| Identification code | mo_B0273_0m_4 |
| Empirical formula | C36H60Br2Fe2N2O2Si4Zn2 |
| Formula weight | 1067.48 |
| Temperature/K | 99.99 |
| Crystal system | triclinic |
| Space group | P-1 |
| a/Å | 9.606(3) |
| b/Å | 14.581(6) |
| c/Å | 15.922(6) |
| α/° | 88.661(11) |
| β/° | 86.404(8) |
| γ/° | 77.905(11) |
| Volume/Å3 | 2176.1(13) |
| Z | 2 |
| ρcalcg/cm3 | 1.629 |
| μ/mm‑1 | 3.722 |
| F(000) | 1088.0 |
| Crystal size/mm3 | 0.157 × 0.143 × 0.08 |
| Radiation | MoKα (λ = 0.71073) |
| 2Θ range for data collection/° | 4.344 to 51.996 |
| Index ranges | -11 ≤ h ≤ 11, -17 ≤ k ≤ 17, 0 ≤ l ≤ 19 |
| Reflections collected | 11416 |
| Independent reflections | 11416 [Rint = ?, Rsigma = 0.0452] |
| Data/restraints/parameters | 11416/0/467 |
| Goodness-of-fit on F2 | 1.171 |
| Final R indexes [I>=2σ (I)] | R1 = 0.0482, wR2 = 0.0923 |
| Final R indexes [all data] | R1 = 0.0643, wR2 = 0.1001 |
| Largest diff. peak/hole / e Å-3 | 0.59/-0.94 |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| Br1 | 8148.3(7) | -1123.0(5) | 3882.4(4) | 20.70(17) |
| Zn1 | 6215.3(8) | -3.6(5) | 4417.0(5) | 11.34(16) |
| Fe1 | 4729.8(10) | 1041.1(6) | 1543.3(6) | 12.6(2) |
| Si1 | 3344.7(18) | 144.6(12) | 3485.0(11) | 12.2(4) |
| Si2 | 8398.9(19) | 1053.6(13) | 1486.1(11) | 15.1(4) |
| O1 | 4175(4) | -10(3) | 4359(3) | 14.3(9) |
| N1 | 6389(5) | 1342(4) | 4049(3) | 12.5(11) |
| C1 | 4750(6) | 271(4) | 2647(4) | 11.2(13) |
| C2 | 5767(6) | 881(4) | 2624(4) | 11.8(13) |
| C3 | 6778(6) | 650(4) | 1912(4) | 11.9(13) |
| C4 | 6377(7) | -121(4) | 1504(4) | 15.0(14) |
| C5 | 5155(7) | -338(4) | 1943(4) | 14.1(14) |
| C6 | 2689(7) | 1798(5) | 1422(4) | 21.5(16) |
| C7 | 3647(7) | 2412(5) | 1467(4) | 18.7(15) |
| C8 | 4682(7) | 2192(5) | 784(4) | 20.5(15) |
| C9 | 4373(7) | 1461(5) | 327(4) | 18.6(15) |
| C10 | 3145(7) | 1204(5) | 723(4) | 22.1(16) |
| C11 | 2698(7) | -935(4) | 3243(4) | 18.1(14) |
| C12 | 1811(7) | 1149(5) | 3601(4) | 19.2(15) |
| C13 | 5670(6) | 1646(4) | 3245(4) | 11.1(13) |
| C14 | 5713(7) | 2015(4) | 4713(4) | 16.4(14) |
| C15 | 7925(6) | 1351(4) | 3945(4) | 14.2(13) |
| C16 | 8489(7) | 2255(5) | 1818(4) | 20.0(15) |
| C17 | 9967(7) | 153(5) | 1819(4) | 18.6(15) |
| C18 | 8469(7) | 1050(5) | 311(4) | 20.8(15) |
| Br2 | 12679.5(8) | -6274.1(5) | 3632.2(4) | 23.36(17) |
| Zn2 | 11077.8(8) | -5070.3(5) | 4320.6(5) | 12.26(17) |
| Fe2 | 8954.2(10) | -3786.4(6) | 1634.6(6) | 13.7(2) |
| Si3 | 7960.1(18) | -4664.0(12) | 3649.1(11) | 12.2(4) |
| Si4 | 12639.4(19) | -3955.9(13) | 1207.1(12) | 17.2(4) |
| O2 | 8987(4) | -4934(3) | 4437(3) | 13.1(9) |
| N2 | 11376(5) | -3758(3) | 3921(3) | 12.9(11) |
| C19 | 9201(6) | -4618(4) | 2699(4) | 12.7(13) |
| C20 | 10311(6) | -4086(4) | 2585(4) | 12.8(13) |
| C21 | 11078(7) | -4316(4) | 1782(4) | 13.7(13) |
| C22 | 10432(7) | -4999(4) | 1417(4) | 18.2(14) |
| C23 | 9306(7) | -5180(4) | 1970(4) | 15.5(14) |
| C24 | 6866(8) | -3090(6) | 1623(5) | 31.0(18) |
| C25 | 7763(9) | -2461(5) | 1807(5) | 33(2) |
| C26 | 8758(8) | -2474(5) | 1116(5) | 27.6(18) |
| C27 | 8492(8) | -3093(5) | 518(4) | 26.4(17) |
