| Identification code | mo_B0175_0m |
| Empirical formula | C33H50Br2Fe2N2O3Si2Zn2 |
| Formula weight | 981.19 |
| Temperature/K | 100.01 |
| Crystal system | monoclinic |
| Space group | P21/c |
| a/Å | 17.5299(5) |
| b/Å | 9.4853(3) |
| c/Å | 23.4559(7) |
| α/° | 90 |
| β/° | 103.372(2) |
| γ/° | 90 |
| Volume/Å3 | 3794.4(2) |
| Z | 4 |
| ρcalcg/cm3 | 1.718 |
| μ/mm‑1 | 4.203 |
| F(000) | 1984.0 |
| Crystal size/mm3 | 0.09 × 0.071 × 0.036 |
| Radiation | MoKα (λ = 0.71073) |
| 2Θ range for data collection/° | 4.65 to 63.188 |
| Index ranges | -25 ≤ h ≤ 25, -11 ≤ k ≤ 13, -34 ≤ l ≤ 25 |
| Reflections collected | 43076 |
| Independent reflections | 12661 [Rint = 0.0594, Rsigma = 0.0669] |
| Data/restraints/parameters | 12661/0/425 |
| Goodness-of-fit on F2 | 1.018 |
| Final R indexes [I>=2σ (I)] | R1 = 0.0363, wR2 = 0.0671 |
| Final R indexes [all data] | R1 = 0.0729, wR2 = 0.0769 |
| Largest diff. peak/hole / e Å-3 | 0.64/-0.79 |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| Br1 | 990.4(2) | 7263.9(3) | 5855.9(2) | 22.96(6) |
| Zn1 | 297.8(2) | 8566.3(3) | 5057.0(2) | 13.62(6) |
| Fe1 | 1187.5(2) | 9698.1(4) | 3108.1(2) | 15.81(7) |
| Si1 | 1439.3(3) | 10770.6(7) | 4610.6(3) | 14.66(13) |
| O1 | 652.0(9) | 10430.1(16) | 4848.0(7) | 15.7(3) |
| N1 | 9.3(10) | 7376(2) | 4297.3(8) | 14.1(4) |
| C1 | 1479.7(12) | 9494(2) | 4011.7(10) | 14.0(4) |
| C2 | 932.4(12) | 8429(2) | 3732.3(10) | 14.0(4) |
| C3 | 1281.7(13) | 7628(3) | 3341.5(10) | 16.8(5) |
| C4 | 2038.7(13) | 8189(3) | 3366.6(11) | 18.4(5) |
| C5 | 2160.6(13) | 9325(3) | 3772.3(10) | 16.4(5) |
| C6 | 400.8(18) | 11299(3) | 2880.3(13) | 36.3(7) |
| C7 | 154.4(15) | 10125(3) | 2524.4(12) | 29.9(6) |
| C8 | 738.9(16) | 9793(3) | 2223.6(12) | 31.3(6) |
| C9 | 1353.2(17) | 10774(4) | 2391.9(14) | 43.6(9) |
| C10 | 1146(2) | 11714(3) | 2802.6(14) | 45.4(9) |
| C11 | 1447.1(15) | 12619(3) | 4352.0(12) | 26.6(6) |
| C12 | 2332.8(13) | 10445(3) | 5196.8(11) | 25.2(6) |
| C13 | 97.2(12) | 8229(3) | 3778.3(10) | 15.3(5) |
| C14 | 467.1(14) | 6042(2) | 4332.0(11) | 19.2(5) |
| C15 | -834.7(13) | 6998(3) | 4203.7(11) | 19.3(5) |
| Br2 | 6169.0(2) | 7729.1(3) | 5711.5(2) | 23.24(6) |
| Zn2 | 5308.6(2) | 6415.5(3) | 4997.0(2) | 13.07(6) |
| Fe2 | 6293.8(2) | 5580.5(4) | 3063.8(2) | 16.02(7) |
| Si2 | 6310.4(3) | 4033.5(7) | 4482.8(3) | 13.70(13) |
| O2 | 5599.0(9) | 4509.0(16) | 4785.5(7) | 15.4(3) |
| N2 | 4908(1) | 7515(2) | 4224.2(8) | 14.6(4) |
| C16 | 6444.8(13) | 5468(2) | 3966.3(10) | 15.8(5) |
| C17 | 5915.1(12) | 6586(2) | 3710.7(10) | 14.9(4) |
| C18 | 6314.6(13) | 7547(3) | 3413.8(10) | 17.2(5) |
| C19 | 7096.0(13) | 7040(3) | 3474.2(10) | 17.9(5) |
| C20 | 7173.5(13) | 5774(3) | 3807.7(10) | 16.6(5) |
| C21 | 5795.2(19) | 3756(3) | 2702.2(13) | 37.2(8) |
| C22 | 5317.7(15) | 4920(4) | 2467.2(13) | 36.2(8) |
