3(4) | |
| C7 | Fe1 | C1 | 120.9(4) | C20 | Fe2 | C23 | 170.7(4) | |
| C7 | Fe1 | C2 | 108.3(4) | C21 | Fe2 | C17 | 41.2(2) | |
| C7 | Fe1 | C3 | 126.2(4) | C21 | Fe2 | C22 | 119.5(4) | |
| C7 | Fe1 | C4 | 162.4(5) | C21 | Fe2 | C23 | 147.7(4) | |
| C7 | Fe1 | C5 | 156.0(5) | C22 | Fe2 | C23 | 37.0(4) | |
| C7 | Fe1 | C6 | 39.7(4) | C24 | Fe2 | C17 | 142.3(4) | |
| C7 | Fe1 | C8 | 40.6(5) | C24 | Fe2 | C20 | 134.7(4) | |
| C7 | Fe1 | C9 | 68.4(5) | C24 | Fe2 | C21 | 174.9(4) | |
| C7 | Fe1 | C10 | 67.3(4) | C24 | Fe2 | C22 | 64.3(4) | |
| C8 | Fe1 | C1 | 155.2(5) | C24 | Fe2 | C23 | 37.4(4) | |
| C8 | Fe1 | C2 | 119.9(4) | C25 | Fe2 | C17 | 173.3(5) | |
| C8 | Fe1 | C3 | 106.9(4) | C25 | Fe2 | C18 | 144.5(5) | |
| C8 | Fe1 | C4 | 124.3(5) | C25 | Fe2 | C19 | 113.2(4) | |
| C8 | Fe1 | C5 | 162.2(6) | C25 | Fe2 | C20 | 108.8(3) | |
| C8 | Fe1 | C6 | 66.9(5) | C25 | Fe2 | C21 | 133.1(5) | |
| C8 | Fe1 | C9 | 40.7(4) | C25 | Fe2 | C22 | 68.7(4) | |
| C8 | Fe1 | C10 | 66.7(4) | C25 | Fe2 | C23 | 68.4(4) | |
| C9 | Fe1 | C1 | 163.2(4) | C25 | Fe2 | C24 | 43.7(4) | |
| C9 | Fe1 | C2 | 154.1(4) | C25 | Fe2 | C26 | 42.2(5) | |
| C9 | Fe1 | C4 | 105.6(4) | C26 | Fe2 | C17 | 133.0(4) | |
| C9 | Fe1 | C6 | 67.1(4) | C26 | Fe2 | C18 | 169.3(3) | |
| C10 | Fe1 | C1 | 128.1(4) | C26 | Fe2 | C19 | 149.6(4) | |
| C10 | Fe1 | C2 | 165.2(3) | C26 | Fe2 | C20 | 120.1(3) | |
| C10 | Fe1 | C4 | 119.3(3) | C26 | Fe2 | C21 | 112.7(4) | |
| C10 | Fe1 | C5 | 109.6(3) | C26 | Fe2 | C22 | 38.6(3) | |
| C10 | Fe1 | C6 | 40.0(3) | C26 | Fe2 | C23 | 64.2(4) | |
| C10 | Fe1 | C9 | 39.2(4) | C26 | Fe2 | C24 | 67.7(4) | |
| C1 | Si1 | C16 | 109.4(3) | C30 | Si2 | C17 | 106.5(3) | |
| C14 | Si1 | C1 | 107.1(3) | C31 | Si2 | C17 | 110.9(3) | |
| C14 | Si1 | C15 | 109.7(4) | C31 | Si2 | C30 | 109.2(4) | |
| C14 | Si1 | C16 | 110.5(4) | C31 | Si2 | C32 | 107.4(3) | |
| C15 | Si1 | C1 | 112.5(3) | C32 | Si2 | C17 | 112.8(3) | |
| C15 | Si1 | C16 | 107.6(4) | C32 | Si2 | C30 | 110.1(4) | |
| C11 | N1 | C12 | 113.3(5) | C28 | N2 | C27 | 112.3(5) | |
| C13 | N1 | C11 | 110.3(5) | C29 | N2 | C27 | 110.7(5) | |
| C13 | N1 | C12 | 110.2(5) | C29 | N2 | C28 | 110.9(5) | |
| Si1 | C1 | Fe1 | 127.1(3) | Si2 | C17 | Fe2 | 127.1(3) | |
| C2 | C1 | Fe1 | 68.6(4) | C18 | C17 | Fe2 | 68.3(4) | |
| C2 | C1 | Si1 | 129.8(5) | C18 | C17 | Si2 | 131.6(5) | |
| C5 | C1 | Fe1 | 68.1(4) | C18 | C17 | C21 | 106.0(5) | |