| C28 | 7322(8) | -3470(5) | 828(5) | 25.9(17) |
| C29 | 6954(7) | -5594(5) | 3467(4) | 22.9(16) |
| C30 | 6647(7) | -3553(4) | 3884(5) | 19.5(15) |
| C31 | 10495(6) | -3373(4) | 3204(4) | 11.1(13) |
| C32 | 12919(7) | -3848(5) | 3679(5) | 23.8(16) |
| C33 | 11011(8) | -3092(4) | 4633(4) | 19.2(15) |
| C34 | 12943(7) | -2791(4) | 1525(4) | 19.4(15) |
| C35 | 12334(8) | -3875(5) | 62(4) | 26.0(17) |
| C36 | 14246(7) | -4903(5) | 1379(5) | 27.8(17) |
| Atom | U11 | U22 | U33 | U23 | U13 | U12 |
|---|---|---|---|---|---|---|
| Br1 | 20.9(4) | 14.4(3) | 23.1(4) | -2.0(3) | 2.9(3) | 3.6(3) |
| Zn1 | 10.8(3) | 11.5(4) | 11.4(4) | 0.6(3) | 0.1(3) | -2.1(3) |
| Fe1 | 13.7(5) | 13.6(5) | 10.6(5) | 0.8(4) | -1.9(4) | -2.9(4) |
| Si1 | 12.3(8) | 14.0(9) | 11.5(9) | 1.2(7) | -1.7(7) | -4.9(7) |
| Si2 | 14.6(9) | 16.4(9) | 14.2(9) | 0.0(7) | 1.1(7) | -3.5(7) |
| O1 | 15(2) | 16(2) | 12(2) | 5.2(19) | -0.8(19) | -6.4(18) |
| N1 | 11(3) | 12(3) | 15(3) | -2(2) | -2(2) | -4(2) |
| C1 | 11(3) | 10(3) | 13(3) | -1(2) | -4(2) | -1(2) |
| C2 | 13(3) | 12(3) | 10(3) | 4(3) | -6(2) | -3(3) |
| C3 | 13(3) | 12(3) | 8(3) | 5(2) | -4(2) | 4(2) |
| C4 | 19(3) | 12(3) | 12(3) | 5(3) | -3(3) | 1(3) |
| C5 | 18(3) | 10(3) | 15(3) | -4(3) | -7(3) | -5(3) |
| C6 | 17(3) | 30(4) | 16(4) | 11(3) | -7(3) | 1(3) |
| C7 | 26(4) | 17(4) | 11(3) | 0(3) | -4(3) | 2(3) |
| C8 | 19(4) | 21(4) | 21(4) | 6(3) | -7(3) | -3(3) |
| C9 | 25(4) | 24(4) | 9(3) | 5(3) | -6(3) | -8(3) |
| C10 | 26(4) | 28(4) | 16(4) | 6(3) | -12(3) | -13(3) |
| C11 | 20(3) | 17(3) | 19(4) | 3(3) | -3(3) | -10(3) |
| C12 | 14(3) | 24(4) | 19(4) | 4(3) | -2(3) | -3(3) |
| C13 | 8(3) | 11(3) | 12(3) | 2(3) | -1(2) | 0(2) |
| C14 | 26(4) | 11(3) | 12(3) | -1(3) | 0(3) | -2(3) |
| C15 | 16(3) | 13(3) | 14(3) | 2(3) | -1(3) | -5(3) |
| C16 | 18(3) | 23(4) | 19(4) | 2(3) | 2(3) | -4(3) |
| C17 | 14(3) | 19(4) | 22(4) | -1(3) | 4(3) | -4(3) |
| C18 | 19(3) | 23(4) | 20(4) | 1(3) | 3(3) | -5(3) |
| Br2 | 25.8(4) | 16.0(3) | 23.4(4) | -2.7(3) | 3.6(3) | 5.6(3) |
| Zn2 | 11.2(4) | 11.4(4) | 13.4(4) | 0.4(3) | 0.5(3) | -1.2(3) |
| Fe2 | 15.1(5) | 13.2(5) | 12.7(5) | 0.9(4) | -2.9(4) | -2.2(4) |
| Si3 | 12.3(8) | 12.6(9) | 12.3(9) | 1.1(7) | -1.4(7) | -3.6(7) |
| Si4 | 15.3(9) | 16.3(10) | 19.2(10) | 0.2(8) | 4.0(7) | -3.3(7) |
| O2 | 14(2) | 9(2) | 16(2) | 0.2(19) | -1.2(19) | -0.6(17) |
| N2 | 13(3) | 12(3) | 14(3) | 2(2) | -1(2) | -4(2) |
| C19 | 13(3) | 11(3) | 13(3) | 4(2) | -1(3) | 3(3) |
| C20 | 9(3) | 11(3) | 16(3) | 2(3) | 2(2) | 3(2) |
| C21 | 19(3) | 10(3) | 12(3) | 3(3) | -1(3) | -4(3) |
| C22 | 26(4) | 11(3) | 17(4) | -1(3) | -2(3) | 0(3) |
| C23 | 21(3) | 9(3) | 17(3) | -1(3) | -6(3) | -3(3) |
| C24 | 19(4) | 41(5) | 27(4) | 9(4) | -5(3) | 7(3) |
| C25 | 48(5) | 17(4) | 27(4) | -2(3) | -23(4) | 13(4) |
| C26 | 28(4) | 16(4) | 40(5) | 12(3) | -18(4) | -5(3) |
| C27 | 34(4) | 29(4) | 13(4) | 8(3) | -7(3) | 3(3) |
| C28 | 25(4) | 24(4) | 30(4) | 6(3) | -10(3) | -7(3) |
| C29 | 23(4) | 27(4) | 21(4) | 3(3) | -5(3) | -13(3) |
| C30 | 10(3) | 19(4) | 28(4) | 1(3) | 1(3) | 0(3) |
