| Identification code | 3113 |
| Empirical formula | C55H74Br4Fe4N4O5Si2Zn2 |
| Formula weight | 1601.14 |
| Temperature/K | 173 |
| Crystal system | monoclinic |
| Space group | C2/c |
| a/Å | 47.515(3) |
| b/Å | 10.31587(19) |
| c/Å | 33.897(2) |
| α/° | 90 |
| β/° | 132.838(10) |
| γ/° | 90 |
| Volume/Å3 | 12183.5(18) |
| Z | 8 |
| ρcalcg/cm3 | 1.746 |
| μ/mm‑1 | 4.414 |
| F(000) | 6432.0 |
| Crystal size/mm3 | 0.2 × 0.2 × 0.1 |
| Radiation | MoKα (λ = 0.71073) |
| 2Θ range for data collection/° | 4.676 to 56 |
| Index ranges | -62 ≤ h ≤ 62, -13 ≤ k ≤ 13, -44 ≤ l ≤ 43 |
| Reflections collected | 155041 |
| Independent reflections | 14607 [Rint = 0.0441, Rsigma = 0.0233] |
| Data/restraints/parameters | 14607/4/709 |
| Goodness-of-fit on F2 | 1.046 |
| Final R indexes [I>=2σ (I)] | R1 = 0.0432, wR2 = 0.1153 |
| Final R indexes [all data] | R1 = 0.0562, wR2 = 0.1243 |
| Largest diff. peak/hole / e Å-3 | 1.70/-0.58 |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| Br1 | 726.1(2) | 2207.3(4) | 6714.0(2) | 46.54(11) |
| Br2 | 748.5(2) | 1111.8(4) | 7878.1(2) | 44.62(11) |
| Zn1 | 849.0(2) | 2798.3(4) | 7511.3(2) | 31.67(10) |
| Fe1 | 1415.0(2) | 7495.7(5) | 7714.6(2) | 27.95(11) |
| Fe2 | -198.2(2) | 7784.4(5) | 6205.4(2) | 36.28(13) |
| Si1 | 588.9(3) | 5662.3(9) | 7140.3(4) | 28.02(18) |
| O1 | 537.8(7) | 4300(2) | 7323.6(10) | 30.8(5) |
| O2 | 580.7(8) | 5411(3) | 6653.3(11) | 38.9(6) |
| N1 | 1430.5(8) | 3326(3) | 8076.4(12) | 33.1(6) |
| N2 | -207.0(9) | 3787(3) | 6651.5(14) | 44.5(8) |
| C1 | 1058.2(9) | 6395(3) | 7720.8(13) | 28.1(6) |
| C2 | 1426.9(9) | 5778(3) | 8014.7(13) | 27.7(6) |
| C3 | 1720.7(10) | 6620(4) | 8441.4(14) | 32.5(7) |
| C4 | 1542.3(11) | 7755(4) | 8415.5(15) | 34.0(7) |
| C5 | 1139.6(10) | 7619(3) | 7981.8(14) | 31.1(7) |
| C6 | 1137.8(12) | 7827(5) | 6931.3(16) | 48(1) |
| C7 | 1474.1(12) | 7092(4) | 7187.9(16) | 41.1(9) |
| C8 | 1792.8(11) | 7840(3) | 7628.4(15) | 33.9(7) |
| C9 | 1645.3(11) | 9025(4) | 7632.6(16) | 37.8(8) |
| C10 | 1244.1(13) | 9017(4) | 7207.7(18) | 47.6(10) |
| C11 | 1510.3(10) | 4495(3) | 7899.0(15) | 33.2(7) |
| C12 | 1566.0(14) | 3530(4) | 8614.0(16) | 49.8(10) |
| C13 | 1641.2(12) | 2212(4) | 8108.8(19) | 49.5(10) |
| C14 | 166.9(10) | 6660(3) | 6883.8(14) | 33.0(7) |
| C15 | -218(1) | 6142(4) | 6507.7(14) | 34.7(7) |
| C16 | -476.1(11) | 7071(4) | 6426.0(16) | 40.1(8) |
| C17 | -260.3(11) | 8173(4) | 6736.5(17) | 47.9(10) |
| C18 | 132.4(11) | 7933(4) | 7016.5(16) | 41.9(9) |
| C19 | 4.8(15) | 7727(6) | 5833(2) | 65.3(15) |
| C20 | -376.9(15) | 7326(5) | 5477.8(19) | 55.2(11) |
| C21 | -599.7(13) | 8335(5) | 5416.9(17) | 53.8(11) |
| C22 | -360.8(18) | 9378(5) | 5731(2) | 70.8(16) |
| C23 | 22.1(17) | 8986(7) | 5997(2) | 79(2) |
| C24 | -326.6(11) | 4837(4) | 6251.2(15) | 39.0(8) |
| C25 | -257.9(15) | 2486(4) | 6436(2) | 71.7(17) |
| C26 | -409.1(14) | 3940(6) | 6844(2) | 71.1(17) |
| Br3 | -2337.8(2) | 10819.0(4) | 3953.8(2) | 48.71(11) |
| Br4 | -1228.7(2) | 12088.2(4) | 4944.8(2) | 44.11(10) |
| Zn2 | -1657.7(2) | 10369.5(4) | 4667.0(2) | 32.27(10) |
| Fe3 | -1985.3(2) | 5661.0(5) | 4916.0(2) | 30.01(11) |
| Fe4 | -1845.6(2) | 5376.6(5) | 3373.6(2) | 34.94(12) |
| Si2 | -1757.0(3) | 7492.2(9) | 4266.0(4) | 28.25(19) |
| O3 | -1546.9(7) | 8892(2) | 4449.3(10) | 31.1(5) |
| O4 | -2223.2(7) | 7701(2) | 3759.4(10) | 35.0(5) |
| N3 | -1585.2(8) | 9761(3) | 5319.2(12) | 31.9(6) |
| N4 | -1435.9(9) | 9434(3) | 3801.2(13) | 36.1(7) |
| C27 | -1648.7(9) | 6701(3) | 4849.7(13) | 28.8(6) |
| C28 | -1662.2(10) | 7308(3) | 5223.9(14) | 30.0(7) |
| C29 | -1515.8(10) | 6406(4) | 5647.0(14) | 33.6(7) |
| C30 | -1418(1) | 5238(4) | 5539.2(14) | 33.2(7) |