| C5 | C1 | Si1 | 124.2(5) | C21 | C17 | Fe2 | 68.6(4) | |
| C5 | C1 | C2 | 106.0(6) | C21 | C17 | Si2 | 122.4(5) | |
| C1 | C2 | Fe1 | 70.6(4) | C17 | C18 | Fe2 | 70.5(4) | |
| C1 | C2 | C11 | 128.2(6) | C17 | C18 | C27 | 126.1(5) | |
| C3 | C2 | Fe1 | 68.6(4) | C19 | C18 | Fe2 | 69.3(4) | |
| C3 | C2 | C1 | 107.8(5) | C19 | C18 | C17 | 108.3(6) | |
| C3 | C2 | C11 | 124.0(6) | C19 | C18 | C27 | 125.5(6) | |
| C11 | C2 | Fe1 | 125.1(4) | C27 | C18 | Fe2 | 126.2(5) | |
| C2 | C3 | Fe1 | 70.2(4) | C18 | C19 | Fe2 | 69.5(4) | |
| C4 | C3 | Fe1 | 70.1(4) | C20 | C19 | Fe2 | 70.2(4) | |
| C4 | C3 | C2 | 109.4(6) | C20 | C19 | C18 | 108.2(6) | |
| C3 | C4 | Fe1 | 69.1(4) | C19 | C20 | Fe2 | 69.5(4) | |
| C3 | C4 | C5 | 106.3(6) | C19 | C20 | C21 | 109.0(6) | |
| C5 | C4 | Fe1 | 69.4(3) | C21 | C20 | Fe2 | 69.8(4) | |
| C1 | C5 | Fe1 | 71.1(4) | C17 | C21 | Fe2 | 70.2(4) | |
| C4 | C5 | Fe1 | 69.8(4) | C20 | C21 | Fe2 | 69.7(4) | |
| C4 | C5 | C1 | 110.4(6) | C20 | C21 | C17 | 108.5(6) | |
| C7 | C6 | Fe1 | 68.7(5) | C23 | C22 | Fe2 | 71.5(6) | |
| C7 | C6 | C10 | 107.9(10) | C23 | C22 | C26 | 109.4(11) | |
| C10 | C6 | Fe1 | 69.7(4) | C26 | C22 | Fe2 | 69.1(5) | |
| C6 | C7 | Fe1 | 71.6(5) | C22 | C23 | Fe2 | 71.4(6) | |
| C6 | C7 | C8 | 107.6(10) | C22 | C23 | C24 | 112.3(11) | |
| C8 | C7 | Fe1 | 70.1(5) | C24 | C23 | Fe2 | 70.0(6) | |
| C7 | C8 | Fe1 | 69.3(6) | C23 | C24 | Fe2 | 72.7(6) | |
| C7 | C8 | C9 | 108.3(11) | C23 | C24 | C25 | 108.6(10) | |
| C9 | C8 | Fe1 | 70.6(6) | C25 | C24 | Fe2 | 67.4(5) | |
| C8 | C9 | Fe1 | 68.7(5) | C24 | C25 | Fe2 | 68.8(5) | |
| C10 | C9 | Fe1 | 70.1(5) | C26 | C25 | Fe2 | 69.4(5) | |
| C10 | C9 | C8 | 106.4(10) | C26 | C25 | C24 | 99.5(7) | |
| C6 | C10 | Fe1 | 70.4(4) | C22 | C26 | Fe2 | 72.3(5) | |
| C9 | C10 | Fe1 | 70.7(5) | C22 | C26 | C25 | 110.1(10) | |
| C9 | C10 | C6 | 109.7(10) | C25 | C26 | Fe2 | 68.4(5) | |
| N1 | C11 | C2 | 112.3(5) | C18 | C27 | N2 | 112.1(5) |
| D | H | A | d(D-H)/Å | d(H-A)/Å | d(D-A)/Å | D-H-A/° |
|---|---|---|---|---|---|---|
| N1 | H1 | Cl1 | 1.00 | 2.11 | 3.062(6) | 159.2 |
| N2 | H2 | Cl2 | 1.00 | 2.12 | 3.071(5) | 158.0 |
| A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|---|---|
| Fe1 | C1 | C2 | C3 | -58.7(4) | Fe2 | C17 | C18 | C19 | 59.2(5) | |
| Fe1 | C1 | C2 | C11 | 119.9(6) | Fe2 | C17 | C18 | C27 | -121.1(7) | |
| Fe1 | C1 | C5 | C4 | 58.9(5) | Fe2 | C17 | C21 | C20 | -59.4(5) | |
