| Identification code | 3260_twin1_hklf4 |
| Empirical formula | C37H59Fe2N2O5Si2 |
| Formula weight | 779.74 |
| Temperature/K | 173 |
| Crystal system | triclinic |
| Space group | P-1 |
| a/Å | 12.4955(17) |
| b/Å | 13.3231(18) |
| c/Å | 14.0840(17) |
| α/° | 64.660(12) |
| β/° | 81.873(11) |
| γ/° | 69.240(13) |
| Volume/Å3 | 1981.4(5) |
| Z | 2 |
| ρcalcg/cm3 | 1.307 |
| μ/mm‑1 | 0.834 |
| F(000) | 830.0 |
| Crystal size/mm3 | 0.1 × 0.1 × 0.01 |
| Radiation | MoKα (λ = 0.71073) |
| 2Θ range for data collection/° | 5.696 to 51.998 |
| Index ranges | -15 ≤ h ≤ 15, -13 ≤ k ≤ 16, -12 ≤ l ≤ 17 |
| Reflections collected | 15878 |
| Independent reflections | 7620 [Rint = 0.1129, Rsigma = 0.3177] |
| Data/restraints/parameters | 7620/6/466 |
| Goodness-of-fit on F2 | 0.658 |
| Final R indexes [I>=2σ (I)] | R1 = 0.0499, wR2 = 0.0646 |
| Final R indexes [all data] | R1 = 0.1540, wR2 = 0.0769 |
| Largest diff. peak/hole / e Å-3 | 0.48/-0.56 |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| Fe1 | 9763.0(5) | 2585.1(5) | 9996.1(5) | 26.9(2) |
| Si1 | 9800.1(10) | 4340.8(10) | 7252.7(10) | 23.9(3) |
| O1 | 10840(2) | 3178(2) | 7239(2) | 30.3(8) |
| O2 | 8791(2) | 4782(2) | 6399(2) | 24.1(8) |
| N1 | 7780(3) | 2979(3) | 7422(3) | 25.7(10) |
| C1 | 9115(3) | 3892(3) | 8563(3) | 20.6(11) |
| C2 | 8559(3) | 3016(3) | 8929(3) | 20.4(11) |
| C3 | 8031(3) | 2951(3) | 9919(4) | 28.9(13) |
| C4 | 8262(3) | 3771(3) | 10175(3) | 28.8(12) |
| C5 | 8915(3) | 4346(3) | 9352(4) | 29.9(13) |
| C6 | 11459(4) | 1859(4) | 9775(4) | 39.9(14) |
| C7 | 11321(4) | 2260(4) | 10572(4) | 41.0(14) |
| C8 | 10680(4) | 1682(4) | 11380(4) | 44.9(15) |
| C9 | 10418(4) | 905(4) | 11092(4) | 42.6(15) |
| C10 | 10895(4) | 1014(4) | 10102(4) | 33.7(13) |
| C11 | 8561(3) | 2292(3) | 8358(4) | 26.8(12) |
| C12 | 6572(3) | 3209(3) | 7740(4) | 35.6(14) |
| C13 | 8013(4) | 2296(3) | 6773(3) | 35.7(13) |
| C14 | 10338(4) | 5610(4) | 6912(4) | 26.9(12) |
| C15 | 11282(4) | 5253(4) | 7682(4) | 47.6(15) |
| C16 | 9361(4) | 6691(3) | 6947(3) | 38.7(14) |
| C17 | 10825(3) | 5941(3) | 5795(3) | 34.5(13) |
| Fe2 | 4497.8(5) | 10023.4(5) | 8123.9(5) | 27.8(2) |
| Si2 | 3473.9(10) | 9713.2(10) | 6055(1) | 23.1(3) |
| O3 | 4514(2) | 8727(2) | 5753(2) | 24.2(8) |
| O4 | 3484(2) | 11033(2) | 5243(2) | 25.8(8) |
| N2 | 5396(3) | 6882(3) | 7486(3) | 27.4(10) |
| C18 | 3683(3) | 9374(3) | 7456(3) | 23.4(11) |
| C19 | 4596(3) | 8449(3) | 8175(4) | 23.4(12) |
| C20 | 4380(4) | 8441(4) | 9196(4) | 34.5(13) |
| C21 | 3340(4) | 9364(3) | 9137(4) | 30.9(13) |
| C22 | 2900(4) | 9924(4) | 8086(4) | 28.4(13) |
| C23 | 5211(4) | 11133(4) | 6928(4) | 39.0(13) |
| C24 | 6039(4) | 10279(4) | 7682(4) | 40.9(14) |
| C25 | 5716(5) | 10360(5) | 8661(4) | 49.6(15) |
| C26 | 4664(5) | 11270(5) | 8503(5) | 46.5(15) |
| C27 | 4346(4) | 11768(4) | 7435(5) | 49.7(16) |
