| Identification code | mo_B0167_0m |
| Empirical formula | C38H60Fe2N2O4Si2 |
| Formula weight | 776.76 |
| Temperature/K | 100.01 |
| Crystal system | triclinic |
| Space group | P-1 |
| a/Å | 7.622(8) |
| b/Å | 9.880(8) |
| c/Å | 14.226(12) |
| α/° | 76.29(3) |
| β/° | 85.20(3) |
| γ/° | 70.52(3) |
| Volume/Å3 | 981.2(15) |
| Z | 1 |
| ρcalcg/cm3 | 1.315 |
| μ/mm‑1 | 0.840 |
| F(000) | 414.0 |
| Crystal size/mm3 | 0.345 × 0.172 × 0.08 |
| Radiation | MoKα (λ = 0.71073) |
| 2Θ range for data collection/° | 4.788 to 57.612 |
| Index ranges | -10 ≤ h ≤ 10, -11 ≤ k ≤ 13, -19 ≤ l ≤ 19 |
| Reflections collected | 23027 |
| Independent reflections | 5104 [Rint = 0.0371, Rsigma = 0.0295] |
| Data/restraints/parameters | 5104/0/224 |
| Goodness-of-fit on F2 | 1.048 |
| Final R indexes [I>=2σ (I)] | R1 = 0.0373, wR2 = 0.0858 |
| Final R indexes [all data] | R1 = 0.0497, wR2 = 0.0913 |
| Largest diff. peak/hole / e Å-3 | 0.72/-0.45 |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| Fe1 | 2000.8(4) | 6859.2(3) | 5423.0(2) | 20.46(8) |
| Si1 | 2707.8(7) | 7578.1(6) | 7634.1(4) | 21.41(11) |
| O1 | 2676(2) | 9267.8(16) | 7180.0(11) | 36.4(4) |
| O2 | 4825(2) | 6439.3(18) | 7699.4(11) | 35.4(3) |
| N1 | 2329(3) | 3420(2) | 8121.7(13) | 40.7(5) |
| C1 | 1453(2) | 6980(2) | 6846.5(13) | 21.1(3) |
| C2 | 1639(3) | 5534(2) | 6724.6(13) | 24.6(4) |
| C3 | 292(3) | 5690(3) | 6043.6(15) | 37.0(5) |
| C4 | -737(3) | 7194(3) | 5739.5(17) | 42.7(6) |
| C5 | -26(3) | 7992(3) | 6231.1(15) | 33.4(5) |
| C6 | 4438(2) | 5758(2) | 4823.1(12) | 19.8(3) |
| C7 | 2968(3) | 6267(2) | 4142.5(12) | 23.2(4) |
| C8 | 2220(3) | 7816(2) | 3991.6(15) | 29.7(4) |
| C9 | 3223(3) | 8279(2) | 4578.2(15) | 29.5(4) |
| C10 | 4584(2) | 7012(2) | 5097.3(13) | 22.1(4) |
| C11 | 3016(3) | 4109(2) | 7201.8(15) | 31.8(5) |
| C12 | 865(4) | 2874(3) | 7983.2(19) | 52.8(8) |
| C13 | 3865(5) | 2228(3) | 8633.3(19) | 61.3(8) |
| C14 | 1471(3) | 7694(2) | 8822.9(14) | 32.5(5) |
| C15 | 1231(5) | 6228(3) | 9320.6(18) | 56.8(8) |
| C16 | -478(4) | 8847(3) | 8625(2) | 50.9(7) |
| C17 | 2481(4) | 8217(4) | 9468.6(18) | 52.8(7) |
| C18 | 3980(4) | 9740(3) | 6538.6(17) | 45.7(6) |
| C19 | 6368(4) | 6517(4) | 8155(2) | 58.6(8) |
| Atom | U11 | U22 | U33 | U23 | U13 | U12 |
|---|---|---|---|---|---|---|
| Fe1 | 18.65(13) | 28.38(15) | 20.23(13) | -9.36(10) | 2.37(9) | -13.11(10) |
| Si1 | 28.0(3) | 23.8(3) | 19.5(2) | -7.40(19) | 2.69(19) | -16.5(2) |
| O1 | 56(1) | 28.3(8) | 35.5(8) | -11.6(6) | 15.5(7) | -28.1(7) |
| O2 | 25.3(7) | 45.0(9) | 40.0(8) | -10.5(7) | -6.6(6) | -14.5(6) |
| N1 | 74.0(14) | 31.7(10) | 26.9(9) | -12.2(8) | 20.5(9) | -31.9(10) |
