| Identification code | mo_B0257_0m |
| Empirical formula | C63H71Br3Fe3N3O6Si4Zn1.25 |
| Formula weight | 1567.58 |
| Temperature/K | 123.01 |
| Crystal system | trigonal |
| Space group | P321 |
| a/Å | 16.1933(6) |
| b/Å | 16.1933(6) |
| c/Å | 15.5940(7) |
| α/° | 90 |
| β/° | 90 |
| γ/° | 120 |
| Volume/Å3 | 3541.3(3) |
| Z | 2 |
| ρcalcg/cm3 | 1.470 |
| μ/mm‑1 | 2.827 |
| F(000) | 1589.0 |
| Crystal size/mm3 | 0.822 × 0.758 × 0.566 |
| Radiation | MoKα (λ = 0.71073) |
| 2Θ range for data collection/° | 2.904 to 58.166 |
| Index ranges | -21 ≤ h ≤ 22, -22 ≤ k ≤ 21, -21 ≤ l ≤ 21 |
| Reflections collected | 45279 |
| Independent reflections | 6334 [Rint = 0.0586, Rsigma = 0.0352] |
| Data/restraints/parameters | 6334/19/272 |
| Goodness-of-fit on F2 | 1.064 |
| Final R indexes [I>=2σ (I)] | R1 = 0.0622, wR2 = 0.1677 |
| Final R indexes [all data] | R1 = 0.0699, wR2 = 0.1746 |
| Largest diff. peak/hole / e Å-3 | 2.73/-1.77 |
| Flack parameter | 0.017(5) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| Br1 | 3333 | 6667 | 10442.1(7) | 29.1(3) |
| Zn1 | 3333 | 6667 | 8914.1(7) | 19.2(3) |
| Fe1 | 2576.8(9) | 2831.1(8) | 6845.5(8) | 32.0(3) |
| Si1 | 3567.9(13) | 5253.8(13) | 7598.4(11) | 20.9(4) |
| Si2 | 3333 | 6667 | 6464.0(18) | 20.8(5) |
| O1 | 3732(4) | 5992(4) | 6817(3) | 26.8(10) |
| O2 | 3192(4) | 5483(3) | 8471(3) | 24.3(10) |
| N1 | 1999(5) | 3899(4) | 9231(3) | 28.1(12) |
| C1 | 2608(5) | 4057(5) | 7252(4) | 23.1(12) |
| C2 | 2005(5) | 3252(5) | 7792(5) | 27.5(13) |
| C3 | 1267(7) | 2541(5) | 7276(5) | 37.2(16) |
| C4 | 1373(7) | 2869(6) | 6423(5) | 41.6(19) |
| C5 | 2216(6) | 3805(6) | 6408(5) | 31.5(15) |
| C6 | 3955(8) | 3080(9) | 6818(8) | 61(3) |
| C7 | 3410(15) | 2380(15) | 7390(8) | 86(5) |
| C8 | 2669(13) | 1644(11) | 6995(17) | 122(9) |
| C9 | 2760(12) | 1908(12) | 6095(12) | 89(5) |
| C10 | 3578(10) | 2819(12) | 6035(8) | 69(4) |
| C11 | 2136(5) | 3178(5) | 8728(5) | 27.5(14) |
| C12 | 2313(8) | 3944(7) | 10134(5) | 47(2) |
| C13 | 1006(6) | 3714(6) | 9167(6) | 42(2) |
| C14 | 4752(5) | 5344(6) | 7773(4) | 25.7(12) |
| C15 | 4895(5) | 4885(6) | 8466(5) | 33.0(16) |
| C16 | 5737(7) | 4889(7) | 8601(7) | 48(2) |
| C17 | 6480(7) | 5365(9) | 7994(6) | 50(2) |
| C18 | 6393(7) | 5869(9) | 7323(7) | 53(3) |
| C19 | 5500(6) | 5825(7) | 7207(5) | 37.9(19) |
| C20 | 3407(19) | 6758(16) | 5272(5) | 29(3) |
