| Identification code | 3111 |
| Empirical formula | C49H58Br2Fe4N2O4Si2Zn |
| Formula weight | 1243.74 |
| Temperature/K | 150 |
| Crystal system | monoclinic |
| Space group | P21/n |
| a/Å | 22.0084(17) |
| b/Å | 11.8011(5) |
| c/Å | 23.1333(18) |
| α/° | 90 |
| β/° | 115.664(9) |
| γ/° | 90 |
| Volume/Å3 | 5415.5(7) |
| Z | 4 |
| ρcalcg/cm3 | 1.525 |
| μ/mm‑1 | 3.044 |
| F(000) | 2520.0 |
| Crystal size/mm3 | 0.2 × 0.1 × 0.1 |
| Radiation | MoKα (λ = 0.71073) |
| 2Θ range for data collection/° | 4.84 to 51.998 |
| Index ranges | -28 ≤ h ≤ 17, -15 ≤ k ≤ 16, -28 ≤ l ≤ 31 |
| Reflections collected | 50421 |
| Independent reflections | 10638 [Rint = 0.0716, Rsigma = 0.0880] |
| Data/restraints/parameters | 10638/42/591 |
| Goodness-of-fit on F2 | 1.066 |
| Final R indexes [I>=2σ (I)] | R1 = 0.0563, wR2 = 0.1282 |
| Final R indexes [all data] | R1 = 0.0859, wR2 = 0.1390 |
| Largest diff. peak/hole / e Å-3 | 1.48/-0.67 |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| Br1 | 8972.7(3) | 40.5(4) | 7303.3(3) | 38.11(17) |
| Br2 | 8902.1(4) | 2424.9(5) | 8405.7(3) | 44.08(18) |
| Zn1 | 9083.7(3) | 2062.6(5) | 7469.5(3) | 25.41(16) |
| Fe1 | 11679.6(4) | 3171.4(6) | 6920.8(4) | 22.10(18) |
| Fe2 | 10436.7(5) | 5670.7(7) | 8347.7(5) | 42.5(2) |
| Fe3 | 7762.2(4) | 6390.8(6) | 5637.6(4) | 28.1(2) |
| Fe4 | 8530.2(4) | 1837.3(6) | 5092.0(4) | 28.0(2) |
| Si1 | 10178.7(7) | 3438.3(11) | 7193.0(7) | 19.5(3) |
| Si2 | 8704.8(7) | 3832.4(11) | 6324.2(7) | 21.2(3) |
| O1 | 8489.1(18) | 3040(3) | 6769.9(17) | 27.3(8) |
| O2 | 9975.2(17) | 2409(3) | 7532.1(16) | 23.4(8) |
| O3 | 9524.6(17) | 3991(3) | 6597.9(16) | 22.1(8) |
| N1 | 10795(2) | 662(4) | 7756(2) | 28.1(10) |
| N2 | 7500(3) | 4032(4) | 6983(2) | 36.3(12) |
| C0AA | 8381(3) | 3327(4) | 5487(3) | 23.9(12) |
| C1 | 10729(3) | 2799(4) | 6846(2) | 19.2(11) |
| C1AA | 9162(3) | 825(4) | 5813(3) | 35.3(14) |
| C2 | 11197(2) | 1875(4) | 7130(2) | 19.6(11) |
| C2AA | 8531(3) | 291(5) | 5486(3) | 41.6(16) |
| C3 | 11450(3) | 1509(4) | 6689(3) | 28.5(13) |
| C3AA | 8666(3) | 3530(4) | 5046(3) | 28.3(12) |
| C4 | 11159(3) | 2190(4) | 6138(2) | 25.3(12) |
| C4AA | 8961(3) | 627(4) | 4757(3) | 35.0(14) |
| C5 | 10718(3) | 2973(4) | 6232(2) | 24.4(12) |
| C5AA | 8227(3) | 3105(5) | 4427(3) | 39.1(15) |
| C6 | 12262(3) | 4132(6) | 7702(3) | 47.3(18) |
| C6AA | 9430(3) | 1030(5) | 5367(3) | 38.9(15) |
| C7 | 12665(3) | 3324(6) | 7562(4) | 61(2) |
| C7AA | 8411(3) | 169(4) | 4835(3) | 39.1(15) |
| C8 | 12577(3) | 3555(6) | 6927(4) | 53(2) |
| C8AA | 7668(3) | 2620(5) | 4482(3) | 46.0(18) |
| C9 | 12153(3) | 4474(5) | 6705(3) | 46.0(17) |
| C9AA | 7764(3) | 2748(4) | 5128(3) | 38.2(15) |
| C10 | 11962(3) | 4818(5) | 7168(3) | 41.7(16) |
| C11 | 10657(3) | 4519(5) | 7790(3) | 37.2(15) |
| C12 | 11036(4) | 4249(7) | 8468(4) | 72(3) |
| C13 | 11422(5) | 5073(8) | 8835(5) | 86(3) |
| C14 | 11362(3) | 5940(6) | 8416(4) | 57(2) |
| C15 | 10852(5) | 5648(6) | 7724(5) | 81(3) |
| C16 | 9427(3) | 5762(7) | 8039(3) | 57(2) |
| C17 | 9733(4) | 5333(6) | 8661(4) | 53.7(19) |
| C18 | 10195(4) | 6148(6) | 9053(4) | 54.3(19) |
| C19 | 10153(4) | 7072(5) | 8676(4) | 56(2) |
| C20 | 9683(4) | 6839(6) | 8047(4) | 60(2) |
| C21 | 8369(3) | 5279(4) | 6341(2) | 19.5(11) |
| C22 | 7753(3) | 5580(4) | 6395(3) | 26.0(12) |
| C23 | 7751(3) | 6770(5) | 6492(3) | 31.6(13) |
| C24 | 8331(3) | 7229(4) | 6471(3) | 31.1(13) |
| C25 | 8698(3) | 6328(4) | 6382(2) | 27.8(12) |
| C26 | 7415(3) | 5649(5) | 4763(3) | 40.4(15) |
| C27 | 7820(5) | 6517(9) | 4786(3) | 82(3) |
| C28 | 7591(8) | 7443(8) | 4905(5) | 129(5) |
| C29 | 6999(7) | 7278(10) | 4963(4) | 130(5) |
| C30 | 6882(4) | 6064(8) | 4865(3) | 68(2) |
| C31 | 11366(3) | 1374(4) | 7775(3) | 28.1(12) |
| C32 | 10629(3) | -287(4) | 7292(3) | 37.1(15) |
| C33 | 10933(3) | 241(5) | 8398(3) | 46.3(17) |
| C34 | 7233(3) | 4751(5) | 6381(3) | 37.4(15) |
| C35 | 7674(3) | 4708(5) | 7569(3) | 42.9(16) |
| C36 | 6993(3) | 3129(5) | 6936(3) | 48.3(17) |
| O4 | 10777(3) | 7406(4) | 6473(3) | 70.4(16) |
| C37 | 10264(4) | 7197(5) | 6024(3) | 38.9(15) |
| C38 | 10131(4) | 6042(5) | 5718(4) | 54.5(19) |
| C39 | 9710(4) | 8048(5) | 5750(3) | 51.2(18) |