| C23 | 5767.5(15) | 5812(3) | 2191.5(12) | 29.4(6) |
| C24 | 6518.1(15) | 5208(3) | 2257.6(11) | 24.9(6) |
| C25 | 6539.7(17) | 3937(3) | 2572.9(12) | 30.2(6) |
| C26 | 7264.8(13) | 3912(3) | 5034.0(11) | 22.3(5) |
| C27 | 6073.4(15) | 2278(3) | 4130.2(12) | 23.9(5) |
| C28 | 5060.9(12) | 6709(3) | 3712.4(11) | 17.0(5) |
| C29 | 5265.9(14) | 8948(2) | 4245.4(11) | 20.8(5) |
| C30 | 4044.9(13) | 7695(3) | 4124.7(11) | 22.4(5) |
| O3 | 6665.4(15) | 523(3) | 2736.6(16) | 81.2(10) |
| C31 | 7104(3) | -542(4) | 1973.4(19) | 80.2(15) |
| C32 | 7214.7(18) | 113(3) | 2543.6(16) | 42.5(8) |
| C33 | 8024.2(18) | 245(4) | 2900.6(16) | 45.7(8) |
| Atom | U11 | U22 | U33 | U23 | U13 | U12 |
|---|---|---|---|---|---|---|
| Br1 | 24.88(12) | 22.73(13) | 19.16(13) | 4.19(10) | 0.75(9) | 1.99(11) |
| Zn1 | 13.37(11) | 12.87(13) | 15.17(14) | -0.44(10) | 4.45(10) | -0.45(10) |
| Fe1 | 15.26(14) | 18.49(17) | 13.67(18) | 2.94(13) | 3.34(12) | -1.35(13) |
| Si1 | 13.1(3) | 14.0(3) | 18.1(3) | -2.7(3) | 6.1(2) | -2.8(3) |
| O1 | 14.6(7) | 13.5(8) | 20.8(9) | -0.8(6) | 7.7(6) | -1.9(6) |
| N1 | 13.7(8) | 14.9(10) | 13.8(10) | 0.6(7) | 3.4(7) | -1.9(8) |
| C1 | 12.4(9) | 12.2(11) | 16.8(12) | 3.0(9) | 2.0(8) | -1.0(8) |
| C2 | 12.7(9) | 14.9(11) | 14.2(12) | 0.8(9) | 2.3(8) | -1.7(9) |
| C3 | 18.6(10) | 16.6(11) | 16.1(12) | 0.6(9) | 5.7(9) | -1(1) |
| C4 | 15.9(10) | 20.7(12) | 20.5(13) | -0.8(10) | 7.8(9) | 1.9(10) |
| C5 | 13.5(9) | 19.9(12) | 15.3(12) | 2.0(9) | 2.5(8) | -1.0(9) |
| C6 | 45.3(17) | 34.4(17) | 27.4(17) | 10.6(13) | 4.8(13) | 17.9(15) |
| C7 | 20.5(12) | 37.1(16) | 28.5(16) | 13.1(13) | -1.6(11) | 0.1(12) |
| C8 | 36.2(14) | 38.3(17) | 16.8(14) | 5.1(12) | 0.5(11) | 6.6(14) |
| C9 | 25.8(13) | 74(3) | 30.4(18) | 32.5(17) | 4.7(12) | -0.7(16) |
| C10 | 59(2) | 26.9(16) | 36.5(19) | 18.6(14) | -17.4(16) | -14.4(16) |
| C11 | 32.5(13) | 17.8(13) | 35.4(17) | -2.0(11) | 20.2(12) | -3.8(11) |
| C12 | 17.2(11) | 36.2(16) | 21.7(14) | -9.6(11) | 3.7(10) | -3.8(11) |
| C13 | 13.4(9) | 17.4(11) | 14.6(12) | 0.5(9) | 2.5(8) | -1.0(9) |
| C14 | 23.8(11) | 14.4(11) | 20.8(13) | 1.1(9) | 7.8(10) | 0.9(10) |
| C15 | 16.7(10) | 19.0(12) | 23.7(14) | -2.7(10) | 7.6(9) | -5.9(10) |
| Br2 | 20.56(11) | 26.05(13) | 21.43(14) | -5.29(10) | 1.47(9) | -6.56(11) |
| Zn2 | 12.90(11) | 11.79(13) | 14.86(14) | 0.49(10) | 3.92(10) | -0.39(10) |
| Fe2 | 15.10(14) | 19.52(17) | 13.95(18) | -3.07(13) | 4.42(12) | -0.34(14) |
| Si2 | 12.1(3) | 12.3(3) | 17.3(3) | 0.3(2) | 4.5(2) | 0.5(2) |
| O2 | 15.2(7) | 12.3(8) | 20.4(9) | 0.2(6) | 7.8(6) | -0.5(6) |
| N2 | 14.1(8) | 14.7(10) | 15.5(10) | 1.0(7) | 4.5(7) | 0.6(8) |
| C16 | 16.5(10) | 15.6(12) | 15.2(12) | -3.5(9) | 3.5(9) | -0.5(9) |
| C17 | 16(1) | 16.4(11) | 12.6(11) | -1.7(9) | 3.9(8) | -0.2(9) |