| C21 | 3760(20) | 6250(20) | 4839(10) | 43(5) |
| C22 | 3840(20) | 6304(18) | 3950(10) | 200(40) |
| C23 | 3562(15) | 6863(15) | 3495(5) | 39(6) |
| C24 | 3210(20) | 7369(19) | 3929(11) | 200(40) |
| C25 | 3130(20) | 7316(17) | 4817(11) | 43(5) |
| Br2 | 540.5(17) | 1552.0(17) | 10787(3) | 84.4(11) |
| Br3 | 0 | 0 | 8601(5) | 156(4) |
| Zn2 | 0 | 0 | 10000 | 45.6(11) |
| Atom | U11 | U22 | U33 | U23 | U13 | U12 |
|---|---|---|---|---|---|---|
| Br1 | 35.2(4) | 35.2(4) | 16.7(5) | 0 | 0 | 17.62(19) |
| Zn1 | 20.1(3) | 20.1(3) | 17.4(5) | 0 | 0 | 10.07(17) |
| Fe1 | 37.8(6) | 29.9(5) | 33.3(6) | -8.7(4) | -1.1(5) | 20.7(5) |
| Si1 | 23.7(8) | 22.1(8) | 18.7(8) | 1.9(6) | 3.1(6) | 12.9(7) |
| Si2 | 22.5(8) | 22.5(8) | 17.4(12) | 0 | 0 | 11.2(4) |
| O1 | 34(3) | 32(3) | 21(2) | 6.1(19) | 4.8(19) | 21(2) |
| O2 | 27(2) | 23(2) | 23(2) | 1.7(18) | 7.5(19) | 12.1(19) |
| N1 | 42(4) | 28(3) | 24(2) | 9(2) | 11(3) | 25(3) |
| C1 | 26(3) | 23(3) | 21(3) | -3(2) | 0(2) | 12(3) |
| C2 | 32(3) | 24(3) | 27(3) | 1(3) | -1(3) | 15(3) |
| C3 | 29(4) | 22(3) | 51(4) | -7(3) | 6(4) | 6(3) |
| C4 | 44(5) | 48(5) | 40(4) | -17(3) | -15(4) | 29(4) |
| C5 | 36(4) | 42(4) | 25(3) | -8(3) | -4(3) | 25(3) |
| C6 | 54(6) | 66(7) | 87(9) | -34(6) | -15(6) | 49(6) |
| C7 | 149(16) | 135(14) | 52(7) | 7(8) | 9(8) | 129(14) |
| C8 | 96(12) | 50(7) | 250(30) | 45(11) | 87(15) | 59(9) |
| C9 | 83(8) | 85(8) | 115(10) | -60(7) | -8(7) | 55(7) |
| C10 | 78(8) | 103(10) | 57(7) | 2(7) | 24(6) | 68(8) |
| C11 | 31(3) | 22(3) | 30(3) | 5(3) | 5(3) | 13(3) |
| C12 | 76(7) | 55(5) | 20(3) | 10(3) | 14(4) | 40(5) |
| C13 | 42(5) | 36(4) | 54(5) | 17(4) | 21(4) | 25(4) |
| C14 | 22(3) | 28(3) | 25(3) | -2(3) | -2(3) | 11(3) |
| C15 | 24(3) | 32(4) | 41(4) | 6(3) | -2(3) | 13(3) |
| C16 | 46(5) | 43(5) | 61(6) | 2(4) | -18(4) | 27(4) |
| C17 | 34(4) | 80(7) | 49(5) | -16(5) | -11(4) | 37(5) |
| C18 | 34(5) | 87(8) | 41(5) | -10(5) | -4(4) | 33(5) |
| C19 | 29(4) | 64(6) | 24(4) | 2(4) | 3(3) | 25(4) |
| C20 | 29(4) | 29(4) | 29(4) | -0.2(14) | -0.1(14) | 14(2) |
| C21 | 79(15) | 44(11) | 24(6) | 18(7) | 25(8) | 45(10) |
| C22 | 530(120) | 180(40) | 30(8) | 66(18) | 90(30) | 280(60) |
| C23 | 39(6) | 39(6) | 38(6) | 0.0(14) | 0.2(14) | 19(3) |
| C24 | 530(120) | 180(40) | 30(8) | 66(18) | 90(30) | 280(60) |
| C25 | 79(15) | 44(11) | 24(6) | 18(7) | 25(8) | 45(10) |
