| Identification code | mo_B0174_0m |
| Empirical formula | C15H22ClFeNOSiZn |
| Formula weight | 417.09 |
| Temperature/K | 99.99 |
| Crystal system | triclinic |
| Space group | P-1 |
| a/Å | 7.7381(7) |
| b/Å | 11.9130(9) |
| c/Å | 19.5044(19) |
| α/° | 86.737(3) |
| β/° | 89.057(3) |
| γ/° | 88.737(3) |
| Volume/Å3 | 1794.4(3) |
| Z | 4 |
| ρcalcg/cm3 | 1.544 |
| μ/mm‑1 | 2.358 |
| F(000) | 856.0 |
| Crystal size/mm3 | 0.14 × 0.136 × 0.095 |
| Radiation | MoKα (λ = 0.71073) |
| 2Θ range for data collection/° | 4.184 to 56 |
| Index ranges | -10 ≤ h ≤ 10, -12 ≤ k ≤ 15, -25 ≤ l ≤ 25 |
| Reflections collected | 40192 |
| Independent reflections | 8657 [Rint = 0.0445, Rsigma = 0.0386] |
| Data/restraints/parameters | 8657/0/387 |
| Goodness-of-fit on F2 | 1.022 |
| Final R indexes [I>=2σ (I)] | R1 = 0.0300, wR2 = 0.0565 |
| Final R indexes [all data] | R1 = 0.0468, wR2 = 0.0611 |
| Largest diff. peak/hole / e Å-3 | 0.81/-0.70 |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| Zn1 | 5076.5(3) | 5135.2(2) | 9266.7(2) | 15.98(6) |
| Fe1 | 2568.5(4) | 1826.2(3) | 8183.2(2) | 21.10(8) |
| Cl1 | 7339.0(7) | 5142.6(5) | 8577.3(3) | 29.77(13) |
| Si1 | 4394.3(8) | 2583.7(5) | 9777.7(3) | 20.82(13) |
| O1 | 4833.3(19) | 3865.9(12) | 9960.2(7) | 19.0(3) |
| N1 | 2739(2) | 5387.6(15) | 8783.8(9) | 21.2(4) |
| C1 | 4168(3) | 2631.4(17) | 8826.6(11) | 17.1(4) |
| C2 | 3130(3) | 3428.7(17) | 8408.5(11) | 18.5(4) |
| C3 | 3499(3) | 3261.1(18) | 7702.3(11) | 22.0(5) |
| C4 | 4743(3) | 2367.7(19) | 7668.0(12) | 24.4(5) |
| C5 | 5153(3) | 1988.6(18) | 8348.4(11) | 19.6(4) |
| C6 | 960(4) | 786(3) | 8748.2(15) | 48.5(8) |
| C7 | -12(3) | 1575(2) | 8306(2) | 56.2(10) |
| C8 | 494(4) | 1388(2) | 7632.2(17) | 45.0(8) |
| C9 | 1747(4) | 532(2) | 7636.3(14) | 36.7(6) |
| C10 | 2025(3) | 161(2) | 8316.3(13) | 34.2(6) |
| C11 | 2430(4) | 2120(2) | 10273.6(13) | 39.0(7) |
| C12 | 6215(4) | 1574(2) | 9991.6(13) | 37.0(6) |
| C13 | 1899(3) | 4279.4(18) | 8688.2(12) | 21.6(5) |
| C14 | 3026(3) | 5987(2) | 8105.8(12) | 30.5(6) |
| C15 | 1544(3) | 6070(2) | 9207.0(14) | 34.1(6) |
| Zn2 | 10354.2(3) | 5094.9(2) | 5711.0(2) | 15.09(6) |
| Fe2 | 7415.4(4) | 8375.0(3) | 6710.3(2) | 23.17(8) |
| Cl2 | 12746.6(7) | 5454.1(5) | 6240.0(3) | 24.51(12) |
| Si2 | 8691.8(8) | 7362.4(5) | 5067.6(3) | 21.02(13) |
| O2 | 9485.1(18) | 6108.7(11) | 4947.0(7) | 18.1(3) |
| N2 | 8231(2) | 4744.1(14) | 6335.7(9) | 17.0(4) |
| C16 | 8899(3) | 7536.4(17) | 6007.1(11) | 16.9(4) |
| C17 | 8261(3) | 6779.7(17) | 6555.3(10) | 17.0(4) |
| C18 | 8873(3) | 7133.3(18) | 7194.4(11) | 23.3(5) |
| C19 | 9883(3) | 8099.6(19) | 7055.1(12) | 25.7(5) |
| C20 | 9901(3) | 8345.4(18) | 6335.6(11) | 21.4(5) |
| C21 | 5302(4) | 9134(3) | 6256.6(17) | 50.9(8) |