| C31 | 9(3) | 9(3) | 14(3) | 4(3) | -2(2) | 1(2) |
| C32 | 12(3) | 27(4) | 34(4) | 6(3) | -6(3) | -7(3) |
| C33 | 33(4) | 12(3) | 15(3) | -1(3) | -6(3) | -7(3) |
| C34 | 23(4) | 18(4) | 18(4) | 3(3) | 4(3) | -8(3) |
| C35 | 29(4) | 30(4) | 19(4) | 0(3) | 11(3) | -10(3) |
| C36 | 17(4) | 22(4) | 41(5) | 0(3) | 6(3) | 1(3) |
| Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
|---|---|---|---|---|---|---|
| Br1 | Zn1 | 2.3308(11) | Br2 | Zn2 | 2.3231(11) | |
| Zn1 | Zn11 | 2.8889(16) | Zn2 | Zn22 | 2.8794(16) | |
| Zn1 | O11 | 1.961(4) | Zn2 | O2 | 1.973(4) | |
| Zn1 | O1 | 1.970(4) | Zn2 | O22 | 1.976(4) | |
| Zn1 | N1 | 2.072(5) | Zn2 | N2 | 2.073(5) | |
| Fe1 | C1 | 2.062(6) | Fe2 | C19 | 2.058(6) | |
| Fe1 | C2 | 2.027(6) | Fe2 | C20 | 2.039(6) | |
| Fe1 | C3 | 2.049(6) | Fe2 | C21 | 2.051(6) | |
| Fe1 | C4 | 2.061(6) | Fe2 | C22 | 2.044(7) | |
| Fe1 | C5 | 2.060(6) | Fe2 | C23 | 2.053(6) | |
| Fe1 | C6 | 2.056(6) | Fe2 | C24 | 2.051(7) | |
| Fe1 | C7 | 2.055(7) | Fe2 | C25 | 2.044(7) | |
| Fe1 | C8 | 2.040(7) | Fe2 | C26 | 2.043(7) | |
| Fe1 | C9 | 2.045(6) | Fe2 | C27 | 2.052(7) | |
| Fe1 | C10 | 2.040(7) | Fe2 | C28 | 2.060(7) | |
| Si1 | O1 | 1.635(4) | Si3 | O2 | 1.634(4) | |
| Si1 | C1 | 1.872(6) | Si3 | C19 | 1.875(6) | |
| Si1 | C11 | 1.866(6) | Si3 | C29 | 1.860(7) | |
| Si1 | C12 | 1.850(7) | Si3 | C30 | 1.862(6) | |
| Si2 | C3 | 1.861(6) | Si4 | C21 | 1.870(7) | |
| Si2 | C16 | 1.862(7) | Si4 | C34 | 1.869(7) | |
| Si2 | C17 | 1.874(7) | Si4 | C35 | 1.861(7) | |
| Si2 | C18 | 1.868(7) | Si4 | C36 | 1.872(7) | |
| O1 | Zn11 | 1.961(4) | O2 | Zn22 | 1.976(4) | |
| N1 | C13 | 1.507(8) | N2 | C31 | 1.492(7) | |
| N1 | C14 | 1.482(8) | N2 | C32 | 1.488(8) | |
| N1 | C15 | 1.477(8) | N2 | C33 | 1.487(8) | |
| C1 | C2 | 1.451(8) | C19 | C20 | 1.446(9) | |
| C1 | C5 | 1.430(8) | C19 | C23 | 1.423(8) | |
| C2 | C3 | 1.444(9) | C20 | C21 | 1.445(9) | |
| C2 | C13 | 1.492(8) | C20 | C31 | 1.493(8) | |
| C3 | C4 | 1.442(9) | C21 | C22 | 1.430(9) | |
| C4 | C5 | 1.417(9) | C22 | C23 | 1.416(9) | |
| C6 | C7 | 1.417(10) | C24 | C25 | 1.429(11) | |
| C6 | C10 | 1.416(10) | C24 | C28 | 1.400(11) | |
| C7 | C8 | 1.422(9) | C25 | C26 | 1.408(11) | |
| C8 | C9 | 1.397(9) | C26 | C27 | 1.400(10) | |
| C9 | C10 | 1.418(9) | C27 | C28 | 1.409(10) |
| Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|
| Br1 | Zn1 | Zn11 | 136.20(5) | Br2 | Zn2 | Zn22 | 136.25(5) | |
| O1 | Zn1 | Br1 | 127.29(13) | O22 | Zn2 | Br2 | 117.75(13) | |
| O11 | Zn1 | Br1 | 117.04(13) | O2 | Zn2 | Br2 | 126.00(12) | |
| O1 | Zn1 | Zn11 | 42.59(13) | O2 | Zn2 | Zn22 | 43.23(12) | |
| O11 | Zn1 | Zn11 | 42.82(12) | O22 | Zn2 | Zn22 | 43.15(12) | |
| O11 | Zn1 | O1 | 85.41(18) | O2 | Zn2 | O22 | 86.38(18) | |
| O11 | Zn1 | N1 | 107.13(19) | O22 | Zn2 | N2 | 106.51(19) | |
| O1 | Zn1 | N1 | 104.62(18) | O2 | Zn2 | N2 | 104.39(18) | |
| N1 | Zn1 | Br1 | 111.64(14) | N2 | Zn2 | Br2 | 112.11(15) | |
| N1 | Zn1 | Zn11 | 111.84(15) | N2 | Zn2 | Zn22 | 111.43(15) | |
| C2 | Fe1 | C1 | 41.6(2) | C19 | Fe2 | C28 | 131.6(3) | |
| C2 | Fe1 | C3 | 41.5(2) | C20 | Fe2 | C19 | 41.3(2) | |