| C18 | 18.3(10) | 16.4(12) | 17.0(12) | 0.7(9) | 4.5(9) | -1.0(9) |
| C19 | 16.5(10) | 19.5(12) | 18.7(13) | 0.2(9) | 6.2(9) | -1.7(10) |
| C20 | 14.8(10) | 18.5(12) | 16.9(12) | -1.1(9) | 4.5(9) | -0.3(9) |
| C21 | 57.5(19) | 34.9(17) | 21.9(16) | -12.9(12) | 14.3(14) | -24.8(16) |
| C22 | 20.3(12) | 62(2) | 25.5(16) | -24.9(15) | 4.4(11) | -9.9(14) |
| C23 | 29.4(13) | 37.3(16) | 18.7(14) | -6.8(12) | 0.0(11) | 3.9(13) |
| C24 | 26.2(12) | 33.2(15) | 17.6(14) | -6.1(11) | 10(1) | -2.3(12) |
| C25 | 40.7(15) | 27.8(15) | 20.8(15) | -11.4(11) | 4.7(12) | 5.9(13) |
| C26 | 16.1(10) | 26.0(13) | 24.9(14) | 7.1(11) | 4.6(10) | 0.5(10) |
| C27 | 26.4(12) | 16.3(12) | 31.0(15) | -1.9(11) | 10.3(11) | -0.6(11) |
| C28 | 15.6(10) | 18.1(12) | 16.8(12) | -0.7(9) | 2.7(9) | 1.2(9) |
| C29 | 28.5(12) | 14.3(11) | 20.5(13) | 1.2(9) | 7.5(10) | 1.4(10) |
| C30 | 16.1(10) | 28.8(14) | 23.7(14) | 4.8(11) | 7.3(10) | 6.5(11) |
| O3 | 51.9(15) | 45.7(17) | 161(3) | 23.7(18) | 55.4(19) | 7.5(14) |
| C31 | 86(3) | 49(2) | 77(3) | -16(2) | -41(2) | 14(2) |
| C32 | 36.1(15) | 19.4(14) | 71(3) | 5.7(15) | 11.8(16) | -3.5(14) |
| C33 | 44.6(18) | 43.7(19) | 47(2) | 1.8(16) | 7.4(15) | -13.1(17) |
| Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
|---|---|---|---|---|---|---|
| Br1 | Zn1 | 2.3365(4) | Zn2 | O2 | 1.9729(16) | |
| Zn1 | Zn11 | 2.9034(5) | Zn2 | O22 | 1.9839(15) | |
| Zn1 | O1 | 1.9728(16) | Zn2 | N2 | 2.0681(19) | |
| Zn1 | O11 | 1.9747(15) | Fe2 | C16 | 2.075(2) | |
| Zn1 | N1 | 2.0710(19) | Fe2 | C17 | 2.030(2) | |
| Fe1 | C1 | 2.071(2) | Fe2 | C18 | 2.035(2) | |
| Fe1 | C2 | 2.024(2) | Fe2 | C19 | 2.048(2) | |
| Fe1 | C3 | 2.035(2) | Fe2 | C20 | 2.052(2) | |
| Fe1 | C4 | 2.055(2) | Fe2 | C21 | 2.034(3) | |
| Fe1 | C5 | 2.057(2) | Fe2 | C22 | 2.042(3) | |
| Fe1 | C6 | 2.037(3) | Fe2 | C23 | 2.052(3) | |
| Fe1 | C7 | 2.042(3) | Fe2 | C24 | 2.049(3) | |
| Fe1 | C8 | 2.044(3) | Fe2 | C25 | 2.042(3) | |
| Fe1 | C9 | 2.043(3) | Si2 | O2 | 1.6346(16) | |
| Fe1 | C10 | 2.038(3) | Si2 | C16 | 1.873(2) | |
| Si1 | O1 | 1.6354(15) | Si2 | C26 | 1.866(2) | |
| Si1 | C1 | 1.868(2) | Si2 | C27 | 1.863(3) | |
| Si1 | C11 | 1.857(3) | O2 | Zn22 | 1.9839(15) | |
| Si1 | C12 | 1.856(3) | N2 | C28 | 1.499(3) | |
| O1 | Zn11 | 1.9747(15) | N2 | C29 | 1.494(3) | |
| N1 | C13 | 1.499(3) | N2 | C30 | 1.486(3) | |
| N1 | C14 | 1.491(3) | C16 | C17 | 1.445(3) | |
| N1 | C15 | 1.489(3) | C16 | C20 | 1.440(3) | |
| C1 | C2 | 1.442(3) | C17 | C18 | 1.426(3) | |
| C1 | C5 | 1.441(3) | C17 | C28 | 1.503(3) | |
| C2 | C3 | 1.433(3) | C18 | C19 | 1.427(3) | |
| C2 | C13 | 1.505(3) | C19 | C20 | 1.422(3) | |
| C3 | C4 | 1.418(3) | C21 | C22 | 1.418(5) | |
| C4 | C5 | 1.421(3) | C21 | C25 | 1.417(4) | |
| C6 | C7 | 1.399(4) | C22 | C23 | 1.411(4) | |
| C6 | C10 | 1.417(5) | C23 | C24 | 1.410(4) | |