| C1 | 20.3(8) | 27.0(9) | 20.2(8) | -10.4(7) | 4.3(6) | -10.6(7) |
| C2 | 29.9(10) | 33.4(10) | 22.2(9) | -14.1(8) | 12.9(7) | -23.2(8) |
| C3 | 36.5(11) | 68.6(16) | 30.2(11) | -27.6(11) | 16.4(9) | -41.1(12) |
| C4 | 19(1) | 85(2) | 32.3(11) | -23.1(12) | 3.9(8) | -21.4(11) |
| C5 | 21.9(9) | 44.1(13) | 31.3(11) | -15.5(9) | 1.2(8) | -2.4(8) |
| C6 | 20.4(8) | 27.7(9) | 16.0(8) | -5.8(7) | 4.9(6) | -14.5(7) |
| C7 | 25.3(9) | 33.9(10) | 14.9(8) | -5.5(7) | 2.6(7) | -16.2(8) |
| C8 | 29.6(10) | 33.4(11) | 25.7(10) | 2.4(8) | -4.3(8) | -14.7(8) |
| C9 | 28.2(10) | 27.2(10) | 36.0(11) | -2.9(8) | -0.2(8) | -15.4(8) |
| C10 | 20.2(8) | 28.9(10) | 23.8(9) | -8.3(7) | 4.0(7) | -15.7(7) |
| C11 | 47.0(12) | 26.5(10) | 28.5(10) | -10.5(8) | 17.2(9) | -21.4(9) |
| C12 | 87(2) | 47.3(14) | 45.4(14) | -22.4(12) | 39.1(14) | -51.0(15) |
| C13 | 107(3) | 45.6(16) | 34.5(13) | 3.3(11) | 3.8(15) | -37.6(17) |
| C14 | 52.5(13) | 35.4(11) | 23.1(9) | -13.5(8) | 10.5(9) | -29.5(10) |
| C15 | 114(3) | 45.1(14) | 27.3(11) | -13.8(10) | 22.6(14) | -47.4(16) |
| C16 | 57.4(16) | 63.2(17) | 43.9(14) | -29.0(13) | 23.0(12) | -28.6(14) |
| C17 | 72.6(18) | 81(2) | 31.6(12) | -33.9(13) | 13.7(12) | -48.9(16) |
| C18 | 78.0(18) | 43.6(13) | 34.2(12) | -12.5(10) | 18.1(12) | -45.7(13) |
| C19 | 33.1(13) | 108(3) | 42.5(14) | -20.1(15) | -6.8(11) | -28.9(15) |
| Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
|---|---|---|---|---|---|---|
| Fe1 | C1 | 2.057(2) | N1 | C12 | 1.436(3) | |
| Fe1 | C2 | 2.055(2) | N1 | C13 | 1.450(4) | |
| Fe1 | C3 | 2.034(2) | C1 | C2 | 1.439(3) | |
| Fe1 | C4 | 2.030(3) | C1 | C5 | 1.427(3) | |
| Fe1 | C5 | 2.030(2) | C2 | C3 | 1.417(3) | |
| Fe1 | C6 | 2.047(2) | C2 | C11 | 1.492(3) | |
| Fe1 | C7 | 2.048(2) | C3 | C4 | 1.409(4) | |
| Fe1 | C8 | 2.050(3) | C4 | C5 | 1.419(3) | |
| Fe1 | C9 | 2.041(2) | C6 | C61 | 1.445(4) | |
| Fe1 | C10 | 2.031(3) | C6 | C7 | 1.422(3) | |
| Si1 | O1 | 1.634(2) | C6 | C10 | 1.424(3) | |
| Si1 | O2 | 1.626(2) | C7 | C8 | 1.412(3) | |
| Si1 | C1 | 1.841(2) | C8 | C9 | 1.419(3) | |
| Si1 | C14 | 1.875(2) | C9 | C10 | 1.418(3) | |
| O1 | C18 | 1.412(3) | C14 | C15 | 1.517(3) | |
| O2 | C19 | 1.421(3) | C14 | C16 | 1.541(4) | |
| N1 | C11 | 1.466(3) | C14 | C17 | 1.521(3) |
| Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|
| C2 | Fe1 | C1 | 40.96(8) | C18 | O1 | Si1 | 127.68(16) | |
| C3 | Fe1 | C1 | 68.69(8) | C19 | O2 | Si1 | 127.22(19) | |
| C3 | Fe1 | C2 | 40.53(8) | C12 | N1 | C11 | 112.1(2) | |
| C3 | Fe1 | C6 | 117.51(11) | C12 | N1 | C13 | 110.0(2) | |
| C3 | Fe1 | C7 | 108.08(9) | C13 | N1 | C11 | 109.1(2) | |