| C28 | 5660(3) | 7607(3) | 7920(3) | 32.0(13) |
| C29 | 4763(4) | 6145(3) | 8241(4) | 44.2(15) |
| C30 | 6467(3) | 6166(3) | 7192(3) | 36.9(13) |
| C31 | 2078(3) | 9632(3) | 5855(4) | 25.4(12) |
| C32 | 1050(3) | 10615(3) | 6015(4) | 41.4(14) |
| C33 | 2017(4) | 9758(4) | 4723(4) | 49.0(15) |
| C34 | 1938(4) | 8447(3) | 6610(4) | 48.7(16) |
| O5 | 7915(3) | 6810(3) | 4525(3) | 33.9(9) |
| C35 | 5846(5) | 5504(5) | 4680(5) | 60.2(18) |
| C36 | 5932(4) | 4543(5) | 4511(4) | 57.5(17) |
| C37 | 5085(6) | 4032(4) | 4817(5) | 57.7(18) |
| Atom | U11 | U22 | U33 | U23 | U13 | U12 |
|---|---|---|---|---|---|---|
| Fe1 | 32.0(4) | 21.9(4) | 23.4(5) | -7.9(4) | 2.2(4) | -7.5(3) |
| Si1 | 29.8(8) | 20.6(7) | 21.3(9) | -7.4(7) | 4.0(7) | -11.1(6) |
| O1 | 34.0(18) | 25.7(17) | 28(2) | -11.9(17) | 8.9(16) | -8.1(15) |
| O2 | 27.6(18) | 20.3(16) | 25(2) | -5.5(16) | 4.4(16) | -15.0(15) |
| N1 | 25(2) | 24(2) | 28(3) | -12(2) | 3(2) | -7.8(18) |
| C1 | 15(2) | 18(3) | 32(3) | -17(2) | -3(2) | 1(2) |
| C2 | 21(3) | 14(2) | 22(3) | -3(2) | 0(2) | -6(2) |
| C3 | 29(3) | 30(3) | 36(3) | -16(3) | 13(2) | -19(2) |
| C4 | 33(3) | 32(3) | 24(3) | -14(3) | 8(2) | -12(2) |
| C5 | 31(3) | 19(3) | 36(3) | -10(3) | 5(2) | -7(2) |
| C6 | 34(3) | 34(3) | 40(4) | -13(3) | -6(3) | 1(3) |
| C7 | 42(3) | 32(3) | 51(4) | -19(3) | -14(3) | -7(3) |
| C8 | 54(4) | 38(3) | 33(4) | -13(3) | -9(3) | -3(3) |
| C9 | 49(3) | 29(3) | 29(4) | -1(3) | -3(3) | -2(3) |
| C10 | 44(3) | 22(3) | 26(3) | -11(3) | -5(3) | 3(2) |
| C11 | 28(3) | 18(3) | 36(3) | -11(3) | 5(3) | -12(2) |
| C12 | 36(3) | 35(3) | 41(4) | -16(3) | 3(3) | -18(2) |
| C13 | 47(3) | 30(3) | 35(3) | -17(3) | 2(3) | -14(2) |
| C14 | 33(3) | 33(3) | 24(3) | -15(3) | 6(2) | -20(2) |
| C15 | 57(4) | 54(3) | 48(4) | -23(3) | 10(3) | -37(3) |
| C16 | 68(4) | 25(3) | 31(3) | -10(3) | 14(3) | -32(3) |
| C17 | 39(3) | 32(3) | 36(4) | -9(3) | 8(3) | -25(2) |
| Fe2 | 33.9(4) | 28.2(4) | 25.0(5) | -9.0(4) | 1.6(4) | -17.2(3) |
| Si2 | 22.3(7) | 21.1(7) | 27.3(9) | -9.8(7) | 1.3(6) | -8.9(6) |
| O3 | 20.1(17) | 20.6(17) | 26(2) | -5.0(17) | 2.3(15) | -6.8(14) |
| O4 | 26.3(18) | 17.7(16) | 26(2) | -3.2(16) | 4.1(16) | -7.2(14) |
| N2 | 23(2) | 20(2) | 32(3) | -9(2) | 6.7(19) | -3.7(18) |
| C18 | 28(3) | 19(3) | 23(3) | -6(2) | 1(2) | -10(2) |
| C19 | 20(3) | 24(3) | 24(3) | -7(3) | 8(2) | -11(2) |
| C20 | 39(3) | 30(3) | 24(3) | 1(3) | 3(3) | -16(2) |
| C21 | 35(3) | 30(3) | 32(3) | -17(3) | 15(3) | -17(2) |
| C22 | 26(3) | 26(3) | 39(4) | -17(3) | 2(3) | -13(2) |
| C23 | 51(3) | 56(4) | 26(3) | -12(3) | 6(3) | -43(3) |
| C24 | 33(3) | 37(3) | 53(4) | -16(3) | 4(3) | -16(3) |
| C25 | 68(4) | 63(4) | 31(4) | -9(3) | -10(3) | -44(3) |
| C26 | 59(4) | 60(4) | 48(4) | -31(4) | 16(3) | -46(3) |
| C27 | 56(4) | 26(3) | 62(5) | -6(3) | 2(4) | -23(3) |
| C28 | 31(3) | 30(3) | 28(3) | -8(3) | 5(2) | -8(2) |