| C7 | C8 | 1.407(4) | C24 | C25 | 1.410(4) | |
| C8 | C9 | 1.409(4) | O3 | C32 | 1.219(4) | |
| C9 | C10 | 1.420(5) | C31 | C32 | 1.447(5) | |
| Br2 | Zn2 | 2.3381(4) | C32 | C33 | 1.477(4) | |
| Zn2 | Zn22 | 2.8963(5) |
| Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|
| Br1 | Zn1 | Zn11 | 132.710(17) | O2 | Zn2 | Br2 | 120.50(5) | |
| O11 | Zn1 | Br1 | 117.37(5) | O2 | Zn2 | Zn22 | 43.10(4) | |
| O1 | Zn1 | Br1 | 122.55(5) | O22 | Zn2 | Zn22 | 42.80(4) | |
| O1 | Zn1 | Zn11 | 42.67(4) | O2 | Zn2 | O22 | 85.90(6) | |
| O11 | Zn1 | Zn11 | 42.62(5) | O22 | Zn2 | N2 | 108.56(7) | |
| O1 | Zn1 | O11 | 85.30(6) | O2 | Zn2 | N2 | 107.26(7) | |
| O1 | Zn1 | N1 | 107.63(7) | N2 | Zn2 | Br2 | 113.06(5) | |
| O11 | Zn1 | N1 | 108.38(7) | N2 | Zn2 | Zn22 | 114.84(5) | |
| N1 | Zn1 | Br1 | 112.33(5) | C17 | Fe2 | C16 | 41.22(9) | |
| N1 | Zn1 | Zn11 | 114.86(5) | C17 | Fe2 | C18 | 41.07(9) | |
| C2 | Fe1 | C1 | 41.21(9) | C17 | Fe2 | C19 | 68.81(9) | |
| C2 | Fe1 | C3 | 41.34(9) | C17 | Fe2 | C20 | 68.50(9) | |
| C2 | Fe1 | C4 | 68.85(9) | C17 | Fe2 | C21 | 121.90(11) | |
| C2 | Fe1 | C5 | 68.47(9) | C17 | Fe2 | C22 | 106.82(10) | |
| C2 | Fe1 | C6 | 112.55(11) | C17 | Fe2 | C23 | 123.08(10) | |
| C2 | Fe1 | C7 | 107.02(10) | C17 | Fe2 | C24 | 159.51(10) | |
| C2 | Fe1 | C8 | 131.55(11) | C17 | Fe2 | C25 | 158.18(11) | |
| C2 | Fe1 | C9 | 171.61(13) | C18 | Fe2 | C16 | 69.47(9) | |
| C2 | Fe1 | C10 | 144.78(13) | C18 | Fe2 | C19 | 40.93(9) | |
| C3 | Fe1 | C1 | 69.45(9) | C18 | Fe2 | C20 | 68.59(9) | |
| C3 | Fe1 | C4 | 40.57(9) | C18 | Fe2 | C22 | 119.45(11) | |
| C3 | Fe1 | C5 | 68.21(9) | C18 | Fe2 | C23 | 105.43(11) | |
| C3 | Fe1 | C6 | 142.88(11) | C18 | Fe2 | C24 | 122.75(11) | |
| C3 | Fe1 | C7 | 112.06(11) | C18 | Fe2 | C25 | 160.17(11) | |
| C3 | Fe1 | C8 | 107.69(11) | C19 | Fe2 | C16 | 69.11(9) | |
| C3 | Fe1 | C9 | 133.25(13) | C19 | Fe2 | C20 | 40.58(9) | |
| C3 | Fe1 | C10 | 173.88(13) | C19 | Fe2 | C23 | 119.86(11) | |
| C4 | Fe1 | C1 | 69.03(9) | C19 | Fe2 | C24 | 107.03(10) | |
| C4 | Fe1 | C5 | 40.41(9) | C20 | Fe2 | C16 | 40.85(8) | |
| C5 | Fe1 | C1 | 40.85(8) | C20 | Fe2 | C23 | 156.08(10) | |
| C6 | Fe1 | C1 | 109.29(11) | C21 | Fe2 | C16 | 108.84(11) | |
| C6 | Fe1 | C4 | 175.91(12) | C21 | Fe2 | C18 | 156.10(11) | |
| C6 | Fe1 | C5 | 135.99(12) | C21 | Fe2 | C19 | 162.45(12) | |
| C6 | Fe1 | C7 | 40.10(12) | C21 | Fe2 | C20 | 126.64(12) | |
| C6 | Fe1 | C8 | 67.83(12) | C21 | Fe2 | C22 | 40.71(13) | |
| C6 | Fe1 | C9 | 68.19(13) | C21 | Fe2 | C23 | 67.95(13) | |
| C6 | Fe1 | C10 | 40.69(13) | C21 | Fe2 | C24 | 67.92(11) | |
| C7 | Fe1 | C1 | 132.51(10) | C21 | Fe2 | C25 | 40.69(12) | |
| C7 | Fe1 | C4 | 143.74(11) | C22 | Fe2 | C16 | 124.91(11) | |
| C7 | Fe1 | C5 | 173.25(11) | C22 | Fe2 | C19 | 154.80(12) | |