| C3 | Fe1 | C8 | 128.43(9) | Si1 | C1 | Fe1 | 128.09(10) | |
| C3 | Fe1 | C9 | 166.73(9) | C2 | C1 | Fe1 | 69.47(10) | |
| C4 | Fe1 | C1 | 69.02(8) | C2 | C1 | Si1 | 130.93(15) | |
| C4 | Fe1 | C2 | 68.51(10) | C5 | C1 | Fe1 | 68.55(12) | |
| C4 | Fe1 | C3 | 40.57(11) | C5 | C1 | Si1 | 122.37(16) | |
| C4 | Fe1 | C6 | 150.69(9) | C5 | C1 | C2 | 106.68(18) | |
| C4 | Fe1 | C7 | 117.54(9) | C1 | C2 | Fe1 | 69.57(11) | |
| C4 | Fe1 | C8 | 108.04(10) | C1 | C2 | C11 | 127.19(18) | |
| C4 | Fe1 | C9 | 128.77(11) | C3 | C2 | Fe1 | 68.92(13) | |
| C4 | Fe1 | C10 | 167.18(10) | C3 | C2 | C1 | 107.84(19) | |
| C5 | Fe1 | C1 | 40.86(8) | C3 | C2 | C11 | 124.96(19) | |
| C5 | Fe1 | C2 | 68.48(10) | C11 | C2 | Fe1 | 125.97(14) | |
| C5 | Fe1 | C3 | 68.34(11) | C2 | C3 | Fe1 | 70.54(12) | |
| C5 | Fe1 | C4 | 40.92(10) | C4 | C3 | Fe1 | 69.55(14) | |
| C5 | Fe1 | C6 | 167.01(8) | C4 | C3 | C2 | 108.95(19) | |
| C5 | Fe1 | C7 | 151.29(8) | C3 | C4 | Fe1 | 69.87(12) | |
| C5 | Fe1 | C8 | 118.25(10) | C3 | C4 | C5 | 107.6(2) | |
| C5 | Fe1 | C9 | 108.55(11) | C5 | C4 | Fe1 | 69.53(12) | |
| C5 | Fe1 | C10 | 128.75(9) | C1 | C5 | Fe1 | 70.59(12) | |
| C6 | Fe1 | C1 | 128.31(8) | C4 | C5 | Fe1 | 69.55(14) | |
| C6 | Fe1 | C2 | 107.77(9) | C4 | C5 | C1 | 108.9(2) | |
| C6 | Fe1 | C7 | 40.63(7) | C61 | C6 | Fe1 | 126.08(17) | |
| C6 | Fe1 | C8 | 68.32(9) | C7 | C6 | Fe1 | 69.73(12) | |
| C7 | Fe1 | C1 | 166.69(8) | C7 | C6 | C61 | 126.1(2) | |
| C7 | Fe1 | C2 | 128.38(9) | C7 | C6 | C10 | 107.41(17) | |
| C7 | Fe1 | C8 | 40.30(9) | C10 | C6 | Fe1 | 68.96(11) | |
| C8 | Fe1 | C1 | 151.62(9) | C10 | C6 | C61 | 126.5(2) | |
| C8 | Fe1 | C2 | 166.29(8) | C6 | C7 | Fe1 | 69.63(12) | |
| C9 | Fe1 | C1 | 118.04(9) | C8 | C7 | Fe1 | 69.92(12) | |
| C9 | Fe1 | C2 | 151.70(8) | C8 | C7 | C6 | 108.56(17) | |
| C9 | Fe1 | C6 | 68.46(10) | C7 | C8 | Fe1 | 69.78(11) | |
| C9 | Fe1 | C7 | 68.04(9) | C7 | C8 | C9 | 107.86(18) | |
| C9 | Fe1 | C8 | 40.58(8) | C9 | C8 | Fe1 | 69.36(13) | |
| C10 | Fe1 | C1 | 107.76(8) | C8 | C9 | Fe1 | 70.07(13) | |
| C10 | Fe1 | C2 | 117.78(8) | C10 | C9 | Fe1 | 69.24(13) | |
| C10 | Fe1 | C3 | 151.10(10) | C10 | C9 | C8 | 108.16(19) | |
| C10 | Fe1 | C6 | 40.87(8) | C6 | C10 | Fe1 | 70.17(10) | |
| C10 | Fe1 | C7 | 68.42(8) | C9 | C10 | Fe1 | 69.99(12) | |
| C10 | Fe1 | C8 | 68.52(8) | C9 | C10 | C6 | 108.00(17) | |
| C10 | Fe1 | C9 | 40.77(8) | N1 | C11 | C2 | 112.70(18) | |
| O1 | Si1 | C1 | 110.75(10) | C15 | C14 | Si1 | 110.79(16) | |
| O1 | Si1 | C14 | 103.32(9) | C15 | C14 | C16 | 108.1(2) | |
| O2 | Si1 | O1 | 110.90(10) | C15 | C14 | C17 | 111.3(2) | |