| Atom | U11 | U22 | U33 | U23 | U13 | U12 |
|---|---|---|---|---|---|---|
| Br1 | 33.3(4) | 23.8(3) | 62.9(4) | 1.7(3) | 26.1(3) | -5.4(3) |
| Br2 | 42.9(4) | 50.4(4) | 51.8(4) | 0.9(3) | 32.7(3) | -3.0(3) |
| Zn1 | 17.2(3) | 23.6(3) | 37.8(4) | 5.7(3) | 14.2(3) | 0.9(3) |
| Fe1 | 13.0(4) | 20.3(4) | 32.8(4) | -1.5(3) | 9.8(3) | -2.0(3) |
| Fe2 | 34.3(5) | 41.3(5) | 60.3(6) | -30.6(4) | 28.4(5) | -13.8(4) |
| Fe3 | 30.4(5) | 18.7(4) | 30.4(4) | 2.4(3) | 8.7(4) | 4.6(3) |
| Fe4 | 23.1(4) | 19.8(4) | 34.4(5) | -4.7(3) | 6.1(4) | 0.6(3) |
| Si1 | 12.3(7) | 18.1(7) | 28.1(8) | -3.1(6) | 8.8(6) | -2.0(6) |
| Si2 | 15.2(8) | 18.3(7) | 30.7(8) | 1.8(6) | 10.6(6) | 2.4(6) |
| O1 | 19(2) | 26.3(19) | 41(2) | 9.6(16) | 17.0(18) | 5.4(16) |
| O2 | 13.4(19) | 24.7(18) | 29(2) | 5.5(15) | 6.6(16) | 3.4(15) |
| O3 | 19(2) | 19.2(17) | 32(2) | 1.9(14) | 14.6(17) | 4.4(15) |
| N1 | 18(2) | 27(2) | 36(3) | 16(2) | 9(2) | 10(2) |
| N2 | 27(3) | 41(3) | 50(3) | 12(2) | 26(3) | 8(2) |
| C0AA | 26(3) | 10(2) | 35(3) | 2(2) | 14(3) | 7(2) |
| C1 | 16(3) | 15(2) | 23(3) | 0.8(19) | 5(2) | -1(2) |
| C1AA | 30(4) | 25(3) | 37(3) | -1(2) | 2(3) | 11(3) |
| C2 | 10(3) | 18(2) | 25(3) | 1(2) | 2(2) | -1(2) |
| C2AA | 40(4) | 22(3) | 67(5) | 0(3) | 27(4) | 1(3) |
| C3 | 16(3) | 22(3) | 45(4) | -11(2) | 11(3) | -4(2) |
| C3AA | 31(3) | 19(2) | 35(3) | 0(2) | 14(3) | 5(2) |
| C4 | 22(3) | 28(3) | 23(3) | -8(2) | 8(2) | -2(2) |
| C4AA | 37(4) | 25(3) | 45(4) | -13(3) | 20(3) | 0(3) |
| C5 | 15(3) | 26(3) | 28(3) | -4(2) | 6(2) | -4(2) |
| C5AA | 48(4) | 29(3) | 34(4) | -3(3) | 12(3) | 7(3) |
| C6 | 39(4) | 60(4) | 40(4) | -14(3) | 15(3) | -32(4) |
| C6AA | 23(3) | 25(3) | 66(4) | -5(3) | 18(3) | 3(3) |
| C7 | 21(4) | 35(4) | 94(6) | 18(4) | -8(4) | -14(3) |
| C7AA | 26(3) | 22(3) | 59(4) | -16(3) | 9(3) | -4(3) |
| C8 | 27(4) | 55(4) | 90(6) | -29(4) | 39(4) | -18(3) |
| C8AA | 30(4) | 36(3) | 41(4) | -9(3) | -13(3) | 12(3) |
| C9 | 39(4) | 43(4) | 57(4) | -1(3) | 22(3) | -24(3) |
| C9AA | 24(3) | 23(3) | 60(4) | -1(3) | 11(3) | 1(3) |
| C10 | 23(3) | 27(3) | 74(5) | -18(3) | 20(3) | -16(3) |
| C11 | 23(3) | 44(3) | 52(4) | -28(3) | 22(3) | -10(3) |
| C12 | 36(4) | 94(6) | 64(5) | -47(5) | 0(4) | 24(4) |
| C13 | 60(6) | 93(7) | 106(8) | -44(6) | 38(6) | -12(5) |
| C14 | 36(4) | 56(4) | 93(6) | -56(4) | 39(4) | -37(4) |
| C15 | 108(7) | 57(5) | 139(8) | -59(5) | 110(7) | -49(5) |
| C16 | 19(3) | 104(6) | 42(4) | -29(4) | 10(3) | 3(4) |
| C17 | 61(5) | 47(4) | 77(6) | -19(4) | 53(5) | -11(4) |
| C18 | 55(5) | 64(5) | 52(4) | -12(4) | 30(4) | 10(4) |
| C19 | 73(6) | 33(4) | 74(5) | -26(4) | 43(5) | 1(4) |
| C20 | 69(6) | 46(4) | 60(5) | -5(4) | 22(4) | 14(4) |
| C21 | 16(3) | 19(2) | 24(3) | 2(2) | 9(2) | 0(2) |
| C22 | 18(3) | 25(3) | 37(3) | 7(2) | 14(3) | 7(2) |
| C23 | 28(3) | 32(3) | 29(3) | -2(2) | 6(3) | 13(3) |
| C24 | 34(4) | 22(3) | 33(3) | -5(2) | 10(3) | 4(3) |
| C25 | 24(3) | 26(3) | 34(3) | 1(2) | 13(3) | -1(2) |
| C26 | 50(4) | 35(3) | 20(3) | -5(2) | 0(3) | 11(3) |
| C27 | 81(6) | 131(7) | 35(4) | -1(5) | 26(4) | -56(6) |
| C28 | 232(13) | 43(4) | 39(5) | 25(4) | -10(8) | -36(6) |
| C29 | 160(10) | 119(7) | 35(5) | -20(5) | -29(6) | 128(7) |
| C30 | 29(4) | 126(7) | 35(4) | -4(4) | -1(3) | 2(4) |
| C31 | 19(3) | 27(3) | 33(3) | 2(2) | 5(2) | 0(2) |
| C32 | 26(3) | 18(3) | 63(4) | 2(3) | 16(3) | 2(2) |
| C33 | 35(4) | 48(4) | 51(4) | 22(3) | 14(3) | 3(3) |
| C34 | 26(3) | 36(3) | 58(4) | 13(3) | 26(3) | 12(3) |
| C35 | 40(4) | 52(4) | 46(4) | 8(3) | 28(3) | 8(3) |
| C36 | 43(4) | 41(4) | 71(5) | 10(3) | 34(4) | -1(3) |
| O4 | 40(3) | 59(3) | 77(4) | -10(3) | -7(3) | 3(3) |
| C37 | 45(4) | 30(3) | 35(4) | 1(3) | 12(3) | -2(3) |
| C38 | 61(5) | 35(3) | 79(5) | -16(3) | 42(4) | -12(4) |
| C39 | 50(5) | 29(3) | 64(5) | 6(3) | 15(4) | 6(3) |
| Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
|---|---|---|---|---|---|---|
| Br1 | Zn1 | 2.4126(8) | N1 | C31 | 1.496(7) | |
| Br2 | Zn1 | 2.4046(9) | N1 | C32 | 1.484(7) | |
| Zn1 | O1 | 1.956(3) | N1 | C33 | 1.468(7) | |
| Zn1 | O2 | 1.947(3) | N2 | C34 | 1.515(7) | |
| Fe1 | C1 | 2.070(5) | N2 | C35 | 1.474(8) | |