| C7 | Fe1 | C8 | 40.30(11) | C22 | Fe2 | C20 | 162.89(12) | |
| C7 | Fe1 | C9 | 67.82(11) | C22 | Fe2 | C23 | 40.32(12) | |
| C8 | Fe1 | C1 | 171.51(10) | C22 | Fe2 | C24 | 67.92(11) | |
| C8 | Fe1 | C4 | 114.38(11) | C22 | Fe2 | C25 | 68.42(12) | |
| C8 | Fe1 | C5 | 146.44(10) | C23 | Fe2 | C16 | 160.84(10) | |
| C9 | Fe1 | C1 | 147.10(12) | C24 | Fe2 | C16 | 157.87(10) | |
| C9 | Fe1 | C4 | 111.04(12) | C24 | Fe2 | C20 | 122.22(10) | |
| C9 | Fe1 | C5 | 117.25(10) | C24 | Fe2 | C23 | 40.23(10) | |
| C9 | Fe1 | C8 | 40.33(12) | C25 | Fe2 | C16 | 122.84(11) | |
| C10 | Fe1 | C1 | 115.34(12) | C25 | Fe2 | C19 | 124.71(11) | |
| C10 | Fe1 | C4 | 136.19(12) | C25 | Fe2 | C20 | 109.43(11) | |
| C10 | Fe1 | C5 | 112.55(11) | C25 | Fe2 | C23 | 67.95(11) | |
| C10 | Fe1 | C7 | 67.95(12) | C25 | Fe2 | C24 | 40.33(11) | |
| C10 | Fe1 | C8 | 68.13(13) | O2 | Si2 | C16 | 107.65(9) | |
| C10 | Fe1 | C9 | 40.72(14) | O2 | Si2 | C26 | 111.58(10) | |
| O1 | Si1 | C1 | 108.05(9) | O2 | Si2 | C27 | 108.98(10) | |
| O1 | Si1 | C11 | 111.61(10) | C26 | Si2 | C16 | 105.44(11) | |
| O1 | Si1 | C12 | 110.43(10) | C27 | Si2 | C16 | 114.24(11) | |
| C11 | Si1 | C1 | 111.23(11) | C27 | Si2 | C26 | 108.95(12) | |
| C12 | Si1 | C1 | 106.08(11) | Zn2 | O2 | Zn22 | 94.10(6) | |
| C12 | Si1 | C11 | 109.30(13) | Si2 | O2 | Zn2 | 129.00(9) | |
| Zn1 | O1 | Zn11 | 94.70(6) | Si2 | O2 | Zn22 | 136.67(10) | |
| Si1 | O1 | Zn1 | 126.90(9) | C28 | N2 | Zn2 | 110.96(14) | |
| Si1 | O1 | Zn11 | 138.00(10) | C29 | N2 | Zn2 | 112.02(14) | |
| C13 | N1 | Zn1 | 110.74(14) | C29 | N2 | C28 | 109.83(18) | |
| C14 | N1 | Zn1 | 113.24(14) | C30 | N2 | Zn2 | 108.83(14) | |
| C14 | N1 | C13 | 110.32(17) | C30 | N2 | C28 | 107.29(18) | |
| C15 | N1 | Zn1 | 107.15(14) | C30 | N2 | C29 | 107.75(18) | |
| C15 | N1 | C13 | 107.19(17) | Si2 | C16 | Fe2 | 133.80(12) | |
| C15 | N1 | C14 | 107.93(18) | C17 | C16 | Fe2 | 67.72(13) | |
| Si1 | C1 | Fe1 | 131.70(12) | C17 | C16 | Si2 | 129.54(16) | |
| C2 | C1 | Fe1 | 67.63(13) | C20 | C16 | Fe2 | 68.75(13) | |
| C2 | C1 | Si1 | 131.20(16) | C20 | C16 | Si2 | 124.44(17) | |
| C5 | C1 | Fe1 | 69.07(13) | C20 | C16 | C17 | 105.5(2) | |
| C5 | C1 | Si1 | 122.96(17) | C16 | C17 | Fe2 | 71.06(13) | |
| C5 | C1 | C2 | 105.6(2) | C16 | C17 | C28 | 126.9(2) | |
| C1 | C2 | Fe1 | 71.16(13) | C18 | C17 | Fe2 | 69.67(13) | |
| C1 | C2 | C13 | 127.7(2) | C18 | C17 | C16 | 109.32(19) | |
| C3 | C2 | Fe1 | 69.75(13) | C18 | C17 | C28 | 123.6(2) | |
| C3 | C2 | C1 | 108.93(19) | C28 | C17 | Fe2 | 122.47(16) | |
| C3 | C2 | C13 | 123.1(2) | C17 | C18 | Fe2 | 69.26(13) | |
| C13 | C2 | Fe1 | 120.56(15) | C17 | C18 | C19 | 107.7(2) | |
| C2 | C3 | Fe1 | 68.91(13) | C19 | C18 | Fe2 | 70.02(14) | |
| C4 | C3 | Fe1 | 70.49(14) | C18 | C19 | Fe2 | 69.05(13) | |
| C4 | C3 | C2 | 108.0(2) | C20 | C19 | Fe2 | 69.87(13) | |