| O2 | Si1 | C1 | 105.80(10) | C16 | C14 | Si1 | 108.18(16) | |
| O2 | Si1 | C14 | 115.34(11) | C17 | C14 | Si1 | 111.02(17) | |
| C1 | Si1 | C14 | 110.81(11) | C17 | C14 | C16 | 107.3(2) |
| A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|---|---|
| Fe1 | C1 | C2 | C3 | -58.46(14) | C1 | C2 | C3 | Fe1 | 58.87(13) | |
| Fe1 | C1 | C2 | C11 | 120.27(19) | C1 | C2 | C3 | C4 | -0.3(2) | |
| Fe1 | C1 | C5 | C4 | 59.18(15) | C1 | C2 | C11 | N1 | 90.2(2) | |
| Fe1 | C2 | C3 | C4 | -59.13(15) | C2 | C1 | C5 | Fe1 | -59.26(13) | |
| Fe1 | C2 | C11 | N1 | -179.31(14) | C2 | C1 | C5 | C4 | -0.1(2) | |
| Fe1 | C3 | C4 | C5 | -59.53(16) | C2 | C3 | C4 | Fe1 | 59.74(14) | |
| Fe1 | C4 | C5 | C1 | -59.82(15) | C2 | C3 | C4 | C5 | 0.2(2) | |
| Fe1 | C6 | C7 | C8 | 59.27(13) | C3 | C2 | C11 | N1 | -91.3(2) | |
| Fe1 | C6 | C10 | C9 | -60.02(14) | C3 | C4 | C5 | Fe1 | 59.74(15) | |
| Fe1 | C7 | C8 | C9 | 59.11(15) | C3 | C4 | C5 | C1 | -0.1(2) | |
| Fe1 | C8 | C9 | C10 | 58.95(14) | C5 | C1 | C2 | Fe1 | 58.68(14) | |
| Fe1 | C9 | C10 | C6 | 60.13(13) | C5 | C1 | C2 | C3 | 0.2(2) | |
| Si1 | C1 | C2 | Fe1 | -123.17(17) | C5 | C1 | C2 | C11 | 178.95(18) | |
| Si1 | C1 | C2 | C3 | 178.36(14) | C61 | C6 | C7 | Fe1 | 120.5(2) | |
| Si1 | C1 | C2 | C11 | -2.9(3) | C61 | C6 | C7 | C8 | 179.8(2) | |
| Si1 | C1 | C5 | Fe1 | 122.39(14) | C61 | C6 | C10 | Fe1 | -120.0(2) | |
| Si1 | C1 | C5 | C4 | -178.42(14) | C61 | C6 | C10 | C9 | 180.0(2) | |
| O1 | Si1 | O2 | C19 | 54.0(2) | C6 | C7 | C8 | Fe1 | -59.10(13) | |
| O1 | Si1 | C1 | Fe1 | 59.25(15) | C6 | C7 | C8 | C9 | 0.0(2) | |
| O1 | Si1 | C1 | C2 | 154.41(17) | C7 | C6 | C10 | Fe1 | 59.36(13) | |
| O1 | Si1 | C1 | C5 | -27.70(18) | C7 | C6 | C10 | C9 | -0.7(2) | |
| O1 | Si1 | C14 | C15 | 175.54(19) | C7 | C8 | C9 | Fe1 | -59.37(14) | |
| O1 | Si1 | C14 | C16 | 57.25(17) | C7 | C8 | C9 | C10 | -0.4(2) | |
| O1 | Si1 | C14 | C17 | -60.2(2) | C8 | C9 | C10 | Fe1 | -59.47(15) | |
| O2 | Si1 | O1 | C18 | 27.1(2) | C8 | C9 | C10 | C6 | 0.7(2) | |
| O2 | Si1 | C1 | Fe1 | -61.00(15) | C10 | C6 | C7 | Fe1 | -58.88(12) | |
| O2 | Si1 | C1 | C2 | 34.16(19) | C10 | C6 | C7 | C8 | 0.4(2) | |
| O2 | Si1 | C1 | C5 | -147.94(16) | C11 | C2 | C3 | Fe1 | -119.90(18) | |
| O2 | Si1 | C14 | C15 | -63.3(2) | C11 | C2 | C3 | C4 | -179.04(18) | |
| O2 | Si1 | C14 | C16 | 178.43(14) | C12 | N1 | C11 | C2 | 70.2(2) | |
| O2 | Si1 | C14 | C17 | 61.0(2) | C13 | N1 | C11 | C2 | -167.79(19) | |
| C1 | Si1 | O1 | C18 | -90.0(2) | C14 | Si1 | O1 | C18 | 151.3(2) | |
| C1 | Si1 | O2 | C19 | 174.2(2) | C14 | Si1 | O2 | C19 | -63.0(2) | |
