| Identification code | mo_B0673_0m |
| Empirical formula | C29H35FeNO2Si2 |
| Formula weight | 541.61 |
| Temperature/K | 100.01 |
| Crystal system | triclinic |
| Space group | P-1 |
| a/Å | 8.4627(9) |
| b/Å | 12.9654(13) |
| c/Å | 13.1700(10) |
| α/° | 73.895(2) |
| β/° | 73.944(3) |
| γ/° | 84.816(3) |
| Volume/Å3 | 1334.0(2) |
| Z | 2 |
| ρcalcg/cm3 | 1.348 |
| μ/mm‑1 | 0.682 |
| F(000) | 572.0 |
| Crystal size/mm3 | 0.356 × 0.246 × 0.17 |
| Radiation | MoKα (λ = 0.71073) |
| 2Θ range for data collection/° | 5.01 to 66.456 |
| Index ranges | -13 ≤ h ≤ 13, -19 ≤ k ≤ 19, -16 ≤ l ≤ 20 |
| Reflections collected | 36672 |
| Independent reflections | 10182 [Rint = 0.0326, Rsigma = 0.0368] |
| Data/restraints/parameters | 10182/0/325 |
| Goodness-of-fit on F2 | 1.032 |
| Final R indexes [I>=2σ (I)] | R1 = 0.0351, wR2 = 0.0781 |
| Final R indexes [all data] | R1 = 0.0487, wR2 = 0.0831 |
| Largest diff. peak/hole / e Å-3 | 0.81/-0.40 |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| Fe1 | 3078.4(2) | 2618.6(2) | 3652.9(2) | 9.29(4) |
| Si1 | 6767.6(4) | 1873.1(3) | 2128.9(3) | 10.73(6) |
| Si2 | 6904.6(4) | 3304.8(2) | 3597.8(3) | 9.79(6) |
| O1 | 7471.4(10) | 2369.7(7) | 2937.4(7) | 12.17(15) |
| O2 | 7148.8(12) | 2702.0(8) | 911.7(7) | 17.55(18) |
| N1 | 4454.3(14) | 2737.0(9) | 196.2(8) | 16.2(2) |
| C1 | 4502.1(14) | 1702.0(9) | 2688.5(9) | 11.05(19) |
| C2 | 3194.1(15) | 2249.9(9) | 2220.4(10) | 13.0(2) |
| C3 | 1657.5(15) | 1928.9(10) | 2996(1) | 15.3(2) |
| C4 | 1961.8(16) | 1197.6(10) | 3950(1) | 15.7(2) |
| C5 | 3698.7(15) | 1050.6(9) | 3762(1) | 13.5(2) |
| C6 | 4648.0(14) | 3549.8(9) | 3948.8(9) | 11.7(2) |
| C7 | 3644.6(15) | 4194.6(9) | 3279(1) | 14.1(2) |
| C8 | 1954.8(16) | 4039.5(10) | 3860.5(11) | 16.6(2) |
| C9 | 1879.6(16) | 3298.7(11) | 4897.9(11) | 17.4(2) |
| C10 | 3520.4(15) | 3001.6(10) | 4953.6(10) | 14.9(2) |
| C11 | 3349.4(17) | 3071.1(11) | 1131.4(10) | 18.9(2) |
| C12 | 3840.1(19) | 1792.8(12) | 33.0(12) | 24.3(3) |
| C13 | 4628(2) | 3637.0(13) | -791.6(11) | 27.0(3) |
| C14 | 7860.2(15) | 551.5(10) | 2055.6(10) | 14.4(2) |
| C15 | 6994.1(19) | -26.0(12) | 1488.3(15) | 28.1(3) |
| C16 | 9647.9(17) | 755.5(12) | 1368.7(12) | 22.2(3) |
| C17 | 7867(2) | -173.6(11) | 3194.1(12) | 27.6(3) |
| C18 | 7988.9(15) | 4569.4(9) | 2730.1(9) | 12.1(2) |
| C19 | 7618.7(17) | 5539.3(10) | 3024.5(10) | 16.8(2) |
| C20 | 8496.6(19) | 6465.5(11) | 2407.5(11) | 22.1(3) |
| C21 | 9758.8(19) | 6441.4(11) | 1475.5(11) | 22.8(3) |
| C22 | 10130.5(17) | 5493.8(11) | 1158.8(11) | 20.7(3) |
| C23 | 9250.1(16) | 4569.1(10) | 1778.5(10) | 16.6(2) |