| C3 | C4 | Fe1 | 68.94(13) | C20 | C19 | C18 | 107.9(2) | |
| C3 | C4 | C5 | 107.9(2) | C16 | C20 | Fe2 | 70.40(13) | |
| C5 | C4 | Fe1 | 69.86(13) | C19 | C20 | Fe2 | 69.55(13) | |
| C1 | C5 | Fe1 | 70.09(13) | C19 | C20 | C16 | 109.6(2) | |
| C4 | C5 | Fe1 | 69.72(13) | C22 | C21 | Fe2 | 69.98(16) | |
| C4 | C5 | C1 | 109.6(2) | C25 | C21 | Fe2 | 69.99(16) | |
| C7 | C6 | Fe1 | 70.14(16) | C25 | C21 | C22 | 108.2(3) | |
| C7 | C6 | C10 | 108.2(3) | C21 | C22 | Fe2 | 69.32(16) | |
| C10 | C6 | Fe1 | 69.66(17) | C23 | C22 | Fe2 | 70.22(15) | |
| C6 | C7 | Fe1 | 69.76(16) | C23 | C22 | C21 | 107.6(2) | |
| C6 | C7 | C8 | 108.5(3) | C22 | C23 | Fe2 | 69.46(16) | |
| C8 | C7 | Fe1 | 69.90(15) | C24 | C23 | Fe2 | 69.76(15) | |
| C7 | C8 | Fe1 | 69.80(16) | C24 | C23 | C22 | 108.2(3) | |
| C7 | C8 | C9 | 108.1(3) | C23 | C24 | Fe2 | 70.01(15) | |
| C9 | C8 | Fe1 | 69.81(16) | C23 | C24 | C25 | 108.4(2) | |
| C8 | C9 | Fe1 | 69.86(16) | C25 | C24 | Fe2 | 69.58(15) | |
| C8 | C9 | C10 | 107.8(3) | C21 | C25 | Fe2 | 69.32(16) | |
| C10 | C9 | Fe1 | 69.43(17) | C24 | C25 | Fe2 | 70.09(15) | |
| C6 | C10 | Fe1 | 69.65(16) | C24 | C25 | C21 | 107.5(3) | |
| C6 | C10 | C9 | 107.5(3) | N2 | C28 | C17 | 113.87(19) | |
| C9 | C10 | Fe1 | 69.85(18) | O3 | C32 | C31 | 122.2(4) | |
| N1 | C13 | C2 | 114.25(18) | O3 | C32 | C33 | 120.0(4) | |
| Br2 | Zn2 | Zn22 | 132.096(17) | C31 | C32 | C33 | 117.8(3) | |
| O22 | Zn2 | Br2 | 118.29(5) |
| A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|---|---|
| Zn1 | N1 | C13 | C2 | 76.4(2) | Zn2 | N2 | C28 | C17 | -68.1(2) | |
| Fe1 | C1 | C2 | C3 | 59.76(16) | Fe2 | C16 | C17 | C18 | -59.37(16) | |
| Fe1 | C1 | C2 | C13 | -114.5(2) | Fe2 | C16 | C17 | C28 | 116.9(2) | |
| Fe1 | C1 | C5 | C4 | -58.64(17) | Fe2 | C16 | C20 | C19 | 58.66(17) | |
| Fe1 | C2 | C3 | C4 | 59.91(17) | Fe2 | C17 | C18 | C19 | -59.70(17) | |
| Fe1 | C2 | C13 | N1 | -174.24(15) | Fe2 | C17 | C28 | N2 | -178.95(15) | |
| Fe1 | C3 | C4 | C5 | 59.23(17) | Fe2 | C18 | C19 | C20 | -59.30(17) | |
| Fe1 | C4 | C5 | C1 | 58.86(16) | Fe2 | C19 | C20 | C16 | -59.18(17) | |
| Fe1 | C6 | C7 | C8 | -59.38(19) | Fe2 | C21 | C22 | C23 | 60.03(19) | |
| Fe1 | C6 | C10 | C9 | 59.9(2) | Fe2 | C21 | C25 | C24 | -59.92(19) | |
| Fe1 | C7 | C8 | C9 | -59.6(2) | Fe2 | C22 | C23 | C24 | 59.21(19) | |
| Fe1 | C8 | C9 | C10 | -59.3(2) | Fe2 | C23 | C24 | C25 | 59.18(19) | |
| Fe1 | C9 | C10 | C6 | -59.7(2) | Fe2 | C24 | C25 | C21 | 59.44(18) | |
| Si1 | C1 | C2 | Fe1 | 126.6(2) | Si2 | C16 | C17 | Fe2 | -129.2(2) | |
| Si1 | C1 | C2 | C3 | -173.67(18) | Si2 | C16 | C17 | C18 | 171.45(18) | |
| Si1 | C1 | C2 | C13 | 12.0(4) | Si2 | C16 | C17 | C28 | -12.3(4) | |
| Si1 | C1 | C5 | Fe1 | -126.93(17) | Si2 | C16 | C20 | Fe2 | 129.33(18) | |