| C31 | -1496.6(10) | 5423(3) | 5058.6(14) | 32.3(7) |
| C32 | -2531.3(11) | 5657(4) | 4174.0(16) | 42.7(9) |
| C33 | -2526.3(10) | 6178(4) | 4565.6(15) | 38.0(8) |
| C34 | -2378.6(11) | 5223(4) | 4966.2(17) | 41.6(9) |
| C35 | -2294.9(12) | 4109(4) | 4821.6(19) | 48.1(10) |
| C36 | -2386.4(12) | 4377(4) | 4333.7(19) | 50.8(11) |
| C37 | -1826.2(10) | 8599(3) | 5180.1(15) | 33.6(7) |
| C38 | -1175.4(11) | 9522(4) | 5797.5(15) | 38.4(8) |
| C39 | -1723.6(12) | 10841(4) | 5437.9(18) | 42.8(9) |
| C40 | -1560.6(10) | 6560(3) | 4026.7(14) | 31.4(7) |
| C41 | -1558.3(11) | 7088(3) | 3631.9(14) | 33.8(7) |
| C42 | -1373.8(11) | 6181(4) | 3553.1(15) | 38.4(8) |
| C43 | -1262.2(11) | 5098(4) | 3885.2(15) | 38.1(8) |
| C44 | -1372.0(11) | 5325(4) | 4178.8(15) | 36.0(8) |
| C45 | -2378.9(14) | 5125(6) | 3109(3) | 70.9(17) |
| C46 | -2404.6(14) | 5689(5) | 2716(3) | 82(2) |
| C47 | -2233.2(14) | 4828(5) | 2589.3(19) | 60.5(13) |
| C48 | -2110.4(12) | 3742(4) | 2921.9(18) | 44.9(9) |
| C49 | -2201.1(14) | 3946(5) | 3236(2) | 57.1(12) |
| C50 | -1698.6(11) | 8396(4) | 3387.1(15) | 38.2(8) |
| C51 | -1035.6(12) | 9307(4) | 4040.1(19) | 48(1) |
| C52 | -1592.0(13) | 10749(4) | 3572.0(17) | 44.3(9) |
| O5 | -641(2) | 2371(7) | 4414(3) | 145(2) |
| C53 | -197(4) | 3596(11) | 5297(4) | 215(8) |
| C54 | -334(2) | 2410(9) | 4916(4) | 101(2) |
| C55 | -49(3) | 1551(14) | 5145(4) | 171(5) |
| Atom | U11 | U22 | U33 | U23 | U13 | U12 |
|---|---|---|---|---|---|---|
| Br1 | 60.8(3) | 40.5(2) | 39.8(2) | -1.08(16) | 34.8(2) | 6.27(18) |
| Br2 | 61.3(3) | 29.25(18) | 55.9(2) | 5.37(16) | 44.8(2) | 1.84(16) |
| Zn1 | 33.4(2) | 27.0(2) | 34.7(2) | 1.88(15) | 23.18(19) | 2.04(15) |
| Fe1 | 27.7(2) | 27.9(2) | 28.9(2) | 1.44(18) | 19.5(2) | 0.46(18) |
| Fe2 | 28.2(3) | 31.3(3) | 36.2(3) | 5.3(2) | 16.7(2) | 1.83(19) |
| Si1 | 27.5(4) | 26.9(4) | 28.9(4) | 0.6(3) | 18.8(4) | 0.3(3) |
| O1 | 30.1(12) | 27.1(11) | 34.9(12) | 2.3(9) | 21.9(11) | 1.1(9) |
| O2 | 52.2(16) | 33.3(14) | 38.3(14) | -0.4(11) | 33.6(13) | 0.8(12) |
| N1 | 33.9(15) | 26.5(14) | 33.5(15) | 3.0(11) | 20.8(13) | 3.9(12) |
| N2 | 29.9(16) | 37.6(17) | 48.4(19) | 9.4(14) | 19.6(15) | -2.3(13) |
| C1 | 31.0(17) | 27.2(16) | 30.7(16) | 0.8(12) | 22.8(15) | -0.2(12) |
| C2 | 29.1(16) | 27.8(16) | 27.0(15) | 3.0(12) | 19.4(14) | 0.5(12) |
| C3 | 28.6(17) | 35.4(18) | 29.1(16) | 2.8(14) | 17.8(15) | -0.4(14) |
| C4 | 35.8(18) | 36.1(18) | 32.9(17) | -3.2(14) | 24.5(16) | -4.7(14) |
| C5 | 30.6(17) | 33.6(17) | 32.1(17) | -1.2(13) | 22.5(15) | 0.0(13) |
| C6 | 37(2) | 67(3) | 29.0(18) | 9.4(18) | 18.4(17) | -9.8(19) |
| C7 | 57(2) | 41(2) | 43(2) | -9.0(16) | 41(2) | -11.1(17) |
| C8 | 35.1(18) | 36.1(18) | 38.5(18) | 1.0(14) | 28.1(17) | -1.2(14) |
| C9 | 47(2) | 29.9(17) | 45(2) | 1.9(15) | 34.3(19) | -2.5(15) |
| C10 | 46(2) | 48(2) | 52(2) | 19.9(19) | 35(2) | 11.9(18) |
| C11 | 27.6(16) | 31.9(17) | 35.5(18) | 3.5(14) | 19.6(15) | 4.6(13) |
| C12 | 62(3) | 38(2) | 33.1(19) | 4.0(16) | 26(2) | -5.6(19) |
| C13 | 38(2) | 33(2) | 60(3) | 0.3(18) | 27(2) | 6.3(16) |
| C14 | 32.4(17) | 32.4(17) | 29.3(16) | 4.0(13) | 19.0(15) | 3.7(14) |
| C15 | 32.0(18) | 35.7(18) | 32.7(17) | 3.1(14) | 20.5(16) | 0.3(14) |
| C16 | 30.5(18) | 44(2) | 40(2) | 4.3(16) | 21.6(17) | 5.0(15) |
| C17 | 35(2) | 50(2) | 46(2) | 1.6(18) | 22.4(19) | 13.5(17) |
| C18 | 32.8(19) | 41(2) | 36.5(19) | -1.3(16) | 17.6(17) | 6.2(15) |
| C19 | 49(3) | 85(4) | 66(3) | 44(3) | 41(3) | 25(3) |
| C20 | 70(3) | 53(3) | 49(2) | 7(2) | 43(3) | 0(2) |
| C21 | 36(2) | 76(3) | 37(2) | 18(2) | 20.0(18) | 11(2) |
| C22 | 92(4) | 41(3) | 60(3) | 21(2) | 44(3) | 16(3) |