| C22 | 4782(3) | 8379(2) | 6807.2(17) | 41.1(7) |
| C23 | 5517(4) | 8710(2) | 7411.3(16) | 41.8(7) |
| C24 | 6473(4) | 9674(2) | 7249.0(16) | 42.8(7) |
| C25 | 6361(4) | 9956(2) | 6540.1(16) | 43.0(7) |
| C26 | 6427(4) | 7480(2) | 4746.1(14) | 40.5(7) |
| C27 | 9975(4) | 8477(2) | 4601.7(13) | 40.9(7) |
| C28 | 7163(3) | 5784.5(17) | 6458.3(11) | 19.8(4) |
| C29 | 7098(3) | 3922.6(18) | 6028.8(12) | 25.6(5) |
| C30 | 8884(3) | 4247.1(19) | 6998.1(11) | 25.1(5) |
| Atom | U11 | U22 | U33 | U23 | U13 | U12 |
|---|---|---|---|---|---|---|
| Zn1 | 16.16(12) | 18.12(13) | 13.80(12) | -1.96(9) | 0.06(9) | -1.01(9) |
| Fe1 | 20.60(16) | 17.47(16) | 25.95(17) | -5.80(13) | -4.91(13) | -1.64(12) |
| Cl1 | 21.7(3) | 42.4(3) | 25.7(3) | -7.5(3) | 7.9(2) | -5.4(2) |
| Si1 | 28.2(3) | 16.6(3) | 17.9(3) | -2.1(2) | -0.8(2) | -3.1(2) |
| O1 | 25.4(8) | 17.0(7) | 14.9(7) | -2.3(6) | -0.4(6) | -2.0(6) |
| N1 | 20.2(9) | 16.9(9) | 27.2(10) | -5.7(8) | -4.8(8) | 0.8(7) |
| C1 | 15.6(10) | 15.3(10) | 21.1(11) | -4.5(8) | -1.0(8) | -2.3(8) |
| C2 | 16.6(10) | 16.4(10) | 23.2(11) | -5.0(8) | -2.2(8) | -2.0(8) |
| C3 | 27.1(12) | 18.6(11) | 20.8(11) | -4.0(9) | -3.7(9) | -2.8(9) |
| C4 | 28.7(12) | 23.8(12) | 21.3(11) | -7.1(9) | 3.1(9) | -0.7(10) |
| C5 | 18.0(11) | 18.2(11) | 23.0(11) | -3.6(9) | -1.1(9) | 0.4(8) |
| C6 | 50.6(18) | 60(2) | 37.8(16) | -14.1(14) | 11.3(14) | -40.4(16) |
| C7 | 19.9(14) | 34.1(16) | 118(3) | -32.3(18) | 8.9(16) | -10.6(12) |
| C8 | 44.0(17) | 28.9(14) | 64(2) | -2.1(14) | -28.5(15) | -10.4(12) |
| C9 | 51.4(17) | 22.4(13) | 37.9(15) | -9.0(11) | -10.3(13) | -9.4(12) |
| C10 | 39.6(15) | 21.4(12) | 41.7(15) | 3.3(11) | -11.3(12) | -8.0(11) |
| C11 | 55.2(18) | 36.3(15) | 26.4(13) | -7.2(11) | 12.7(12) | -19.1(13) |
| C12 | 55.0(17) | 22.3(13) | 34.1(14) | -1.4(11) | -19.4(13) | 4.8(12) |
| C13 | 18.3(11) | 18.7(11) | 28.5(12) | -6.9(9) | -4.4(9) | -0.7(9) |
| C14 | 37.6(14) | 22.2(12) | 31.9(13) | 3.6(10) | -15.8(11) | -2.6(10) |
| C15 | 21.3(12) | 28.4(13) | 54.7(17) | -22.9(12) | -4.6(11) | 5.7(10) |
| Zn2 | 16.90(12) | 14.88(12) | 13.63(12) | -1.87(9) | -0.55(9) | -0.74(9) |
| Fe2 | 23.41(17) | 16.12(16) | 30.34(18) | -6.93(13) | 7.76(14) | -0.21(13) |
| Cl2 | 17.8(3) | 29.8(3) | 26.5(3) | -5.0(2) | -4.4(2) | -2.2(2) |
| Si2 | 31.2(3) | 13.8(3) | 18.2(3) | -2.0(2) | -3.5(3) | 2.6(2) |
| O2 | 24.8(8) | 14.7(7) | 14.8(7) | -1.3(6) | -1.9(6) | 0.8(6) |
| N2 | 19.4(9) | 14.0(9) | 17.9(9) | -2.8(7) | -0.1(7) | -2.0(7) |
| C16 | 15.6(10) | 15.5(10) | 20.0(11) | -5.5(8) | 2.9(8) | 1.6(8) |
| C17 | 16.5(10) | 15.3(10) | 19.5(11) | -5.6(8) | 1.7(8) | 1.5(8) |
| C18 | 29.3(12) | 21.5(11) | 19.5(11) | -4.9(9) | 3.3(9) | -2.0(9) |
| C19 | 30.1(13) | 22.4(12) | 25.8(12) | -9.5(9) | -3.7(10) | -4.1(10) |