| Si1 | C1 | C5 | C4 | 174.42(17) | Si2 | C16 | C20 | C19 | -172.01(17) | |
| O1 | Si1 | C1 | Fe1 | 100.75(15) | O2 | Si2 | C16 | Fe2 | -114.84(15) | |
| O1 | Si1 | C1 | C2 | 4.9(2) | O2 | Si2 | C16 | C17 | -18.5(2) | |
| O1 | Si1 | C1 | C5 | -168.83(18) | O2 | Si2 | C16 | C20 | 152.37(19) | |
| C1 | Si1 | O1 | Zn11 | -123.02(15) | C16 | Si2 | O2 | Zn22 | 139.24(14) | |
| C1 | Si1 | O1 | Zn1 | 47.76(14) | C16 | Si2 | O2 | Zn2 | -33.76(15) | |
| C1 | C2 | C3 | Fe1 | -60.63(16) | C16 | C17 | C18 | Fe2 | 60.22(16) | |
| C1 | C2 | C3 | C4 | -0.7(3) | C16 | C17 | C18 | C19 | 0.5(3) | |
| C1 | C2 | C13 | N1 | -85.2(3) | C16 | C17 | C28 | N2 | 91.2(3) | |
| C2 | C1 | C5 | Fe1 | 57.99(15) | C17 | C16 | C20 | Fe2 | -57.97(15) | |
| C2 | C1 | C5 | C4 | -0.6(3) | C17 | C16 | C20 | C19 | 0.7(3) | |
| C2 | C3 | C4 | Fe1 | -58.91(16) | C17 | C18 | C19 | Fe2 | 59.22(16) | |
| C2 | C3 | C4 | C5 | 0.3(3) | C17 | C18 | C19 | C20 | -0.1(3) | |
| C3 | C2 | C13 | N1 | 101.2(3) | C18 | C17 | C28 | N2 | -93.0(3) | |
| C3 | C4 | C5 | Fe1 | -58.65(17) | C18 | C19 | C20 | Fe2 | 58.79(17) | |
| C3 | C4 | C5 | C1 | 0.2(3) | C18 | C19 | C20 | C16 | -0.4(3) | |
| C5 | C1 | C2 | Fe1 | -58.92(15) | C20 | C16 | C17 | Fe2 | 58.63(16) | |
| C5 | C1 | C2 | C3 | 0.8(3) | C20 | C16 | C17 | C18 | -0.7(3) | |
| C5 | C1 | C2 | C13 | -173.5(2) | C20 | C16 | C17 | C28 | 175.5(2) | |
| C6 | C7 | C8 | Fe1 | 59.29(19) | C21 | C22 | C23 | Fe2 | -59.46(19) | |
| C6 | C7 | C8 | C9 | -0.3(3) | C21 | C22 | C23 | C24 | -0.2(3) | |
| C7 | C6 | C10 | Fe1 | -59.8(2) | C22 | C21 | C25 | Fe2 | 59.77(19) | |
| C7 | C6 | C10 | C9 | 0.0(3) | C22 | C21 | C25 | C24 | -0.2(3) | |
| C7 | C8 | C9 | Fe1 | 59.55(19) | C22 | C23 | C24 | Fe2 | -59.02(19) | |
| C7 | C8 | C9 | C10 | 0.3(3) | C22 | C23 | C24 | C25 | 0.2(3) | |
| C8 | C9 | C10 | Fe1 | 59.5(2) | C23 | C24 | C25 | Fe2 | -59.44(18) | |
| C8 | C9 | C10 | C6 | -0.2(3) | C23 | C24 | C25 | C21 | 0.0(3) | |
| C10 | C6 | C7 | Fe1 | 59.5(2) | C25 | C21 | C22 | Fe2 | -59.78(19) | |
| C10 | C6 | C7 | C8 | 0.1(3) | C25 | C21 | C22 | C23 | 0.2(3) | |
| C11 | Si1 | O1 | Zn1 | 170.35(13) | C26 | Si2 | O2 | Zn2 | 81.47(15) | |
| C11 | Si1 | O1 | Zn11 | -0.42(19) | C26 | Si2 | O2 | Zn22 | -105.52(16) | |
| C11 | Si1 | C1 | Fe1 | -22.08(18) | C26 | Si2 | C16 | Fe2 | 125.93(16) | |
| C11 | Si1 | C1 | C2 | -118.0(2) | C26 | Si2 | C16 | C17 | -137.7(2) | |
| C11 | Si1 | C1 | C5 | 68.3(2) | C26 | Si2 | C16 | C20 | 33.1(2) | |
| C12 | Si1 | O1 | Zn1 | -67.85(15) | C27 | Si2 | O2 | Zn22 | 14.83(18) | |
| C12 | Si1 | O1 | Zn11 | 121.38(16) | C27 | Si2 | O2 | Zn2 | -158.17(13) | |
| C12 | Si1 | C1 | Fe1 | -140.83(15) | C27 | Si2 | C16 | Fe2 | 6.3(2) | |
| C12 | Si1 | C1 | C2 | 123.3(2) | C27 | Si2 | C16 | C17 | 102.7(2) | |
| C12 | Si1 | C1 | C5 | -50.4(2) | C27 | Si2 | C16 | C20 | -86.5(2) | |