| Br2 | 44.8(11) | 45.5(11) | 175(3) | 31.1(15) | 37.4(15) | 31.8(10) |
| Br3 | 197(6) | 197(6) | 75(4) | 0 | 0 | 98(3) |
| Zn2 | 30.8(13) | 30.8(13) | 75(4) | 0 | 0 | 15.4(7) |
| Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
|---|---|---|---|---|---|---|
| Br1 | Zn1 | 2.3828(15) | C4 | C5 | 1.446(13) | |
| Zn1 | O2 | 1.941(5) | C6 | C7 | 1.36(2) | |
| Zn1 | O21 | 1.941(5) | C6 | C10 | 1.337(17) | |
| Zn1 | O22 | 1.941(5) | C7 | C8 | 1.35(3) | |
| Fe1 | C1 | 2.060(7) | C8 | C9 | 1.45(3) | |
| Fe1 | C2 | 2.033(7) | C9 | C10 | 1.41(2) | |
| Fe1 | C3 | 2.042(9) | C14 | C15 | 1.396(10) | |
| Fe1 | C4 | 2.087(10) | C14 | C19 | 1.381(11) | |
| Fe1 | C5 | 2.053(8) | C15 | C16 | 1.377(11) | |
| Fe1 | C6 | 2.061(11) | C16 | C17 | 1.418(15) | |
| Fe1 | C7 | 2.015(12) | C17 | C18 | 1.378(16) | |
| Fe1 | C8 | 2.015(12) | C18 | C19 | 1.422(12) | |
| Fe1 | C9 | 2.033(11) | C20 | C21 | 1.3900 | |
| Fe1 | C10 | 2.064(10) | C20 | C25 | 1.3900 | |
| Si1 | O1 | 1.633(5) | C21 | C22 | 1.3900 | |
| Si1 | O2 | 1.608(5) | C22 | C23 | 1.3900 | |
| Si1 | C1 | 1.858(7) | C23 | C24 | 1.3900 | |
| Si1 | C14 | 1.869(7) | C24 | C25 | 1.3900 | |
| Si2 | O12 | 1.618(5) | Br2 | Br33 | 2.407(4) | |
| Si2 | O11 | 1.618(5) | Br2 | Zn2 | 2.528(3) | |
| Si2 | O1 | 1.618(5) | Br3 | Br24 | 2.407(4) | |
| Si2 | C20 | 1.864(9) | Br3 | Br23 | 2.407(4) | |
| N1 | C11 | 1.512(9) | Br3 | Br25 | 2.407(4) | |
| N1 | C12 | 1.487(10) | Br3 | Zn2 | 2.182(8) | |
| N1 | C13 | 1.484(11) | Zn2 | Br25 | 2.528(3) | |
| C1 | C2 | 1.445(10) | Zn2 | Br26 | 2.528(3) | |
| C1 | C5 | 1.428(10) | Zn2 | Br23 | 2.528(3) | |
| C2 | C3 | 1.424(10) | Zn2 | Br24 | 2.528(3) | |
| C2 | C11 | 1.488(10) | Zn2 | Br27 | 2.528(3) | |
| C3 | C4 | 1.410(12) | Zn2 | Br33 | 2.182(8) |
| Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|
| O21 | Zn1 | Br1 | 110.85(14) | C3 | C2 | C11 | 125.8(7) | |
| O22 | Zn1 | Br1 | 110.85(14) | C11 | C2 | Fe1 | 125.3(5) | |
| O2 | Zn1 | Br1 | 110.85(14) | C2 | C3 | Fe1 | 69.2(5) | |
| O21 | Zn1 | O22 | 108.05(15) | C4 | C3 | Fe1 | 71.7(5) | |
| O22 | Zn1 | O2 | 108.05(15) | C4 | C3 | C2 | 109.5(7) | |
| O21 | Zn1 | O2 | 108.05(15) | C3 | C4 | Fe1 | 68.3(5) | |
| C1 | Fe1 | C4 | 69.0(3) | C3 | C4 | C5 | 106.4(7) | |
| C1 | Fe1 | C6 | 108.4(4) | C5 | C4 | Fe1 | 68.3(5) | |
| C1 | Fe1 | C10 | 123.8(5) | C1 | C5 | Fe1 | 70.0(4) | |
| C2 | Fe1 | C1 | 41.4(3) | C1 | C5 | C4 | 109.7(7) | |