| C20 | 20.5(11) | 18.5(11) | 25.5(12) | -3.8(9) | 2.9(9) | -3.0(9) |
| C21 | 41.9(17) | 57(2) | 53.9(19) | -13.3(16) | -5.6(14) | 34.9(15) |
| C22 | 23.7(13) | 26.9(14) | 73(2) | -8.5(14) | 7.0(13) | 2.9(11) |
| C23 | 40.8(16) | 34.2(15) | 50.1(17) | -7.7(13) | 21.2(13) | 3.3(12) |
| C24 | 46.8(17) | 26.0(14) | 56.5(19) | -18.2(13) | 19.3(14) | 3.4(12) |
| C25 | 44.0(17) | 20.6(13) | 62(2) | 2.5(13) | 23.5(14) | 11.4(12) |
| C26 | 46.8(17) | 35.0(15) | 40.7(16) | -12.2(12) | -22.7(13) | 17.6(12) |
| C27 | 77(2) | 18.9(12) | 26.4(13) | -1.7(10) | 10.0(13) | -5.3(13) |
| C28 | 15.8(10) | 17.4(11) | 26.5(12) | -4.5(9) | 3.0(9) | -0.8(8) |
| C29 | 24.7(12) | 19.0(11) | 34.0(13) | -7.9(10) | 3.3(10) | -7.7(9) |
| C30 | 31.1(13) | 24.0(12) | 19.6(11) | 2.4(9) | 1.8(9) | 1.6(10) |
| Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
|---|---|---|---|---|---|---|
| Zn1 | Zn11 | 2.8610(6) | Zn2 | Zn22 | 2.8586(5) | |
| Zn1 | Cl1 | 2.1898(6) | Zn2 | Cl2 | 2.1960(6) | |
| Zn1 | O11 | 1.9763(14) | Zn2 | O22 | 1.9787(14) | |
| Zn1 | O1 | 1.9806(14) | Zn2 | O2 | 1.9808(14) | |
| Zn1 | N1 | 2.0616(18) | Zn2 | N2 | 2.0652(17) | |
| Fe1 | C1 | 2.066(2) | Fe2 | C16 | 2.062(2) | |
| Fe1 | C2 | 2.041(2) | Fe2 | C17 | 2.034(2) | |
| Fe1 | C3 | 2.042(2) | Fe2 | C18 | 2.038(2) | |
| Fe1 | C4 | 2.043(2) | Fe2 | C19 | 2.048(2) | |
| Fe1 | C5 | 2.046(2) | Fe2 | C20 | 2.047(2) | |
| Fe1 | C6 | 2.041(3) | Fe2 | C21 | 2.042(3) | |
| Fe1 | C7 | 2.034(3) | Fe2 | C22 | 2.044(3) | |
| Fe1 | C8 | 2.040(3) | Fe2 | C23 | 2.039(3) | |
| Fe1 | C9 | 2.043(2) | Fe2 | C24 | 2.034(2) | |
| Fe1 | C10 | 2.039(2) | Fe2 | C25 | 2.048(2) | |
| Si1 | O1 | 1.6322(15) | Si2 | O2 | 1.6302(15) | |
| Si1 | C1 | 1.864(2) | Si2 | C16 | 1.866(2) | |
| Si1 | C11 | 1.865(3) | Si2 | C26 | 1.871(3) | |
| Si1 | C12 | 1.869(3) | Si2 | C27 | 1.862(3) | |
| O1 | Zn11 | 1.9763(14) | O2 | Zn22 | 1.9787(14) | |
| N1 | C13 | 1.507(3) | N2 | C28 | 1.503(3) | |
| N1 | C14 | 1.482(3) | N2 | C29 | 1.485(3) | |
| N1 | C15 | 1.489(3) | N2 | C30 | 1.482(3) | |
| C1 | C2 | 1.453(3) | C16 | C17 | 1.446(3) | |
| C1 | C5 | 1.438(3) | C16 | C20 | 1.435(3) | |
| C2 | C3 | 1.426(3) | C17 | C18 | 1.429(3) | |
| C2 | C13 | 1.495(3) | C17 | C28 | 1.496(3) | |
| C3 | C4 | 1.423(3) | C18 | C19 | 1.417(3) | |
| C4 | C5 | 1.416(3) | C19 | C20 | 1.417(3) | |
| C6 | C7 | 1.446(5) | C21 | C22 | 1.420(4) | |
| C6 | C10 | 1.402(4) | C21 | C25 | 1.431(4) | |
| C7 | C8 | 1.394(5) | C22 | C23 | 1.397(4) | |
| C8 | C9 | 1.391(4) | C23 | C24 | 1.398(4) | |
| C9 | C10 | 1.392(4) | C24 | C25 | 1.408(4) |
| Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|
| Cl1 | Zn1 | Zn11 | 129.18(2) | Cl2 | Zn2 | Zn22 | 131.53(2) | |
| O1 | Zn1 | Zn11 | 43.63(4) | O22 | Zn2 | Zn22 | 43.81(4) | |