| Fe1 | C2 | C3 | C4 | -59.3(5) | Fe2 | C18 | C19 | C20 | 59.8(5) | |
| Fe1 | C2 | C11 | N1 | -131.5(5) | Fe2 | C18 | C27 | N2 | 129.5(5) | |
| Fe1 | C3 | C4 | C5 | -59.8(4) | Fe2 | C19 | C20 | C21 | 58.8(5) | |
| Fe1 | C4 | C5 | C1 | -59.6(4) | Fe2 | C20 | C21 | C17 | 59.7(5) | |
| Fe1 | C6 | C7 | C8 | 61.2(6) | Fe2 | C22 | C23 | C24 | -58.1(8) | |
| Fe1 | C6 | C10 | C9 | -60.0(6) | Fe2 | C22 | C26 | C25 | 58.1(6) | |
| Fe1 | C7 | C8 | C9 | 60.1(7) | Fe2 | C23 | C24 | C25 | -58.1(7) | |
| Fe1 | C8 | C9 | C10 | 60.2(6) | Fe2 | C24 | C25 | C26 | -63.4(6) | |
| Fe1 | C9 | C10 | C6 | 59.8(6) | Fe2 | C25 | C26 | C22 | -60.4(7) | |
| Si1 | C1 | C2 | Fe1 | -121.2(5) | Si2 | C17 | C18 | Fe2 | 121.0(6) | |
| Si1 | C1 | C2 | C3 | -179.9(5) | Si2 | C17 | C18 | C19 | -179.8(5) | |
| Si1 | C1 | C2 | C11 | -1.3(10) | Si2 | C17 | C18 | C27 | -0.2(11) | |
| Si1 | C1 | C5 | Fe1 | 120.9(5) | Si2 | C17 | C21 | Fe2 | -121.2(5) | |
| Si1 | C1 | C5 | C4 | 179.7(5) | Si2 | C17 | C21 | C20 | 179.4(5) | |
| C1 | C2 | C3 | Fe1 | 60.0(4) | C17 | C18 | C19 | Fe2 | -59.9(5) | |
| C1 | C2 | C3 | C4 | 0.7(7) | C17 | C18 | C19 | C20 | -0.1(8) | |
| C1 | C2 | C11 | N1 | 136.4(7) | C17 | C18 | C27 | N2 | -139.3(7) | |
| C2 | C1 | C5 | Fe1 | -58.4(4) | C18 | C17 | C21 | Fe2 | 58.3(5) | |
| C2 | C1 | C5 | C4 | 0.5(7) | C18 | C17 | C21 | C20 | -1.1(7) | |
| C2 | C3 | C4 | Fe1 | 59.4(4) | C18 | C19 | C20 | Fe2 | -59.4(5) | |
| C2 | C3 | C4 | C5 | -0.4(7) | C18 | C19 | C20 | C21 | -0.6(8) | |
| C3 | C2 | C11 | N1 | -45.2(9) | C19 | C18 | C27 | N2 | 40.3(9) | |
| C3 | C4 | C5 | Fe1 | 59.6(4) | C19 | C20 | C21 | Fe2 | -58.6(5) | |
| C3 | C4 | C5 | C1 | -0.1(7) | C19 | C20 | C21 | C17 | 1.1(8) | |
| C5 | C1 | C2 | Fe1 | 58.0(4) | C21 | C17 | C18 | Fe2 | -58.5(4) | |
| C5 | C1 | C2 | C3 | -0.7(7) | C21 | C17 | C18 | C19 | 0.7(8) | |
| C5 | C1 | C2 | C11 | 178.0(6) | C21 | C17 | C18 | C27 | -179.6(6) | |
| C6 | C7 | C8 | Fe1 | -62.2(6) | C22 | C23 | C24 | Fe2 | 58.9(8) | |
| C6 | C7 | C8 | C9 | -2.1(11) | C22 | C23 | C24 | C25 | 0.9(12) | |
| C7 | C6 | C10 | Fe1 | 58.2(6) | C23 | C22 | C26 | Fe2 | -60.4(8) | |
| C7 | C6 | C10 | C9 | -1.8(10) | C23 | C22 | C26 | C25 | -2.3(11) | |
| C7 | C8 | C9 | Fe1 | -59.2(7) | C23 | C24 | C25 | Fe2 | 61.3(8) | |
| C7 | C8 | C9 | C10 | 1.0(11) | C23 | C24 | C25 | C26 | -2.1(10) | |
| C8 | C9 | C10 | Fe1 | -59.3(6) | C24 | C25 | C26 | Fe2 | 63.0(6) | |