| Fe1 | C2 | 2.037(5) | N2 | C36 | 1.512(8) | |
| Fe1 | C3 | 2.039(5) | C0AA | C3AA | 1.431(7) | |
| Fe1 | C4 | 2.034(5) | C0AA | C9AA | 1.423(8) | |
| Fe1 | C5 | 2.038(5) | C1 | C2 | 1.446(7) | |
| Fe1 | C6 | 2.046(6) | C1 | C5 | 1.425(7) | |
| Fe1 | C7 | 2.037(6) | C1AA | C2AA | 1.409(8) | |
| Fe1 | C8 | 2.020(6) | C1AA | C6AA | 1.415(8) | |
| Fe1 | C9 | 2.038(6) | C2 | C3 | 1.427(7) | |
| Fe1 | C10 | 2.044(5) | C2 | C31 | 1.494(7) | |
| Fe2 | C11 | 2.070(5) | C2AA | C7AA | 1.419(9) | |
| Fe2 | C12 | 2.077(7) | C3 | C4 | 1.405(7) | |
| Fe2 | C13 | 2.086(10) | C3AA | C5AA | 1.428(8) | |
| Fe2 | C14 | 1.998(6) | C4 | C5 | 1.423(7) | |
| Fe2 | C15 | 2.014(7) | C4AA | C6AA | 1.421(8) | |
| Fe2 | C16 | 2.022(6) | C4AA | C7AA | 1.406(8) | |
| Fe2 | C17 | 2.014(7) | C5AA | C8AA | 1.413(9) | |
| Fe2 | C18 | 2.002(6) | C6 | C7 | 1.432(10) | |
| Fe2 | C19 | 2.028(6) | C6 | C10 | 1.383(9) | |
| Fe2 | C20 | 2.035(7) | C7 | C8 | 1.422(10) | |
| Fe3 | C21 | 2.066(5) | C8 | C9 | 1.376(9) | |
| Fe3 | C22 | 2.003(5) | C8AA | C9AA | 1.422(9) | |
| Fe3 | C23 | 2.038(5) | C9 | C10 | 1.372(9) | |
| Fe3 | C24 | 2.042(5) | C11 | C12 | 1.457(10) | |
| Fe3 | C25 | 2.034(6) | C11 | C15 | 1.427(9) | |
| Fe3 | C26 | 2.025(5) | C12 | C13 | 1.329(11) | |
| Fe3 | C27 | 2.035(7) | C13 | C14 | 1.375(12) | |
| Fe3 | C28 | 2.001(8) | C14 | C15 | 1.544(11) | |
| Fe3 | C29 | 2.021(8) | C16 | C17 | 1.393(10) | |
| Fe3 | C30 | 2.025(7) | C16 | C20 | 1.387(10) | |
| Fe4 | C0AA | 2.072(5) | C17 | C18 | 1.409(10) | |
| Fe4 | C1AA | 2.033(5) | C18 | C19 | 1.374(9) | |
| Fe4 | C2AA | 2.039(6) | C19 | C20 | 1.399(10) | |
| Fe4 | C3AA | 2.030(5) | C21 | C22 | 1.459(7) | |
| Fe4 | C4AA | 2.042(5) | C21 | C25 | 1.415(7) | |
| Fe4 | C5AA | 2.040(6) | C22 | C23 | 1.422(7) | |
| Fe4 | C6AA | 2.035(6) | C22 | C34 | 1.495(7) | |
| Fe4 | C7AA | 2.041(5) | C23 | C24 | 1.408(8) | |
| Fe4 | C8AA | 2.032(6) | C24 | C25 | 1.403(7) | |
| Fe4 | C9AA | 2.032(6) | C26 | C27 | 1.344(10) | |
| Si1 | O2 | 1.611(3) | C26 | C30 | 1.383(9) | |
| Si1 | O3 | 1.636(4) | C27 | C28 | 1.283(15) | |
| Si1 | C1 | 1.877(5) | C28 | C29 | 1.381(17) | |
| Si1 | C11 | 1.840(6) | C29 | C30 | 1.456(14) | |
| Si2 | O1 | 1.609(4) | O4 | C37 | 1.183(8) | |
| Si2 | O3 | 1.644(4) | C37 | C38 | 1.506(8) | |
| Si2 | C0AA | 1.849(5) | C37 | C39 | 1.492(9) | |
| Si2 | C21 | 1.868(5) |
| Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|
| Br2 | Zn1 | Br1 | 105.94(3) | C8AA | Fe4 | C5AA | 40.6(3) | |
| O1 | Zn1 | Br1 | 117.76(11) | C8AA | Fe4 | C6AA | 156.9(3) | |
| O1 | Zn1 | Br2 | 109.13(10) | C8AA | Fe4 | C7AA | 105.8(2) | |
| O2 | Zn1 | Br1 | 104.41(10) | C8AA | Fe4 | C9AA | 41.0(3) | |
| O2 | Zn1 | Br2 | 116.80(10) | C9AA | Fe4 | C0AA | 40.5(2) | |
| O2 | Zn1 | O1 | 103.24(14) | C9AA | Fe4 | C1AA | 124.2(3) | |
| C2 | Fe1 | C1 | 41.24(18) | C9AA | Fe4 | C2AA | 107.2(3) | |
| C2 | Fe1 | C3 | 41.0(2) | C9AA | Fe4 | C4AA | 156.2(2) | |
| C2 | Fe1 | C5 | 68.1(2) | C9AA | Fe4 | C5AA | 68.7(3) | |
| C2 | Fe1 | C6 | 113.5(2) | C9AA | Fe4 | C6AA | 161.4(3) | |
| C2 | Fe1 | C9 | 179.4(3) | C9AA | Fe4 | C7AA | 121.2(2) | |
| C2 | Fe1 | C10 | 140.7(2) | O2 | Si1 | O3 | 112.42(19) | |
| C3 | Fe1 | C1 | 69.4(2) | O2 | Si1 | C1 | 105.79(19) | |
| C3 | Fe1 | C6 | 139.0(3) | O2 | Si1 | C11 | 110.3(2) | |
| C3 | Fe1 | C10 | 177.0(2) | O3 | Si1 | C1 | 107.2(2) | |
| C4 | Fe1 | C1 | 69.2(2) | O3 | Si1 | C11 | 111.4(2) | |
| C4 | Fe1 | C2 | 68.5(2) | C11 | Si1 | C1 | 109.5(2) | |
| C4 | Fe1 | C3 | 40.3(2) | O1 | Si2 | O3 | 113.49(19) | |
| C4 | Fe1 | C5 | 40.9(2) | O1 | Si2 | C0AA | 113.4(2) | |
| C4 | Fe1 | C6 | 176.1(3) | O1 | Si2 | C21 | 106.8(2) | |
| C4 | Fe1 | C7 | 135.3(3) | O3 | Si2 | C0AA | 107.5(2) | |
| C4 | Fe1 | C9 | 111.2(2) | O3 | Si2 | C21 | 105.5(2) | |
| C4 | Fe1 | C10 | 140.9(3) | C0AA | Si2 | C21 | 109.9(2) | |
| C5 | Fe1 | C1 | 40.60(19) | Si2 | O1 | Zn1 | 126.6(2) | |
| C5 | Fe1 | C3 | 68.2(2) | Si1 | O2 | Zn1 | 127.3(2) | |
| C5 | Fe1 | C6 | 142.7(3) | Si1 | O3 | Si2 | 134.3(2) | |
| C5 | Fe1 | C10 | 114.5(2) | C32 | N1 | C31 | 112.7(4) | |
| C6 | Fe1 | C1 | 114.6(2) | C33 | N1 | C31 | 110.9(4) | |
| C7 | Fe1 | C1 | 143.0(3) | C33 | N1 | C32 | 110.8(4) | |