| O11 | Zn1 | Zn11 | 43.75(4) | O2 | Zn2 | Zn22 | 43.76(4) | |
| O11 | Zn1 | Cl1 | 116.00(5) | O22 | Zn2 | Cl2 | 116.18(4) | |
| O1 | Zn1 | Cl1 | 118.36(5) | O2 | Zn2 | Cl2 | 121.07(5) | |
| O11 | Zn1 | O1 | 87.39(6) | O22 | Zn2 | O2 | 87.57(6) | |
| O11 | Zn1 | N1 | 108.90(7) | O2 | Zn2 | N2 | 105.70(7) | |
| O1 | Zn1 | N1 | 108.01(7) | O22 | Zn2 | N2 | 106.34(6) | |
| N1 | Zn1 | Zn11 | 115.96(5) | N2 | Zn2 | Zn22 | 112.47(5) | |
| N1 | Zn1 | Cl1 | 114.85(6) | N2 | Zn2 | Cl2 | 115.91(5) | |
| C2 | Fe1 | C1 | 41.44(8) | C17 | Fe2 | C16 | 41.35(8) | |
| C2 | Fe1 | C3 | 40.89(8) | C17 | Fe2 | C18 | 41.10(8) | |
| C2 | Fe1 | C4 | 68.76(9) | C17 | Fe2 | C19 | 68.66(8) | |
| C2 | Fe1 | C5 | 68.61(8) | C17 | Fe2 | C20 | 68.46(8) | |
| C2 | Fe1 | C6 | 125.17(10) | C17 | Fe2 | C21 | 124.67(11) | |
| C2 | Fe1 | C9 | 159.20(10) | C17 | Fe2 | C22 | 108.56(10) | |
| C3 | Fe1 | C1 | 69.43(8) | C17 | Fe2 | C23 | 122.04(10) | |
| C3 | Fe1 | C4 | 40.77(9) | C17 | Fe2 | C24 | 156.97(11) | |
| C3 | Fe1 | C5 | 68.36(9) | C17 | Fe2 | C25 | 161.44(11) | |
| C3 | Fe1 | C9 | 121.28(10) | C18 | Fe2 | C16 | 69.53(8) | |
| C4 | Fe1 | C1 | 69.20(9) | C18 | Fe2 | C19 | 40.57(9) | |
| C4 | Fe1 | C5 | 40.52(9) | C18 | Fe2 | C20 | 68.28(9) | |
| C5 | Fe1 | C1 | 40.95(8) | C18 | Fe2 | C21 | 158.12(12) | |
| C6 | Fe1 | C1 | 109.94(10) | C18 | Fe2 | C22 | 120.34(11) | |
| C6 | Fe1 | C3 | 159.69(12) | C18 | Fe2 | C23 | 103.79(11) | |
| C6 | Fe1 | C4 | 159.31(12) | C18 | Fe2 | C25 | 156.80(11) | |
| C6 | Fe1 | C5 | 125.32(12) | C19 | Fe2 | C16 | 69.13(8) | |
| C6 | Fe1 | C9 | 67.80(11) | C20 | Fe2 | C16 | 40.89(8) | |
| C7 | Fe1 | C1 | 127.41(11) | C20 | Fe2 | C19 | 40.49(9) | |
| C7 | Fe1 | C2 | 109.94(10) | C20 | Fe2 | C25 | 109.39(10) | |
| C7 | Fe1 | C3 | 121.68(12) | C21 | Fe2 | C16 | 111.01(10) | |
| C7 | Fe1 | C4 | 155.03(13) | C21 | Fe2 | C19 | 161.25(12) | |
| C7 | Fe1 | C5 | 164.06(13) | C21 | Fe2 | C20 | 127.36(12) | |
| C7 | Fe1 | C6 | 41.57(13) | C21 | Fe2 | C22 | 40.69(12) | |
| C7 | Fe1 | C8 | 40.02(13) | C21 | Fe2 | C25 | 40.96(12) | |
| C7 | Fe1 | C9 | 67.70(12) | C22 | Fe2 | C16 | 126.73(10) | |
| C7 | Fe1 | C10 | 68.13(12) | C22 | Fe2 | C19 | 154.28(11) | |
| C8 | Fe1 | C1 | 163.25(10) | C22 | Fe2 | C20 | 164.30(11) | |
| C8 | Fe1 | C2 | 125.02(10) | C22 | Fe2 | C25 | 68.21(11) | |
| C8 | Fe1 | C3 | 106.37(10) | C23 | Fe2 | C16 | 160.73(10) | |
| C8 | Fe1 | C4 | 118.87(12) | C23 | Fe2 | C19 | 118.20(11) | |
| C8 | Fe1 | C5 | 154.03(11) | C23 | Fe2 | C20 | 154.92(11) | |
| C8 | Fe1 | C6 | 68.08(12) | C23 | Fe2 | C21 | 68.20(13) | |
| C8 | Fe1 | C9 | 39.85(11) | C23 | Fe2 | C22 | 40.03(12) | |
| C9 | Fe1 | C1 | 156.28(10) | C23 | Fe2 | C25 | 68.09(11) | |
| C9 | Fe1 | C4 | 104.27(10) | C24 | Fe2 | C16 | 158.87(10) | |
| C9 | Fe1 | C5 | 119.57(10) | C24 | Fe2 | C18 | 119.69(11) | |