| C24 | 7427.7(14) | 2809.1(9) | 4944.7(9) | 11.8(2) |
| C25 | 7597.0(17) | 1710.4(10) | 5420.6(10) | 17.4(2) |
| C26 | 7823.3(19) | 1333.2(10) | 6472.5(11) | 21.4(3) |
| C27 | 7891.9(17) | 2052.8(10) | 7068.5(10) | 18.0(2) |
| C28 | 7731.0(16) | 3146(1) | 6612.4(10) | 16.6(2) |
| C29 | 7495.1(16) | 3516.7(10) | 5566.1(10) | 15.3(2) |
| Atom | U11 | U22 | U33 | U23 | U13 | U12 |
|---|---|---|---|---|---|---|
| Fe1 | 9.05(8) | 9.86(7) | 9.13(7) | -3.20(5) | -1.68(6) | -1.00(5) |
| Si1 | 10.82(15) | 10.91(13) | 10.36(13) | -3.42(11) | -1.62(11) | -1.44(11) |
| Si2 | 9.51(14) | 10.48(13) | 10.28(13) | -4.19(10) | -2.36(11) | -0.95(11) |
| O1 | 11.0(4) | 13.8(4) | 14.2(4) | -7.7(3) | -3.6(3) | 0.7(3) |
| O2 | 16.5(4) | 20.5(4) | 12.4(4) | 1.1(3) | -2.5(3) | -5.9(3) |
| N1 | 17.8(5) | 20.8(5) | 10.1(4) | -3.8(4) | -3.5(4) | -1.7(4) |
| C1 | 12.2(5) | 10.3(4) | 11.5(5) | -4.4(4) | -2.7(4) | -0.8(4) |
| C2 | 14.8(5) | 14.0(5) | 11.6(5) | -5.1(4) | -4.3(4) | 0.7(4) |
| C3 | 11.8(5) | 18.4(5) | 18.8(5) | -8.8(4) | -5.2(4) | -0.7(4) |
| C4 | 14.2(6) | 12.8(5) | 18.3(5) | -3.6(4) | -0.5(4) | -5.0(4) |
| C5 | 14.3(5) | 10.5(5) | 14.0(5) | -1.8(4) | -1.9(4) | -1.4(4) |
| C6 | 11.3(5) | 12.4(5) | 12.8(5) | -6.2(4) | -2.2(4) | -1.0(4) |
| C7 | 14.3(5) | 10.4(5) | 18.7(5) | -4.7(4) | -5.1(4) | -0.3(4) |
| C8 | 12.7(5) | 15.9(5) | 24.3(6) | -10.7(5) | -5.6(5) | 3.4(4) |
| C9 | 12.3(5) | 25.0(6) | 16.7(5) | -11.9(5) | 0.0(4) | -1.8(5) |
| C10 | 14.0(5) | 20.7(6) | 11.2(5) | -6.7(4) | -2.3(4) | -2.1(4) |
| C11 | 23.6(7) | 20.2(6) | 12.1(5) | -4.0(4) | -5.8(5) | 5.8(5) |
| C12 | 26.1(7) | 30.7(7) | 20.0(6) | -12.5(5) | -5.4(5) | -4.6(6) |
| C13 | 34.8(8) | 30.7(7) | 12.2(6) | 0.1(5) | -6.1(6) | -2.5(6) |
| C14 | 13.3(5) | 14.5(5) | 16.7(5) | -7.8(4) | -2.3(4) | -0.1(4) |
| C15 | 23.2(7) | 26.3(7) | 45.6(9) | -25.1(7) | -11.6(7) | 2.3(6) |
| C16 | 14.5(6) | 25.7(6) | 25.6(7) | -11.0(5) | -0.7(5) | 2.3(5) |
| C17 | 33.7(8) | 17.6(6) | 23.6(7) | -1.5(5) | -1.6(6) | 8.8(6) |
| C18 | 11.9(5) | 13.5(5) | 11.4(5) | -2.4(4) | -4.2(4) | -1.7(4) |
| C19 | 23.2(6) | 14.8(5) | 12.4(5) | -4.1(4) | -3.0(5) | -3.4(5) |
| C20 | 35.3(8) | 15.5(5) | 16.1(6) | -4.0(4) | -6.0(5) | -7.3(5) |
| C21 | 28.9(7) | 21.4(6) | 16.6(6) | 1.1(5) | -6.0(5) | -12.1(5) |
| C22 | 17.8(6) | 25.2(6) | 15.1(5) | -1.1(5) | -0.4(5) | -5.5(5) |
| C23 | 14.7(6) | 18.5(5) | 15.4(5) | -4.4(4) | -1.8(4) | -0.9(4) |
| C24 | 10.1(5) | 13.6(5) | 12.1(5) | -4.3(4) | -2.6(4) | -0.2(4) |
| C25 | 24.0(6) | 13.0(5) | 17.1(5) | -4.7(4) | -7.3(5) | -1.2(5) |
| C26 | 30.6(7) | 14.2(5) | 19.6(6) | -1.1(4) | -10.1(5) | -0.3(5) |
