| Identification code | 3075 |
| Empirical formula | C41H50Br2Fe2N2O4Si2Zn |
| Formula weight | 1027.90 |
| Temperature/K | 173 |
| Crystal system | triclinic |
| Space group | P-1 |
| a/Å | 10.9344(4) |
| b/Å | 14.4572(5) |
| c/Å | 15.7160(6) |
| α/° | 65.850(4) |
| β/° | 75.359(3) |
| γ/° | 87.591(3) |
| Volume/Å3 | 2188.05(15) |
| Z | 2 |
| ρcalcg/cm3 | 1.560 |
| μ/mm‑1 | 3.120 |
| F(000) | 1044.0 |
| Crystal size/mm3 | 0.08 × 0.06 × 0.05 |
| Radiation | MoKα (λ = 0.71073) |
| 2Θ range for data collection/° | 4.628 to 53.994 |
| Index ranges | -13 ≤ h ≤ 13, -18 ≤ k ≤ 18, -20 ≤ l ≤ 19 |
| Reflections collected | 32328 |
| Independent reflections | 9491 [Rint = 0.0481, Rsigma = 0.0530] |
| Data/restraints/parameters | 9491/2/501 |
| Goodness-of-fit on F2 | 1.022 |
| Final R indexes [I>=2σ (I)] | R1 = 0.0359, wR2 = 0.0678 |
| Final R indexes [all data] | R1 = 0.0564, wR2 = 0.0754 |
| Largest diff. peak/hole / e Å-3 | 0.53/-0.48 |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| Br1 | 9141.9(3) | 2479.8(2) | 4167.7(2) | 26.84(8) |
| Br2 | 12102.9(3) | 2641.1(2) | 5179.1(3) | 29.82(9) |
| Zn1 | 9870.8(3) | 2228.0(2) | 5562.8(2) | 17.37(8) |
| Fe1 | 7927.9(4) | -2168.9(3) | 9120.6(3) | 18.83(10) |
| Fe2 | 6983.1(4) | 4245.2(3) | 8331.6(3) | 20.49(10) |
| Si1 | 9140.6(7) | 433.4(6) | 7607.5(6) | 15.40(17) |
| Si2 | 8167.3(7) | 2450.3(6) | 7354.2(6) | 15.77(17) |
| O1 | 9290.1(18) | 814.4(13) | 6465.9(14) | 17.5(4) |
| O2 | 8654.0(18) | 1337.8(13) | 7967.3(14) | 17.9(4) |
| O3 | 9129.4(17) | 3031.4(13) | 6302.1(14) | 17.4(4) |
| N1 | 7613(2) | -223.9(18) | 6192.2(18) | 20.5(5) |
| N2 | 10721(2) | 4232.5(18) | 6507.3(18) | 21.6(6) |
| C1 | 7878(3) | -627(2) | 8294(2) | 17.1(6) |
| C2 | 7296(3) | -1248(2) | 7957(2) | 19.4(6) |
| C3 | 6254(3) | -1866(2) | 8720(2) | 22.5(7) |
| C4 | 6200(3) | -1659(2) | 9535(2) | 24.1(7) |
| C5 | 7175(3) | -912(2) | 9279(2) | 19.9(6) |
| C6 | 9114(3) | -3149(2) | 8732(2) | 30.0(8) |
| C7 | 8117(3) | -3699(2) | 9561(2) | 28.1(8) |
| C8 | 8188(3) | -3396(2) | 10298(2) | 29.1(8) |
| C9 | 9219(3) | -2661(2) | 9931(3) | 32.6(8) |
| C10 | 9787(3) | -2511(2) | 8971(3) | 30.2(8) |
| C11 | 7699(3) | -1249(2) | 6971(2) | 22.0(7) |
| C12 | 8031(3) | -256(2) | 5226(2) | 29.8(8) |
| C13 | 6331(3) | 153(2) | 6350(2) | 31.0(8) |
| C14 | 10656(3) | 36.3(19) | 7936(2) | 17.0(6) |
| C15 | 11672(3) | -156(2) | 7301(2) | 26.0(7) |
| C16 | 12732(3) | -591(2) | 7597(3) | 32.3(8) |
| C17 | 12802(3) | -833(2) | 8526(3) | 32.2(8) |
| C18 | 11817(3) | -631(2) | 9167(2) | 30.4(8) |
| C19 | 10769(3) | -195(2) | 8860(2) | 23.6(7) |
| C20 | 8141(3) | 3168(2) | 8103(2) | 17.1(6) |
| C21 | 8861(3) | 4089(2) | 7876(2) | 20.3(6) |
| C22 | 8627(3) | 4276(2) | 8728(2) | 27.6(7) |
| C23 | 7759(3) | 3502(2) | 9473(2) | 28.4(7) |
| C24 | 7462(3) | 2820(2) | 9103(2) | 23.2(7) |
| C25 | 6152(4) | 4925(3) | 7220(3) | 45.7(10) |
| C26 | 6481(3) | 5636(3) | 7519(3) | 50.0(12) |
| C27 | 5829(4) | 5331(3) | 8511(3) | 47.1(11) |
| C28 | 5098(3) | 4423(3) | 8786(3) | 37.0(9) |
| C29 | 5309(3) | 4189(3) | 7994(3) | 38.7(9) |