| C29 | 49(3) | 29(3) | 45(4) | -7(3) | 11(3) | -16(3) |
| C30 | 37(3) | 31(3) | 38(4) | -16(3) | -1(3) | -2(2) |
| C31 | 16(3) | 21(3) | 44(4) | -16(3) | 9(2) | -12(2) |
| C32 | 27(3) | 43(3) | 51(4) | -15(3) | 3(3) | -14(2) |
| C33 | 36(3) | 64(4) | 59(4) | -34(4) | -11(3) | -14(3) |
| C34 | 37(3) | 35(3) | 74(5) | -18(3) | 3(3) | -19(2) |
| O5 | 44(2) | 30(2) | 21(2) | -10.2(19) | 2.5(18) | -4.9(17) |
| C35 | 49(4) | 50(4) | 77(5) | -5(4) | -1(4) | -36(3) |
| C36 | 41(4) | 58(4) | 51(4) | -8(4) | -11(3) | -4(3) |
| C37 | 63(4) | 34(3) | 72(5) | -7(4) | -41(4) | -15(3) |
| Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
|---|---|---|---|---|---|---|
| Fe1 | C1 | 2.053(4) | Fe2 | C20 | 2.044(4) | |
| Fe1 | C2 | 2.035(4) | Fe2 | C21 | 2.036(4) | |
| Fe1 | C3 | 2.051(4) | Fe2 | C22 | 2.056(4) | |
| Fe1 | C4 | 2.045(4) | Fe2 | C23 | 2.049(4) | |
| Fe1 | C5 | 2.035(4) | Fe2 | C24 | 2.039(5) | |
| Fe1 | C6 | 2.035(4) | Fe2 | C25 | 2.047(5) | |
| Fe1 | C7 | 2.046(5) | Fe2 | C26 | 2.030(5) | |
| Fe1 | C8 | 2.051(5) | Fe2 | C27 | 2.047(4) | |
| Fe1 | C9 | 2.041(4) | Si2 | O3 | 1.645(3) | |
| Fe1 | C10 | 2.025(4) | Si2 | O4 | 1.640(3) | |
| Si1 | O1 | 1.638(3) | Si2 | C18 | 1.861(5) | |
| Si1 | O2 | 1.637(3) | Si2 | C31 | 1.852(4) | |
| Si1 | C1 | 1.862(4) | N2 | C28 | 1.486(5) | |
| Si1 | C14 | 1.888(4) | N2 | C29 | 1.463(4) | |
| N1 | C11 | 1.491(5) | N2 | C30 | 1.466(4) | |
| N1 | C12 | 1.473(5) | C18 | C19 | 1.452(5) | |
| N1 | C13 | 1.484(5) | C18 | C22 | 1.444(5) | |
| C1 | C2 | 1.439(5) | C19 | C20 | 1.421(6) | |
| C1 | C5 | 1.433(5) | C19 | C28 | 1.519(5) | |
| C2 | C3 | 1.436(5) | C20 | C21 | 1.421(5) | |
| C2 | C11 | 1.496(5) | C21 | C22 | 1.430(6) | |
| C3 | C4 | 1.413(6) | C23 | C24 | 1.391(6) | |
| C4 | C5 | 1.419(5) | C23 | C27 | 1.430(6) | |
| C6 | C7 | 1.403(6) | C24 | C25 | 1.419(6) | |
| C6 | C10 | 1.416(6) | C25 | C26 | 1.403(6) | |
| C7 | C8 | 1.400(6) | C26 | C27 | 1.411(6) | |
| C8 | C9 | 1.408(6) | C31 | C32 | 1.547(5) | |
| C9 | C10 | 1.405(6) | C31 | C33 | 1.540(6) | |
| C14 | C15 | 1.521(6) | C31 | C34 | 1.537(5) | |
| C14 | C16 | 1.537(5) | C35 | C36 | 1.366(6) | |
| C14 | C17 | 1.539(5) | C35 | C371 | 1.368(7) | |
| Fe2 | C18 | 2.065(4) | C36 | C37 | 1.377(7) | |
| Fe2 | C19 | 2.027(4) | C37 | C351 | 1.368(7) |
| Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|
| C2 | Fe1 | C1 | 41.22(14) | C19 | Fe2 | C21 | 68.61(15) | |
| C2 | Fe1 | C3 | 41.16(15) | C19 | Fe2 | C22 | 68.48(15) | |
| C2 | Fe1 | C4 | 68.63(17) | C19 | Fe2 | C23 | 121.56(18) | |
| C2 | Fe1 | C7 | 158.72(19) | C19 | Fe2 | C24 | 109.20(17) | |
| C2 | Fe1 | C8 | 158.18(19) | C19 | Fe2 | C25 | 126.1(2) | |
| C2 | Fe1 | C9 | 121.3(2) | C19 | Fe2 | C26 | 162.2(2) | |
| C3 | Fe1 | C1 | 69.54(16) | C19 | Fe2 | C27 | 156.4(2) | |
| C3 | Fe1 | C8 | 123.3(2) | C20 | Fe2 | C18 | 69.89(18) | |