| C10 | Fe1 | C1 | 122.99(9) | C24 | Fe2 | C19 | 104.71(11) | |
| C10 | Fe1 | C2 | 160.27(10) | C24 | Fe2 | C20 | 121.62(10) | |
| C10 | Fe1 | C3 | 157.45(10) | C24 | Fe2 | C21 | 68.08(12) | |
| C10 | Fe1 | C4 | 121.74(10) | C24 | Fe2 | C22 | 67.35(12) | |
| C10 | Fe1 | C5 | 107.56(10) | C24 | Fe2 | C23 | 40.14(11) | |
| C10 | Fe1 | C6 | 40.19(12) | C24 | Fe2 | C25 | 40.35(11) | |
| C10 | Fe1 | C8 | 67.04(11) | C25 | Fe2 | C16 | 124.87(10) | |
| C10 | Fe1 | C9 | 39.89(10) | C25 | Fe2 | C19 | 122.53(11) | |
| O1 | Si1 | C1 | 105.45(9) | O2 | Si2 | C16 | 104.96(8) | |
| O1 | Si1 | C11 | 109.20(10) | O2 | Si2 | C26 | 109.65(10) | |
| O1 | Si1 | C12 | 112.12(10) | O2 | Si2 | C27 | 111.82(11) | |
| C1 | Si1 | C11 | 114.72(11) | C16 | Si2 | C26 | 114.66(11) | |
| C1 | Si1 | C12 | 106.66(11) | C27 | Si2 | C16 | 107.88(11) | |
| C11 | Si1 | C12 | 108.72(13) | C27 | Si2 | C26 | 107.93(14) | |
| Zn11 | O1 | Zn1 | 92.61(6) | Zn22 | O2 | Zn2 | 92.43(6) | |
| Si1 | O1 | Zn11 | 142.33(9) | Si2 | O2 | Zn22 | 144.04(9) | |
| Si1 | O1 | Zn1 | 124.19(8) | Si2 | O2 | Zn2 | 122.39(8) | |
| C13 | N1 | Zn1 | 110.47(13) | C28 | N2 | Zn2 | 111.76(12) | |
| C14 | N1 | Zn1 | 109.22(14) | C29 | N2 | Zn2 | 111.18(13) | |
| C14 | N1 | C13 | 109.67(17) | C29 | N2 | C28 | 107.97(16) | |
| C14 | N1 | C15 | 109.36(19) | C30 | N2 | Zn2 | 107.31(13) | |
| C15 | N1 | Zn1 | 110.23(14) | C30 | N2 | C28 | 109.70(16) | |
| C15 | N1 | C13 | 107.88(17) | C30 | N2 | C29 | 108.87(17) | |
| Si1 | C1 | Fe1 | 133.11(11) | Si2 | C16 | Fe2 | 133.01(11) | |
| C2 | C1 | Fe1 | 68.37(11) | C17 | C16 | Fe2 | 68.28(11) | |
| C2 | C1 | Si1 | 126.92(15) | C17 | C16 | Si2 | 126.22(15) | |
| C5 | C1 | Fe1 | 68.78(11) | C20 | C16 | Fe2 | 68.99(12) | |
| C5 | C1 | Si1 | 127.02(16) | C20 | C16 | Si2 | 127.71(16) | |
| C5 | C1 | C2 | 105.59(18) | C20 | C16 | C17 | 105.60(18) | |
| C1 | C2 | Fe1 | 70.19(11) | C16 | C17 | Fe2 | 70.37(11) | |
| C1 | C2 | C13 | 124.57(19) | C16 | C17 | C28 | 124.95(18) | |
| C3 | C2 | Fe1 | 69.60(12) | C18 | C17 | Fe2 | 69.61(12) | |
| C3 | C2 | C1 | 108.67(18) | C18 | C17 | C16 | 108.78(18) | |
| C3 | C2 | C13 | 126.8(2) | C18 | C17 | C28 | 126.3(2) | |
| C13 | C2 | Fe1 | 126.40(15) | C28 | C17 | Fe2 | 126.63(14) | |
| C2 | C3 | Fe1 | 69.51(12) | C17 | C18 | Fe2 | 69.29(12) | |
| C4 | C3 | Fe1 | 69.67(13) | C19 | C18 | Fe2 | 70.10(13) | |
| C4 | C3 | C2 | 108.09(19) | C19 | C18 | C17 | 107.96(19) | |
| C3 | C4 | Fe1 | 69.57(13) | C18 | C19 | Fe2 | 69.33(13) | |
| C5 | C4 | Fe1 | 69.83(13) | C18 | C19 | C20 | 107.99(19) | |
| C5 | C4 | C3 | 107.99(19) | C20 | C19 | Fe2 | 69.70(13) | |
| C1 | C5 | Fe1 | 70.26(12) | C16 | C20 | Fe2 | 70.12(12) | |
| C4 | C5 | Fe1 | 69.65(13) | C19 | C20 | Fe2 | 69.81(13) | |