| C23 | 60(3) | 91(4) | 52(3) | 17(3) | 24(3) | -32(3) |
| C24 | 32.4(18) | 36.6(19) | 36.9(19) | 4.3(15) | 19.2(16) | -1.9(15) |
| C25 | 49(3) | 36(2) | 68(3) | 2(2) | 15(2) | -10(2) |
| C26 | 41(2) | 99(4) | 72(3) | 41(3) | 38(3) | 7(3) |
| Br3 | 34.1(2) | 40.2(2) | 46.6(2) | -2.43(17) | 17.43(18) | 8.44(16) |
| Br4 | 44.9(2) | 29.61(18) | 50.7(2) | -0.16(15) | 29.7(2) | -5.06(15) |
| Zn2 | 33.0(2) | 27.0(2) | 34.3(2) | -0.76(15) | 21.96(18) | 1.62(15) |
| Fe3 | 28.9(2) | 28.5(2) | 33.5(2) | -0.71(19) | 21.6(2) | 0.38(18) |
| Fe4 | 34.6(3) | 30.3(3) | 38.8(3) | -4.1(2) | 24.5(2) | 0.8(2) |
| Si2 | 29.0(5) | 25.9(4) | 29.6(4) | -0.1(3) | 19.8(4) | 1.8(3) |
| O3 | 34.1(12) | 25.6(11) | 34.4(12) | -0.5(9) | 23.6(11) | 0.9(9) |
| O4 | 29.5(13) | 32.0(13) | 33.4(13) | -1.6(10) | 17.4(11) | 2.7(10) |
| N3 | 32.0(15) | 29.4(14) | 35.3(15) | -4.3(12) | 23.3(13) | -1.6(11) |
| N4 | 43.5(17) | 32.2(15) | 35.9(16) | 0.9(12) | 28.4(15) | -2.8(13) |
| C27 | 27.1(16) | 30.2(16) | 30.1(16) | -1.0(13) | 19.9(14) | 0.7(13) |
| C28 | 27.4(16) | 30.1(16) | 30.8(16) | -5.2(13) | 19.2(14) | -2.7(13) |
| C29 | 31.6(17) | 38.1(18) | 30.3(17) | -2.2(14) | 20.7(15) | -1.5(14) |
| C30 | 27.4(16) | 36.2(18) | 33.5(17) | 4.3(14) | 19.7(15) | 3.2(14) |
| C31 | 30.8(17) | 32.8(17) | 36.8(18) | 2.1(14) | 24.4(16) | 3.3(13) |
| C32 | 31.0(19) | 52(2) | 37.3(19) | -2.5(17) | 20.0(17) | -7.6(16) |
| C33 | 26.8(17) | 38.5(19) | 42(2) | 2.4(15) | 20.6(16) | 3.1(14) |
| C34 | 35.0(19) | 47(2) | 49(2) | 6.0(17) | 30.8(19) | 0.8(16) |
| C35 | 37(2) | 34(2) | 65(3) | 6.6(18) | 32(2) | -0.3(16) |
| C36 | 42(2) | 47(2) | 62(3) | -22(2) | 35(2) | -13.4(18) |
| C37 | 33.6(18) | 33.0(18) | 40.0(19) | -2.8(14) | 27.4(16) | -0.2(14) |
| C38 | 34.9(19) | 36.6(19) | 36.8(19) | -4.0(15) | 21.6(17) | -0.5(15) |
| C39 | 51(2) | 32.7(19) | 54(2) | -7.0(17) | 39(2) | 0.6(16) |
| C40 | 30.9(17) | 29.8(16) | 32.7(17) | -0.4(13) | 21.3(15) | 1.0(13) |
| C41 | 36.1(18) | 33.5(18) | 30.5(17) | -1.4(14) | 22.1(16) | -1.9(14) |
| C42 | 39(2) | 45(2) | 36.7(19) | -2.2(16) | 27.8(17) | -0.3(16) |
| C43 | 35.9(19) | 41(2) | 40.9(19) | 0.4(16) | 27.6(17) | 6.0(15) |
| C44 | 37.0(19) | 37.0(19) | 33.7(18) | 3.6(14) | 24.0(16) | 5.9(15) |
| C45 | 45(3) | 64(3) | 98(4) | -38(3) | 46(3) | -16(2) |
| C46 | 37(3) | 41(3) | 74(4) | -14(2) | 1(3) | 4(2) |
| C47 | 56(3) | 51(3) | 41(2) | -10(2) | 20(2) | -13(2) |
| C48 | 50(2) | 34(2) | 57(2) | -13.5(17) | 39(2) | -10.5(17) |
| C49 | 60(3) | 52(3) | 79(3) | -23(2) | 55(3) | -18(2) |
| C50 | 42(2) | 36.5(19) | 32.2(18) | -0.8(15) | 23.7(17) | -4.6(16) |
| C51 | 46(2) | 45(2) | 57(3) | -1.4(19) | 36(2) | -4.5(18) |
| C52 | 59(3) | 35(2) | 44(2) | 4.6(16) | 37(2) | 1.6(17) |
| O5 | 139(6) | 133(6) | 133(6) | -3(4) | 81(5) | 1(4) |
| C53 | 307(18) | 124(9) | 94(7) | 25(6) | 89(9) | -39(11) |
| C54 | 73(5) | 106(6) | 83(5) | -6(4) | 37(4) | -4(4) |
| C55 | 149(10) | 227(14) | 97(7) | 40(8) | 67(7) | -11(10) |
| Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
|---|---|---|---|---|---|---|
| Br1 | Zn1 | 2.4230(6) | Zn2 | O3 | 1.917(2) | |
| Br2 | Zn1 | 2.3680(5) | Zn2 | N3 | 2.089(3) | |
| Zn1 | O1 | 1.926(2) | Fe3 | C27 | 2.061(3) | |
| Zn1 | N1 | 2.098(3) | Fe3 | C28 | 2.038(3) | |
| Fe1 | C1 | 2.052(3) | Fe3 | C29 | 2.047(4) | |
| Fe1 | C2 | 2.024(3) | Fe3 | C30 | 2.043(3) | |
| Fe1 | C3 | 2.032(3) | Fe3 | C31 | 2.040(3) | |
| Fe1 | C4 | 2.032(4) | Fe3 | C32 | 2.045(4) | |
| Fe1 | C5 | 2.040(3) | Fe3 | C33 | 2.038(4) | |
| Fe1 | C6 | 2.036(4) | Fe3 | C34 | 2.039(4) | |
| Fe1 | C7 | 2.030(4) | Fe3 | C35 | 2.047(4) | |
| Fe1 | C8 | 2.036(3) | Fe3 | C36 | 2.042(4) | |
| Fe1 | C9 | 2.044(4) | Fe4 | C40 | 2.037(3) | |