| C4 | Fe1 | C1 | 69.38(16) | C20 | Fe2 | C22 | 68.66(17) | |
| C4 | Fe1 | C3 | 40.36(15) | C20 | Fe2 | C23 | 156.31(18) | |
| C4 | Fe1 | C7 | 124.94(19) | C20 | Fe2 | C25 | 107.7(2) | |
| C4 | Fe1 | C8 | 109.57(19) | C20 | Fe2 | C27 | 161.2(2) | |
| C5 | Fe1 | C1 | 41.05(15) | C21 | Fe2 | C18 | 69.66(18) | |
| C5 | Fe1 | C2 | 68.43(17) | C21 | Fe2 | C20 | 40.75(14) | |
| C5 | Fe1 | C3 | 68.24(16) | C21 | Fe2 | C22 | 40.90(16) | |
| C5 | Fe1 | C4 | 40.70(14) | C21 | Fe2 | C23 | 162.04(19) | |
| C5 | Fe1 | C6 | 123.21(18) | C21 | Fe2 | C24 | 155.9(2) | |
| C5 | Fe1 | C7 | 109.95(18) | C21 | Fe2 | C25 | 119.9(2) | |
| C5 | Fe1 | C8 | 125.4(2) | C21 | Fe2 | C27 | 124.18(19) | |
| C5 | Fe1 | C9 | 160.61(19) | C22 | Fe2 | C18 | 41.03(14) | |
| C6 | Fe1 | C1 | 105.99(17) | C23 | Fe2 | C18 | 107.28(18) | |
| C6 | Fe1 | C2 | 121.57(19) | C23 | Fe2 | C22 | 125.5(2) | |
| C6 | Fe1 | C3 | 158.1(2) | C24 | Fe2 | C18 | 125.68(19) | |
| C6 | Fe1 | C4 | 159.85(19) | C24 | Fe2 | C20 | 121.73(19) | |
| C6 | Fe1 | C7 | 40.21(17) | C24 | Fe2 | C22 | 162.5(2) | |
| C6 | Fe1 | C8 | 67.82(19) | C24 | Fe2 | C23 | 39.80(16) | |
| C6 | Fe1 | C9 | 68.18(18) | C24 | Fe2 | C25 | 40.66(18) | |
| C7 | Fe1 | C1 | 123.38(18) | C24 | Fe2 | C27 | 67.66(18) | |
| C7 | Fe1 | C3 | 159.6(2) | C25 | Fe2 | C18 | 163.4(2) | |
| C7 | Fe1 | C8 | 39.96(16) | C25 | Fe2 | C22 | 154.7(2) | |
| C8 | Fe1 | C1 | 160.21(19) | C25 | Fe2 | C23 | 67.95(19) | |
| C9 | Fe1 | C1 | 156.91(19) | C25 | Fe2 | C27 | 67.8(2) | |
| C9 | Fe1 | C3 | 107.10(18) | C26 | Fe2 | C18 | 154.6(2) | |
| C9 | Fe1 | C4 | 123.69(18) | C26 | Fe2 | C20 | 124.4(2) | |
| C9 | Fe1 | C7 | 67.47(19) | C26 | Fe2 | C21 | 106.39(19) | |
| C9 | Fe1 | C8 | 40.25(17) | C26 | Fe2 | C22 | 119.71(19) | |
| C10 | Fe1 | C1 | 120.63(17) | C26 | Fe2 | C23 | 68.37(19) | |
| C10 | Fe1 | C2 | 105.46(18) | C26 | Fe2 | C24 | 67.95(19) | |
| C10 | Fe1 | C3 | 121.77(19) | C26 | Fe2 | C25 | 40.26(17) | |
| C10 | Fe1 | C4 | 158.51(18) | C26 | Fe2 | C27 | 40.48(18) | |
| C10 | Fe1 | C5 | 158.21(18) | C27 | Fe2 | C18 | 119.8(2) | |
| C10 | Fe1 | C6 | 40.82(16) | C27 | Fe2 | C22 | 107.10(19) | |
| C10 | Fe1 | C7 | 67.76(19) | C27 | Fe2 | C23 | 40.86(17) | |
| C10 | Fe1 | C8 | 67.83(18) | O3 | Si2 | C18 | 107.39(17) | |
| C10 | Fe1 | C9 | 40.43(16) | O3 | Si2 | C31 | 109.38(17) | |
| O1 | Si1 | C1 | 107.24(16) | O4 | Si2 | O3 | 109.28(15) | |
| O1 | Si1 | C14 | 111.11(17) | O4 | Si2 | C18 | 113.54(18) | |
| O2 | Si1 | O1 | 111.61(17) | O4 | Si2 | C31 | 106.34(17) | |
| O2 | Si1 | C1 | 105.47(17) | C31 | Si2 | C18 | 110.9(2) | |
| O2 | Si1 | C14 | 107.21(18) | C29 | N2 | C28 | 111.0(3) | |
| C1 | Si1 | C14 | 114.1(2) | C29 | N2 | C30 | 111.1(3) | |
| C12 | N1 | C11 | 111.1(3) | C30 | N2 | C28 | 109.0(3) | |
| C12 | N1 | C13 | 108.4(3) | Si2 | C18 | Fe2 | 130.9(2) | |
| C13 | N1 | C11 | 109.1(3) | C19 | C18 | Fe2 | 67.8(2) | |