| C4 | C5 | C1 | 109.66(19) | C19 | C20 | C16 | 109.67(19) | |
| C7 | C6 | Fe1 | 68.95(16) | C22 | C21 | Fe2 | 69.73(16) | |
| C10 | C6 | Fe1 | 69.81(15) | C22 | C21 | C25 | 107.2(3) | |
| C10 | C6 | C7 | 106.4(3) | C25 | C21 | Fe2 | 69.76(16) | |
| C6 | C7 | Fe1 | 69.49(15) | C21 | C22 | Fe2 | 69.58(15) | |
| C8 | C7 | Fe1 | 70.24(16) | C23 | C22 | Fe2 | 69.80(15) | |
| C8 | C7 | C6 | 107.1(3) | C23 | C22 | C21 | 108.6(3) | |
| C7 | C8 | Fe1 | 69.74(16) | C22 | C23 | Fe2 | 70.16(16) | |
| C9 | C8 | Fe1 | 70.18(15) | C22 | C23 | C24 | 108.0(3) | |
| C9 | C8 | C7 | 109.2(3) | C24 | C23 | Fe2 | 69.76(15) | |
| C8 | C9 | Fe1 | 69.97(14) | C23 | C24 | Fe2 | 70.11(15) | |
| C8 | C9 | C10 | 108.0(3) | C23 | C24 | C25 | 109.3(3) | |
| C10 | C9 | Fe1 | 69.88(14) | C25 | C24 | Fe2 | 70.34(14) | |
| C6 | C10 | Fe1 | 70.00(15) | C21 | C25 | Fe2 | 69.29(15) | |
| C9 | C10 | Fe1 | 70.23(14) | C24 | C25 | Fe2 | 69.31(15) | |
| C9 | C10 | C6 | 109.2(3) | C24 | C25 | C21 | 107.0(3) | |
| C2 | C13 | N1 | 112.48(17) | C17 | C28 | N2 | 112.06(16) |
| A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|---|---|
| Zn1 | N1 | C13 | C2 | -46.6(2) | Zn2 | N2 | C28 | C17 | -39.5(2) | |
| Fe1 | C1 | C2 | C3 | -59.15(14) | Fe2 | C16 | C17 | C18 | -59.20(15) | |
| Fe1 | C1 | C2 | C13 | 121.2(2) | Fe2 | C16 | C17 | C28 | 121.6(2) | |
| Fe1 | C1 | C5 | C4 | 58.63(15) | Fe2 | C16 | C20 | C19 | 58.73(16) | |
| Fe1 | C2 | C3 | C4 | -59.19(15) | Fe2 | C17 | C18 | C19 | -59.66(16) | |
| Fe1 | C2 | C13 | N1 | -179.05(14) | Fe2 | C17 | C28 | N2 | 178.31(14) | |
| Fe1 | C3 | C4 | C5 | -59.48(15) | Fe2 | C18 | C19 | C20 | -59.17(16) | |
| Fe1 | C4 | C5 | C1 | -59.00(15) | Fe2 | C19 | C20 | C16 | -58.92(15) | |
| Fe1 | C6 | C7 | C8 | 60.49(19) | Fe2 | C21 | C22 | C23 | 59.09(19) | |
| Fe1 | C6 | C10 | C9 | -59.45(18) | Fe2 | C21 | C25 | C24 | -59.30(18) | |
| Fe1 | C7 | C8 | C9 | 59.25(19) | Fe2 | C22 | C23 | C24 | 59.74(18) | |
| Fe1 | C8 | C9 | C10 | 59.77(18) | Fe2 | C23 | C24 | C25 | 59.64(18) | |
| Fe1 | C9 | C10 | C6 | 59.31(18) | Fe2 | C24 | C25 | C21 | 59.29(17) | |
| Si1 | C1 | C2 | Fe1 | -128.43(17) | Si2 | C16 | C17 | Fe2 | -128.19(16) | |
| Si1 | C1 | C2 | C3 | 172.42(16) | Si2 | C16 | C17 | C18 | 172.60(15) | |
| Si1 | C1 | C2 | C13 | -7.2(3) | Si2 | C16 | C17 | C28 | -6.6(3) | |
| Si1 | C1 | C5 | Fe1 | 128.71(17) | Si2 | C16 | C20 | Fe2 | 128.80(17) | |
| Si1 | C1 | C5 | C4 | -172.66(16) | Si2 | C16 | C20 | C19 | -172.47(16) | |
| O1 | Si1 | C1 | Fe1 | -143.63(13) | O2 | Si2 | C16 | Fe2 | -146.84(14) | |
| O1 | Si1 | C1 | C2 | -49.5(2) | O2 | Si2 | C16 | C17 | -53.64(19) | |
| O1 | Si1 | C1 | C5 | 121.49(18) | O2 | Si2 | C16 | C20 | 117.33(19) | |
| C1 | Si1 | O1 | Zn1 | -0.79(13) | C16 | Si2 | O2 | Zn22 | 165.40(14) | |