| Fe1 | C10 | 2.044(4) | Fe4 | C41 | 2.030(4) | |
| Fe2 | C14 | 2.054(3) | Fe4 | C42 | 2.057(4) | |
| Fe2 | C15 | 2.015(4) | Fe4 | C43 | 2.059(4) | |
| Fe2 | C16 | 2.046(4) | Fe4 | C44 | 2.041(4) | |
| Fe2 | C17 | 2.052(5) | Fe4 | C45 | 2.050(5) | |
| Fe2 | C18 | 2.044(4) | Fe4 | C46 | 2.018(5) | |
| Fe2 | C19 | 2.045(5) | Fe4 | C47 | 2.030(5) | |
| Fe2 | C20 | 2.045(5) | Fe4 | C48 | 2.038(4) | |
| Fe2 | C21 | 2.043(4) | Fe4 | C49 | 2.044(5) | |
| Fe2 | C22 | 2.048(5) | Si2 | O3 | 1.620(2) | |
| Fe2 | C23 | 2.034(5) | Si2 | O4 | 1.652(3) | |
| Si1 | O1 | 1.620(2) | Si2 | C27 | 1.860(3) | |
| Si1 | O2 | 1.645(3) | Si2 | C40 | 1.866(4) | |
| Si1 | C1 | 1.857(4) | N3 | C37 | 1.496(4) | |
| Si1 | C14 | 1.862(4) | N3 | C38 | 1.479(5) | |
| N1 | C11 | 1.506(5) | N3 | C39 | 1.482(5) | |
| N1 | C12 | 1.478(5) | N4 | C50 | 1.514(5) | |
| N1 | C13 | 1.478(5) | N4 | C51 | 1.482(5) | |
| N2 | C24 | 1.513(5) | N4 | C52 | 1.487(5) | |
| N2 | C25 | 1.467(6) | C27 | C28 | 1.455(5) | |
| N2 | C26 | 1.491(6) | C27 | C31 | 1.438(5) | |
| C1 | C2 | 1.447(5) | C28 | C29 | 1.432(5) | |
| C1 | C5 | 1.436(5) | C28 | C37 | 1.498(5) | |
| C2 | C3 | 1.431(5) | C29 | C30 | 1.426(5) | |
| C2 | C11 | 1.508(5) | C30 | C31 | 1.415(5) | |
| C3 | C4 | 1.413(5) | C32 | C33 | 1.417(6) | |
| C4 | C5 | 1.420(5) | C32 | C36 | 1.416(6) | |
| C6 | C7 | 1.413(6) | C33 | C34 | 1.418(5) | |
| C6 | C10 | 1.413(7) | C34 | C35 | 1.409(6) | |
| C7 | C8 | 1.429(5) | C35 | C36 | 1.422(7) | |
| C8 | C9 | 1.414(5) | C40 | C41 | 1.452(5) | |
| C9 | C10 | 1.405(6) | C40 | C44 | 1.437(5) | |
| C14 | C15 | 1.444(5) | C41 | C42 | 1.426(5) | |
| C14 | C18 | 1.433(5) | C41 | C50 | 1.484(5) | |
| C15 | C16 | 1.428(5) | C42 | C43 | 1.408(6) | |
| C15 | C24 | 1.491(5) | C43 | C44 | 1.423(5) | |
| C16 | C17 | 1.408(6) | C45 | C46 | 1.380(9) | |
| C17 | C18 | 1.427(5) | C45 | C49 | 1.372(8) | |
| C19 | C20 | 1.393(7) | C46 | C47 | 1.454(8) | |
| C19 | C23 | 1.393(9) | C47 | C48 | 1.405(7) | |
| C20 | C21 | 1.396(7) | C48 | C49 | 1.410(6) | |
| C21 | C22 | 1.391(8) | O5 | C54 | 1.286(10) | |
| C22 | C23 | 1.434(9) | C53 | C54 | 1.564(14) | |
| Br3 | Zn2 | 2.4246(7) | C54 | C55 | 1.339(14) | |
| Br4 | Zn2 | 2.3611(6) |
| Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|
| Br2 | Zn1 | Br1 | 114.77(2) | O3 | Zn2 | Br4 | 111.23(7) | |
| O1 | Zn1 | Br1 | 106.56(7) | O3 | Zn2 | N3 | 106.12(11) | |
| O1 | Zn1 | Br2 | 112.38(7) | N3 | Zn2 | Br3 | 105.18(8) | |
| O1 | Zn1 | N1 | 109.36(11) | N3 | Zn2 | Br4 | 109.09(8) | |
| N1 | Zn1 | Br1 | 104.63(9) | C28 | Fe3 | C27 | 41.57(13) | |
| N1 | Zn1 | Br2 | 108.77(8) | C28 | Fe3 | C29 | 41.03(14) | |
| C2 | Fe1 | C1 | 41.56(13) | C28 | Fe3 | C30 | 69.15(14) | |
| C2 | Fe1 | C3 | 41.32(14) | C28 | Fe3 | C31 | 68.86(14) | |
| C2 | Fe1 | C4 | 69.10(14) | C28 | Fe3 | C32 | 121.02(16) | |
| C2 | Fe1 | C5 | 68.83(14) | C28 | Fe3 | C34 | 123.78(16) | |
| C2 | Fe1 | C6 | 125.07(17) | C28 | Fe3 | C35 | 160.59(17) | |
| C2 | Fe1 | C7 | 106.80(15) | C28 | Fe3 | C36 | 156.79(18) | |
| C2 | Fe1 | C8 | 119.89(14) | C29 | Fe3 | C27 | 69.44(14) | |
| C2 | Fe1 | C9 | 155.39(15) | C30 | Fe3 | C27 | 69.40(14) | |
| C2 | Fe1 | C10 | 162.52(17) | C30 | Fe3 | C29 | 40.81(14) | |
| C3 | Fe1 | C1 | 69.89(14) | C30 | Fe3 | C32 | 161.71(16) | |
| C3 | Fe1 | C5 | 68.60(14) | C30 | Fe3 | C35 | 107.28(16) | |
| C3 | Fe1 | C6 | 161.99(18) | C31 | Fe3 | C27 | 41.04(13) | |
| C3 | Fe1 | C8 | 106.15(15) | C31 | Fe3 | C29 | 68.31(14) | |
| C3 | Fe1 | C9 | 120.04(15) | C31 | Fe3 | C30 | 40.56(14) | |
| C3 | Fe1 | C10 | 155.29(18) | C31 | Fe3 | C32 | 125.37(16) | |
| C4 | Fe1 | C1 | 69.65(14) | C31 | Fe3 | C35 | 121.61(16) | |