| C8 | C9 | C10 | C6 | 0.5(10) | C24 | C25 | C26 | C22 | 2.6(10) | |
| C10 | C6 | C7 | Fe1 | -58.8(6) | C26 | C22 | C23 | Fe2 | 59.0(7) | |
| C10 | C6 | C7 | C8 | 2.4(10) | C26 | C22 | C23 | C24 | 0.9(13) | |
| C11 | C2 | C3 | Fe1 | -118.7(6) | C27 | C18 | C19 | Fe2 | 120.4(7) | |
| C11 | C2 | C3 | C4 | -178.0(6) | C27 | C18 | C19 | C20 | -179.7(7) | |
| C12 | N1 | C11 | C2 | -59.0(7) | C28 | N2 | C27 | C18 | 63.7(7) | |
| C13 | N1 | C11 | C2 | 176.8(5) | C29 | N2 | C27 | C18 | -171.8(6) | |
| C14 | Si1 | C1 | Fe1 | 74.8(5) | C30 | Si2 | C17 | Fe2 | -81.0(5) | |
| C14 | Si1 | C1 | C2 | 166.9(6) | C30 | Si2 | C17 | C18 | -173.9(7) | |
| C14 | Si1 | C1 | C5 | -12.2(6) | C30 | Si2 | C17 | C21 | 5.5(7) | |
| C15 | Si1 | C1 | Fe1 | -45.8(5) | C31 | Si2 | C17 | Fe2 | 160.4(4) | |
| C15 | Si1 | C1 | C2 | 46.3(7) | C31 | Si2 | C17 | C18 | 67.4(7) | |
| C15 | Si1 | C1 | C5 | -132.8(6) | C31 | Si2 | C17 | C21 | -113.2(6) | |
| C16 | Si1 | C1 | Fe1 | -165.4(4) | C32 | Si2 | C17 | Fe2 | 39.9(5) | |
| C16 | Si1 | C1 | C2 | -73.3(7) | C32 | Si2 | C17 | C18 | -53.0(8) | |
| C16 | Si1 | C1 | C5 | 107.6(6) | C32 | Si2 | C17 | C21 | 126.3(6) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| H1 | 1198 | 2332 | 4289 | 29 |
| H3 | 1841 | 2380 | 2832 | 32 |
| H4 | 1490 | 2571 | 1268 | 34 |
| H5 | -105 | 4236 | 830 | 30 |
| H6 | 1865 | 7158 | 1055 | 66 |
| H7 | 2771 | 6109 | 2439 | 100 |
| H8 | 4191 | 4465 | 2150 | 119 |
| H9 | 4033 | 4422 | 602 | 88 |
| H10 | 2583 | 6072 | -44 | 67 |
| H11A | 1333 | 4453 | 3659 | 32 |
| H11B | -223 | 4481 | 3797 | 32 |
| H12A | -792 | 1275 | 5014 | 53 |
| H12B | -767 | 1821 | 3962 | 53 |
| H12C | -1547 | 2487 | 4605 | 53 |
| H13A | 1221 | 3623 | 5180 | 40 |
| H13B | 653 | 2252 | 5718 | 40 |
| H13C | -319 | 3345 | 5472 | 40 |
| H14A | -743 | 6742 | 502 | 63 |
| H14B | -2203 | 7037 | 828 | 63 |
| H14C | -1911 | 5749 | 674 | 63 |
| H15A | -309 | 6554 | 2968 | 70 |
| H15B | -1442 | 7412 | 2593 | 70 |
| H15C | -70 | 7477 | 1967 | 70 |
| H16A | -3271 | 4416 | 2593 | 61 |
| H16B | -3537 | 5708 | 2745 | 61 |
| H16C | -2772 | 4704 | 3403 | 61 |
| H2 | -5876 | 7323 | 4388 | 25 |
| H19 | -5877 | 7380 | 2958 | 36 |
| H20 | -4804 | 7551 | 1412 | 32 |
| H21 | -2979 | 9176 | 923 | 31 |
| H22 | -4804 | 12135 | 994 | 87 |
| H23 | -6093 | 11512 | 2445 | 94 |
| H24 | -7657 | 9886 | 2628 | 85 |
| H25 | -7337 | 9319 | 1121 | 138 |
| H26 | -5521 | 10948 | 114 | 80 |
| H27A | -5556 | 9487 | 3788 | 33 |