| C7 | Fe1 | C2 | 113.2(2) | C35 | N2 | C34 | 112.7(5) | |
| C7 | Fe1 | C3 | 109.9(2) | C35 | N2 | C36 | 109.7(5) | |
| C7 | Fe1 | C5 | 175.7(3) | C36 | N2 | C34 | 110.4(5) | |
| C7 | Fe1 | C6 | 41.1(3) | Si2 | C0AA | Fe4 | 132.3(3) | |
| C7 | Fe1 | C9 | 67.4(3) | C3AA | C0AA | Fe4 | 68.0(3) | |
| C7 | Fe1 | C10 | 67.3(3) | C3AA | C0AA | Si2 | 127.1(4) | |
| C8 | Fe1 | C1 | 176.0(3) | C9AA | C0AA | Fe4 | 68.2(3) | |
| C8 | Fe1 | C2 | 140.9(3) | C9AA | C0AA | Si2 | 127.2(4) | |
| C8 | Fe1 | C3 | 110.3(2) | C9AA | C0AA | C3AA | 105.4(5) | |
| C8 | Fe1 | C4 | 107.8(2) | Si1 | C1 | Fe1 | 134.0(3) | |
| C8 | Fe1 | C5 | 135.4(3) | C2 | C1 | Fe1 | 68.2(3) | |
| C8 | Fe1 | C6 | 68.5(3) | C2 | C1 | Si1 | 124.9(4) | |
| C8 | Fe1 | C7 | 41.0(3) | C5 | C1 | Fe1 | 68.5(3) | |
| C8 | Fe1 | C9 | 39.7(3) | C5 | C1 | Si1 | 129.2(4) | |
| C8 | Fe1 | C10 | 66.9(3) | C5 | C1 | C2 | 105.3(4) | |
| C9 | Fe1 | C1 | 138.2(2) | C2AA | C1AA | Fe4 | 70.0(3) | |
| C9 | Fe1 | C3 | 139.1(2) | C2AA | C1AA | C6AA | 108.0(5) | |
| C9 | Fe1 | C5 | 111.3(2) | C6AA | C1AA | Fe4 | 69.7(3) | |
| C9 | Fe1 | C6 | 66.9(3) | C1 | C2 | Fe1 | 70.6(3) | |
| C9 | Fe1 | C10 | 39.3(2) | C1 | C2 | C31 | 124.9(4) | |
| C10 | Fe1 | C1 | 113.5(2) | C3 | C2 | Fe1 | 69.6(3) | |
| C10 | Fe1 | C6 | 39.5(3) | C3 | C2 | C1 | 109.0(4) | |
| C11 | Fe2 | C12 | 41.1(3) | C3 | C2 | C31 | 126.1(5) | |
| C11 | Fe2 | C13 | 69.2(3) | C31 | C2 | Fe1 | 127.2(4) | |
| C12 | Fe2 | C13 | 37.2(3) | C1AA | C2AA | Fe4 | 69.5(3) | |
| C14 | Fe2 | C11 | 69.4(2) | C1AA | C2AA | C7AA | 107.7(6) | |
| C14 | Fe2 | C12 | 63.4(3) | C7AA | C2AA | Fe4 | 69.7(3) | |
| C14 | Fe2 | C13 | 39.3(3) | C2 | C3 | Fe1 | 69.4(3) | |
| C14 | Fe2 | C15 | 45.3(3) | C4 | C3 | Fe1 | 69.6(3) | |
| C14 | Fe2 | C16 | 161.1(4) | C4 | C3 | C2 | 108.0(5) | |
| C14 | Fe2 | C17 | 156.8(3) | C0AA | C3AA | Fe4 | 71.2(3) | |
| C14 | Fe2 | C18 | 120.7(3) | C5AA | C3AA | Fe4 | 69.8(3) | |
| C14 | Fe2 | C19 | 108.0(3) | C5AA | C3AA | C0AA | 109.9(5) | |
| C14 | Fe2 | C20 | 124.9(4) | C3 | C4 | Fe1 | 70.1(3) | |
| C15 | Fe2 | C11 | 40.9(3) | C3 | C4 | C5 | 107.9(5) | |
| C15 | Fe2 | C12 | 68.1(4) | C5 | C4 | Fe1 | 69.7(3) | |
| C15 | Fe2 | C13 | 72.2(4) | C6AA | C4AA | Fe4 | 69.3(3) | |
| C15 | Fe2 | C16 | 121.2(4) | C7AA | C4AA | Fe4 | 69.8(3) | |
| C15 | Fe2 | C19 | 126.0(3) | C7AA | C4AA | C6AA | 107.4(5) | |
| C15 | Fe2 | C20 | 108.7(4) | C1 | C5 | Fe1 | 70.9(3) | |
| C16 | Fe2 | C11 | 109.5(3) | C4 | C5 | Fe1 | 69.4(3) | |
| C16 | Fe2 | C12 | 128.9(3) | C4 | C5 | C1 | 109.8(4) | |
| C16 | Fe2 | C13 | 159.3(4) | C3AA | C5AA | Fe4 | 69.1(3) | |
| C16 | Fe2 | C19 | 67.6(3) | C8AA | C5AA | Fe4 | 69.4(3) | |
| C16 | Fe2 | C20 | 40.0(3) | C8AA | C5AA | C3AA | 106.8(5) | |
| C17 | Fe2 | C11 | 121.2(2) | C7 | C6 | Fe1 | 69.1(4) | |
| C17 | Fe2 | C12 | 109.5(4) | C10 | C6 | Fe1 | 70.2(3) | |
| C17 | Fe2 | C13 | 121.4(4) | C10 | C6 | C7 | 106.9(6) | |
| C17 | Fe2 | C15 | 155.9(3) | C1AA | C6AA | Fe4 | 69.6(3) | |
| C17 | Fe2 | C16 | 40.4(3) | C1AA | C6AA | C4AA | 108.2(5) | |
| C17 | Fe2 | C19 | 67.5(3) | C4AA | C6AA | Fe4 | 69.9(3) | |
| C17 | Fe2 | C20 | 67.4(3) | C6 | C7 | Fe1 | 69.8(4) | |
| C18 | Fe2 | C11 | 155.3(3) | C8 | C7 | Fe1 | 68.9(4) | |
| C18 | Fe2 | C12 | 119.7(3) | C8 | C7 | C6 | 106.6(6) | |
| C18 | Fe2 | C13 | 103.6(3) | C2AA | C7AA | Fe4 | 69.6(3) | |
| C18 | Fe2 | C15 | 161.7(3) | C4AA | C7AA | Fe4 | 69.9(3) | |
| C18 | Fe2 | C16 | 68.5(3) | C4AA | C7AA | C2AA | 108.7(5) | |
| C18 | Fe2 | C17 | 41.1(3) | C7 | C8 | Fe1 | 70.1(4) | |
| C18 | Fe2 | C19 | 39.9(3) | C9 | C8 | Fe1 | 70.8(4) | |
| C18 | Fe2 | C20 | 67.9(3) | C9 | C8 | C7 | 107.7(6) | |
| C19 | Fe2 | C11 | 164.1(3) | C5AA | C8AA | Fe4 | 70.0(4) | |
| C19 | Fe2 | C12 | 152.8(3) | C5AA | C8AA | C9AA | 108.2(5) | |
| C19 | Fe2 | C13 | 119.3(3) | C9AA | C8AA | Fe4 | 69.5(3) | |
| C19 | Fe2 | C20 | 40.3(3) | C8 | C9 | Fe1 | 69.5(4) | |
| C20 | Fe2 | C11 | 127.5(3) | C10 | C9 | Fe1 | 70.6(3) | |
| C20 | Fe2 | C12 | 165.9(3) | C10 | C9 | C8 | 109.2(6) | |
| C20 | Fe2 | C13 | 156.5(3) | C0AA | C9AA | Fe4 | 71.3(3) | |
| C22 | Fe3 | C21 | 41.98(19) | C8AA | C9AA | Fe4 | 69.5(3) | |
| C22 | Fe3 | C23 | 41.2(2) | C8AA | C9AA | C0AA | 109.6(6) | |