| C2 | Fe1 | C3 | 40.9(3) | C4 | C5 | Fe1 | 70.8(5) | |
| C2 | Fe1 | C4 | 68.3(3) | C7 | C6 | Fe1 | 68.7(8) | |
| C2 | Fe1 | C5 | 68.4(3) | C10 | C6 | Fe1 | 71.2(7) | |
| C2 | Fe1 | C6 | 125.4(4) | C10 | C6 | C7 | 109.3(13) | |
| C2 | Fe1 | C10 | 160.0(5) | C6 | C7 | Fe1 | 72.3(7) | |
| C3 | Fe1 | C1 | 69.1(3) | C8 | C7 | Fe1 | 70.5(9) | |
| C3 | Fe1 | C4 | 39.9(4) | C8 | C7 | C6 | 110.9(14) | |
| C3 | Fe1 | C5 | 67.9(3) | C7 | C8 | Fe1 | 70.5(7) | |
| C3 | Fe1 | C6 | 161.8(5) | C7 | C8 | C9 | 105.5(13) | |
| C3 | Fe1 | C10 | 158.3(5) | C9 | C8 | Fe1 | 69.7(8) | |
| C5 | Fe1 | C1 | 40.6(3) | C8 | C9 | Fe1 | 68.3(7) | |
| C5 | Fe1 | C4 | 40.9(3) | C10 | C9 | Fe1 | 71.1(7) | |
| C5 | Fe1 | C6 | 122.6(5) | C10 | C9 | C8 | 106.1(14) | |
| C5 | Fe1 | C10 | 109.3(5) | C6 | C10 | Fe1 | 71.0(6) | |
| C6 | Fe1 | C4 | 157.5(5) | C6 | C10 | C9 | 108.2(14) | |
| C6 | Fe1 | C10 | 37.8(5) | C9 | C10 | Fe1 | 68.7(7) | |
| C7 | Fe1 | C1 | 121.4(6) | C2 | C11 | N1 | 111.4(6) | |
| C7 | Fe1 | C2 | 108.4(4) | C15 | C14 | Si1 | 120.5(6) | |
| C7 | Fe1 | C3 | 125.8(6) | C19 | C14 | Si1 | 121.9(5) | |
| C7 | Fe1 | C4 | 161.4(7) | C19 | C14 | C15 | 117.5(7) | |
| C7 | Fe1 | C5 | 156.6(7) | C16 | C15 | C14 | 122.9(8) | |
| C7 | Fe1 | C6 | 39.1(6) | C15 | C16 | C17 | 118.0(9) | |
| C7 | Fe1 | C9 | 66.8(7) | C18 | C17 | C16 | 121.3(8) | |
| C7 | Fe1 | C10 | 65.4(5) | C17 | C18 | C19 | 118.0(9) | |
| C8 | Fe1 | C1 | 155.0(8) | C14 | C19 | C18 | 122.0(9) | |
| C8 | Fe1 | C2 | 120.0(7) | C21 | C20 | Si2 | 117.9(11) | |
| C8 | Fe1 | C3 | 107.8(5) | C21 | C20 | C25 | 120.0 | |
| C8 | Fe1 | C4 | 125.5(7) | C25 | C20 | Si2 | 122.1(11) | |
| C8 | Fe1 | C5 | 163.1(8) | C20 | C21 | C22 | 120.0 | |
| C8 | Fe1 | C6 | 66.4(6) | C21 | C22 | C23 | 120.0 | |
| C8 | Fe1 | C7 | 39.0(8) | C24 | C23 | C22 | 120.0 | |
| C8 | Fe1 | C9 | 42.0(8) | C25 | C24 | C23 | 120.0 | |
| C8 | Fe1 | C10 | 68.2(6) | C24 | C25 | C20 | 120.0 | |
| C9 | Fe1 | C1 | 160.6(6) | Br33 | Br2 | Zn2 | 52.41(18) | |
| C9 | Fe1 | C2 | 157.3(6) | Br23 | Br3 | Br24 | 105.3(2) | |
| C9 | Fe1 | C3 | 122.4(5) | Br23 | Br3 | Br25 | 105.3(2) | |
| C9 | Fe1 | C4 | 108.8(5) | Br24 | Br3 | Br25 | 105.3(2) | |
| C9 | Fe1 | C5 | 125.2(6) | Zn2 | Br3 | Br25 | 66.6(2) | |
| C9 | Fe1 | C6 | 65.8(5) | Zn2 | Br3 | Br23 | 66.6(2) | |
| C9 | Fe1 | C10 | 40.2(6) | Zn2 | Br3 | Br24 | 66.6(2) | |
| C10 | Fe1 | C4 | 123.8(5) | Br24 | Zn2 | Br23 | 98.41(10) | |