| Si1 | C1 | Fe1 | 130.95(19) | C19 | C18 | Si2 | 128.3(3) | |
| C2 | C1 | Fe1 | 68.7(2) | C22 | C18 | Fe2 | 69.2(2) | |
| C2 | C1 | Si1 | 122.7(3) | C22 | C18 | Si2 | 126.4(3) | |
| C5 | C1 | Fe1 | 68.8(2) | C22 | C18 | C19 | 105.0(4) | |
| C5 | C1 | Si1 | 131.4(3) | C18 | C19 | Fe2 | 70.6(2) | |
| C5 | C1 | C2 | 105.6(4) | C18 | C19 | C28 | 127.3(4) | |
| C1 | C2 | Fe1 | 70.1(2) | C20 | C19 | Fe2 | 70.2(3) | |
| C1 | C2 | C11 | 124.3(4) | C20 | C19 | C18 | 110.0(3) | |
| C3 | C2 | Fe1 | 70.0(3) | C20 | C19 | C28 | 122.7(4) | |
| C3 | C2 | C1 | 109.0(4) | C28 | C19 | Fe2 | 124.6(3) | |
| C3 | C2 | C11 | 126.7(4) | C19 | C20 | Fe2 | 68.9(2) | |
| C11 | C2 | Fe1 | 125.3(3) | C21 | C20 | Fe2 | 69.3(2) | |
| C2 | C3 | Fe1 | 68.8(2) | C21 | C20 | C19 | 107.4(4) | |
| C4 | C3 | Fe1 | 69.6(2) | C20 | C21 | Fe2 | 69.9(2) | |
| C4 | C3 | C2 | 107.7(4) | C20 | C21 | C22 | 108.5(4) | |
| C3 | C4 | Fe1 | 70.0(2) | C22 | C21 | Fe2 | 70.3(2) | |
| C3 | C4 | C5 | 108.0(4) | C18 | C22 | Fe2 | 69.8(2) | |
| C5 | C4 | Fe1 | 69.2(2) | C21 | C22 | Fe2 | 68.8(2) | |
| C1 | C5 | Fe1 | 70.2(2) | C21 | C22 | C18 | 109.1(4) | |
| C4 | C5 | Fe1 | 70.1(2) | C24 | C23 | Fe2 | 69.7(3) | |
| C4 | C5 | C1 | 109.7(4) | C24 | C23 | C27 | 107.5(5) | |
| C7 | C6 | Fe1 | 70.3(3) | C27 | C23 | Fe2 | 69.5(3) | |
| C7 | C6 | C10 | 107.2(4) | C23 | C24 | Fe2 | 70.5(3) | |
| C10 | C6 | Fe1 | 69.2(2) | C23 | C24 | C25 | 109.0(4) | |
| C6 | C7 | Fe1 | 69.5(3) | C25 | C24 | Fe2 | 70.0(3) | |
| C8 | C7 | Fe1 | 70.2(3) | C24 | C25 | Fe2 | 69.4(3) | |
| C8 | C7 | C6 | 108.8(4) | C26 | C25 | Fe2 | 69.3(3) | |
| C7 | C8 | Fe1 | 69.8(3) | C26 | C25 | C24 | 107.4(5) | |
| C7 | C8 | C9 | 107.9(4) | C25 | C26 | Fe2 | 70.5(3) | |
| C9 | C8 | Fe1 | 69.5(3) | C25 | C26 | C27 | 108.5(5) | |
| C8 | C9 | Fe1 | 70.3(3) | C27 | C26 | Fe2 | 70.4(3) | |
| C10 | C9 | Fe1 | 69.2(3) | C23 | C27 | Fe2 | 69.6(2) | |
| C10 | C9 | C8 | 107.9(5) | C26 | C27 | Fe2 | 69.1(3) | |
| C6 | C10 | Fe1 | 70.0(2) | C26 | C27 | C23 | 107.6(4) | |
| C9 | C10 | Fe1 | 70.4(3) | N2 | C28 | C19 | 113.1(4) | |
| C9 | C10 | C6 | 108.2(5) | C32 | C31 | Si2 | 112.6(3) | |
| N1 | C11 | C2 | 112.3(3) | C33 | C31 | Si2 | 108.7(3) | |
| C15 | C14 | Si1 | 109.7(3) | C33 | C31 | C32 | 108.2(4) | |
| C15 | C14 | C16 | 109.6(4) | C34 | C31 | Si2 | 111.5(3) | |
| C15 | C14 | C17 | 109.0(4) | C34 | C31 | C32 | 107.6(3) | |
| C16 | C14 | Si1 | 110.8(3) | C34 | C31 | C33 | 108.0(4) | |
| C16 | C14 | C17 | 108.5(4) | C36 | C35 | C371 | 120.0(5) | |
| C17 | C14 | Si1 | 109.3(3) | C35 | C36 | C37 | 121.6(5) | |
| C19 | Fe2 | C18 | 41.55(15) | C351 | C37 | C36 | 118.4(5) | |
| C19 | Fe2 | C20 | 40.86(16) |
| D | H | A | d(D-H)/Å | d(H-A)/Å | d(D-A)/Å | D-H-A/° |
|---|---|---|---|---|---|---|
| O2 | H2 | N1 | 0.939(18) | 1.96(2) | 2.848(4) | 158(3) |
| O3 | H3A | N2 | 0.991(19) | 1.67(3) | 2.630(4) | 161(5) |