| C1 | Si1 | O1 | Zn11 | 165.15(14) | C16 | Si2 | O2 | Zn2 | 1.66(12) | |
| C1 | C2 | C3 | Fe1 | 59.52(14) | C16 | C17 | C18 | Fe2 | 59.67(14) | |
| C1 | C2 | C3 | C4 | 0.3(2) | C16 | C17 | C18 | C19 | 0.0(2) | |
| C1 | C2 | C13 | N1 | 91.1(3) | C16 | C17 | C28 | N2 | 87.8(2) | |
| C2 | C1 | C5 | Fe1 | -58.74(13) | C17 | C16 | C20 | Fe2 | -58.75(13) | |
| C2 | C1 | C5 | C4 | -0.1(2) | C17 | C16 | C20 | C19 | 0.0(2) | |
| C2 | C3 | C4 | Fe1 | 59.09(15) | C17 | C18 | C19 | Fe2 | 59.16(15) | |
| C2 | C3 | C4 | C5 | -0.4(3) | C17 | C18 | C19 | C20 | 0.0(3) | |
| C3 | C2 | C13 | N1 | -88.5(3) | C18 | C17 | C28 | N2 | -91.3(2) | |
| C3 | C4 | C5 | Fe1 | 59.32(16) | C18 | C19 | C20 | Fe2 | 58.94(16) | |
| C3 | C4 | C5 | C1 | 0.3(3) | C18 | C19 | C20 | C16 | 0.0(3) | |
| C5 | C1 | C2 | Fe1 | 59.01(14) | C20 | C16 | C17 | Fe2 | 59.21(14) | |
| C5 | C1 | C2 | C3 | -0.1(2) | C20 | C16 | C17 | C18 | 0.0(2) | |
| C5 | C1 | C2 | C13 | -179.81(19) | C20 | C16 | C17 | C28 | -179.22(19) | |
| C6 | C7 | C8 | Fe1 | -60.00(18) | C21 | C22 | C23 | Fe2 | -58.95(18) | |
| C6 | C7 | C8 | C9 | -0.8(3) | C21 | C22 | C23 | C24 | 0.8(3) | |
| C7 | C6 | C10 | Fe1 | 59.49(17) | C22 | C21 | C25 | Fe2 | 59.98(17) | |
| C7 | C6 | C10 | C9 | 0.0(3) | C22 | C21 | C25 | C24 | 0.7(3) | |
| C7 | C8 | C9 | Fe1 | -58.98(19) | C22 | C23 | C24 | Fe2 | -59.99(18) | |
| C7 | C8 | C9 | C10 | 0.8(3) | C22 | C23 | C24 | C25 | -0.4(3) | |
| C8 | C9 | C10 | Fe1 | -59.82(18) | C23 | C24 | C25 | Fe2 | -59.49(19) | |
| C8 | C9 | C10 | C6 | -0.5(3) | C23 | C24 | C25 | C21 | -0.2(3) | |
| C10 | C6 | C7 | Fe1 | -60.05(18) | C25 | C21 | C22 | Fe2 | -60.00(18) | |
| C10 | C6 | C7 | C8 | 0.4(3) | C25 | C21 | C22 | C23 | -0.9(3) | |
| C11 | Si1 | O1 | Zn11 | 41.40(18) | C26 | Si2 | O2 | Zn2 | -121.97(13) | |
| C11 | Si1 | O1 | Zn1 | -124.55(13) | C26 | Si2 | O2 | Zn22 | 41.77(19) | |
| C11 | Si1 | C1 | Fe1 | -23.45(19) | C26 | Si2 | C16 | Fe2 | -26.47(19) | |
| C11 | Si1 | C1 | C2 | 70.7(2) | C26 | Si2 | C16 | C17 | 66.7(2) | |
| C11 | Si1 | C1 | C5 | -118.3(2) | C26 | Si2 | C16 | C20 | -122.3(2) | |
| C12 | Si1 | O1 | Zn11 | -79.16(18) | C27 | Si2 | O2 | Zn2 | 118.35(12) | |
| C12 | Si1 | O1 | Zn1 | 114.89(13) | C27 | Si2 | O2 | Zn22 | -77.90(18) | |
| C12 | Si1 | C1 | Fe1 | 96.99(16) | C27 | Si2 | C16 | Fe2 | 93.79(17) | |
| C12 | Si1 | C1 | C2 | -168.90(18) | C27 | Si2 | C16 | C17 | -173.01(19) | |
| C12 | Si1 | C1 | C5 | 2.1(2) | C27 | Si2 | C16 | C20 | -2.0(2) | |
| C13 | C2 | C3 | Fe1 | -120.8(2) | C28 | C17 | C18 | Fe2 | -121.1(2) | |
| C13 | C2 | C3 | C4 | 180.0(2) | C28 | C17 | C18 | C19 | 179.2(2) | |
| C14 | N1 | C13 | C2 | 73.9(2) | C29 | N2 | C28 | C17 | -162.07(18) | |
| C15 | N1 | C13 | C2 | -167.13(19) | C30 | N2 | C28 | C17 | 79.4(2) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| H3 | 3000 | 3674 | 7321 | 26 |