| C22 | Fe3 | C24 | 68.9(2) | C6 | C10 | Fe1 | 70.3(3) | |
| C22 | Fe3 | C25 | 68.5(2) | C9 | C10 | Fe1 | 70.1(3) | |
| C22 | Fe3 | C26 | 121.6(2) | C9 | C10 | C6 | 109.6(6) | |
| C22 | Fe3 | C27 | 155.6(4) | Si1 | C11 | Fe2 | 135.3(3) | |
| C22 | Fe3 | C29 | 127.0(5) | C12 | C11 | Fe2 | 69.7(3) | |
| C22 | Fe3 | C30 | 108.2(3) | C12 | C11 | Si1 | 122.0(5) | |
| C23 | Fe3 | C21 | 69.6(2) | C15 | C11 | Fe2 | 67.5(3) | |
| C23 | Fe3 | C24 | 40.4(2) | C15 | C11 | Si1 | 131.9(6) | |
| C24 | Fe3 | C21 | 69.0(2) | C15 | C11 | C12 | 105.1(6) | |
| C25 | Fe3 | C21 | 40.38(19) | C11 | C12 | Fe2 | 69.2(4) | |
| C25 | Fe3 | C23 | 67.7(2) | C13 | C12 | Fe2 | 71.8(5) | |
| C25 | Fe3 | C24 | 40.3(2) | C13 | C12 | C11 | 115.9(9) | |
| C25 | Fe3 | C27 | 110.9(3) | C12 | C13 | Fe2 | 71.0(5) | |
| C26 | Fe3 | C21 | 110.3(2) | C12 | C13 | C14 | 104.8(9) | |
| C26 | Fe3 | C23 | 155.0(3) | C14 | C13 | Fe2 | 66.9(5) | |
| C26 | Fe3 | C24 | 164.5(3) | C13 | C14 | Fe2 | 73.8(5) | |
| C26 | Fe3 | C25 | 129.4(2) | C13 | C14 | C15 | 111.6(6) | |
| C26 | Fe3 | C27 | 38.7(3) | C15 | C14 | Fe2 | 67.9(3) | |
| C26 | Fe3 | C30 | 39.9(3) | C11 | C15 | Fe2 | 71.7(4) | |
| C27 | Fe3 | C21 | 121.2(4) | C11 | C15 | C14 | 102.4(7) | |
| C27 | Fe3 | C23 | 162.9(3) | C14 | C15 | Fe2 | 66.8(4) | |
| C27 | Fe3 | C24 | 127.5(3) | C17 | C16 | Fe2 | 69.5(4) | |
| C28 | Fe3 | C21 | 151.8(5) | C20 | C16 | Fe2 | 70.5(4) | |
| C28 | Fe3 | C22 | 165.3(5) | C20 | C16 | C17 | 108.0(6) | |
| C28 | Fe3 | C23 | 127.5(4) | C16 | C17 | Fe2 | 70.1(4) | |
| C28 | Fe3 | C24 | 108.2(3) | C16 | C17 | C18 | 107.9(7) | |
| C28 | Fe3 | C25 | 119.3(5) | C18 | C17 | Fe2 | 69.0(4) | |
| C28 | Fe3 | C26 | 64.6(3) | C17 | C18 | Fe2 | 69.9(4) | |
| C28 | Fe3 | C27 | 37.1(4) | C19 | C18 | Fe2 | 71.1(4) | |
| C28 | Fe3 | C29 | 40.2(5) | C19 | C18 | C17 | 107.6(7) | |
| C28 | Fe3 | C30 | 67.2(4) | C18 | C19 | Fe2 | 69.1(4) | |
| C29 | Fe3 | C21 | 167.1(5) | C18 | C19 | C20 | 108.7(7) | |
| C29 | Fe3 | C23 | 106.2(3) | C20 | C19 | Fe2 | 70.1(4) | |
| C29 | Fe3 | C24 | 116.3(3) | C16 | C20 | Fe2 | 69.5(4) | |
| C29 | Fe3 | C25 | 150.5(4) | C16 | C20 | C19 | 107.9(7) | |
| C29 | Fe3 | C26 | 68.0(3) | C19 | C20 | Fe2 | 69.6(4) | |
| C29 | Fe3 | C27 | 66.1(5) | Si2 | C21 | Fe3 | 133.7(3) | |
| C29 | Fe3 | C30 | 42.2(4) | C22 | C21 | Fe3 | 66.7(3) | |
| C30 | Fe3 | C21 | 128.3(3) | C22 | C21 | Si2 | 128.0(4) | |
| C30 | Fe3 | C23 | 119.3(3) | C25 | C21 | Fe3 | 68.6(3) | |
| C30 | Fe3 | C24 | 152.5(3) | C25 | C21 | Si2 | 127.2(4) | |
| C30 | Fe3 | C25 | 166.2(3) | C25 | C21 | C22 | 104.4(4) | |
| C30 | Fe3 | C27 | 66.2(3) | C21 | C22 | Fe3 | 71.3(3) | |
| C1AA | Fe4 | C0AA | 108.6(2) | C21 | C22 | C34 | 124.7(5) | |
| C1AA | Fe4 | C2AA | 40.5(2) | C23 | C22 | Fe3 | 70.7(3) | |
| C1AA | Fe4 | C4AA | 68.6(2) | C23 | C22 | C21 | 108.7(5) | |
| C1AA | Fe4 | C5AA | 159.0(3) | C23 | C22 | C34 | 126.5(5) | |
| C1AA | Fe4 | C6AA | 40.7(2) | C34 | C22 | Fe3 | 126.2(4) | |
| C1AA | Fe4 | C7AA | 68.2(2) | C22 | C23 | Fe3 | 68.1(3) | |
| C2AA | Fe4 | C0AA | 122.1(2) | C24 | C23 | Fe3 | 70.0(3) | |
| C2AA | Fe4 | C4AA | 68.4(2) | C24 | C23 | C22 | 108.0(5) | |
| C2AA | Fe4 | C5AA | 158.4(3) | C23 | C24 | Fe3 | 69.7(3) | |
| C2AA | Fe4 | C7AA | 40.7(2) | C25 | C24 | Fe3 | 69.5(3) | |
| C3AA | Fe4 | C0AA | 40.8(2) | C25 | C24 | C23 | 107.6(5) | |
| C3AA | Fe4 | C1AA | 123.9(2) | C21 | C25 | Fe3 | 71.0(3) | |
| C3AA | Fe4 | C2AA | 158.8(2) | C24 | C25 | Fe3 | 70.2(3) | |
| C3AA | Fe4 | C4AA | 124.5(2) | C24 | C25 | C21 | 111.2(5) | |
| C3AA | Fe4 | C5AA | 41.1(2) | C27 | C26 | Fe3 | 71.1(4) | |
| C3AA | Fe4 | C6AA | 109.4(2) | C27 | C26 | C30 | 108.8(7) | |
| C3AA | Fe4 | C7AA | 159.7(2) | C30 | C26 | Fe3 | 70.0(4) | |
| C3AA | Fe4 | C8AA | 68.3(2) | C26 | C27 | Fe3 | 70.3(4) | |
| C3AA | Fe4 | C9AA | 68.0(2) | C28 | C27 | Fe3 | 70.0(6) | |
| C4AA | Fe4 | C0AA | 161.6(2) | C28 | C27 | C26 | 109.9(10) | |
| C5AA | Fe4 | C0AA | 69.4(2) | C27 | C28 | Fe3 | 72.9(5) | |
| C5AA | Fe4 | C4AA | 106.3(2) | C27 | C28 | C29 | 112.1(9) | |
| C5AA | Fe4 | C7AA | 122.0(2) | C29 | C28 | Fe3 | 70.7(6) | |
| C6AA | Fe4 | C0AA | 125.3(2) | C28 | C29 | Fe3 | 69.1(5) | |