| C2 | Fe1 | C4 | 68.5(2) | C20 | Fe2 | C21 | 41.4(2) | |
| C2 | Fe1 | C5 | 68.5(2) | C20 | Fe2 | C22 | 68.4(3) | |
| C2 | Fe1 | C6 | 125.1(3) | C20 | Fe2 | C23 | 68.3(2) | |
| C2 | Fe1 | C7 | 107.9(3) | C20 | Fe2 | C24 | 131.7(3) | |
| C2 | Fe1 | C8 | 121.7(3) | C20 | Fe2 | C25 | 108.3(3) | |
| C2 | Fe1 | C9 | 156.3(3) | C20 | Fe2 | C26 | 115.6(3) | |
| C2 | Fe1 | C10 | 161.6(3) | C20 | Fe2 | C27 | 147.5(3) | |
| C3 | Fe1 | C1 | 70.3(2) | C20 | Fe2 | C28 | 170.6(3) | |
| C3 | Fe1 | C4 | 41.1(2) | C21 | Fe2 | C19 | 70.0(2) | |
| C3 | Fe1 | C5 | 69.1(2) | C21 | Fe2 | C23 | 68.9(3) | |
| C3 | Fe1 | C6 | 161.2(3) | C21 | Fe2 | C27 | 115.3(3) | |
| C3 | Fe1 | C7 | 123.7(3) | C21 | Fe2 | C28 | 147.6(3) | |
| C4 | Fe1 | C1 | 68.6(2) | C22 | Fe2 | C19 | 68.6(3) | |
| C5 | Fe1 | C1 | 40.6(2) | C22 | Fe2 | C21 | 40.9(2) | |
| C5 | Fe1 | C4 | 40.2(2) | C22 | Fe2 | C23 | 40.4(3) | |
| C6 | Fe1 | C1 | 108.1(3) | C22 | Fe2 | C24 | 148.1(3) | |
| C6 | Fe1 | C4 | 157.1(3) | C22 | Fe2 | C27 | 109.8(3) | |
| C6 | Fe1 | C5 | 122.6(3) | C22 | Fe2 | C28 | 117.0(3) | |
| C7 | Fe1 | C1 | 122.1(2) | C23 | Fe2 | C19 | 40.5(2) | |
| C7 | Fe1 | C4 | 160.8(3) | C23 | Fe2 | C28 | 110.3(3) | |
| C7 | Fe1 | C5 | 157.8(3) | C24 | Fe2 | C19 | 108.7(3) | |
| C7 | Fe1 | C6 | 40.3(3) | C24 | Fe2 | C21 | 170.6(3) | |
| C8 | Fe1 | C1 | 157.9(3) | C24 | Fe2 | C23 | 116.5(3) | |
| C8 | Fe1 | C3 | 106.3(3) | C24 | Fe2 | C27 | 67.5(3) | |
| C8 | Fe1 | C4 | 123.9(3) | C24 | Fe2 | C28 | 39.8(3) | |
| C8 | Fe1 | C5 | 160.1(3) | C25 | Fe2 | C19 | 115.5(3) | |
| C8 | Fe1 | C6 | 67.8(3) | C25 | Fe2 | C21 | 130.6(3) | |
| C8 | Fe1 | C7 | 40.6(3) | C25 | Fe2 | C22 | 170.1(3) | |
| C8 | Fe1 | C9 | 40.0(3) | C25 | Fe2 | C23 | 148.2(3) | |
| C9 | Fe1 | C1 | 160.6(3) | C25 | Fe2 | C24 | 40.9(3) | |
| C9 | Fe1 | C3 | 119.8(3) | C25 | Fe2 | C27 | 67.6(3) | |
| C9 | Fe1 | C4 | 107.2(3) | C25 | Fe2 | C28 | 67.7(3) | |
| C9 | Fe1 | C5 | 124.2(3) | C26 | Fe2 | C19 | 147.7(3) | |
| C9 | Fe1 | C6 | 67.9(3) | C26 | Fe2 | C21 | 107.9(3) | |
| C9 | Fe1 | C7 | 68.0(3) | C26 | Fe2 | C22 | 131.7(3) | |
| C10 | Fe1 | C1 | 124.1(3) | C26 | Fe2 | C23 | 170.7(3) | |
| C10 | Fe1 | C3 | 155.8(3) | C26 | Fe2 | C24 | 67.9(3) | |
| C10 | Fe1 | C4 | 121.3(3) | C26 | Fe2 | C25 | 40.3(3) | |
| C10 | Fe1 | C5 | 108.0(3) | C26 | Fe2 | C27 | 40.0(3) | |
| C10 | Fe1 | C6 | 40.4(3) | C26 | Fe2 | C28 | 67.4(3) | |
| C10 | Fe1 | C7 | 68.1(3) | C27 | Fe2 | C19 | 170.7(3) | |
| C10 | Fe1 | C8 | 67.8(3) | C27 | Fe2 | C23 | 132.6(3) | |
| C10 | Fe1 | C9 | 40.6(3) | C27 | Fe2 | C28 | 40.1(3) | |
| O1 | Si1 | C1 | 105.0(2) | O2 | Si3 | C19 | 105.4(3) | |
| O1 | Si1 | C11 | 109.8(3) | O2 | Si3 | C29 | 111.5(3) | |
| O1 | Si1 | C12 | 109.5(3) | O2 | Si3 | C30 | 109.3(3) | |
| C11 | Si1 | C1 | 107.0(3) | C29 | Si3 | C19 | 107.3(3) | |
| C12 | Si1 | C1 | 115.9(3) | C29 | Si3 | C30 | 108.1(3) | |
| C12 | Si1 | C11 | 109.6(3) | C30 | Si3 | C19 | 115.1(3) | |
| C3 | Si2 | C16 | 114.2(3) | C21 | Si4 | C36 | 107.4(3) | |
| C3 | Si2 | C17 | 106.4(3) | C34 | Si4 | C21 | 114.2(3) | |
| C3 | Si2 | C18 | 109.6(3) | C34 | Si4 | C36 | 110.8(3) | |