| C30 | 9685(3) | 4775(2) | 6913(2) | 26.0(7) |
| C31 | 11467(3) | 3659(3) | 7200(2) | 32.9(8) |
| C32 | 11563(3) | 4975(2) | 5588(2) | 30.9(8) |
| C33 | 6540(3) | 2214(2) | 7282(2) | 20.0(6) |
| C34 | 6117(3) | 2716(2) | 6459(2) | 28.1(7) |
| C35 | 4885(3) | 2544(3) | 6440(3) | 37.5(9) |
| C36 | 4053(3) | 1849(3) | 7255(3) | 37.1(9) |
| C37 | 4448(3) | 1337(2) | 8081(3) | 32.8(8) |
| C38 | 5674(3) | 1510(2) | 8102(2) | 25.2(7) |
| O4 | 5400(4) | 2343(3) | 2672(5) | 157(3) |
| C39 | 5661(5) | 2795(5) | 3884(4) | 100(2) |
| C40 | 5978(5) | 2843(4) | 2912(5) | 68.3(16) |
| C41 | 7055(5) | 3581(4) | 2219(3) | 85.6(18) |
| Atom | U11 | U22 | U33 | U23 | U13 | U12 |
|---|---|---|---|---|---|---|
| Br1 | 39.1(2) | 22.25(16) | 20.50(17) | -7.25(14) | -12.48(14) | 1.76(13) |
| Br2 | 19.73(17) | 30.39(18) | 38.4(2) | -17.17(16) | -0.12(14) | -2.64(13) |
| Zn1 | 20.22(18) | 15.62(17) | 14.31(18) | -5.80(14) | -1.58(13) | 0.01(13) |
| Fe1 | 20.7(2) | 13.7(2) | 18.5(2) | -4.63(18) | -2.29(18) | -0.10(16) |
| Fe2 | 25.2(2) | 16.3(2) | 18.8(2) | -7.85(19) | -3.53(18) | 6.08(17) |
| Si1 | 18.8(4) | 12.5(4) | 14.3(4) | -5.7(3) | -3.0(3) | 1.3(3) |
| Si2 | 17.6(4) | 13.3(4) | 16.0(4) | -6.7(3) | -2.6(3) | 1.2(3) |
| O1 | 22.8(11) | 14.2(10) | 15(1) | -5.7(9) | -4.1(8) | -0.5(8) |
| O2 | 22.5(11) | 14.7(10) | 16.7(11) | -7.7(9) | -3.5(8) | 3.3(8) |
| O3 | 18.6(11) | 15.4(10) | 16.3(11) | -6.6(9) | -1.4(8) | 0.6(8) |
| N1 | 25.8(14) | 19.3(13) | 18.8(14) | -10.0(11) | -6.0(11) | -0.6(11) |
| N2 | 20.6(14) | 17.8(13) | 26.2(15) | -9.6(12) | -4.5(11) | -0.6(10) |
| C1 | 20.6(15) | 12.4(13) | 16.4(15) | -4.8(12) | -4.2(12) | 5.9(11) |
| C2 | 22.1(16) | 16.8(14) | 20.1(16) | -8.2(13) | -6.2(12) | 3.3(12) |
| C3 | 17.0(16) | 19.1(15) | 29.1(18) | -8.7(14) | -4.2(13) | 0.2(12) |
| C4 | 21.2(16) | 22.4(16) | 21.4(17) | -7.1(14) | 3.4(13) | 1.9(13) |
| C5 | 22.4(16) | 17.8(14) | 18.2(16) | -8.9(13) | -0.3(12) | 1.8(12) |
| C6 | 32.6(19) | 18.6(16) | 30.7(19) | -7.1(15) | -1.0(15) | 9.8(14) |
| C7 | 31.6(19) | 13.2(15) | 37(2) | -7.4(15) | -8.6(15) | 1.0(13) |
| C8 | 30.9(19) | 18.6(16) | 27.3(19) | 1.2(14) | -7.3(14) | -1.4(13) |
| C9 | 36(2) | 23.8(17) | 36(2) | -4.4(16) | -19.7(16) | 2.4(15) |
| C10 | 20.6(17) | 19.2(16) | 41(2) | -3.2(15) | -6.4(15) | 2.5(13) |
| C11 | 27.1(17) | 16.3(15) | 23.3(17) | -9.1(13) | -6.2(13) | 2.6(12) |
| C12 | 45(2) | 24.9(17) | 22.2(18) | -13.7(15) | -5.8(15) | -2.5(15) |
| C13 | 31.1(19) | 31.7(18) | 33(2) | -14.6(16) | -11.9(15) | 7.3(15) |
| C14 | 18.9(15) | 10.6(13) | 20.4(16) | -6.1(12) | -3.5(12) | -1.4(11) |
| C15 | 26.4(18) | 22.4(16) | 22.6(17) | -6.7(14) | 1.0(13) | -1.6(13) |
| C16 | 19.9(17) | 27.6(18) | 38(2) | -9.5(16) | 4.6(15) | 3.3(14) |
| C17 | 23.4(18) | 20.7(16) | 46(2) | -5.1(16) | -13.7(16) | 2.3(13) |
| C18 | 38(2) | 26.7(17) | 30.5(19) | -8.8(16) | -20.0(16) | 4.3(15) |
| C19 | 27.3(18) | 23.5(16) | 24.1(17) | -12.6(14) | -9.1(14) | 5.9(13) |
| C20 | 19.4(15) | 15.8(14) | 16.7(15) | -8.1(13) | -3.8(12) | 4.4(11) |
| C21 | 21.3(16) | 17.0(14) | 24.8(17) | -11.3(14) | -5.4(13) | 3.3(12) |