| C6AA | Fe4 | C2AA | 68.2(2) | C28 | C29 | C30 | 103.5(8) | |
| C6AA | Fe4 | C4AA | 40.8(2) | C30 | C29 | Fe3 | 69.1(4) | |
| C6AA | Fe4 | C5AA | 122.4(3) | C26 | C30 | Fe3 | 70.0(4) | |
| C6AA | Fe4 | C7AA | 68.0(2) | C26 | C30 | C29 | 105.6(8) | |
| C7AA | Fe4 | C0AA | 157.2(2) | C29 | C30 | Fe3 | 68.7(5) | |
| C7AA | Fe4 | C4AA | 40.3(2) | C2 | C31 | N1 | 110.4(4) | |
| C8AA | Fe4 | C0AA | 69.0(2) | C22 | C34 | N2 | 111.0(5) | |
| C8AA | Fe4 | C1AA | 159.7(3) | O4 | C37 | C38 | 121.3(6) | |
| C8AA | Fe4 | C2AA | 122.5(3) | O4 | C37 | C39 | 121.8(6) | |
| C8AA | Fe4 | C4AA | 120.1(3) | C39 | C37 | C38 | 116.9(6) |
| D | H | A | d(D-H)/Å | d(H-A)/Å | d(D-A)/Å | D-H-A/° |
|---|---|---|---|---|---|---|
| N1 | H1 | O2 | 0.99(2) | 1.70(3) | 2.639(5) | 156(6) |
| N2 | H2 | O1 | 1.00(2) | 1.75(4) | 2.698(6) | 158(8) |
| A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|---|---|
| Fe1 | C1 | C2 | C3 | -59.2(3) | C1 | C2 | C3 | Fe1 | 59.8(3) | |
| Fe1 | C1 | C2 | C31 | 122.3(5) | C1 | C2 | C3 | C4 | 0.7(6) | |
| Fe1 | C1 | C5 | C4 | 58.6(4) | C1 | C2 | C31 | N1 | 73.9(6) | |
| Fe1 | C2 | C3 | C4 | -59.1(4) | C1AA | C2AA | C7AA | Fe4 | -59.4(4) | |
| Fe1 | C2 | C31 | N1 | 165.1(3) | C1AA | C2AA | C7AA | C4AA | -0.2(6) | |
| Fe1 | C3 | C4 | C5 | -59.7(4) | C2 | C1 | C5 | Fe1 | -58.5(3) | |
| Fe1 | C4 | C5 | C1 | -59.5(4) | C2 | C1 | C5 | C4 | 0.1(5) | |
| Fe1 | C6 | C7 | C8 | 59.3(4) | C2 | C3 | C4 | Fe1 | 59.0(3) | |
| Fe1 | C6 | C10 | C9 | -59.3(4) | C2 | C3 | C4 | C5 | -0.7(6) | |
| Fe1 | C7 | C8 | C9 | 61.2(4) | C2AA | C1AA | C6AA | Fe4 | 59.7(4) | |
| Fe1 | C8 | C9 | C10 | 59.6(4) | C2AA | C1AA | C6AA | C4AA | 0.3(6) | |
| Fe1 | C9 | C10 | C6 | 59.4(4) | C3 | C2 | C31 | N1 | -104.3(6) | |
| Fe2 | C11 | C12 | C13 | -56.2(6) | C3 | C4 | C5 | Fe1 | 59.9(4) | |
| Fe2 | C11 | C15 | C14 | 60.1(4) | C3 | C4 | C5 | C1 | 0.4(6) | |
| Fe2 | C12 | C13 | C14 | -58.7(6) | C3AA | C0AA | C9AA | Fe4 | 58.1(3) | |
| Fe2 | C13 | C14 | C15 | -57.6(5) | C3AA | C0AA | C9AA | C8AA | -1.0(6) | |
| Fe2 | C14 | C15 | C11 | -63.6(4) | C3AA | C5AA | C8AA | Fe4 | -59.2(4) | |
| Fe2 | C16 | C17 | C18 | 58.9(5) | C3AA | C5AA | C8AA | C9AA | 0.1(6) | |
| Fe2 | C16 | C20 | C19 | -59.2(5) | C5 | C1 | C2 | Fe1 | 58.8(3) | |
| Fe2 | C17 | C18 | C19 | 61.4(5) | C5 | C1 | C2 | C3 | -0.5(5) | |
| Fe2 | C18 | C19 | C20 | 59.1(5) | C5 | C1 | C2 | C31 | -178.9(5) | |
| Fe2 | C19 | C20 | C16 | 59.2(5) | C5AA | C8AA | C9AA | Fe4 | -59.6(4) | |
| Fe3 | C21 | C22 | C23 | -61.1(4) | C5AA | C8AA | C9AA | C0AA | 0.6(6) | |
| Fe3 | C21 | C22 | C34 | 121.7(5) | C6 | C7 | C8 | Fe1 | -59.9(4) | |
| Fe3 | C21 | C25 | C24 | 58.8(4) | C6 | C7 | C8 | C9 | 1.3(7) | |
| Fe3 | C22 | C23 | C24 | -58.8(4) | C6AA | C1AA | C2AA | Fe4 | -59.6(4) | |
| Fe3 | C22 | C34 | N2 | 161.1(4) | C6AA | C1AA | C2AA | C7AA | -0.1(6) | |
| Fe3 | C23 | C24 | C25 | -59.4(4) | C6AA | C4AA | C7AA | Fe4 | 59.4(4) | |
| Fe3 | C24 | C25 | C21 | -59.3(4) | C6AA | C4AA | C7AA | C2AA | 0.4(6) | |
| Fe3 | C26 | C27 | C28 | -58.9(6) | C7 | C6 | C10 | Fe1 | 59.6(4) | |
| Fe3 | C26 | C30 | C29 | 59.9(5) | C7 | C6 | C10 | C9 | 0.3(7) | |
| Fe3 | C27 | C28 | C29 | -60.1(8) | C7 | C8 | C9 | Fe1 | -60.7(4) | |
| Fe3 | C28 | C29 | C30 | -61.0(6) | C7 | C8 | C9 | C10 | -1.1(7) | |
| Fe3 | C29 | C30 | C26 | -60.7(5) | C7AA | C4AA | C6AA | Fe4 | -59.7(4) | |
| Fe4 | C0AA | C3AA | C5AA | 59.3(4) | C7AA | C4AA | C6AA | C1AA | -0.5(6) | |
| Fe4 | C0AA | C9AA | C8AA | -59.1(4) | C8 | C9 | C10 | Fe1 | -58.9(4) | |
| Fe4 | C1AA | C2AA | C7AA | 59.5(4) | C8 | C9 | C10 | C6 | 0.5(7) | |
| Fe4 | C1AA | C6AA | C4AA | -59.4(4) | C9AA | C0AA | C3AA | Fe4 | -58.2(3) | |
| Fe4 | C2AA | C7AA | C4AA | 59.2(4) | C9AA | C0AA | C3AA | C5AA | 1.1(6) | |
| Fe4 | C3AA | C5AA | C8AA | 59.4(4) | C10 | C6 | C7 | Fe1 | -60.3(4) | |
| Fe4 | C4AA | C6AA | C1AA | 59.2(4) | C10 | C6 | C7 | C8 | -1.0(7) | |
| Fe4 | C4AA | C7AA | C2AA | -58.9(4) | C11 | Si1 | O2 | Zn1 | 107.3(3) | |
| Fe4 | C5AA | C8AA | C9AA | 59.3(4) | C11 | Si1 | O3 | Si2 | -115.7(3) | |
| Fe4 | C8AA | C9AA | C0AA | 60.2(4) | C11 | Si1 | C1 | Fe1 | -7.9(4) | |
| Si1 | C1 | C2 | Fe1 | -129.3(4) | C11 | Si1 | C1 | C2 | 84.6(5) | |