| O1 | Si1 | C1 | 107.0(3) | Br26 | Zn2 | Br25 | 95.83(10) | |
| O1 | Si1 | C14 | 105.5(3) | Br25 | Zn2 | Br2 | 69.61(15) | |
| O2 | Si1 | O1 | 113.8(3) | Br23 | Zn2 | Br25 | 98.41(10) | |
| O2 | Si1 | C1 | 105.7(3) | Br24 | Zn2 | Br27 | 95.83(10) | |
| O2 | Si1 | C14 | 110.5(3) | Br27 | Zn2 | Br25 | 162.64(10) | |
| C1 | Si1 | C14 | 114.5(3) | Br24 | Zn2 | Br26 | 69.61(15) | |
| O12 | Si2 | O1 | 109.02(19) | Br23 | Zn2 | Br2 | 95.83(10) | |
| O11 | Si2 | O1 | 109.02(19) | Br27 | Zn2 | Br26 | 98.41(10) | |
| O11 | Si2 | O12 | 109.02(19) | Br24 | Zn2 | Br2 | 162.64(10) | |
| O12 | Si2 | C20 | 105.8(8) | Br27 | Zn2 | Br2 | 98.41(10) | |
| O1 | Si2 | C20 | 111.2(7) | Br24 | Zn2 | Br25 | 98.41(10) | |
| O11 | Si2 | C20 | 112.6(8) | Br26 | Zn2 | Br23 | 162.64(10) | |
| Si2 | O1 | Si1 | 140.8(3) | Br26 | Zn2 | Br2 | 98.41(10) | |
| Si1 | O2 | Zn1 | 131.1(3) | Br27 | Zn2 | Br23 | 69.61(15) | |
| C12 | N1 | C11 | 110.5(6) | Br3 | Zn2 | Br25 | 60.94(8) | |
| C13 | N1 | C11 | 111.8(7) | Br3 | Zn2 | Br27 | 119.06(8) | |
| C13 | N1 | C12 | 112.5(7) | Br33 | Zn2 | Br25 | 119.06(8) | |
| Si1 | C1 | Fe1 | 134.4(4) | Br3 | Zn2 | Br23 | 60.94(8) | |
| C2 | C1 | Fe1 | 68.3(4) | Br33 | Zn2 | Br2 | 60.94(8) | |
| C2 | C1 | Si1 | 127.3(5) | Br3 | Zn2 | Br26 | 119.06(8) | |
| C5 | C1 | Fe1 | 69.4(4) | Br33 | Zn2 | Br27 | 60.94(8) | |
| C5 | C1 | Si1 | 125.9(6) | Br3 | Zn2 | Br24 | 60.94(8) | |
| C5 | C1 | C2 | 106.0(6) | Br33 | Zn2 | Br24 | 119.06(8) | |
| C1 | C2 | Fe1 | 70.3(4) | Br33 | Zn2 | Br23 | 119.06(8) | |
| C1 | C2 | C11 | 125.8(6) | Br3 | Zn2 | Br2 | 119.06(8) | |
| C3 | C2 | Fe1 | 69.9(5) | Br33 | Zn2 | Br26 | 60.94(8) | |
| C3 | C2 | C1 | 108.3(6) | Br3 | Zn2 | Br33 | 180.0 |
| D | H | A | d(D-H)/Å | d(H-A)/Å | d(D-A)/Å | D-H-A/° |
|---|---|---|---|---|---|---|
| N1 | H1 | O2 | 1.00 | 1.61 | 2.600(8) | 170.6 |
| A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|---|---|
| Fe1 | C1 | C2 | C3 | -59.8(6) | C1 | C2 | C3 | Fe1 | 60.0(5) | |
| Fe1 | C1 | C2 | C11 | 119.9(7) | C1 | C2 | C3 | C4 | -0.6(10) | |
| Fe1 | C1 | C5 | C4 | 59.9(6) | C1 | C2 | C11 | N1 | 65.5(9) | |
| Fe1 | C2 | C3 | C4 | -60.7(7) | C2 | C1 | C5 | Fe1 | -58.8(5) | |
| Fe1 | C2 | C11 | N1 | 155.6(5) | C2 | C1 | C5 | C4 | 1.1(9) | |
| Fe1 | C3 | C4 | C5 | -57.8(6) | C2 | C3 | C4 | Fe1 | 59.1(6) | |
| Fe1 | C4 | C5 | C1 | -59.4(5) | C2 | C3 | C4 | C5 | 1.3(10) | |