| C16 | Si2 | C17 | 111.9(3) | C35 | Si4 | C21 | 108.7(3) | |
| C16 | Si2 | C18 | 107.6(3) | C35 | Si4 | C34 | 107.0(3) | |
| C18 | Si2 | C17 | 107.0(3) | C35 | Si4 | C36 | 108.6(3) | |
| Zn11 | O1 | Zn1 | 94.59(18) | Zn2 | O2 | Zn22 | 93.62(18) | |
| Si1 | O1 | Zn11 | 140.8(3) | Si3 | O2 | Zn2 | 123.2(2) | |
| Si1 | O1 | Zn1 | 123.4(2) | Si3 | O2 | Zn22 | 141.4(3) | |
| C13 | N1 | Zn1 | 112.3(4) | C31 | N2 | Zn2 | 113.0(4) | |
| C14 | N1 | Zn1 | 109.7(4) | C32 | N2 | Zn2 | 107.4(4) | |
| C14 | N1 | C13 | 107.8(5) | C32 | N2 | C31 | 110.5(5) | |
| C15 | N1 | Zn1 | 107.3(4) | C33 | N2 | Zn2 | 109.4(4) | |
| C15 | N1 | C13 | 110.5(5) | C33 | N2 | C31 | 108.7(5) | |
| C15 | N1 | C14 | 109.1(5) | C33 | N2 | C32 | 107.6(5) | |
| Si1 | C1 | Fe1 | 133.4(3) | Si3 | C19 | Fe2 | 130.6(3) | |
| C2 | C1 | Fe1 | 67.9(3) | C20 | C19 | Fe2 | 68.6(3) | |
| C2 | C1 | Si1 | 129.0(5) | C20 | C19 | Si3 | 127.9(5) | |
| C5 | C1 | Fe1 | 69.7(4) | C23 | C19 | Fe2 | 69.6(4) | |
| C5 | C1 | Si1 | 124.5(5) | C23 | C19 | Si3 | 125.5(5) | |
| C5 | C1 | C2 | 106.0(5) | C23 | C19 | C20 | 106.4(5) | |
| C1 | C2 | Fe1 | 70.5(3) | C19 | C20 | Fe2 | 70.0(3) | |
| C1 | C2 | C13 | 122.3(5) | C19 | C20 | C31 | 122.3(5) | |
| C3 | C2 | Fe1 | 70.1(3) | C21 | C20 | Fe2 | 69.8(4) | |
| C3 | C2 | C1 | 109.7(5) | C21 | C20 | C19 | 109.2(5) | |
| C3 | C2 | C13 | 128.0(6) | C21 | C20 | C31 | 128.4(6) | |
| C13 | C2 | Fe1 | 123.6(4) | C31 | C20 | Fe2 | 123.0(4) | |
| Si2 | C3 | Fe1 | 128.6(3) | Si4 | C21 | Fe2 | 127.7(3) | |
| C2 | C3 | Fe1 | 68.4(3) | C20 | C21 | Fe2 | 68.9(3) | |
| C2 | C3 | Si2 | 135.8(5) | C20 | C21 | Si4 | 134.8(5) | |
| C4 | C3 | Fe1 | 69.9(3) | C22 | C21 | Fe2 | 69.3(4) | |
| C4 | C3 | Si2 | 118.4(5) | C22 | C21 | Si4 | 119.3(5) | |
| C4 | C3 | C2 | 105.7(5) | C22 | C21 | C20 | 105.9(5) | |
| C3 | C4 | Fe1 | 69.0(3) | C21 | C22 | Fe2 | 69.8(4) | |
| C5 | C4 | Fe1 | 69.9(4) | C23 | C22 | Fe2 | 70.1(4) | |
| C5 | C4 | C3 | 109.2(6) | C23 | C22 | C21 | 109.4(6) | |
| C1 | C5 | Fe1 | 69.8(4) | C19 | C23 | Fe2 | 69.9(3) | |
| C4 | C5 | Fe1 | 69.9(4) | C22 | C23 | Fe2 | 69.4(4) | |
| C4 | C5 | C1 | 109.4(5) | C22 | C23 | C19 | 109.1(6) | |
| C7 | C6 | Fe1 | 69.8(4) | C25 | C24 | Fe2 | 69.3(4) | |
| C10 | C6 | Fe1 | 69.2(4) | C28 | C24 | Fe2 | 70.4(4) | |
| C10 | C6 | C7 | 108.1(6) | C28 | C24 | C25 | 107.7(7) | |
| C6 | C7 | Fe1 | 69.9(4) | C24 | C25 | Fe2 | 69.8(4) | |
| C6 | C7 | C8 | 107.2(6) | C26 | C25 | Fe2 | 69.8(4) | |
| C8 | C7 | Fe1 | 69.1(4) | C26 | C25 | C24 | 107.4(7) | |
| C7 | C8 | Fe1 | 70.3(4) | C25 | C26 | Fe2 | 69.9(4) | |
| C9 | C8 | Fe1 | 70.2(4) | C27 | C26 | Fe2 | 70.3(4) | |
| C9 | C8 | C7 | 108.9(6) | C27 | C26 | C25 | 108.4(7) | |
| C8 | C9 | Fe1 | 69.8(4) | C26 | C27 | Fe2 | 69.7(4) | |
| C8 | C9 | C10 | 108.0(6) | C26 | C27 | C28 | 108.2(7) | |
| C10 | C9 | Fe1 | 69.5(4) | C28 | C27 | Fe2 | 70.3(4) | |
| C6 | C10 | Fe1 | 70.4(4) | C24 | C28 | Fe2 | 69.7(4) | |
| C6 | C10 | C9 | 107.9(6) | C24 | C28 | C27 | 108.3(7) | |
| C9 | C10 | Fe1 | 69.9(4) | C27 | C28 | Fe2 | 69.6(4) | |
| C2 | C13 | N1 | 114.5(5) | N2 | C31 | C20 | 114.8(5) |