| C22 | 33.2(19) | 25.2(17) | 36(2) | -20.5(16) | -16.5(15) | 10.0(14) |
| C23 | 39(2) | 28.9(17) | 20.0(17) | -12.7(15) | -9.4(14) | 14.0(15) |
| C24 | 31.0(18) | 16.3(15) | 20.6(17) | -6.9(13) | -6.4(13) | 8.6(13) |
| C25 | 43(2) | 63(3) | 30(2) | -17(2) | -13.9(18) | 25(2) |
| C26 | 29(2) | 19.0(18) | 73(3) | 9(2) | -11(2) | 5.5(15) |
| C27 | 47(2) | 52(2) | 80(3) | -55(2) | -36(2) | 34(2) |
| C28 | 25.6(19) | 40(2) | 35(2) | -9.9(18) | -1.2(15) | 11.1(16) |
| C29 | 33(2) | 37(2) | 60(3) | -28(2) | -22.0(19) | 14.7(16) |
| C30 | 22.1(17) | 18.1(15) | 37(2) | -13.5(15) | -2.7(14) | 0.9(12) |
| C31 | 27.6(19) | 41(2) | 31(2) | -14.3(17) | -12.8(15) | 10.1(15) |
| C32 | 33.3(19) | 21.0(16) | 32(2) | -9.6(15) | 1.8(15) | -8.3(14) |
| C33 | 20.2(16) | 18.2(15) | 24.0(17) | -13.1(14) | -2.6(13) | 2.9(12) |
| C34 | 28.8(18) | 23.7(17) | 30.8(19) | -10.6(15) | -7.0(15) | 1.1(14) |
| C35 | 36(2) | 37(2) | 50(2) | -21.1(19) | -25.1(18) | 10.0(16) |
| C36 | 20.6(18) | 42(2) | 60(3) | -33(2) | -11.0(17) | 4.5(15) |
| C37 | 21.8(18) | 34.8(19) | 42(2) | -22.9(18) | 5.6(15) | -7.8(14) |
| C38 | 24.1(17) | 27.8(17) | 25.3(18) | -15.3(15) | -1.3(13) | -0.5(13) |
| O4 | 119(4) | 134(4) | 366(8) | -194(5) | -167(5) | 90(3) |
| C39 | 43(3) | 148(6) | 74(4) | -10(4) | -19(3) | 9(3) |
| C40 | 56(3) | 60(3) | 132(5) | -61(3) | -65(3) | 36(2) |
| C41 | 75(4) | 134(5) | 49(3) | -36(3) | -28(3) | 43(4) |
| Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
|---|---|---|---|---|---|---|
| Br1 | Zn1 | 2.4043(5) | C1 | C2 | 1.448(4) | |
| Br2 | Zn1 | 2.4001(4) | C1 | C5 | 1.436(4) | |
| Zn1 | O1 | 1.9683(18) | C2 | C3 | 1.433(4) | |
| Zn1 | O3 | 1.9763(18) | C2 | C11 | 1.499(4) | |
| Fe1 | C1 | 2.077(3) | C3 | C4 | 1.416(4) | |
| Fe1 | C2 | 2.040(3) | C4 | C5 | 1.411(4) | |
| Fe1 | C3 | 2.056(3) | C6 | C7 | 1.422(4) | |
| Fe1 | C4 | 2.047(3) | C6 | C10 | 1.419(5) | |
| Fe1 | C5 | 2.045(3) | C7 | C8 | 1.415(5) | |
| Fe1 | C6 | 2.053(3) | C8 | C9 | 1.415(4) | |
| Fe1 | C7 | 2.048(3) | C9 | C10 | 1.407(5) | |
| Fe1 | C8 | 2.046(3) | C14 | C15 | 1.395(4) | |
| Fe1 | C9 | 2.051(3) | C14 | C19 | 1.387(4) | |
| Fe1 | C10 | 2.050(3) | C15 | C16 | 1.387(4) | |
| Fe2 | C20 | 2.054(3) | C16 | C17 | 1.378(5) | |
| Fe2 | C21 | 2.032(3) | C17 | C18 | 1.387(5) | |
| Fe2 | C22 | 2.053(3) | C18 | C19 | 1.384(4) | |
| Fe2 | C23 | 2.052(3) | C20 | C21 | 1.442(4) | |
| Fe2 | C24 | 2.043(3) | C20 | C24 | 1.439(4) | |
| Fe2 | C25 | 2.041(4) | C21 | C22 | 1.431(4) | |
| Fe2 | C26 | 2.034(3) | C21 | C30 | 1.498(4) | |
| Fe2 | C27 | 2.038(3) | C22 | C23 | 1.407(4) | |
| Fe2 | C28 | 2.046(3) | C23 | C24 | 1.417(4) | |
| Fe2 | C29 | 2.044(4) | C25 | C26 | 1.386(6) | |
| Si1 | O1 | 1.612(2) | C25 | C29 | 1.385(5) | |
| Si1 | O2 | 1.6452(19) | C26 | C27 | 1.426(6) | |
| Si1 | C1 | 1.869(3) | C27 | C28 | 1.414(5) | |
| Si1 | C14 | 1.858(3) | C28 | C29 | 1.382(5) | |
| Si2 | O2 | 1.6485(19) | C33 | C34 | 1.386(4) | |
| Si2 | O3 | 1.614(2) | C33 | C38 | 1.409(4) | |
| Si2 | C20 | 1.855(3) | C34 | C35 | 1.389(4) | |
| Si2 | C33 | 1.865(3) | C35 | C36 | 1.383(5) | |
| N1 | C11 | 1.505(4) | C36 | C37 | 1.375(5) | |