| C4 | Fe1 | C3 | 40.69(15) | C31 | Fe3 | C36 | 108.35(16) | |
| C4 | Fe1 | C5 | 40.84(14) | C32 | Fe3 | C27 | 107.23(15) | |
| C4 | Fe1 | C6 | 156.49(18) | C32 | Fe3 | C29 | 156.41(16) | |
| C4 | Fe1 | C8 | 123.65(15) | C32 | Fe3 | C35 | 68.31(17) | |
| C4 | Fe1 | C9 | 107.22(15) | C33 | Fe3 | C27 | 124.40(15) | |
| C4 | Fe1 | C10 | 120.93(17) | C33 | Fe3 | C28 | 107.02(15) | |
| C5 | Fe1 | C1 | 41.09(13) | C33 | Fe3 | C29 | 120.79(15) | |
| C5 | Fe1 | C9 | 125.21(15) | C33 | Fe3 | C30 | 155.95(15) | |
| C5 | Fe1 | C10 | 108.48(16) | C33 | Fe3 | C31 | 162.08(15) | |
| C6 | Fe1 | C1 | 107.44(15) | C33 | Fe3 | C32 | 40.62(16) | |
| C6 | Fe1 | C5 | 121.80(17) | C33 | Fe3 | C34 | 40.72(16) | |
| C6 | Fe1 | C8 | 68.62(16) | C33 | Fe3 | C35 | 68.03(16) | |
| C6 | Fe1 | C9 | 67.95(17) | C33 | Fe3 | C36 | 68.15(17) | |
| C6 | Fe1 | C10 | 40.52(19) | C34 | Fe3 | C27 | 161.36(15) | |
| C7 | Fe1 | C1 | 120.30(15) | C34 | Fe3 | C29 | 106.77(16) | |
| C7 | Fe1 | C3 | 124.24(16) | C34 | Fe3 | C30 | 120.39(15) | |
| C7 | Fe1 | C4 | 161.11(17) | C34 | Fe3 | C31 | 156.05(15) | |
| C7 | Fe1 | C5 | 156.55(16) | C34 | Fe3 | C32 | 68.54(17) | |
| C7 | Fe1 | C6 | 40.66(18) | C34 | Fe3 | C35 | 40.33(17) | |
| C7 | Fe1 | C8 | 41.16(15) | C34 | Fe3 | C36 | 68.33(18) | |
| C7 | Fe1 | C9 | 68.39(16) | C35 | Fe3 | C27 | 156.72(16) | |
| C7 | Fe1 | C10 | 68.40(18) | C35 | Fe3 | C29 | 123.98(17) | |
| C8 | Fe1 | C1 | 155.88(14) | C36 | Fe3 | C27 | 121.05(17) | |
| C8 | Fe1 | C5 | 161.27(15) | C36 | Fe3 | C29 | 161.20(18) | |
| C8 | Fe1 | C9 | 40.56(15) | C36 | Fe3 | C30 | 124.67(17) | |
| C8 | Fe1 | C10 | 68.33(16) | C36 | Fe3 | C32 | 40.54(18) | |
| C9 | Fe1 | C1 | 161.96(15) | C36 | Fe3 | C35 | 40.71(19) | |
| C9 | Fe1 | C10 | 40.22(17) | C40 | Fe4 | C42 | 69.60(14) | |
| C10 | Fe1 | C1 | 125.08(16) | C40 | Fe4 | C43 | 69.43(14) | |
| C15 | Fe2 | C14 | 41.56(14) | C40 | Fe4 | C44 | 41.26(14) | |
| C15 | Fe2 | C16 | 41.15(15) | C40 | Fe4 | C45 | 105.18(18) | |
| C15 | Fe2 | C17 | 68.53(17) | C40 | Fe4 | C48 | 158.02(16) | |
| C15 | Fe2 | C18 | 68.77(16) | C40 | Fe4 | C49 | 121.09(17) | |
| C15 | Fe2 | C19 | 119.6(2) | C41 | Fe4 | C40 | 41.84(14) | |
| C15 | Fe2 | C20 | 107.12(18) | C41 | Fe4 | C42 | 40.84(15) | |
| C15 | Fe2 | C21 | 125.06(18) | C41 | Fe4 | C43 | 68.42(15) | |
| C15 | Fe2 | C22 | 162.0(2) | C41 | Fe4 | C44 | 68.85(15) | |
| C15 | Fe2 | C23 | 154.4(2) | C41 | Fe4 | C45 | 124.59(19) | |
| C16 | Fe2 | C14 | 69.60(15) | C41 | Fe4 | C47 | 123.53(18) | |
| C16 | Fe2 | C17 | 40.20(17) | C41 | Fe4 | C48 | 159.12(16) | |
| C16 | Fe2 | C22 | 125.6(2) | C41 | Fe4 | C49 | 159.30(17) | |
| C17 | Fe2 | C14 | 69.14(15) | C42 | Fe4 | C43 | 40.02(16) | |
| C18 | Fe2 | C14 | 40.94(15) | C44 | Fe4 | C42 | 68.03(15) | |
| C18 | Fe2 | C16 | 68.41(17) | C44 | Fe4 | C43 | 40.61(14) | |
| C18 | Fe2 | C17 | 40.77(16) | C44 | Fe4 | C45 | 119.5(2) | |
| C18 | Fe2 | C19 | 125.4(2) | C44 | Fe4 | C49 | 106.0(2) | |
| C18 | Fe2 | C20 | 161.64(19) | C45 | Fe4 | C42 | 162.8(2) | |
| C18 | Fe2 | C22 | 122.0(2) | C45 | Fe4 | C43 | 155.1(2) | |
| C19 | Fe2 | C14 | 106.31(16) | C46 | Fe4 | C40 | 120.50(19) | |
| C19 | Fe2 | C16 | 155.2(2) | C46 | Fe4 | C41 | 109.37(19) | |
| C19 | Fe2 | C17 | 163.0(2) | C46 | Fe4 | C42 | 127.9(3) | |
| C19 | Fe2 | C22 | 67.9(2) | C46 | Fe4 | C43 | 163.7(3) | |
| C20 | Fe2 | C14 | 124.19(18) | C46 | Fe4 | C44 | 155.1(3) | |
| C20 | Fe2 | C16 | 121.06(19) | C46 | Fe4 | C45 | 39.7(3) | |
| C20 | Fe2 | C17 | 156.07(19) | C46 | Fe4 | C47 | 42.1(2) | |
| C20 | Fe2 | C19 | 39.8(2) | C46 | Fe4 | C48 | 68.03(19) | |
| C20 | Fe2 | C22 | 67.2(2) | C46 | Fe4 | C49 | 66.4(3) | |