| A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|---|---|
| Zn1 | N1 | C13 | C2 | -35.2(6) | Zn2 | N2 | C31 | C20 | -36.1(6) | |
| Fe1 | C1 | C2 | C3 | -59.3(4) | Fe2 | C19 | C20 | C21 | -58.9(4) | |
| Fe1 | C1 | C2 | C13 | 118.1(6) | Fe2 | C19 | C20 | C31 | 117.2(6) | |
| Fe1 | C1 | C5 | C4 | 58.8(4) | Fe2 | C19 | C23 | C22 | 58.5(5) | |
| Fe1 | C2 | C3 | Si2 | 123.7(6) | Fe2 | C20 | C21 | Si4 | 122.7(6) | |
| Fe1 | C2 | C3 | C4 | -60.3(4) | Fe2 | C20 | C21 | C22 | -59.7(4) | |
| Fe1 | C2 | C13 | N1 | 173.2(4) | Fe2 | C20 | C31 | N2 | 171.7(4) | |
| Fe1 | C3 | C4 | C5 | -58.4(4) | Fe2 | C21 | C22 | C23 | -59.1(5) | |
| Fe1 | C4 | C5 | C1 | -58.7(4) | Fe2 | C22 | C23 | C19 | -58.8(4) | |
| Fe1 | C6 | C7 | C8 | 59.3(4) | Fe2 | C24 | C25 | C26 | 60.0(5) | |
| Fe1 | C6 | C10 | C9 | -60.1(5) | Fe2 | C24 | C28 | C27 | -59.1(5) | |
| Fe1 | C7 | C8 | C9 | 59.8(5) | Fe2 | C25 | C26 | C27 | 60.0(5) | |
| Fe1 | C8 | C9 | C10 | 59.2(5) | Fe2 | C26 | C27 | C28 | 60.0(5) | |
| Fe1 | C9 | C10 | C6 | 60.4(5) | Fe2 | C27 | C28 | C24 | 59.2(5) | |
| Si1 | C1 | C2 | Fe1 | -128.8(5) | Si3 | C19 | C20 | Fe2 | -125.6(5) | |
| Si1 | C1 | C2 | C3 | 171.9(4) | Si3 | C19 | C20 | C21 | 175.5(4) | |
| Si1 | C1 | C2 | C13 | -10.6(9) | Si3 | C19 | C20 | C31 | -8.4(9) | |
| Si1 | C1 | C5 | Fe1 | 129.4(5) | Si3 | C19 | C23 | Fe2 | 126.0(5) | |
| Si1 | C1 | C5 | C4 | -171.8(4) | Si3 | C19 | C23 | C22 | -175.5(5) | |
| Si2 | C3 | C4 | Fe1 | -123.8(4) | Si4 | C21 | C22 | Fe2 | -122.5(4) | |
| Si2 | C3 | C4 | C5 | 177.8(4) | Si4 | C21 | C22 | C23 | 178.4(5) | |
| O1 | Si1 | C1 | Fe1 | -146.4(4) | O2 | Si3 | C19 | Fe2 | -146.7(4) | |
| O1 | Si1 | C1 | C2 | -50.6(6) | O2 | Si3 | C19 | C20 | -53.3(6) | |
| O1 | Si1 | C1 | C5 | 119.6(5) | O2 | Si3 | C19 | C23 | 120.6(5) | |
| C1 | Si1 | O1 | Zn1 | 1.8(4) | C19 | Si3 | O2 | Zn22 | 163.7(4) | |
| C1 | Si1 | O1 | Zn11 | 165.8(4) | C19 | Si3 | O2 | Zn2 | 3.9(4) | |
| C1 | C2 | C3 | Fe1 | 59.5(4) | C19 | C20 | C21 | Fe2 | 59.1(4) | |
| C1 | C2 | C3 | Si2 | -176.7(5) | C19 | C20 | C21 | Si4 | -178.2(5) | |
| C1 | C2 | C3 | C4 | -0.8(7) | C19 | C20 | C21 | C22 | -0.6(7) | |
| C1 | C2 | C13 | N1 | 86.3(7) | C19 | C20 | C31 | N2 | 85.7(7) | |
| C2 | C1 | C5 | Fe1 | -58.5(4) | C20 | C19 | C23 | Fe2 | -59.0(4) | |
| C2 | C1 | C5 | C4 | 0.3(7) | C20 | C19 | C23 | C22 | -0.5(7) | |
| C2 | C3 | C4 | Fe1 | 59.4(4) | C20 | C21 | C22 | Fe2 | 59.4(4) | |
| C2 | C3 | C4 | C5 | 1.0(7) | C20 | C21 | C22 | C23 | 0.3(7) | |
| C3 | C2 | C13 | N1 | -96.8(7) | C21 | C20 | C31 | N2 | -99.0(7) | |
| C3 | C4 | C5 | Fe1 | 57.9(4) | C21 | C22 | C23 | Fe2 | 58.9(4) | |
| C3 | C4 | C5 | C1 | -0.8(7) | C21 | C22 | C23 | C19 | 0.1(7) | |
| C5 | C1 | C2 | Fe1 | 59.6(4) | C23 | C19 | C20 | Fe2 | 59.6(4) | |
| C5 | C1 | C2 | C3 | 0.3(7) | C23 | C19 | C20 | C21 | 0.7(7) | |
| C5 | C1 | C2 | C13 | 177.7(5) | C23 | C19 | C20 | C31 | 176.8(5) | |
| C6 | C7 | C8 | Fe1 | -59.8(4) | C24 | C25 | C26 | Fe2 | -60.0(5) | |
| C6 | C7 | C8 | C9 | 0.0(7) | C24 | C25 | C26 | C27 | 0.0(8) | |
| C7 | C6 | C10 | Fe1 | 59.1(4) | C25 | C24 | C28 | Fe2 | 59.5(5) | |