| Si1 | C1 | C2 | C3 | 171.5(4) | C11 | Si1 | C1 | C5 | -105.4(5) | |
| Si1 | C1 | C2 | C31 | -6.9(7) | C11 | C12 | C13 | Fe2 | 54.9(5) | |
| Si1 | C1 | C5 | Fe1 | 130.0(4) | C11 | C12 | C13 | C14 | -3.8(9) | |
| Si1 | C1 | C5 | C4 | -171.4(4) | C12 | C11 | C15 | Fe2 | -59.9(4) | |
| Si1 | C11 | C12 | Fe2 | -131.5(4) | C12 | C11 | C15 | C14 | 0.2(6) | |
| Si1 | C11 | C12 | C13 | 172.3(6) | C12 | C13 | C14 | Fe2 | 61.4(6) | |
| Si1 | C11 | C15 | Fe2 | 131.4(5) | C12 | C13 | C14 | C15 | 3.8(9) | |
| Si1 | C11 | C15 | C14 | -168.4(5) | C13 | C14 | C15 | Fe2 | 61.1(6) | |
| Si2 | C0AA | C3AA | Fe4 | 127.2(4) | C13 | C14 | C15 | C11 | -2.5(8) | |
| Si2 | C0AA | C3AA | C5AA | -173.5(4) | C15 | C11 | C12 | Fe2 | 58.4(4) | |
| Si2 | C0AA | C9AA | Fe4 | -127.3(4) | C15 | C11 | C12 | C13 | 2.2(9) | |
| Si2 | C0AA | C9AA | C8AA | 173.6(4) | C16 | C17 | C18 | Fe2 | -59.5(5) | |
| Si2 | C21 | C22 | Fe3 | -128.2(4) | C16 | C17 | C18 | C19 | 1.9(8) | |
| Si2 | C21 | C22 | C23 | 170.7(4) | C17 | C16 | C20 | Fe2 | 59.7(5) | |
| Si2 | C21 | C22 | C34 | -6.5(8) | C17 | C16 | C20 | C19 | 0.5(8) | |
| Si2 | C21 | C25 | Fe3 | 129.3(4) | C17 | C18 | C19 | Fe2 | -60.7(5) | |
| Si2 | C21 | C25 | C24 | -171.9(4) | C17 | C18 | C19 | C20 | -1.6(8) | |
| O1 | Si2 | O3 | Si1 | 6.1(4) | C18 | C19 | C20 | Fe2 | -58.5(5) | |
| O1 | Si2 | C0AA | Fe4 | -60.9(4) | C18 | C19 | C20 | C16 | 0.7(8) | |
| O1 | Si2 | C0AA | C3AA | -153.9(4) | C20 | C16 | C17 | Fe2 | -60.3(5) | |
| O1 | Si2 | C0AA | C9AA | 32.5(5) | C20 | C16 | C17 | C18 | -1.5(8) | |
| O1 | Si2 | C21 | Fe3 | -125.8(3) | C21 | Si2 | O1 | Zn1 | -128.5(3) | |
| O1 | Si2 | C21 | C22 | -32.8(5) | C21 | Si2 | O3 | Si1 | 122.7(3) | |
| O1 | Si2 | C21 | C25 | 139.0(4) | C21 | Si2 | C0AA | Fe4 | 179.7(3) | |
| O2 | Si1 | O3 | Si2 | 8.6(4) | C21 | Si2 | C0AA | C3AA | 86.6(5) | |
| O2 | Si1 | C1 | Fe1 | -126.8(3) | C21 | Si2 | C0AA | C9AA | -86.9(5) | |
| O2 | Si1 | C1 | C2 | -34.3(5) | C21 | C22 | C23 | Fe3 | 61.5(4) | |
| O2 | Si1 | C1 | C5 | 135.7(4) | C21 | C22 | C23 | C24 | 2.8(6) | |
| O2 | Si1 | C11 | Fe2 | -68.3(5) | C21 | C22 | C34 | N2 | 69.7(7) | |
| O2 | Si1 | C11 | C12 | 24.6(6) | C22 | C21 | C25 | Fe3 | -57.4(3) | |
| O2 | Si1 | C11 | C15 | -168.3(6) | C22 | C21 | C25 | C24 | 1.4(6) | |
| O3 | Si1 | O2 | Zn1 | -17.6(3) | C22 | C23 | C24 | Fe3 | 57.6(4) | |
| O3 | Si1 | C1 | Fe1 | 113.0(3) | C22 | C23 | C24 | C25 | -1.8(6) | |
| O3 | Si1 | C1 | C2 | -154.4(4) | C23 | C22 | C34 | N2 | -107.0(6) | |
| O3 | Si1 | C1 | C5 | 15.5(5) | C23 | C24 | C25 | Fe3 | 59.5(4) | |
| O3 | Si1 | C11 | Fe2 | 57.3(5) | C23 | C24 | C25 | C21 | 0.2(6) | |
| O3 | Si1 | C11 | C12 | 150.1(5) | C25 | C21 | C22 | Fe3 | 58.6(3) | |
| O3 | Si1 | C11 | C15 | -42.8(7) | C25 | C21 | C22 | C23 | -2.5(6) | |
| O3 | Si2 | O1 | Zn1 | -12.7(3) | C25 | C21 | C22 | C34 | -179.7(5) | |
| O3 | Si2 | C0AA | Fe4 | 65.4(4) | C26 | C27 | C28 | Fe3 | 59.1(6) | |
| O3 | Si2 | C0AA | C3AA | -27.7(5) | C26 | C27 | C28 | C29 | -1.0(12) | |
| O3 | Si2 | C0AA | C9AA | 158.8(4) | C27 | C26 | C30 | Fe3 | -60.8(5) | |
| O3 | Si2 | C21 | Fe3 | 113.2(3) | C27 | C26 | C30 | C29 | -0.9(8) | |
| O3 | Si2 | C21 | C22 | -153.8(4) | C27 | C28 | C29 | Fe3 | 61.4(7) | |
| O3 | Si2 | C21 | C25 | 17.9(5) | C27 | C28 | C29 | C30 | 0.4(12) | |
| C0AA | Si2 | O1 | Zn1 | 110.4(3) | C28 | C29 | C30 | Fe3 | 61.0(6) | |
| C0AA | Si2 | O3 | Si1 | -120.1(3) | C28 | C29 | C30 | C26 | 0.3(9) | |
| C0AA | Si2 | C21 | Fe3 | -2.4(4) | C30 | C26 | C27 | Fe3 | 60.1(5) | |
| C0AA | Si2 | C21 | C22 | 90.6(5) | C30 | C26 | C27 | C28 | 1.2(9) | |
| C0AA | Si2 | C21 | C25 | -97.7(5) | C31 | C2 | C3 | Fe1 | -121.8(5) | |
| C0AA | C3AA | C5AA | Fe4 | -60.1(4) | C31 | C2 | C3 | C4 | 179.1(5) | |
| C0AA | C3AA | C5AA | C8AA | -0.8(6) | C32 | N1 | C31 | C2 | 59.7(6) | |
| C1 | Si1 | O2 | Zn1 | -134.3(3) | C33 | N1 | C31 | C2 | -175.4(4) | |
| C1 | Si1 | O3 | Si2 | 124.5(3) | C34 | C22 | C23 | Fe3 | -121.4(6) | |
| C1 | Si1 | C11 | Fe2 | 175.7(4) | C34 | C22 | C23 | C24 | 179.9(5) | |
| C1 | Si1 | C11 | C12 | -91.4(5) | C35 | N2 | C34 | C22 | 62.1(6) | |
| C1 | Si1 | C11 | C15 | 75.7(7) | C36 | N2 | C34 | C22 | -174.9(5) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| H1 | 10400(20) | 1160(40) | 7620(30) | 60(20) |