| C21 | Fe2 | C14 | 161.55(19) | C47 | Fe4 | C40 | 158.62(18) | |
| C21 | Fe2 | C16 | 108.52(17) | C47 | Fe4 | C42 | 109.6(2) | |
| C21 | Fe2 | C17 | 122.02(18) | C47 | Fe4 | C43 | 124.5(2) | |
| C21 | Fe2 | C18 | 156.80(19) | C47 | Fe4 | C44 | 159.66(19) | |
| C21 | Fe2 | C19 | 67.25(19) | C47 | Fe4 | C45 | 69.0(2) | |
| C21 | Fe2 | C20 | 40.0(2) | C47 | Fe4 | C48 | 40.40(19) | |
| C21 | Fe2 | C22 | 39.8(2) | C47 | Fe4 | C49 | 68.1(2) | |
| C22 | Fe2 | C14 | 155.9(2) | C48 | Fe4 | C42 | 123.22(16) | |
| C22 | Fe2 | C17 | 109.2(2) | C48 | Fe4 | C43 | 107.89(17) | |
| C23 | Fe2 | C14 | 119.4(2) | C48 | Fe4 | C44 | 122.64(17) | |
| C23 | Fe2 | C16 | 163.4(3) | C48 | Fe4 | C45 | 67.58(19) | |
| C23 | Fe2 | C17 | 126.9(3) | C48 | Fe4 | C49 | 40.42(17) | |
| C23 | Fe2 | C18 | 108.3(2) | C49 | Fe4 | C42 | 157.56(18) | |
| C23 | Fe2 | C19 | 40.0(3) | C49 | Fe4 | C43 | 121.5(2) | |
| C23 | Fe2 | C20 | 67.2(2) | C49 | Fe4 | C45 | 39.2(2) | |
| C23 | Fe2 | C21 | 67.6(2) | O3 | Si2 | O4 | 108.88(13) | |
| C23 | Fe2 | C22 | 41.1(3) | O3 | Si2 | C27 | 109.29(14) | |
| O1 | Si1 | O2 | 109.91(14) | O3 | Si2 | C40 | 105.46(14) | |
| O1 | Si1 | C1 | 109.37(14) | O4 | Si2 | C27 | 111.61(15) | |
| O1 | Si1 | C14 | 105.30(15) | O4 | Si2 | C40 | 109.19(15) | |
| O2 | Si1 | C1 | 108.64(15) | C27 | Si2 | C40 | 112.19(15) | |
| O2 | Si1 | C14 | 109.60(15) | Si2 | O3 | Zn2 | 126.70(14) | |
| C1 | Si1 | C14 | 113.96(16) | C37 | N3 | Zn2 | 111.6(2) | |
| Si1 | O1 | Zn1 | 122.86(14) | C38 | N3 | Zn2 | 110.9(2) | |
| C11 | N1 | Zn1 | 112.1(2) | C38 | N3 | C37 | 111.5(3) | |
| C12 | N1 | Zn1 | 111.2(3) | C38 | N3 | C39 | 108.9(3) | |
| C12 | N1 | C11 | 111.2(3) | C39 | N3 | Zn2 | 106.1(2) | |
| C12 | N1 | C13 | 108.3(3) | C39 | N3 | C37 | 107.6(3) | |
| C13 | N1 | Zn1 | 105.7(2) | C51 | N4 | C50 | 112.7(3) | |
| C13 | N1 | C11 | 108.1(3) | C51 | N4 | C52 | 111.4(3) | |
| C25 | N2 | C24 | 111.9(4) | C52 | N4 | C50 | 110.9(3) | |
| C25 | N2 | C26 | 112.2(4) | Si2 | C27 | Fe3 | 132.10(18) | |
| C26 | N2 | C24 | 110.8(3) | C28 | C27 | Fe3 | 68.37(19) | |
| Si1 | C1 | Fe1 | 128.27(17) | C28 | C27 | Si2 | 126.5(3) | |
| C2 | C1 | Fe1 | 68.18(18) | C31 | C27 | Fe3 | 68.67(19) | |
| C2 | C1 | Si1 | 124.8(2) | C31 | C27 | Si2 | 127.5(3) | |
| C5 | C1 | Fe1 | 68.98(19) | C31 | C27 | C28 | 105.7(3) | |
| C5 | C1 | Si1 | 129.6(3) | C27 | C28 | Fe3 | 70.07(19) | |
| C5 | C1 | C2 | 105.6(3) | C27 | C28 | C37 | 128.6(3) | |
| C1 | C2 | Fe1 | 70.26(18) | C29 | C28 | Fe3 | 69.8(2) | |
| C1 | C2 | C11 | 128.0(3) | C29 | C28 | C27 | 108.3(3) | |
| C3 | C2 | Fe1 | 69.63(19) | C29 | C28 | C37 | 122.8(3) | |
| C3 | C2 | C1 | 108.8(3) | C37 | C28 | Fe3 | 122.0(2) | |
| C3 | C2 | C11 | 123.2(3) | C28 | C29 | Fe3 | 69.1(2) | |
| C11 | C2 | Fe1 | 124.1(2) | C30 | C29 | Fe3 | 69.5(2) | |
| C2 | C3 | Fe1 | 69.05(19) | C30 | C29 | C28 | 108.3(3) | |
| C4 | C3 | Fe1 | 69.6(2) | C29 | C30 | Fe3 | 69.7(2) | |
| C4 | C3 | C2 | 108.0(3) | C31 | C30 | Fe3 | 69.6(2) | |
| C3 | C4 | Fe1 | 69.7(2) | C31 | C30 | C29 | 107.7(3) | |
| C3 | C4 | C5 | 108.2(3) | C27 | C31 | Fe3 | 70.28(19) | |
| C5 | C4 | Fe1 | 69.9(2) | C30 | C31 | Fe3 | 69.9(2) | |
| C1 | C5 | Fe1 | 69.92(18) | C30 | C31 | C27 | 110.0(3) | |
| C4 | C5 | Fe1 | 69.3(2) | C33 | C32 | Fe3 | 69.4(2) | |
| C4 | C5 | C1 | 109.5(3) | C36 | C32 | Fe3 | 69.6(2) | |
| C7 | C6 | Fe1 | 69.5(2) | C36 | C32 | C33 | 107.5(4) | |
| C7 | C6 | C10 | 108.3(4) | C32 | C33 | Fe3 | 70.0(2) | |
| C10 | C6 | Fe1 | 70.0(2) | C32 | C33 | C34 | 108.4(4) | |
| C6 | C7 | Fe1 | 69.9(2) | C34 | C33 | Fe3 | 69.7(2) | |
| C6 | C7 | C8 | 107.7(4) | C33 | C34 | Fe3 | 69.6(2) | |
| C8 | C7 | Fe1 | 69.7(2) | C35 | C34 | Fe3 | 70.1(2) | |