| C27 | 22.1(6) | 19.0(6) | 12.8(5) | -2.9(4) | -5.8(5) | 0.4(5) |
| C28 | 20.3(6) | 17.6(5) | 13.7(5) | -7.1(4) | -5.2(5) | 2.2(5) |
| C29 | 18.5(6) | 13.5(5) | 14.8(5) | -4.6(4) | -5.6(5) | 1.6(4) |
| Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
|---|---|---|---|---|---|---|
| Fe1 | C1 | 2.0517(11) | C2 | C11 | 1.5104(17) | |
| Fe1 | C2 | 2.0463(12) | C3 | C4 | 1.4206(18) | |
| Fe1 | C3 | 2.0477(12) | C4 | C5 | 1.4257(18) | |
| Fe1 | C4 | 2.0373(12) | C6 | C7 | 1.4406(17) | |
| Fe1 | C5 | 2.0288(12) | C6 | C10 | 1.4384(17) | |
| Fe1 | C6 | 2.0521(11) | C7 | C8 | 1.4257(18) | |
| Fe1 | C7 | 2.0336(12) | C8 | C9 | 1.4241(19) | |
| Fe1 | C8 | 2.0474(12) | C9 | C10 | 1.4233(18) | |
| Fe1 | C9 | 2.0532(12) | C14 | C15 | 1.5390(18) | |
| Fe1 | C10 | 2.0447(12) | C14 | C16 | 1.5361(18) | |
| Si1 | O1 | 1.6442(9) | C14 | C17 | 1.5342(19) | |
| Si1 | O2 | 1.6277(10) | C18 | C19 | 1.4006(17) | |
| Si1 | C1 | 1.8635(12) | C18 | C23 | 1.4037(17) | |
| Si1 | C14 | 1.8858(12) | C19 | C20 | 1.3929(18) | |
| Si2 | O1 | 1.6449(9) | C20 | C21 | 1.392(2) | |
| Si2 | C6 | 1.8561(12) | C21 | C22 | 1.387(2) | |
| Si2 | C18 | 1.8678(12) | C22 | C23 | 1.3930(18) | |
| Si2 | C24 | 1.8725(12) | C24 | C25 | 1.4000(17) | |
| N1 | C11 | 1.4713(17) | C24 | C29 | 1.4023(16) | |
| N1 | C12 | 1.4622(18) | C25 | C26 | 1.3960(18) | |
| N1 | C13 | 1.4692(17) | C26 | C27 | 1.3897(18) | |
| C1 | C2 | 1.4501(16) | C27 | C28 | 1.3878(18) | |
| C1 | C5 | 1.4436(16) | C28 | C29 | 1.3918(17) | |
| C2 | C3 | 1.4264(18) |
| Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|
| C1 | Fe1 | C6 | 107.00(5) | C2 | C1 | Fe1 | 69.08(6) | |
| C1 | Fe1 | C9 | 166.51(5) | C2 | C1 | Si1 | 128.82(9) | |
| C2 | Fe1 | C1 | 41.45(5) | C5 | C1 | Fe1 | 68.43(6) | |
| C2 | Fe1 | C3 | 40.78(5) | C5 | C1 | Si1 | 125.05(9) | |
| C2 | Fe1 | C6 | 128.17(5) | C5 | C1 | C2 | 105.86(10) | |
| C2 | Fe1 | C8 | 117.42(5) | C1 | C2 | Fe1 | 69.48(6) | |
| C2 | Fe1 | C9 | 150.81(5) | C1 | C2 | C11 | 128.02(11) | |
| C3 | Fe1 | C1 | 69.39(5) | C3 | C2 | Fe1 | 69.66(7) | |
| C3 | Fe1 | C6 | 166.53(5) | C3 | C2 | C1 | 108.42(10) | |
| C3 | Fe1 | C9 | 117.20(5) | C3 | C2 | C11 | 123.49(11) | |
| C4 | Fe1 | C1 | 69.89(5) | C11 | C2 | Fe1 | 124.24(8) | |
| C4 | Fe1 | C2 | 69.05(5) | C2 | C3 | Fe1 | 69.56(7) | |
| C4 | Fe1 | C3 | 40.70(5) | C4 | C3 | Fe1 | 69.26(7) | |
| C4 | Fe1 | C6 | 151.60(5) | C4 | C3 | C2 | 108.77(11) | |
| C4 | Fe1 | C8 | 126.85(5) | C3 | C4 | Fe1 | 70.05(7) | |
| C4 | Fe1 | C9 | 106.83(5) | C3 | C4 | C5 | 107.52(11) | |
| C4 | Fe1 | C10 | 117.62(5) | C5 | C4 | Fe1 | 69.16(7) | |