| O4 | H4A | O31 | 0.938(18) | 1.807(19) | 2.742(4) | 175(4) |
| O5 | H5A | O2 | 0.971(19) | 1.92(2) | 2.843(4) | 157(4) |
| O1 | H1 | O52 | 0.996(19) | 1.79(3) | 2.735(4) | 158(4) |
| A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|---|---|
| Fe1 | C1 | C2 | C3 | 59.4(3) | Fe2 | C18 | C19 | C28 | -119.3(4) | |
| Fe1 | C1 | C2 | C11 | -119.8(4) | Fe2 | C18 | C22 | C21 | -57.6(3) | |
| Fe1 | C1 | C5 | C4 | -59.0(3) | Fe2 | C19 | C20 | C21 | 58.8(3) | |
| Fe1 | C2 | C3 | C4 | 59.0(3) | Fe2 | C19 | C28 | N2 | -150.3(3) | |
| Fe1 | C2 | C11 | N1 | -163.5(3) | Fe2 | C20 | C21 | C22 | 60.0(3) | |
| Fe1 | C3 | C4 | C5 | 59.0(3) | Fe2 | C21 | C22 | C18 | 58.2(3) | |
| Fe1 | C4 | C5 | C1 | 59.1(3) | Fe2 | C23 | C24 | C25 | -59.6(3) | |
| Fe1 | C6 | C7 | C8 | 59.4(3) | Fe2 | C23 | C27 | C26 | 58.9(3) | |
| Fe1 | C6 | C10 | C9 | -60.3(3) | Fe2 | C24 | C25 | C26 | -59.1(3) | |
| Fe1 | C7 | C8 | C9 | 59.3(3) | Fe2 | C25 | C26 | C27 | -60.4(3) | |
| Fe1 | C8 | C9 | C10 | 59.1(3) | Fe2 | C26 | C27 | C23 | -59.2(3) | |
| Fe1 | C9 | C10 | C6 | 60.0(3) | Si2 | C18 | C19 | Fe2 | 125.4(3) | |
| Si1 | C1 | C2 | Fe1 | 125.9(3) | Si2 | C18 | C19 | C20 | -175.2(3) | |
| Si1 | C1 | C2 | C3 | -174.8(3) | Si2 | C18 | C19 | C28 | 6.2(6) | |
| Si1 | C1 | C2 | C11 | 6.1(5) | Si2 | C18 | C22 | Fe2 | -126.2(3) | |
| Si1 | C1 | C5 | Fe1 | -126.5(3) | Si2 | C18 | C22 | C21 | 176.2(3) | |
| Si1 | C1 | C5 | C4 | 174.5(3) | O3 | Si2 | C18 | Fe2 | 94.7(3) | |
| O1 | Si1 | C1 | Fe1 | 27.0(3) | O3 | Si2 | C18 | C19 | 1.9(4) | |
| O1 | Si1 | C1 | C2 | -62.3(4) | O3 | Si2 | C18 | C22 | -172.2(3) | |
| O1 | Si1 | C1 | C5 | 124.2(4) | O3 | Si2 | C31 | C32 | -174.3(3) | |
| O1 | Si1 | C14 | C15 | -57.9(3) | O3 | Si2 | C31 | C33 | -54.4(3) | |
| O1 | Si1 | C14 | C16 | -179.0(3) | O3 | Si2 | C31 | C34 | 64.6(3) | |
| O1 | Si1 | C14 | C17 | 61.6(3) | O4 | Si2 | C18 | Fe2 | -26.2(3) | |
| O2 | Si1 | C1 | Fe1 | 146.0(3) | O4 | Si2 | C18 | C19 | -119.1(4) | |
| O2 | Si1 | C1 | C2 | 56.8(3) | O4 | Si2 | C18 | C22 | 66.9(4) | |
| O2 | Si1 | C1 | C5 | -116.7(4) | O4 | Si2 | C31 | C32 | -56.4(4) | |
| O2 | Si1 | C14 | C15 | 179.9(3) | O4 | Si2 | C31 | C33 | 63.5(3) | |
| O2 | Si1 | C14 | C16 | 58.8(4) | O4 | Si2 | C31 | C34 | -177.5(3) | |
| O2 | Si1 | C14 | C17 | -60.6(3) | C18 | Si2 | C31 | C32 | 67.5(3) | |
| C1 | Si1 | C14 | C15 | 63.5(3) | C18 | Si2 | C31 | C33 | -172.6(3) | |
| C1 | Si1 | C14 | C16 | -57.6(4) | C18 | Si2 | C31 | C34 | -53.7(3) | |
| C1 | Si1 | C14 | C17 | -177.0(3) | C18 | C19 | C20 | Fe2 | -59.6(3) | |
| C1 | C2 | C3 | Fe1 | -59.4(3) | C18 | C19 | C20 | C21 | -0.7(5) | |
| C1 | C2 | C3 | C4 | -0.4(5) | C18 | C19 | C28 | N2 | -59.2(5) | |
| C1 | C2 | C11 | N1 | -74.8(5) | C19 | C18 | C22 | Fe2 | 58.7(3) | |
| C2 | C1 | C5 | Fe1 | 59.2(3) | C19 | C18 | C22 | C21 | 1.1(4) | |