| C7 | C8 | Fe1 | 69.2(2) | C35 | C34 | C33 | 107.8(4) | |
| C9 | C8 | Fe1 | 70.0(2) | C34 | C35 | Fe3 | 69.6(2) | |
| C9 | C8 | C7 | 107.3(3) | C34 | C35 | C36 | 108.1(4) | |
| C8 | C9 | Fe1 | 69.4(2) | C36 | C35 | Fe3 | 69.5(2) | |
| C10 | C9 | Fe1 | 69.9(2) | C32 | C36 | Fe3 | 69.9(2) | |
| C10 | C9 | C8 | 108.7(4) | C32 | C36 | C35 | 108.1(4) | |
| C6 | C10 | Fe1 | 69.4(2) | C35 | C36 | Fe3 | 69.8(2) | |
| C9 | C10 | Fe1 | 69.9(2) | N3 | C37 | C28 | 116.5(3) | |
| C9 | C10 | C6 | 108.0(4) | Si2 | C40 | Fe4 | 128.46(18) | |
| N1 | C11 | C2 | 114.6(3) | C41 | C40 | Fe4 | 68.8(2) | |
| Si1 | C14 | Fe2 | 131.05(19) | C41 | C40 | Si2 | 121.8(3) | |
| C15 | C14 | Fe2 | 67.8(2) | C44 | C40 | Fe4 | 69.5(2) | |
| C15 | C14 | Si1 | 121.5(3) | C44 | C40 | Si2 | 132.5(3) | |
| C18 | C14 | Fe2 | 69.2(2) | C44 | C40 | C41 | 105.6(3) | |
| C18 | C14 | Si1 | 132.6(3) | C40 | C41 | Fe4 | 69.3(2) | |
| C18 | C14 | C15 | 105.7(3) | C40 | C41 | C50 | 125.1(3) | |
| C14 | C15 | Fe2 | 70.7(2) | C42 | C41 | Fe4 | 70.6(2) | |
| C14 | C15 | C24 | 125.3(3) | C42 | C41 | C40 | 108.5(3) | |
| C16 | C15 | Fe2 | 70.6(2) | C42 | C41 | C50 | 126.3(3) | |
| C16 | C15 | C14 | 109.1(3) | C50 | C41 | Fe4 | 129.4(3) | |
| C16 | C15 | C24 | 125.6(3) | C41 | C42 | Fe4 | 68.6(2) | |
| C24 | C15 | Fe2 | 125.4(3) | C43 | C42 | Fe4 | 70.1(2) | |
| C15 | C16 | Fe2 | 68.3(2) | C43 | C42 | C41 | 108.4(3) | |
| C17 | C16 | Fe2 | 70.1(3) | C42 | C43 | Fe4 | 69.9(2) | |
| C17 | C16 | C15 | 107.7(3) | C42 | C43 | C44 | 108.1(3) | |
| C16 | C17 | Fe2 | 69.7(2) | C44 | C43 | Fe4 | 69.0(2) | |
| C16 | C17 | C18 | 108.4(4) | C40 | C44 | Fe4 | 69.2(2) | |
| C18 | C17 | Fe2 | 69.3(2) | C43 | C44 | Fe4 | 70.4(2) | |
| C14 | C18 | Fe2 | 69.9(2) | C43 | C44 | C40 | 109.3(3) | |
| C17 | C18 | Fe2 | 69.9(2) | C46 | C45 | Fe4 | 68.9(3) | |
| C17 | C18 | C14 | 109.1(4) | C49 | C45 | Fe4 | 70.2(3) | |
| C20 | C19 | Fe2 | 70.1(3) | C49 | C45 | C46 | 107.9(5) | |
| C20 | C19 | C23 | 108.1(5) | C45 | C46 | Fe4 | 71.4(3) | |
| C23 | C19 | Fe2 | 69.6(3) | C45 | C46 | C47 | 109.2(5) | |
| C19 | C20 | Fe2 | 70.1(3) | C47 | C46 | Fe4 | 69.4(3) | |
| C19 | C20 | C21 | 108.5(5) | C46 | C47 | Fe4 | 68.5(3) | |
| C21 | C20 | Fe2 | 69.9(3) | C48 | C47 | Fe4 | 70.1(3) | |
| C20 | C21 | Fe2 | 70.1(3) | C48 | C47 | C46 | 105.1(5) | |
| C22 | C21 | Fe2 | 70.3(3) | C47 | C48 | Fe4 | 69.5(2) | |
| C22 | C21 | C20 | 108.7(5) | C47 | C48 | C49 | 108.3(4) | |
| C21 | C22 | Fe2 | 69.9(3) | C49 | C48 | Fe4 | 70.0(2) | |
| C21 | C22 | C23 | 106.8(5) | C45 | C49 | Fe4 | 70.7(3) | |
| C23 | C22 | Fe2 | 68.9(3) | C45 | C49 | C48 | 109.6(5) | |
| C19 | C23 | Fe2 | 70.5(3) | C48 | C49 | Fe4 | 69.6(2) | |
| C19 | C23 | C22 | 107.8(5) | C41 | C50 | N4 | 110.6(3) | |
| C22 | C23 | Fe2 | 70.0(3) | O5 | C54 | C53 | 125.3(9) | |
| C15 | C24 | N2 | 110.7(3) | O5 | C54 | C55 | 122.5(10) | |
| Br4 | Zn2 | Br3 | 117.25(2) | C55 | C54 | C53 | 110.5(10) | |
| O3 | Zn2 | Br3 | 107.27(7) |
| D | H | A | d(D-H)/Å | d(H-A)/Å | d(D-A)/Å | D-H-A/° |
|---|---|---|---|---|---|---|
| N2 | H2A | O1 | 0.984(19) | 1.69(2) | 2.652(4) | 163(4) |
| N4 | H4B | O3 | 0.968(19) | 1.70(2) | 2.644(4) | 165(5) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| H3 | 1983 | 6449 | 8692 | 39 |
| H4 | 1667 | 8468 | 8643 | 41 |
| H5 | 957 | 8229 | 7882 | 37 |
| H6 | 889 | 7572 | 6632 | 58 |
| H7 | 1486 | 6269 | 7088 | 49 |
| H8 | 2049 | 7593 | 7868 | 41 |
| H9 | 1790 | 9698 | 7876 | 45 |
| H10 | 1078 | 9679 | 7123 | 57 |
| H11A | 1357 | 4431 | 7515 | 40 |
| H11B | 1778 | 4479 | 8077 | 40 |
| H12A | 1427 | 4235 | 8598 | 75 |
| H12B | 1835 | 3731 | 8868 | 75 |
| H12C | 1524 | 2756 | 8725 | 75 |