| C5 | Fe1 | C1 | 41.43(5) | C1 | C5 | Fe1 | 70.13(6) | |
| C5 | Fe1 | C2 | 69.02(5) | C4 | C5 | Fe1 | 69.79(7) | |
| C5 | Fe1 | C3 | 68.54(5) | C4 | C5 | C1 | 109.42(10) | |
| C5 | Fe1 | C4 | 41.05(5) | Si2 | C6 | Fe1 | 121.50(6) | |
| C5 | Fe1 | C6 | 117.93(5) | C7 | C6 | Fe1 | 68.67(6) | |
| C5 | Fe1 | C7 | 152.44(5) | C7 | C6 | Si2 | 129.41(9) | |
| C5 | Fe1 | C8 | 165.52(5) | C10 | C6 | Fe1 | 69.17(7) | |
| C5 | Fe1 | C9 | 127.80(5) | C10 | C6 | Si2 | 124.39(9) | |
| C5 | Fe1 | C10 | 108.19(5) | C10 | C6 | C7 | 105.85(10) | |
| C6 | Fe1 | C9 | 69.31(5) | C6 | C7 | Fe1 | 70.04(6) | |
| C7 | Fe1 | C1 | 117.78(5) | C8 | C7 | Fe1 | 70.07(7) | |
| C7 | Fe1 | C2 | 107.78(5) | C8 | C7 | C6 | 109.15(11) | |
| C7 | Fe1 | C3 | 127.88(5) | C7 | C8 | Fe1 | 69.03(7) | |
| C7 | Fe1 | C4 | 165.46(5) | C9 | C8 | Fe1 | 69.90(7) | |
| C7 | Fe1 | C6 | 41.29(5) | C9 | C8 | C7 | 107.83(11) | |
| C7 | Fe1 | C8 | 40.89(5) | C8 | C9 | Fe1 | 69.46(7) | |
| C7 | Fe1 | C9 | 68.60(5) | C10 | C9 | Fe1 | 69.36(7) | |
| C7 | Fe1 | C10 | 68.56(5) | C10 | C9 | C8 | 107.85(11) | |
| C8 | Fe1 | C1 | 151.56(5) | C6 | C10 | Fe1 | 69.72(6) | |
| C8 | Fe1 | C3 | 107.16(5) | C9 | C10 | Fe1 | 70.00(7) | |
| C8 | Fe1 | C6 | 69.47(5) | C9 | C10 | C6 | 109.31(11) | |
| C8 | Fe1 | C9 | 40.64(5) | N1 | C11 | C2 | 114.06(10) | |
| C10 | Fe1 | C1 | 128.33(5) | C15 | C14 | Si1 | 108.73(9) | |
| C10 | Fe1 | C2 | 167.21(5) | C16 | C14 | Si1 | 109.60(9) | |
| C10 | Fe1 | C3 | 151.04(5) | C16 | C14 | C15 | 108.42(11) | |
| C10 | Fe1 | C6 | 41.11(5) | C17 | C14 | Si1 | 112.09(9) | |
| C10 | Fe1 | C8 | 68.45(5) | C17 | C14 | C15 | 109.30(12) | |
| C10 | Fe1 | C9 | 40.65(5) | C17 | C14 | C16 | 108.63(11) | |
| O1 | Si1 | C1 | 109.06(5) | C19 | C18 | Si2 | 121.43(9) | |
| O1 | Si1 | C14 | 108.05(5) | C19 | C18 | C23 | 117.70(11) | |
| O2 | Si1 | O1 | 109.29(5) | C23 | C18 | Si2 | 120.83(9) | |
| O2 | Si1 | C1 | 109.19(5) | C20 | C19 | C18 | 121.13(12) | |
| O2 | Si1 | C14 | 109.69(5) | C21 | C20 | C19 | 120.12(12) | |
| C1 | Si1 | C14 | 111.53(5) | C22 | C21 | C20 | 119.76(12) | |
| O1 | Si2 | C6 | 112.97(5) | C21 | C22 | C23 | 119.93(12) | |
| O1 | Si2 | C18 | 108.34(5) | C22 | C23 | C18 | 121.35(12) | |
| O1 | Si2 | C24 | 107.78(5) | C25 | C24 | Si2 | 121.25(9) | |
| C6 | Si2 | C18 | 110.01(5) | C25 | C24 | C29 | 117.38(11) | |
| C6 | Si2 | C24 | 105.22(5) | C29 | C24 | Si2 | 121.05(9) | |
| C18 | Si2 | C24 | 112.55(5) | C26 | C25 | C24 | 121.35(11) | |
| Si1 | O1 | Si2 | 136.87(6) | C27 | C26 | C25 | 120.06(12) | |
| C12 | N1 | C11 | 111.58(11) | C28 | C27 | C26 | 119.61(12) | |