| N1 | C12 | 1.490(4) | C37 | C38 | 1.386(4) | |
| N1 | C13 | 1.482(4) | O4 | C40 | 1.203(5) | |
| N2 | C30 | 1.508(4) | C39 | C40 | 1.450(7) | |
| N2 | C31 | 1.480(4) | C40 | C41 | 1.489(7) | |
| N2 | C32 | 1.493(4) |
| Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|
| Br2 | Zn1 | Br1 | 112.892(17) | O3 | Si2 | C20 | 110.16(12) | |
| O1 | Zn1 | Br1 | 104.44(6) | O3 | Si2 | C33 | 112.33(12) | |
| O1 | Zn1 | Br2 | 115.43(6) | C20 | Si2 | C33 | 111.24(13) | |
| O1 | Zn1 | O3 | 104.07(8) | Si1 | O1 | Zn1 | 121.07(11) | |
| O3 | Zn1 | Br1 | 117.36(6) | Si1 | O2 | Si2 | 128.44(13) | |
| O3 | Zn1 | Br2 | 102.78(6) | Si2 | O3 | Zn1 | 118.34(10) | |
| C2 | Fe1 | C1 | 41.18(11) | C12 | N1 | C11 | 110.2(2) | |
| C2 | Fe1 | C3 | 40.96(11) | C13 | N1 | C11 | 112.4(2) | |
| C2 | Fe1 | C4 | 68.49(12) | C13 | N1 | C12 | 111.4(3) | |
| C2 | Fe1 | C5 | 68.27(12) | C31 | N2 | C30 | 112.7(3) | |
| C2 | Fe1 | C6 | 108.30(13) | C31 | N2 | C32 | 110.7(3) | |
| C2 | Fe1 | C7 | 126.06(13) | C32 | N2 | C30 | 109.9(2) | |
| C2 | Fe1 | C8 | 163.01(12) | Si1 | C1 | Fe1 | 132.69(15) | |
| C2 | Fe1 | C9 | 155.29(12) | C2 | C1 | Fe1 | 68.05(15) | |
| C2 | Fe1 | C10 | 121.09(13) | C2 | C1 | Si1 | 129.6(2) | |
| C3 | Fe1 | C1 | 69.10(11) | C5 | C1 | Fe1 | 68.41(15) | |
| C4 | Fe1 | C1 | 68.85(11) | C5 | C1 | Si1 | 124.8(2) | |
| C4 | Fe1 | C3 | 40.37(12) | C5 | C1 | C2 | 105.3(2) | |
| C4 | Fe1 | C6 | 154.53(13) | C1 | C2 | Fe1 | 70.77(16) | |
| C4 | Fe1 | C7 | 119.51(12) | C1 | C2 | C11 | 126.2(3) | |
| C4 | Fe1 | C9 | 125.63(14) | C3 | C2 | Fe1 | 70.11(17) | |
| C4 | Fe1 | C10 | 163.01(14) | C3 | C2 | C1 | 108.9(3) | |
| C5 | Fe1 | C1 | 40.77(11) | C3 | C2 | C11 | 124.9(3) | |
| C5 | Fe1 | C3 | 67.90(12) | C11 | C2 | Fe1 | 125.5(2) | |
| C5 | Fe1 | C4 | 40.35(11) | C2 | C3 | Fe1 | 68.93(17) | |
| C5 | Fe1 | C6 | 164.00(12) | C4 | C3 | Fe1 | 69.48(17) | |
| C5 | Fe1 | C7 | 154.06(12) | C4 | C3 | C2 | 107.7(3) | |
| C5 | Fe1 | C8 | 119.89(13) | C3 | C4 | Fe1 | 70.15(16) | |
| C5 | Fe1 | C9 | 108.15(13) | C5 | C4 | Fe1 | 69.74(16) | |
| C5 | Fe1 | C10 | 126.73(12) | C5 | C4 | C3 | 108.2(3) | |
| C6 | Fe1 | C1 | 126.42(12) | C1 | C5 | Fe1 | 70.82(15) | |
| C6 | Fe1 | C3 | 120.52(13) | C4 | C5 | Fe1 | 69.92(16) | |
| C7 | Fe1 | C1 | 163.81(12) | C4 | C5 | C1 | 110.0(3) | |
| C7 | Fe1 | C3 | 107.51(12) | C7 | C6 | Fe1 | 69.52(17) | |
| C7 | Fe1 | C6 | 40.57(12) | C10 | C6 | Fe1 | 69.62(18) | |
| C7 | Fe1 | C9 | 68.08(13) | C10 | C6 | C7 | 107.4(3) | |
| C7 | Fe1 | C10 | 67.96(12) | C6 | C7 | Fe1 | 69.91(17) | |
| C8 | Fe1 | C1 | 154.33(13) | C8 | C7 | Fe1 | 69.71(17) | |
| C8 | Fe1 | C3 | 125.32(12) | C8 | C7 | C6 | 107.8(3) | |
| C8 | Fe1 | C4 | 107.26(13) | C7 | C8 | Fe1 | 69.84(18) | |
| C8 | Fe1 | C6 | 68.02(13) | C9 | C8 | Fe1 | 69.95(18) | |
| C8 | Fe1 | C7 | 40.45(13) | C9 | C8 | C7 | 108.3(3) | |
| C8 | Fe1 | C9 | 40.42(12) | C8 | C9 | Fe1 | 69.63(19) | |
| C8 | Fe1 | C10 | 67.68(13) | C10 | C9 | Fe1 | 69.89(19) | |
| C9 | Fe1 | C1 | 119.93(12) | C10 | C9 | C8 | 107.8(3) | |
| C9 | Fe1 | C3 | 162.41(13) | C6 | C10 | Fe1 | 69.90(18) | |