| H13A | 1579 | 1442 | 8195 | 74 |
| H13B | 1912 | 2371 | 8383 | 74 |
| H13C | 1569 | 2100 | 7769 | 74 |
| H16 | -739 | 6967 | 6207 | 48 |
| H17 | -357 | 8929 | 6756 | 57 |
| H18 | 334 | 8510 | 7248 | 50 |
| H19 | 212 | 7240 | 5942 | 78 |
| H20 | -468 | 6522 | 5309 | 66 |
| H21 | -864 | 8314 | 5202 | 65 |
| H22 | -435 | 10175 | 5763 | 85 |
| H23 | 243 | 9484 | 6237 | 95 |
| H24A | -203 | 4692 | 6116 | 47 |
| H24B | -602 | 4801 | 5949 | 47 |
| H25A | -526 | 2334 | 6132 | 107 |
| H25B | -163 | 1851 | 6709 | 107 |
| H25C | -119 | 2423 | 6325 | 107 |
| H26A | -347 | 4768 | 7015 | 107 |
| H26B | -330 | 3264 | 7096 | 107 |
| H26C | -681 | 3886 | 6543 | 107 |
| H29 | -1489 | 6557 | 5942 | 40 |
| H30 | -1320 | 4488 | 5747 | 40 |
| H31 | -1456 | 4808 | 4901 | 39 |
| H32 | -2615 | 6079 | 3868 | 51 |
| H33 | -2606 | 7006 | 4561 | 46 |
| H34 | -2343 | 5316 | 5270 | 50 |
| H35 | -2197 | 3334 | 5012 | 58 |
| H36 | -2356 | 3809 | 4151 | 61 |
| H37A | -2071 | 8699 | 4814 | 40 |
| H37B | -1877 | 8590 | 5413 | 40 |
| H38A | -1079 | 8860 | 5716 | 58 |
| H38B | -1149 | 9243 | 6092 | 58 |
| H38C | -1032 | 10306 | 5895 | 58 |
| H39A | -1588 | 11620 | 5501 | 64 |
| H39B | -1680 | 10635 | 5752 | 64 |
| H39C | -1993 | 10968 | 5138 | 64 |
| H42 | -1334 | 6286 | 3322 | 46 |
| H43 | -1138 | 4363 | 3908 | 46 |
| H44 | -1328 | 4762 | 4430 | 43 |
| H45 | -2466 | 5481 | 3261 | 85 |
| H46 | -2514 | 6492 | 2558 | 98 |
| H47 | -2210 | 4967 | 2341 | 73 |
| H48 | -1990 | 3013 | 2933 | 54 |
| H49 | -2149 | 3370 | 3490 | 68 |
| H50A | -1956 | 8521 | 3244 | 46 |
| H50B | -1709 | 8468 | 3092 | 46 |
| H51A | -934 | 8481 | 4216 | 72 |
| H51B | -882 | 9987 | 4298 | 72 |
| H51C | -1032 | 9368 | 3761 | 72 |
| H52A | -1618 | 10869 | 3268 | 67 |
| H52B | -1420 | 11391 | 3840 | 67 |
| H52C | -1839 | 10836 | 3460 | 67 |
| H53A | 40 | 3386 | 5653 | 322 |
| H53B | -159 | 4330 | 5164 | 322 |
| H53C | -388 | 3800 | 5310 | 322 |
| H55A | 153 | 1748 | 5520 | 257 |
| H55B | -144 | 693 | 5105 | 257 |
| H55C | 49 | 1595 | 4973 | 257 |
| H2A | 68(6) | 3960(50) | 6952(14) | 56(14) |
| H4B | -1438(14) | 9320(50) | 4083(15) | 59(14) |
| H4A | -2316(14) | 8470(30) | 3730(20) | 64(15) |
| H2 | 614(15) | 4590(20) | 6620(20) | 63(15) |
Experimental
Single crystals of C55H74Br4Fe4N4O5Si2Zn2 [3113] 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 [3113]
Crystal Data for C55H74Br4Fe4N4O5Si2Zn2 (M =1601.14 g/mol): monoclinic, space group C2/c (no. 15), a = 47.515(3) Å, b = 10.31587(19) Å, c = 33.897(2) Å, β = 132.838(10)°, V = 12183.5(18) Å3, Z = 8, T = 173 K, μ(MoKα) = 4.414 mm-1, Dcalc = 1.746 g/cm3, 155041 reflections measured (4.676° ≤ 2Θ ≤ 56°), 14607 unique (Rint = 0.0441, Rsigma = 0.0233) which were used in all calculations. The final R1 was 0.0432 (I > 2σ(I)) and wR2 was 0.1243 (all data).
Refinement model description
Number of restraints - 4, 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
O2-H2 = O4-H4A
0.9 with sigma of 0.02
N4-H4B = N2-H2A
1 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
C11(H11A,H11B), C24(H24A,H24B), C37(H37A,H37B), C50(H50A,H50B)
3.b Me refined with riding coordinates:
C53(H53A,H53B,H53C), C55(H55A,H55B,H55C)
3.c Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C16(H16),
C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C29(H29),
C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36),
C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49)
3.d Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C25(H25A,H25B,H25C), C26(H26A,H26B,
H26C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C51(H51A,H51B,H51C), C52(H52A,
H52B,H52C)
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.