| C2 | C1 | C5 | C4 | 0.1(4) | C19 | C20 | C21 | Fe2 | -58.6(3) | |
| C2 | C3 | C4 | Fe1 | -58.5(3) | C19 | C20 | C21 | C22 | 1.4(5) | |
| C2 | C3 | C4 | C5 | 0.5(5) | C20 | C19 | C28 | N2 | 122.4(4) | |
| C3 | C2 | C11 | N1 | 106.2(5) | C20 | C21 | C22 | Fe2 | -59.8(3) | |
| C3 | C4 | C5 | Fe1 | -59.5(3) | C20 | C21 | C22 | C18 | -1.6(5) | |
| C3 | C4 | C5 | C1 | -0.4(5) | C22 | C18 | C19 | Fe2 | -59.6(3) | |
| C5 | C1 | C2 | Fe1 | -59.2(3) | C22 | C18 | C19 | C20 | -0.2(5) | |
| C5 | C1 | C2 | C3 | 0.2(4) | C22 | C18 | C19 | C28 | -178.8(4) | |
| C5 | C1 | C2 | C11 | -178.9(4) | C23 | C24 | C25 | Fe2 | 59.9(3) | |
| C6 | C7 | C8 | Fe1 | -58.9(3) | C23 | C24 | C25 | C26 | 0.8(6) | |
| C6 | C7 | C8 | C9 | 0.4(5) | C24 | C23 | C27 | Fe2 | -59.6(3) | |
| C7 | C6 | C10 | Fe1 | 60.3(3) | C24 | C23 | C27 | C26 | -0.7(5) | |
| C7 | C6 | C10 | C9 | 0.0(5) | C24 | C25 | C26 | Fe2 | 59.1(3) | |
| C7 | C8 | C9 | Fe1 | -59.5(3) | C24 | C25 | C26 | C27 | -1.3(6) | |
| C7 | C8 | C9 | C10 | -0.4(5) | C25 | C26 | C27 | Fe2 | 60.5(3) | |
| C8 | C9 | C10 | Fe1 | -59.8(3) | C25 | C26 | C27 | C23 | 1.2(6) | |
| C8 | C9 | C10 | C6 | 0.2(5) | C27 | C23 | C24 | Fe2 | 59.5(3) | |
| C10 | C6 | C7 | Fe1 | -59.6(3) | C27 | C23 | C24 | C25 | -0.1(5) | |
| C10 | C6 | C7 | C8 | -0.3(5) | C28 | C19 | C20 | Fe2 | 119.1(4) | |
| C11 | C2 | C3 | Fe1 | 119.7(4) | C28 | C19 | C20 | C21 | 177.9(4) | |
| C11 | C2 | C3 | C4 | 178.7(4) | C29 | N2 | C28 | C19 | -61.4(4) | |
| C12 | N1 | C11 | C2 | -72.7(4) | C30 | N2 | C28 | C19 | 175.8(3) | |
| C13 | N1 | C11 | C2 | 167.8(3) | C31 | Si2 | C18 | Fe2 | -145.9(2) | |
| C14 | Si1 | C1 | Fe1 | -96.6(3) | C31 | Si2 | C18 | C19 | 121.3(4) | |
| C14 | Si1 | C1 | C2 | 174.2(3) | C31 | Si2 | C18 | C22 | -52.7(4) | |
| C14 | Si1 | C1 | C5 | 0.7(4) | C35 | C36 | C37 | C351 | -1.4(9) | |
| Fe2 | C18 | C19 | C20 | 59.3(3) | C371 | C35 | C36 | C37 | 1.4(9) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| H2 | 8310(20) | 4330(20) | 6600(30) | 19(12) |
| H3 | 7604 | 2447 | 10328 | 35 |
| H4 | 8022 | 3912 | 10790 | 35 |
| H5 | 9180 | 4943 | 9327 | 36 |
| H6 | 11856 | 2109 | 9136 | 48 |
| H7 | 11615 | 2831 | 10565 | 49 |
| H8 | 10460 | 1794 | 12011 | 54 |
| H9 | 9994 | 396 | 11495 | 51 |
| H10 | 10847 | 593 | 9718 | 40 |
| H11A | 9349 | 1983 | 8128 | 32 |
| H11B | 8324 | 1612 | 8844 | 32 |
| H12A | 6414 | 3625 | 8201 | 53 |
| H12B | 6422 | 2462 | 8117 | 53 |
| H12C | 6077 | 3695 | 7115 | 53 |
| H13A | 7897 | 1537 | 7194 | 53 |
| H13B | 8806 | 2162 | 6531 | 53 |
| H13C | 7491 | 2736 | 6164 | 53 |
| H15A | 11910 | 4573 | 7650 | 71 |
| H15B | 10977 | 5046 | 8396 | 71 |
| H15C | 11566 | 5910 | 7498 | 71 |
| H16A | 9084 | 6515 | 7668 | 58 |
| H16B | 8734 | 6889 | 6484 | 58 |
| H16C | 9643 | 7358 | 6710 | 58 |
| H17A | 10221 | 6176 | 5293 | 52 |
| H17B | 11454 | 5261 | 5761 | 52 |
| H17C | 11111 | 6595 | 5617 | 52 |