| C9 | Fe1 | C6 | 68.01(14) | C9 | C10 | Fe1 | 69.97(18) | |
| C10 | Fe1 | C1 | 108.24(12) | C9 | C10 | C6 | 108.6(3) | |
| C10 | Fe1 | C3 | 155.76(14) | C2 | C11 | N1 | 111.9(2) | |
| C10 | Fe1 | C6 | 40.47(13) | C15 | C14 | Si1 | 121.2(2) | |
| C10 | Fe1 | C9 | 40.14(13) | C19 | C14 | Si1 | 121.1(2) | |
| C21 | Fe2 | C20 | 41.33(11) | C19 | C14 | C15 | 117.3(3) | |
| C21 | Fe2 | C22 | 41.01(12) | C16 | C15 | C14 | 121.0(3) | |
| C21 | Fe2 | C23 | 68.53(12) | C17 | C16 | C15 | 120.3(3) | |
| C21 | Fe2 | C24 | 68.60(12) | C16 | C17 | C18 | 120.0(3) | |
| C21 | Fe2 | C25 | 112.87(14) | C19 | C18 | C17 | 119.0(3) | |
| C21 | Fe2 | C26 | 111.60(13) | C18 | C19 | C14 | 122.4(3) | |
| C21 | Fe2 | C27 | 138.69(14) | Si2 | C20 | Fe2 | 131.84(16) | |
| C21 | Fe2 | C28 | 179.20(13) | C21 | C20 | Fe2 | 68.54(15) | |
| C21 | Fe2 | C29 | 140.87(14) | C21 | C20 | Si2 | 129.4(2) | |
| C22 | Fe2 | C20 | 69.18(11) | C24 | C20 | Fe2 | 69.05(15) | |
| C23 | Fe2 | C20 | 69.14(12) | C24 | C20 | Si2 | 124.5(2) | |
| C23 | Fe2 | C22 | 40.08(13) | C24 | C20 | C21 | 105.7(2) | |
| C24 | Fe2 | C20 | 41.11(11) | C20 | C21 | Fe2 | 70.13(16) | |
| C24 | Fe2 | C22 | 67.86(12) | C20 | C21 | C30 | 127.0(3) | |
| C24 | Fe2 | C23 | 40.48(12) | C22 | C21 | Fe2 | 70.27(17) | |
| C24 | Fe2 | C28 | 112.06(13) | C22 | C21 | C20 | 108.5(3) | |
| C24 | Fe2 | C29 | 111.08(14) | C22 | C21 | C30 | 124.4(3) | |
| C25 | Fe2 | C20 | 110.21(14) | C30 | C21 | Fe2 | 123.7(2) | |
| C25 | Fe2 | C22 | 142.48(15) | C21 | C22 | Fe2 | 68.72(17) | |
| C25 | Fe2 | C23 | 177.24(15) | C23 | C22 | Fe2 | 69.90(19) | |
| C25 | Fe2 | C24 | 137.36(15) | C23 | C22 | C21 | 108.3(3) | |
| C25 | Fe2 | C28 | 67.01(15) | C22 | C23 | Fe2 | 70.02(18) | |
| C25 | Fe2 | C29 | 39.64(15) | C22 | C23 | C24 | 108.2(3) | |
| C26 | Fe2 | C20 | 137.20(15) | C24 | C23 | Fe2 | 69.44(18) | |
| C26 | Fe2 | C22 | 114.31(14) | C20 | C24 | Fe2 | 69.84(16) | |
| C26 | Fe2 | C23 | 142.41(16) | C23 | C24 | Fe2 | 70.08(17) | |
| C26 | Fe2 | C24 | 177.10(17) | C23 | C24 | C20 | 109.3(3) | |
| C26 | Fe2 | C25 | 39.76(16) | C26 | C25 | Fe2 | 69.9(2) | |
| C26 | Fe2 | C27 | 41.01(16) | C29 | C25 | Fe2 | 70.3(2) | |
| C26 | Fe2 | C28 | 67.76(14) | C29 | C25 | C26 | 108.3(4) | |
| C26 | Fe2 | C29 | 66.82(15) | C25 | C26 | Fe2 | 70.4(2) | |
| C27 | Fe2 | C20 | 178.00(15) | C25 | C26 | C27 | 108.0(3) | |
| C27 | Fe2 | C22 | 112.08(13) | C27 | C26 | Fe2 | 69.6(2) | |
| C27 | Fe2 | C23 | 112.85(14) | C26 | C27 | Fe2 | 69.34(19) | |
| C27 | Fe2 | C24 | 140.62(16) | C28 | C27 | Fe2 | 70.05(18) | |
| C27 | Fe2 | C25 | 67.82(16) | C28 | C27 | C26 | 106.4(3) | |
| C27 | Fe2 | C28 | 40.50(15) | C27 | C28 | Fe2 | 69.45(19) | |
| C27 | Fe2 | C29 | 67.32(14) | C29 | C28 | Fe2 | 70.2(2) | |
| C28 | Fe2 | C20 | 139.47(13) | C29 | C28 | C27 | 108.0(3) | |
| C28 | Fe2 | C22 | 138.64(14) | C25 | C29 | Fe2 | 70.1(2) | |
| C28 | Fe2 | C23 | 111.62(14) | C28 | C29 | Fe2 | 70.3(2) | |
| C29 | Fe2 | C20 | 111.48(12) | C28 | C29 | C25 | 109.2(3) | |
| C29 | Fe2 | C22 | 177.70(15) | C21 | C30 | N2 | 112.7(2) | |