| Fe1 | C6 | C7 | C8 | 60.2(9) | C3 | C2 | C11 | N1 | -114.8(8) | |
| Fe1 | C6 | C10 | C9 | -58.9(9) | C3 | C4 | C5 | Fe1 | 57.9(6) | |
| Fe1 | C7 | C8 | C9 | 61.3(9) | C3 | C4 | C5 | C1 | -1.5(10) | |
| Fe1 | C8 | C9 | C10 | 61.4(9) | C5 | C1 | C2 | Fe1 | 59.5(5) | |
| Fe1 | C9 | C10 | C6 | 60.3(8) | C5 | C1 | C2 | C3 | -0.3(8) | |
| Si1 | C1 | C2 | Fe1 | -130.0(6) | C5 | C1 | C2 | C11 | 179.4(7) | |
| Si1 | C1 | C2 | C3 | 170.2(6) | C6 | C7 | C8 | Fe1 | -61.3(9) | |
| Si1 | C1 | C2 | C11 | -10.1(11) | C6 | C7 | C8 | C9 | 0.0(14) | |
| Si1 | C1 | C5 | Fe1 | 130.6(6) | C7 | C6 | C10 | Fe1 | 58.2(8) | |
| Si1 | C1 | C5 | C4 | -169.5(6) | C7 | C6 | C10 | C9 | -0.7(13) | |
| Si1 | C14 | C15 | C16 | 176.7(7) | C7 | C8 | C9 | Fe1 | -61.8(9) | |
| Si1 | C14 | C19 | C18 | -177.9(8) | C7 | C8 | C9 | C10 | -0.4(14) | |
| Si2 | C20 | C21 | C22 | -179.4(17) | C8 | C9 | C10 | Fe1 | -59.6(8) | |
| Si2 | C20 | C25 | C24 | 179.4(18) | C8 | C9 | C10 | C6 | 0.7(14) | |
| O1 | Si1 | O2 | Zn1 | -26.0(5) | C10 | C6 | C7 | Fe1 | -59.7(8) | |
| O1 | Si1 | C1 | Fe1 | 106.0(5) | C10 | C6 | C7 | C8 | 0.4(14) | |
| O1 | Si1 | C1 | C2 | -158.4(6) | C11 | C2 | C3 | Fe1 | -119.7(7) | |
| O1 | Si1 | C1 | C5 | 10.3(7) | C11 | C2 | C3 | C4 | 179.7(8) | |
| O1 | Si1 | C14 | C15 | 172.5(6) | C12 | N1 | C11 | C2 | -169.0(7) | |
| O1 | Si1 | C14 | C19 | -10.5(8) | C13 | N1 | C11 | C2 | 64.8(8) | |
| O11 | Si2 | O1 | Si1 | -23.6(6) | C14 | Si1 | O1 | Si2 | -150.5(5) | |
| O12 | Si2 | O1 | Si1 | 95.3(4) | C14 | Si1 | O2 | Zn1 | 92.5(5) | |
| O12 | Si2 | C20 | C21 | 119.2(14) | C14 | Si1 | C1 | Fe1 | -10.4(6) | |
| O11 | Si2 | C20 | C21 | -121.8(14) | C14 | Si1 | C1 | C2 | 85.1(7) | |
| O1 | Si2 | C20 | C21 | 1.0(16) | C14 | Si1 | C1 | C5 | -106.2(6) | |
| O11 | Si2 | C20 | C25 | 58.9(19) | C14 | C15 | C16 | C17 | -1.3(14) | |
| O12 | Si2 | C20 | C25 | -60.2(18) | C15 | C14 | C19 | C18 | -0.8(14) | |
| O1 | Si2 | C20 | C25 | -178.4(15) | C15 | C16 | C17 | C18 | 4.6(16) | |
| O2 | Si1 | O1 | Si2 | -29.1(7) | C16 | C17 | C18 | C19 | -5.8(16) | |
| O2 | Si1 | C1 | Fe1 | -132.3(5) | C17 | C18 | C19 | C14 | 3.9(16) | |
| O2 | Si1 | C1 | C2 | -36.8(7) | C19 | C14 | C15 | C16 | -0.5(13) | |
| O2 | Si1 | C1 | C5 | 131.9(6) | C20 | Si2 | O1 | Si1 | -148.4(10) | |
| O2 | Si1 | C14 | C15 | 49.0(7) | C20 | C21 | C22 | C23 | 0.0 | |
| O2 | Si1 | C14 | C19 | -133.9(7) | C21 | C20 | C25 | C24 | 0.0 | |