| C7 | C6 | C10 | C9 | -1.0(7) | C25 | C24 | C28 | C27 | 0.4(8) | |
| C7 | C8 | C9 | Fe1 | -59.9(5) | C25 | C26 | C27 | Fe2 | -59.7(5) | |
| C7 | C8 | C9 | C10 | -0.7(8) | C25 | C26 | C27 | C28 | 0.3(8) | |
| C8 | C9 | C10 | Fe1 | -59.4(5) | C26 | C27 | C28 | Fe2 | -59.6(5) | |
| C8 | C9 | C10 | C6 | 1.0(8) | C26 | C27 | C28 | C24 | -0.4(8) | |
| C10 | C6 | C7 | Fe1 | -58.7(5) | C28 | C24 | C25 | Fe2 | -60.2(5) | |
| C10 | C6 | C7 | C8 | 0.6(7) | C28 | C24 | C25 | C26 | -0.2(8) | |
| C11 | Si1 | O1 | Zn1 | 116.4(3) | C29 | Si3 | O2 | Zn22 | -80.1(5) | |
| C11 | Si1 | O1 | Zn11 | -79.6(5) | C29 | Si3 | O2 | Zn2 | 120.0(3) | |
| C11 | Si1 | C1 | Fe1 | 97.0(5) | C29 | Si3 | C19 | Fe2 | 94.3(5) | |
| C11 | Si1 | C1 | C2 | -167.3(5) | C29 | Si3 | C19 | C20 | -172.3(5) | |
| C11 | Si1 | C1 | C5 | 3.0(6) | C29 | Si3 | C19 | C23 | 1.6(6) | |
| C12 | Si1 | O1 | Zn1 | -123.3(3) | C30 | Si3 | O2 | Zn22 | 39.4(5) | |
| C12 | Si1 | O1 | Zn11 | 40.8(5) | C30 | Si3 | O2 | Zn2 | -120.5(3) | |
| C12 | Si1 | C1 | Fe1 | -25.6(6) | C30 | Si3 | C19 | Fe2 | -26.1(6) | |
| C12 | Si1 | C1 | C2 | 70.2(6) | C30 | Si3 | C19 | C20 | 67.3(6) | |
| C12 | Si1 | C1 | C5 | -119.5(5) | C30 | Si3 | C19 | C23 | -118.8(5) | |
| C13 | C2 | C3 | Fe1 | -117.7(6) | C31 | C20 | C21 | Fe2 | -116.7(6) | |
| C13 | C2 | C3 | Si2 | 6.0(10) | C31 | C20 | C21 | Si4 | 6.0(10) | |
| C13 | C2 | C3 | C4 | -178.0(6) | C31 | C20 | C21 | C22 | -176.4(6) | |
| C14 | N1 | C13 | C2 | -156.2(5) | C32 | N2 | C31 | C20 | 84.3(6) | |
| C15 | N1 | C13 | C2 | 84.6(6) | C33 | N2 | C31 | C20 | -157.8(5) | |
| C16 | Si2 | C3 | Fe1 | 75.2(5) | C34 | Si4 | C21 | Fe2 | 73.0(5) | |
| C16 | Si2 | C3 | C2 | -23.2(7) | C34 | Si4 | C21 | C20 | -24.2(7) | |
| C16 | Si2 | C3 | C4 | 161.2(5) | C34 | Si4 | C21 | C22 | 158.4(5) | |
| C17 | Si2 | C3 | Fe1 | -160.9(4) | C35 | Si4 | C21 | Fe2 | -46.5(5) | |
| C17 | Si2 | C3 | C2 | 100.7(6) | C35 | Si4 | C21 | C20 | -143.6(6) | |
| C17 | Si2 | C3 | C4 | -74.8(5) | C35 | Si4 | C21 | C22 | 39.0(6) | |
| C18 | Si2 | C3 | Fe1 | -45.5(5) | C36 | Si4 | C21 | Fe2 | -163.7(4) | |
| C18 | Si2 | C3 | C2 | -144.0(6) | C36 | Si4 | C21 | C20 | 99.1(7) | |
| C18 | Si2 | C3 | C4 | 40.5(6) | C36 | Si4 | C21 | C22 | -78.3(6) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| H4 | 6855 | -434 | 1018 | 18 |
| H5 | 4679 | -814 | 1793 | 17 |
| H6 | 1882 | 1788 | 1796 | 26 |
| H7 | 3605 | 2881 | 1877 | 22 |
| H8 | 5458 | 2494 | 659 | 25 |
| H9 | 4893 | 1185 | -163 | 22 |
| H10 | 2706 | 719 | 551 | 26 |
| H11A | 3481 | -1484 | 3282 | 27 |
| H11B | 2360 | -885 | 2673 | 27 |
| H11C | 1914 | -1004 | 3648 | 27 |
| H12A | 1240 | 1070 | 4119 | 29 |
| H12B | 1220 | 1176 | 3117 | 29 |
| H12C | 2160 | 1732 | 3627 | 29 |
| H13A | 4650 | 1918 | 3386 | 13 |
| H13B | 6101 | 2148 | 2976 | 13 |
| H14A | 4707 | 1983 | 4809 | 25 |
| H14B | 5784 | 2652 | 4532 | 25 |
| H14C | 6202 | 1855 | 5235 | 25 |
| H15A | 8388 | 1110 | 4460 | 21 |
| H15B | 8046 | 1994 | 3836 | 21 |
| H15C | 8359 | 954 | 3471 | 21 |
| H16A | 7571 | 2682 | 1740 | 30 |
| H16B | 9242 | 2474 | 1476 | 30 |