| C29 | Fe2 | C23 | 137.83(15) | C34 | C33 | Si2 | 123.2(2) | |
| C29 | Fe2 | C28 | 39.51(14) | C34 | C33 | C38 | 117.3(3) | |
| O1 | Si1 | O2 | 111.04(10) | C38 | C33 | Si2 | 119.4(2) | |
| O1 | Si1 | C1 | 109.55(12) | C33 | C34 | C35 | 121.7(3) | |
| O1 | Si1 | C14 | 112.15(12) | C36 | C35 | C34 | 119.9(3) | |
| O2 | Si1 | C1 | 105.51(11) | C37 | C36 | C35 | 119.7(3) | |
| O2 | Si1 | C14 | 107.63(11) | C36 | C37 | C38 | 120.5(3) | |
| C14 | Si1 | C1 | 110.75(12) | C37 | C38 | C33 | 120.9(3) | |
| O2 | Si2 | C20 | 104.00(12) | O4 | C40 | C39 | 122.9(6) | |
| O2 | Si2 | C33 | 107.08(11) | O4 | C40 | C41 | 122.0(6) | |
| O3 | Si2 | O2 | 111.70(10) | C39 | C40 | C41 | 115.1(4) |
| D | H | A | d(D-H)/Å | d(H-A)/Å | d(D-A)/Å | D-H-A/° |
|---|---|---|---|---|---|---|
| N1 | H1 | O1 | 0.998(18) | 1.657(19) | 2.638(3) | 166(3) |
| N2 | H2 | O3 | 0.984(18) | 1.71(2) | 2.673(3) | 165(3) |
| A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|---|---|
| Fe1 | C1 | C2 | C3 | 60.0(2) | C3 | C2 | C11 | N1 | 118.9(3) | |
| Fe1 | C1 | C2 | C11 | -120.4(3) | C3 | C4 | C5 | Fe1 | -59.8(2) | |
| Fe1 | C1 | C5 | C4 | -59.1(2) | C3 | C4 | C5 | C1 | -0.2(3) | |
| Fe1 | C2 | C3 | C4 | 58.9(2) | C5 | C1 | C2 | Fe1 | -58.59(18) | |
| Fe1 | C2 | C11 | N1 | -151.8(2) | C5 | C1 | C2 | C3 | 1.4(3) | |
| Fe1 | C3 | C4 | C5 | 59.6(2) | C5 | C1 | C2 | C11 | -179.0(3) | |
| Fe1 | C4 | C5 | C1 | 59.7(2) | C6 | C7 | C8 | Fe1 | 59.8(2) | |
| Fe1 | C6 | C7 | C8 | -59.6(2) | C6 | C7 | C8 | C9 | 0.1(3) | |
| Fe1 | C6 | C10 | C9 | 59.5(2) | C7 | C6 | C10 | Fe1 | -59.5(2) | |
| Fe1 | C7 | C8 | C9 | -59.6(2) | C7 | C6 | C10 | C9 | 0.0(3) | |
| Fe1 | C8 | C9 | C10 | -59.7(2) | C7 | C8 | C9 | Fe1 | 59.5(2) | |
| Fe1 | C9 | C10 | C6 | -59.4(2) | C7 | C8 | C9 | C10 | -0.1(4) | |
| Fe2 | C20 | C21 | C22 | 60.1(2) | C8 | C9 | C10 | Fe1 | 59.5(2) | |
| Fe2 | C20 | C21 | C30 | -117.8(3) | C8 | C9 | C10 | C6 | 0.1(4) | |
| Fe2 | C20 | C24 | C23 | -59.1(2) | C10 | C6 | C7 | Fe1 | 59.5(2) | |
| Fe2 | C21 | C22 | C23 | 58.9(2) | C10 | C6 | C7 | C8 | -0.1(3) | |
| Fe2 | C21 | C30 | N2 | -147.2(2) | C11 | C2 | C3 | Fe1 | 120.0(3) | |
| Fe2 | C22 | C23 | C24 | 59.2(2) | C11 | C2 | C3 | C4 | 178.9(3) | |
| Fe2 | C23 | C24 | C20 | 59.0(2) | C12 | N1 | C11 | C2 | 179.6(2) | |
| Fe2 | C25 | C26 | C27 | -59.7(2) | C13 | N1 | C11 | C2 | -55.5(3) | |
| Fe2 | C25 | C29 | C28 | 59.6(2) | C14 | Si1 | O1 | Zn1 | -85.28(14) | |
| Fe2 | C26 | C27 | C28 | -60.6(2) | C14 | Si1 | O2 | Si2 | 131.26(16) | |
| Fe2 | C27 | C28 | C29 | -59.8(2) | C14 | Si1 | C1 | Fe1 | -12.8(2) | |
| Fe2 | C28 | C29 | C25 | -59.5(3) | C14 | Si1 | C1 | C2 | -108.7(3) | |
| Si1 | C1 | C2 | Fe1 | 128.0(2) | C14 | Si1 | C1 | C5 | 79.0(3) | |
| Si1 | C1 | C2 | C3 | -172.0(2) | C14 | C15 | C16 | C17 | -0.5(5) | |
| Si1 | C1 | C2 | C11 | 7.5(4) | C15 | C14 | C19 | C18 | -2.1(4) | |
| Si1 | C1 | C5 | Fe1 | -127.8(2) | C15 | C16 | C17 | C18 | -0.8(5) | |
| Si1 | C1 | C5 | C4 | 173.1(2) | C16 | C17 | C18 | C19 | 0.6(5) | |
| Si1 | C14 | C15 | C16 | -170.7(2) | C17 | C18 | C19 | C14 | 0.9(5) | |
| Si1 | C14 | C19 | C18 | 170.5(2) | C19 | C14 | C15 | C16 | 1.9(4) | |