| H2 | 7940(20) | 3720(70) | 7020(40) | 110(30) |
| H1AA | 9370 | 1014 | 6256 | 42 |
| H2AA | 8240 | 56 | 5668 | 50 |
| H3 | 11762 | 909 | 6755 | 34 |
| H3AA | 9085 | 3895 | 5150 | 34 |
| H4 | 11241 | 2138 | 5769 | 30 |
| H4AA | 9009 | 660 | 4369 | 42 |
| H5 | 10455 | 3529 | 5930 | 29 |
| H5AA | 8297 | 3142 | 4050 | 47 |
| H6 | 12211 | 4186 | 8088 | 57 |
| H6AA | 9851 | 1378 | 5458 | 47 |
| H7 | 12938 | 2746 | 7838 | 74 |
| H7AA | 8023 | -167 | 4506 | 47 |
| H8 | 12775 | 3148 | 6697 | 63 |
| H8AA | 7292 | 2268 | 4146 | 55 |
| H9 | 12016 | 4816 | 6295 | 55 |
| H9AA | 7462 | 2488 | 5293 | 46 |
| H10 | 11667 | 5433 | 7128 | 50 |
| H12 | 11008 | 3527 | 8637 | 86 |
| H13 | 11683 | 5066 | 9287 | 103 |
| H14 | 11604 | 6634 | 8538 | 69 |
| H15 | 10706 | 6103 | 7350 | 97 |
| H16 | 9101 | 5384 | 7674 | 68 |
| H17 | 9645 | 4617 | 8796 | 64 |
| H18 | 10485 | 6072 | 9497 | 65 |
| H19 | 10402 | 7755 | 8818 | 67 |
| H20 | 9560 | 7332 | 7689 | 72 |
| H23 | 7416 | 7182 | 6560 | 38 |
| H24 | 8452 | 8007 | 6510 | 37 |
| H25 | 9113 | 6410 | 6352 | 33 |
| H26 | 7484 | 4878 | 4690 | 48 |
| H27 | 8218 | 6454 | 4723 | 99 |
| H28 | 7804 | 8159 | 4948 | 155 |
| H29 | 6731 | 7826 | 5048 | 155 |
| H30 | 6515 | 5644 | 4869 | 82 |
| H31A | 11460 | 1989 | 8094 | 34 |
| H31B | 11777 | 903 | 7910 | 34 |
| H32A | 10451 | 16 | 6855 | 56 |
| H32B | 10289 | -775 | 7332 | 56 |
| H32C | 11037 | -730 | 7382 | 56 |
| H33A | 11307 | -301 | 8539 | 69 |
| H33B | 10530 | -134 | 8385 | 69 |
| H33C | 11054 | 878 | 8699 | 69 |
| H34A | 7102 | 4254 | 6001 | 45 |
| H34B | 6826 | 5165 | 6343 | 45 |
| H35A | 7278 | 5139 | 7532 | 64 |
| H35B | 8040 | 5232 | 7624 | 64 |
| H35C | 7819 | 4201 | 7941 | 64 |
| H36A | 6583 | 3489 | 6915 | 73 |
| H36B | 7186 | 2637 | 7314 | 73 |
| H36C | 6883 | 2676 | 6548 | 73 |
| H38A | 10561 | 5661 | 5819 | 82 |
| H38B | 9879 | 6121 | 5252 | 82 |
| H38C | 9867 | 5593 | 5884 | 82 |
| H39A | 9775 | 8639 | 6069 | 77 |
| H39B | 9276 | 7672 | 5635 | 77 |
| H39C | 9715 | 8389 | 5366 | 77 |
| Number | X | Y | Z | Volume | Electron count | Content |
|---|---|---|---|---|---|---|
| 1 | 0.000 | 0.018 | 0.000 | 412.4 | 27.7 | ? |
| 2 | 0.500 | -0.251 | 0.500 | 412.4 | 27.7 | ? |
Experimental
Single crystals of C49H58Br2Fe4N2O4Si2Zn [3111] were []. A suitable crystal was selected and [] on a Xcalibur, Sapphire3 diffractometer. The crystal was kept at 150 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 ShelXL [3] refinement package using Least Squares minimisation.
Crystal structure determination of [3111]
Crystal Data for C49H58Br2Fe4N2O4Si2Zn (M =1243.74 g/mol): monoclinic, space group P21/n (no. 14), a = 22.0084(17) Å, b = 11.8011(5) Å, c = 23.1333(18) Å, β = 115.664(9)°, V = 5415.5(7) Å3, Z = 4, T = 150 K, μ(MoKα) = 3.044 mm-1, Dcalc = 1.525 g/cm3, 50421 reflections measured (4.84° ≤ 2Θ ≤ 51.998°), 10638 unique (Rint = 0.0716, Rsigma = 0.0880) which were used in all calculations. The final R1 was 0.0563 (I > 2σ(I)) and wR2 was 0.1390 (all data).
Refinement model description
Number of restraints - 42, 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. Rigid bond restraints
C26, C27, C28, C29, C30
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C29) ≈ Ueq, Uanis(C28) ≈ Ueq, Uanis(C27) ≈ Ueq, Uanis(C26)
≈ Ueq, Uanis(C30) ≈ Ueq: with sigma of 0.1 and sigma for terminal atoms
of 0.2
5.a Secondary CH2 refined with riding coordinates:
C31(H31A,H31B), C34(H34A,H34B)
5.b Aromatic/amide H refined with riding coordinates:
C1AA(H1AA), C2AA(H2AA), C3(H3), C3AA(H3AA), C4(H4), C4AA(H4AA), C5(H5),
C5AA(H5AA), C6(H6), C6AA(H6AA), C7(H7), C7AA(H7AA), C8(H8), C8AA(H8AA), C9(H9),
C9AA(H9AA), C10(H10), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16),
C17(H17), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C25(H25), C26(H26),
C27(H27), C28(H28), C29(H29), C30(H30)
5.c Idealised Me refined as rotating group:
C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,
H36C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C)
This report has been created with Olex2, compiled on 2015.01.26 svn.r3150 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.