| H3A | 4850(40) | 7940(20) | 6320(30) | 110(20) |
| H4A | 4150(20) | 11160(30) | 4880(30) | 55(16) |
| H20 | 4845 | 7915 | 9805 | 41 |
| H21 | 2996 | 9574 | 9701 | 37 |
| H22 | 2204 | 10556 | 7842 | 34 |
| H23 | 5219 | 11270 | 6208 | 47 |
| H24 | 6712 | 9729 | 7561 | 49 |
| H25 | 6134 | 9886 | 9304 | 59 |
| H26 | 4238 | 11510 | 9028 | 56 |
| H27 | 3679 | 12409 | 7111 | 60 |
| H28A | 6121 | 8065 | 7405 | 38 |
| H28B | 6130 | 7080 | 8568 | 38 |
| H29A | 4070 | 6641 | 8448 | 66 |
| H29B | 5245 | 5580 | 8863 | 66 |
| H29C | 4551 | 5719 | 7918 | 66 |
| H30A | 6953 | 5634 | 7819 | 55 |
| H30B | 6868 | 6680 | 6679 | 55 |
| H30C | 6298 | 5704 | 6884 | 55 |
| H32A | 1109 | 11384 | 5533 | 62 |
| H32B | 1055 | 10530 | 6741 | 62 |
| H32C | 336 | 10553 | 5874 | 62 |
| H33A | 2639 | 9118 | 4617 | 74 |
| H33B | 2093 | 10515 | 4227 | 74 |
| H33C | 1279 | 9721 | 4606 | 74 |
| H34A | 1982 | 8344 | 7337 | 73 |
| H34B | 2550 | 7809 | 6491 | 73 |
| H34C | 1194 | 8432 | 6484 | 73 |
| H5A | 8210(30) | 6270(30) | 5230(18) | 55(17) |
| H5B | 7350(30) | 7470(30) | 4640(30) | 78(18) |
| H35 | 6434 | 5851 | 4448 | 72 |
| H36 | 6591 | 4218 | 4174 | 69 |
| H37 | 5147 | 3374 | 4681 | 69 |
| H1 | 11140(40) | 3130(40) | 6560(20) | 87 |
Experimental
Single crystals of C37H59Fe2N2O5Si2 [3260_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 [3260_twin1_hklf4]
Crystal Data for C37H59Fe2N2O5Si2 (M =779.74 g/mol): triclinic, space group P-1 (no. 2), a = 12.4955(17) Å, b = 13.3231(18) Å, c = 14.0840(17) Å, α = 64.660(12)°, β = 81.873(11)°, γ = 69.240(13)°, V = 1981.4(5) Å3, Z = 2, T = 173 K, μ(MoKα) = 0.834 mm-1, Dcalc = 1.307 g/cm3, 15878 reflections measured (5.696° ≤ 2Θ ≤ 51.998°), 7620 unique (Rint = 0.1129, Rsigma = 0.3177) which were used in all calculations. The final R1 was 0.0499 (I > 2σ(I)) and wR2 was 0.0769 (all data).
Refinement model description
Number of restraints - 6, number of constraints - unknown.
Details:
1. Fixed Uiso
At 1.2 times of:
All C(H,H) groups, H35 of C35, H7 of C7, H6 of C6, H5 of C5, H4 of C4, H3
of C3, H9 of C9, H8 of C8, H10 of C10, H21 of C21, H20 of C20, H25 of C25,
H24 of C24, H23 of C23, H22 of C22, H26 of C26, H27 of C27, H36 of C36, H37
of C37
At 1.5 times of:
All C(H,H,H) groups, H1 of C37
2. Restrained distances
O4-H4A = O5_$1-H5B_$1
1 with sigma of 0.02
O3-H3A
1 with sigma of 0.02
O2-H2 = O5_$1-H5A_$1 = O1-H1
1 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
C11(H11A,H11B), C28(H28A,H28B)
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), C20(H20),
C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C35(H35),
C36(H36), C37(H37)
3.c Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
H16C), C17(H17A,H17B,H17C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,
H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
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.