| Si2 | C20 | C21 | Fe2 | 127.2(2) | C20 | Si2 | O2 | Si1 | -167.09(15) | |
| Si2 | C20 | C21 | C22 | -172.7(2) | C20 | Si2 | O3 | Zn1 | 155.77(12) | |
| Si2 | C20 | C21 | C30 | 9.5(5) | C20 | Si2 | C33 | C34 | 107.2(3) | |
| Si2 | C20 | C24 | Fe2 | -127.1(2) | C20 | Si2 | C33 | C38 | -71.4(2) | |
| Si2 | C20 | C24 | C23 | 173.8(2) | C20 | C21 | C22 | Fe2 | -60.0(2) | |
| Si2 | C33 | C34 | C35 | -178.0(2) | C20 | C21 | C22 | C23 | -1.1(3) | |
| Si2 | C33 | C38 | C37 | 178.3(2) | C20 | C21 | C30 | N2 | -57.7(4) | |
| O1 | Si1 | O2 | Si2 | 8.16(19) | C21 | C20 | C24 | Fe2 | 59.00(19) | |
| O1 | Si1 | C1 | Fe1 | 111.4(2) | C21 | C20 | C24 | C23 | -0.1(3) | |
| O1 | Si1 | C1 | C2 | 15.5(3) | C21 | C22 | C23 | Fe2 | -58.2(2) | |
| O1 | Si1 | C1 | C5 | -156.8(2) | C21 | C22 | C23 | C24 | 1.0(3) | |
| O1 | Si1 | C14 | C15 | -15.9(3) | C22 | C21 | C30 | N2 | 124.8(3) | |
| O1 | Si1 | C14 | C19 | 171.8(2) | C22 | C23 | C24 | Fe2 | -59.5(2) | |
| O2 | Si1 | O1 | Zn1 | 35.18(15) | C22 | C23 | C24 | C20 | -0.6(3) | |
| O2 | Si1 | C1 | Fe1 | -128.99(19) | C24 | C20 | C21 | Fe2 | -59.33(19) | |
| O2 | Si1 | C1 | C2 | 135.1(2) | C24 | C20 | C21 | C22 | 0.7(3) | |
| O2 | Si1 | C1 | C5 | -37.2(3) | C24 | C20 | C21 | C30 | -177.1(3) | |
| O2 | Si1 | C14 | C15 | -138.3(2) | C25 | C26 | C27 | Fe2 | 60.2(2) | |
| O2 | Si1 | C14 | C19 | 49.4(3) | C25 | C26 | C27 | C28 | -0.4(4) | |
| O2 | Si2 | O3 | Zn1 | 40.72(15) | C26 | C25 | C29 | Fe2 | -59.8(3) | |
| O2 | Si2 | C20 | Fe2 | -146.78(18) | C26 | C25 | C29 | C28 | -0.1(4) | |
| O2 | Si2 | C20 | C21 | 117.4(3) | C26 | C27 | C28 | Fe2 | 60.1(2) | |
| O2 | Si2 | C20 | C24 | -54.9(3) | C26 | C27 | C28 | C29 | 0.3(4) | |
| O2 | Si2 | C33 | C34 | -139.7(2) | C27 | C28 | C29 | Fe2 | 59.3(2) | |
| O2 | Si2 | C33 | C38 | 41.7(2) | C27 | C28 | C29 | C25 | -0.1(4) | |
| O3 | Si2 | O2 | Si1 | -48.31(18) | C29 | C25 | C26 | Fe2 | 60.0(3) | |
| O3 | Si2 | C20 | Fe2 | 93.4(2) | C29 | C25 | C26 | C27 | 0.3(4) | |
| O3 | Si2 | C20 | C21 | -2.4(3) | C30 | C21 | C22 | Fe2 | 117.9(3) | |
| O3 | Si2 | C20 | C24 | -174.7(2) | C30 | C21 | C22 | C23 | 176.8(3) | |
| O3 | Si2 | C33 | C34 | -16.8(3) | C31 | N2 | C30 | C21 | -51.5(3) | |
| O3 | Si2 | C33 | C38 | 164.6(2) | C32 | N2 | C30 | C21 | -175.6(3) | |
| C1 | Si1 | O1 | Zn1 | 151.33(12) | C33 | Si2 | O2 | Si1 | 75.06(18) | |
| C1 | Si1 | O2 | Si2 | -110.45(16) | C33 | Si2 | O3 | Zn1 | -79.62(14) | |
| C1 | Si1 | C14 | C15 | 106.9(2) | C33 | Si2 | C20 | Fe2 | -31.8(2) | |
| C1 | Si1 | C14 | C19 | -65.4(3) | C33 | Si2 | C20 | C21 | -127.6(3) | |
| C1 | C2 | C3 | Fe1 | -60.41(19) | C33 | Si2 | C20 | C24 | 60.0(3) | |
| C1 | C2 | C3 | C4 | -1.5(3) | C33 | C34 | C35 | C36 | -0.6(5) | |
| C1 | C2 | C11 | N1 | -60.6(4) | C34 | C33 | C38 | C37 | -0.4(4) | |
| C2 | C1 | C5 | Fe1 | 58.35(18) | C34 | C35 | C36 | C37 | 0.4(5) | |
| C2 | C1 | C5 | C4 | -0.8(3) | C35 | C36 | C37 | C38 | -0.2(5) | |
| C2 | C3 | C4 | Fe1 | -58.5(2) | C36 | C37 | C38 | C33 | 0.2(5) | |