| C12 | N1 | C13 | 110.33(11) | C27 | C28 | C29 | 120.07(11) | |
| C13 | N1 | C11 | 108.85(11) | C28 | C29 | C24 | 121.53(11) | |
| Si1 | C1 | Fe1 | 122.36(6) |
| D | H | A | d(D-H)/Å | d(H-A)/Å | d(D-A)/Å | D-H-A/° |
|---|---|---|---|---|---|---|
| O2 | H2 | N1 | 0.83(2) | 1.87(2) | 2.6900(15) | 169(2) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| H2 | 6400(30) | 2705(17) | 610(18) | 42(6) |
| H3 | 604 | 2165 | 2892 | 18 |
| H4 | 1155 | 867 | 4596 | 19 |
| H5 | 4243 | 595 | 4265 | 16 |
| H7 | 4045 | 4651 | 2564 | 17 |
| H8 | 1042 | 4371 | 3602 | 20 |
| H9 | 907 | 3047 | 5454 | 21 |
| H10 | 3823 | 2517 | 5559 | 18 |
| H11A | 2244 | 3223 | 1001 | 23 |
| H11B | 3759 | 3747 | 1170 | 23 |
| H12A | 3735 | 1198 | 696 | 36 |
| H12B | 4611 | 1586 | -587 | 36 |
| H12C | 2763 | 1962 | -119 | 36 |
| H13A | 3539 | 3869 | -901 | 41 |
| H13B | 5300 | 3407 | -1428 | 41 |
| H13C | 5162 | 4235 | -704 | 41 |
| H15A | 5861 | -185 | 1930 | 42 |
| H15B | 7585 | -697 | 1412 | 42 |
| H15C | 6984 | 437 | 762 | 42 |
| H16A | 9661 | 1210 | 635 | 33 |
| H16B | 10202 | 69 | 1310 | 33 |
| H16C | 10221 | 1117 | 1723 | 33 |
| H17A | 8429 | 189 | 3554 | 41 |
| H17B | 8444 | -850 | 3120 | 41 |
| H17C | 6732 | -323 | 3636 | 41 |
| H19 | 6754 | 5566 | 3656 | 20 |
| H20 | 8234 | 7115 | 2623 | 26 |
| H21 | 10363 | 7072 | 1058 | 27 |
| H22 | 10985 | 5475 | 520 | 25 |
| H23 | 9509 | 3925 | 1552 | 20 |
| H25 | 7557 | 1211 | 5020 | 21 |
| H26 | 7931 | 584 | 6781 | 26 |
| H27 | 8048 | 1798 | 7784 | 22 |
| H28 | 7782 | 3642 | 7015 | 20 |
| H29 | 7377 | 4267 | 5266 | 18 |
Experimental
Single crystals of C29H35FeNO2Si2 [mo_B0673_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 Intrinsic Phasing and refined with the XL [3] refinement package using Least Squares minimisation.
Crystal structure determination of [mo_B0673_0m]
Crystal Data for C29H35FeNO2Si2 (M =541.61 g/mol): triclinic, space group P-1 (no. 2), a = 8.4627(9) Å, b = 12.9654(13) Å, c = 13.1700(10) Å, α = 73.895(2)°, β = 73.944(3)°, γ = 84.816(3)°, V = 1334.0(2) Å3, Z = 2, T = 100.01 K, μ(MoKα) = 0.682 mm-1, Dcalc = 1.348 g/cm3, 36672 reflections measured (5.01° ≤ 2Θ ≤ 66.456°), 10182 unique (Rint = 0.0326, Rsigma = 0.0368) which were used in all calculations. The final R1 was 0.0351 (I > 2σ(I)) and wR2 was 0.0831 (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), C19(H19), C20(H20),
C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29)
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)
This report has been created with Olex2, compiled on 2017.03.02 svn.r3394 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.