| C13 | C2 | C3 | Fe1 | 114.0(2) | C28 | C17 | C18 | Fe2 | -116.2(2) | |
| C13 | C2 | C3 | C4 | 173.9(2) | C28 | C17 | C18 | C19 | -175.9(2) | |
| C14 | N1 | C13 | C2 | -49.8(3) | C29 | N2 | C28 | C17 | 56.3(2) | |
| C15 | N1 | C13 | C2 | -167.05(19) | C30 | N2 | C28 | C17 | 173.1(2) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| H3 | 1047 | 6857 | 3107 | 20 |
| H4 | 2400 | 7863 | 3150 | 22 |
| H5 | 2621 | 9887 | 3871 | 20 |
| H6 | 117 | 11740 | 3131 | 44 |
| H7 | -326 | 9634 | 2491 | 36 |
| H8 | 722 | 9040 | 1954 | 38 |
| H9 | 1822 | 10802 | 2255 | 52 |
| H10 | 1452 | 12481 | 2991 | 55 |
| H11A | 934 | 12850 | 4100 | 40 |
| H11B | 1853 | 12727 | 4130 | 40 |
| H11C | 1558 | 13256 | 4690 | 40 |
| H12A | 2365 | 11145 | 5509 | 38 |
| H12B | 2797 | 10520 | 5033 | 38 |
| H12C | 2308 | 9498 | 5358 | 38 |
| H13A | -142 | 9167 | 3799 | 18 |
| H13B | -198 | 7760 | 3417 | 18 |
| H14A | 1027 | 6263 | 4404 | 29 |
| H14B | 305 | 5526 | 3962 | 29 |
| H14C | 370 | 5460 | 4653 | 29 |
| H15A | -913 | 6426 | 4533 | 29 |
| H15B | -997 | 6458 | 3839 | 29 |
| H15C | -1149 | 7860 | 4177 | 29 |
| H18 | 6100 | 8376 | 3212 | 21 |
| H19 | 7494 | 7471 | 3319 | 21 |
| H20 | 7635 | 5217 | 3910 | 20 |
| H21 | 5642 | 2987 | 2910 | 45 |
| H22 | 4790 | 5072 | 2491 | 43 |
| H23 | 5595 | 6671 | 1995 | 35 |
| H24 | 6938 | 5592 | 2114 | 30 |
| H25 | 6974 | 3315 | 2679 | 36 |
| H26A | 7360 | 4792 | 5259 | 34 |
| H26B | 7689 | 3758 | 4832 | 34 |
| H26C | 7247 | 3124 | 5301 | 34 |
| H27A | 6112 | 1554 | 4433 | 36 |
| H27B | 6445 | 2064 | 3887 | 36 |
| H27C | 5539 | 2293 | 3884 | 36 |
| H28A | 4784 | 7180 | 3346 | 20 |
| H28B | 4839 | 5750 | 3714 | 20 |
| H29A | 5120 | 9503 | 4556 | 31 |
| H29B | 5075 | 9421 | 3868 | 31 |
| H29C | 5838 | 8862 | 4326 | 31 |
| H30A | 3793 | 6767 | 4099 | 34 |
| H30B | 3849 | 8212 | 3758 | 34 |
| H30C | 3924 | 8225 | 4451 | 34 |
| H31A | 7151 | -1568 | 2020 | 120 |
| H31B | 7505 | -198 | 1777 | 120 |
| H31C | 6583 | -306 | 1737 | 120 |
| H33A | 8289 | 1023 | 2751 | 69 |
| H33B | 8309 | -635 | 2879 | 69 |
| H33C | 8011 | 434 | 3309 | 69 |
Experimental
Single crystals of C33H50Br2Fe2N2O3Si2Zn2 [mo_B0175_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_B0175_0m]
Crystal Data for C33H50Br2Fe2N2O3Si2Zn2 (M =981.19 g/mol): monoclinic, space group P21/c (no. 14), a = 17.5299(5) Å, b = 9.4853(3) Å, c = 23.4559(7) Å, β = 103.372(2)°, V = 3794.4(2) Å3, Z = 4, T = 100.01 K, μ(MoKα) = 4.203 mm-1, Dcalc = 1.718 g/cm3, 43076 reflections measured (4.65° ≤ 2Θ ≤ 63.188°), 12661 unique (Rint = 0.0594, Rsigma = 0.0669) which were used in all calculations. The final R1 was 0.0363 (I > 2σ(I)) and wR2 was 0.0769 (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), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C)
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.