| H27B | -4057 | 9362 | 3908 | 33 |
| H28A | -3328 | 7344 | 4779 | 60 |
| H28B | -3780 | 6759 | 4087 | 60 |
| H28C | -4327 | 6171 | 5127 | 60 |
| H29A | -4935 | 8283 | 5592 | 45 |
| H29B | -6033 | 7206 | 5824 | 45 |
| H29C | -6321 | 8584 | 5280 | 45 |
| H30A | -665 | 11776 | 873 | 67 |
| H30B | -1925 | 11396 | 541 | 67 |
| H30C | -857 | 10413 | 842 | 67 |
| H31A | -1503 | 9813 | 3506 | 58 |
| H31B | -341 | 10622 | 2781 | 58 |
| H31C | -696 | 9262 | 2800 | 58 |
| H32A | -3476 | 11687 | 2978 | 66 |
| H32B | -3472 | 12378 | 1941 | 66 |
| H32C | -2238 | 12541 | 2384 | 66 |
Experimental
Single crystals of C16H26ClFeNSi [3193_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 ShelXL [3] refinement package using Least Squares minimisation.
Crystal structure determination of [3193_twin1_hklf4]
Crystal Data for C16H26ClFeNSi (M =351.77 g/mol): triclinic, space group P-1 (no. 2), a = 10.4038(9) Å, b = 11.5162(11) Å, c = 16.0747(16) Å, α = 71.308(9)°, β = 81.097(8)°, γ = 89.850(7)°, V = 1800.1(3) Å3, Z = 4, T = 173.15 K, μ(MoKα) = 1.044 mm-1, Dcalc = 1.298 g/cm3, 8830 reflections measured (4.426° ≤ 2Θ ≤ 52°), 8830 unique (Rint = N/A, Rsigma = 0.1178) which were used in all calculations. The final R1 was 0.0621 (I > 2σ(I)) and wR2 was 0.1843 (all data).
Refinement model description
Number of restraints - 60, number of constraints - unknown.
Details:
1. Twinned data refinement
Scales: 0.7958(13) 0.2042(13)
2. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All N(H) groups
At 1.5 times of:
All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C23) ≈ Ueq, Uanis(C22) ≈ Ueq, Uanis(C26) ≈ Ueq, Uanis(C25)
≈ Ueq, Uanis(C10) ≈ Ueq, Uanis(C6) ≈ Ueq, Uanis(C7) ≈ Ueq,
Uanis(C8) ≈ Ueq, Uanis(C9) ≈ Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C24) ≈ Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.0005
4.a Ternary CH refined with riding coordinates:
N1(H1), N2(H2)
4.b Secondary CH2 refined with riding coordinates:
C11(H11A,H11B), C27(H27A,H27B)
4.c Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C19(H19),
C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26)
4.d Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,
H15C), C16(H16A,H16B,H16C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,
H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C)
This report has been created with Olex2, compiled on 2015.01.26 svn.r3150 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.