| H16C | 8702 | 2241 | 2413 | 30 |
| H17A | 9902 | 76 | 2433 | 28 |
| H17B | 10850 | 360 | 1646 | 28 |
| H17C | 9969 | -446 | 1554 | 28 |
| H18A | 8430 | 424 | 117 | 31 |
| H18B | 9359 | 1217 | 88 | 31 |
| H18C | 7656 | 1509 | 111 | 31 |
| H22 | 10715 | -5287 | 887 | 22 |
| H23 | 8714 | -5609 | 1870 | 19 |
| H24 | 6099 | -3225 | 1976 | 37 |
| H25 | 7699 | -2102 | 2303 | 39 |
| H26 | 9487 | -2121 | 1066 | 33 |
| H27 | 9010 | -3235 | -8 | 32 |
| H28 | 6912 | -3907 | 547 | 31 |
| H29A | 7623 | -6199 | 3397 | 34 |
| H29B | 6425 | -5442 | 2958 | 34 |
| H29C | 6285 | -5632 | 3951 | 34 |
| H30A | 6128 | -3617 | 4425 | 29 |
| H30B | 5972 | -3421 | 3438 | 29 |
| H30C | 7151 | -3037 | 3913 | 29 |
| H31A | 10942 | -2897 | 2903 | 13 |
| H31B | 9540 | -3051 | 3433 | 13 |
| H32A | 13112 | -3227 | 3537 | 36 |
| H32B | 13180 | -4258 | 3190 | 36 |
| H32C | 13483 | -4119 | 4150 | 36 |
| H33A | 10017 | -3057 | 4836 | 29 |
| H33B | 11136 | -2469 | 4442 | 29 |
| H33C | 11640 | -3311 | 5090 | 29 |
| H34A | 12058 | -2318 | 1488 | 29 |
| H34B | 13692 | -2613 | 1149 | 29 |
| H34C | 13238 | -2831 | 2105 | 29 |
| H35A | 12008 | -4433 | -108 | 39 |
| H35B | 13226 | -3838 | -257 | 39 |
| H35C | 11607 | -3313 | -50 | 39 |
| H36A | 14407 | -4962 | 1981 | 42 |
| H36B | 15082 | -4743 | 1072 | 42 |
| H36C | 14089 | -5499 | 1172 | 42 |
Experimental
Single crystals of C36H60Br2Fe2N2O2Si4Zn2 [mo_B0273_0m_4] were []. A suitable crystal was selected and [] on a Bruker SMART APEX2 area detector diffractometer. The crystal was kept at 99.99 K during data collection. Using Olex2 [1], the structure was solved with the ShelXT [2] structure solution program using Direct Methods and refined with the XL [3] refinement package using Least Squares minimisation.
Crystal structure determination of [mo_B0273_0m_4]
Crystal Data for C36H60Br2Fe2N2O2Si4Zn2 (M =1067.48 g/mol): triclinic, space group P-1 (no. 2), a = 9.606(3) Å, b = 14.581(6) Å, c = 15.922(6) Å, α = 88.661(11)°, β = 86.404(8)°, γ = 77.905(11)°, V = 2176.1(13) Å3, Z = 2, T = 99.99 K, μ(MoKα) = 3.722 mm-1, Dcalc = 1.629 g/cm3, 11416 reflections measured (4.344° ≤ 2Θ ≤ 51.996°), 11416 unique (Rint = ?, Rsigma = 0.0452) which were used in all calculations. The final R1 was 0.0482 (I > 2σ(I)) and wR2 was 0.1001 (all data).
Refinement model description
Number of restraints - 0, number of constraints - unknown.
Details:
1. Twinned data refinement
Scales: 0.7583(6) 0.2417(6)
2. 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
3.a Secondary CH2 refined with riding coordinates:
C13(H13A,H13B), C31(H31A,H31B)
3.b Aromatic/amide H refined with riding coordinates:
C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C22(H22), C23(H23),
C24(H24), C25(H25), C26(H26), C27(H27), C28(H28)
3.c Idealised Me refined as rotating group:
C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C29(H29A,
H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C),
C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C)
This report has been created with Olex2, compiled on 2016.02.19 svn.r3266 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.