| C2 | C3 | C4 | C5 | 1.0(3) | C38 | C33 | C34 | C35 | 0.6(4) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| H1 | 8210(30) | 260(20) | 6220(20) | 38(10) |
| H2 | 10250(30) | 3730(20) | 6420(30) | 54(11) |
| H3 | 5700 | -2331 | 8686 | 27 |
| H4 | 5608 | -1970 | 10147 | 29 |
| H5 | 7342 | -638 | 9698 | 24 |
| H6 | 9295 | -3200 | 8130 | 36 |
| H7 | 7512 | -4183 | 9610 | 34 |
| H8 | 7638 | -3643 | 10930 | 35 |
| H9 | 9481 | -2328 | 10273 | 39 |
| H10 | 10502 | -2058 | 8552 | 36 |
| H11A | 7154 | -1760 | 6944 | 26 |
| H11B | 8583 | -1447 | 6854 | 26 |
| H12A | 8891 | -487 | 5135 | 45 |
| H12B | 8025 | 425 | 4723 | 45 |
| H12C | 7452 | -727 | 5186 | 45 |
| H13A | 5718 | -314 | 6338 | 47 |
| H13B | 6329 | 830 | 5838 | 47 |
| H13C | 6098 | 193 | 6978 | 47 |
| H15 | 11637 | 13 | 6657 | 31 |
| H16 | 13411 | -722 | 7156 | 39 |
| H17 | 13524 | -1138 | 8728 | 39 |
| H18 | 11862 | -790 | 9807 | 36 |
| H19 | 10101 | -49 | 9297 | 28 |
| H22 | 8994 | 4828 | 8781 | 33 |
| H23 | 7429 | 3446 | 10114 | 34 |
| H24 | 6903 | 2226 | 9460 | 28 |
| H25 | 6453 | 4939 | 6592 | 55 |
| H26 | 7043 | 6224 | 7131 | 60 |
| H27 | 5876 | 5671 | 8907 | 57 |
| H28 | 4557 | 4040 | 9408 | 44 |
| H29 | 4935 | 3614 | 7982 | 46 |
| H30A | 10073 | 5342 | 6977 | 31 |
| H30B | 9153 | 5070 | 6454 | 31 |
| H31A | 11875 | 4129 | 7366 | 49 |
| H31B | 12117 | 3313 | 6905 | 49 |
| H31C | 10904 | 3154 | 7785 | 49 |
| H32A | 11052 | 5347 | 5141 | 46 |
| H32B | 12185 | 4610 | 5297 | 46 |
| H32C | 12005 | 5455 | 5723 | 46 |
| H34 | 6683 | 3191 | 5893 | 34 |
| H35 | 4616 | 2902 | 5868 | 45 |
| H36 | 3212 | 1725 | 7244 | 44 |
| H37 | 3876 | 860 | 8641 | 39 |
| H38 | 5935 | 1149 | 8678 | 30 |
| H39A | 5467 | 3471 | 3862 | 150 |
| H39B | 6380 | 2564 | 4166 | 150 |
| H39C | 4920 | 2317 | 4279 | 150 |
| H41A | 7298 | 3478 | 1621 | 128 |
| H41B | 7778 | 3475 | 2504 | 128 |
| H41C | 6798 | 4275 | 2076 | 128 |
Experimental
Single crystals of C41H50Br2Fe2N2O4Si2Zn [3075] 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 [3075]
Crystal Data for C41H50Br2Fe2N2O4Si2Zn (M =1027.90 g/mol): triclinic, space group P-1 (no. 2), a = 10.9344(4) Å, b = 14.4572(5) Å, c = 15.7160(6) Å, α = 65.850(4)°, β = 75.359(3)°, γ = 87.591(3)°, V = 2188.05(15) Å3, Z = 2, T = 173 K, μ(MoKα) = 3.120 mm-1, Dcalc = 1.560 g/cm3, 32328 reflections measured (4.628° ≤ 2Θ ≤ 53.994°), 9491 unique (Rint = 0.0481, Rsigma = 0.0530) which were used in all calculations. The final R1 was 0.0359 (I > 2σ(I)) and wR2 was 0.0754 (all data).
Refinement model description
Number of restraints - 2, 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. Restrained distances
N1-H1 = N2-H2
1 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
C11(H11A,H11B), C30(H30A,H30B)
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), C15(H15),
C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C24(H24), C25(H25),
C26(H26), C27(H27), C28(H28), C29(H29), C34(H34), C35(H35), C36(H36),
C37(H37), C38(H38)
3.c Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C31(H31A,H31B,H31C), C32(H32A,H32B,
H32C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C)
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.