| H4 | 5215 | 2077 | 7260 | 29 |
| H5 | 5956 | 1399 | 8471 | 24 |
| H6 | 891 | 707 | 9235 | 58 |
| H7 | -839 | 2119 | 8448 | 67 |
| H8 | 53 | 1782 | 7233 | 54 |
| H9 | 2313 | 249 | 7244 | 44 |
| H10 | 2811 | -424 | 8464 | 41 |
| H11A | 2536 | 2308 | 10754 | 58 |
| H11B | 2316 | 1306 | 10252 | 58 |
| H11C | 1405 | 2504 | 10076 | 58 |
| H12A | 7290 | 1863 | 9784 | 56 |
| H12B | 5974 | 843 | 9812 | 56 |
| H12C | 6336 | 1488 | 10491 | 56 |
| H13A | 1429 | 3981 | 9136 | 26 |
| H13B | 920 | 4403 | 8370 | 26 |
| H14A | 3537 | 6718 | 8171 | 46 |
| H14B | 1919 | 6100 | 7872 | 46 |
| H14C | 3812 | 5538 | 7826 | 46 |
| H15A | 1411 | 5699 | 9666 | 51 |
| H15B | 414 | 6143 | 8987 | 51 |
| H15C | 2021 | 6819 | 9247 | 51 |
| H18 | 8642 | 6782 | 7635 | 28 |
| H19 | 10449 | 8511 | 7386 | 31 |
| H20 | 10488 | 8953 | 6106 | 26 |
| H21 | 5003 | 9101 | 5788 | 61 |
| H22 | 4055 | 7753 | 6771 | 49 |
| H23 | 5389 | 8345 | 7854 | 50 |
| H24 | 7101 | 10075 | 7567 | 51 |
| H25 | 6888 | 10575 | 6296 | 52 |
| H26A | 6390 | 7196 | 4285 | 61 |
| H26B | 6040 | 8270 | 4728 | 61 |
| H26C | 5665 | 7035 | 5057 | 61 |
| H27A | 11173 | 8426 | 4757 | 61 |
| H27B | 9478 | 9217 | 4695 | 61 |
| H27C | 9949 | 8374 | 4107 | 61 |
| H28A | 6398 | 5952 | 6062 | 24 |
| H28B | 6423 | 5645 | 6872 | 24 |
| H29A | 6735 | 4218 | 5573 | 38 |
| H29B | 6076 | 3798 | 6325 | 38 |
| H29C | 7735 | 3209 | 5986 | 38 |
| H30A | 9642 | 3598 | 6913 | 38 |
| H30B | 7907 | 4004 | 7292 | 38 |
| H30C | 9536 | 4810 | 7227 | 38 |
Experimental
Single crystals of C15H22ClFeNOSiZn [mo_B0174_0m] were []. A suitable crystal was selected and [] on a 'Bruker APEX-II CCD' diffractometer. The crystal was kept at 99.99 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_B0174_0m]
Crystal Data for C15H22ClFeNOSiZn (M =417.09 g/mol): triclinic, space group P-1 (no. 2), a = 7.7381(7) Å, b = 11.9130(9) Å, c = 19.5044(19) Å, α = 86.737(3)°, β = 89.057(3)°, γ = 88.737(3)°, V = 1794.4(3) Å3, Z = 4, T = 99.99 K, μ(MoKα) = 2.358 mm-1, Dcalc = 1.544 g/cm3, 40192 reflections measured (4.184° ≤ 2Θ ≤ 56°), 8657 unique (Rint = 0.0445, Rsigma = 0.0386) which were used in all calculations. The final R1 was 0.0300 (I > 2σ(I)) and wR2 was 0.0611 (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:
C13(H13A,H13B), C28(H28A,H28B)
2.b Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C18(H18),
C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25)
2.c Idealised Me refined as rotating group:
C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
H15C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,
H30B,H30C)
This report has been created with Olex2, compiled on 2016.11.07 svn.r3352 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.