| C1 | Si1 | C14 | C15 | 56.9(2) | C14 | Si1 | C1 | Fe1 | 173.31(12) | |
| C1 | Si1 | C14 | C16 | -61.41(18) | C14 | Si1 | C1 | C2 | -91.54(19) | |
| C1 | Si1 | C14 | C17 | -178.86(18) | C14 | Si1 | C1 | C5 | 86.36(19) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| H3 | 112 | 4907 | 5827 | 44 |
| H4 | -1728 | 7601 | 5287 | 51 |
| H5 | -463 | 9030 | 6162 | 40 |
| H7 | 2557 | 5667 | 3840 | 28 |
| H8 | 1222 | 8436 | 3572 | 36 |
| H9 | 3019 | 9267 | 4617 | 35 |
| H10 | 5441 | 7002 | 5549 | 27 |
| H11A | 3319 | 3424 | 6760 | 38 |
| H11B | 4176 | 4282 | 7320 | 38 |
| H12A | -180 | 3690 | 7653 | 79 |
| H12B | 448 | 2423 | 8613 | 79 |
| H12C | 1329 | 2136 | 7589 | 79 |
| H13A | 4384 | 1492 | 8241 | 92 |
| H13B | 3418 | 1770 | 9252 | 92 |
| H13C | 4831 | 2618 | 8752 | 92 |
| H15A | 608 | 5906 | 8881 | 85 |
| H15B | 475 | 6338 | 9907 | 85 |
| H15C | 2454 | 5492 | 9495 | 85 |
| H16A | -356 | 9812 | 8323 | 76 |
| H16B | -1165 | 8900 | 9237 | 76 |
| H16C | -1154 | 8562 | 8190 | 76 |
| H17A | 3676 | 7456 | 9668 | 79 |
| H17B | 1719 | 8405 | 10043 | 79 |
| H17C | 2698 | 9126 | 9111 | 79 |
| H18A | 3350 | 10378 | 5942 | 69 |
| H18B | 4956 | 8882 | 6385 | 69 |
| H18C | 4538 | 10290 | 6843 | 69 |
| H19A | 7444 | 6374 | 7717 | 88 |
| H19B | 6671 | 5746 | 8750 | 88 |
| H19C | 6053 | 7484 | 8313 | 88 |
Experimental
Single crystals of C38H60Fe2N2O4Si2 [mo_B0167_0m] were []. A suitable crystal was selected and [] on a 'Bruker APEX-II CCD' diffractometer. The crystal was kept at 100.01 K during data collection. Using Olex2 [1], the structure was solved with the XT [2] structure solution program using Direct Methods and refined with the XL [3] refinement package using Least Squares minimisation.
Crystal structure determination of [mo_B0167_0m]
Crystal Data for C38H60Fe2N2O4Si2 (M =776.76 g/mol): triclinic, space group P-1 (no. 2), a = 7.622(8) Å, b = 9.880(8) Å, c = 14.226(12) Å, α = 76.29(3)°, β = 85.20(3)°, γ = 70.52(3)°, V = 981.2(15) Å3, Z = 1, T = 100.01 K, μ(MoKα) = 0.840 mm-1, Dcalc = 1.315 g/cm3, 23027 reflections measured (4.788° ≤ 2Θ ≤ 57.612°), 5104 unique (Rint = 0.0371, Rsigma = 0.0295) which were used in all calculations. The final R1 was 0.0373 (I > 2σ(I)) and wR2 was 0.0913 (all data).
Refinement model description
Number of restraints - 0, 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.a Secondary CH2 refined with riding coordinates:
C11(H11A,H11B)
2.b Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10)
2.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), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C)
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.