| C1 | Si1 | O1 | Si2 | 87.2(6) | C21 | C22 | C23 | C24 | 0.0 | |
| C1 | Si1 | O2 | Zn1 | -143.1(4) | C22 | C23 | C24 | C25 | 0.0 | |
| C1 | Si1 | C14 | C15 | -70.2(7) | C23 | C24 | C25 | C20 | 0.0 | |
| C1 | Si1 | C14 | C19 | 106.8(7) | C25 | C20 | C21 | C22 | 0.0 |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| H1 | 2423 | 4538 | 8968 | 34 |
| H3 | 779 | 1938 | 7475 | 45 |
| H4 | 970 | 2540 | 5952 | 50 |
| H5 | 2471 | 4193 | 5913 | 38 |
| H6 | 4516 | 3662 | 6955 | 73 |
| H7 | 3536 | 2408 | 7988 | 104 |
| H8 | 2187 | 1072 | 7250 | 146 |
| H9 | 2341 | 1513 | 5613 | 106 |
| H10 | 3819 | 3184 | 5525 | 83 |
| H11A | 2785 | 3285 | 8834 | 33 |
| H11B | 1671 | 2528 | 8928 | 33 |
| H12A | 1921 | 3323 | 10409 | 71 |
| H12B | 2243 | 4432 | 10444 | 71 |
| H12C | 2984 | 4108 | 10143 | 71 |
| H13A | 865 | 3787 | 8570 | 62 |
| H13B | 935 | 4169 | 9529 | 62 |
| H13C | 564 | 3063 | 9361 | 62 |
| H15 | 4389 | 4556 | 8863 | 40 |
| H16 | 5818 | 4581 | 9086 | 57 |
| H17 | 7050 | 5337 | 8052 | 60 |
| H18 | 6913 | 6235 | 6948 | 64 |
| H19 | 5416 | 6135 | 6726 | 45 |
| H21 | 3953 | 5870 | 5150 | 51 |
| H22 | 4083 | 5959 | 3654 | 243 |
| H23 | 3615 | 6899 | 2888 | 47 |
| H24 | 3016 | 7751 | 3618 | 243 |
| H25 | 2886 | 7662 | 5113 | 51 |
| Atom | Occupancy | Atom | Occupancy | Atom | Occupancy | ||
|---|---|---|---|---|---|---|---|
| C20 | 0.3333 | C21 | 0.3333 | H21 | 0.3333 | ||
| C22 | 0.3333 | H22 | 0.3333 | C23 | 0.3333 | ||
| H23 | 0.3333 | C24 | 0.3333 | H24 | 0.3333 | ||
| C25 | 0.3333 | H25 | 0.3333 | Br2 | 0.5 | ||
| Br3 | 0.5 | Zn2 | 0.5 |
| Number | X | Y | Z | Volume | Electron count | Content |
|---|---|---|---|---|---|---|
| 1 | 0.000 | 0.000 | 0.500 | 364.0 | 154.7 | Aceton und/oder Wasser? |
Experimental
Single crystals of C63H71Br3Fe3N3O6Si4Zn1.25 [mo_B0257_0m] were []. A suitable crystal was selected and [] on a 'Bruker APEX-II CCD' diffractometer. The crystal was kept at 123.01 K during data collection. Using Olex2 [1], the structure was solved with the XT [2] structure solution program using Direct Methods and refined with the XL [3] refinement package using Least Squares minimisation.
Crystal structure determination of [mo_B0257_0m]
Crystal Data for C63H71Br3Fe3N3O6Si4Zn1.25 (M =1567.58 g/mol): trigonal, space group P321 (no. 150), a = 16.1933(6) Å, c = 15.5940(7) Å, V = 3541.3(3) Å3, Z = 2, T = 123.01 K, μ(MoKα) = 2.827 mm-1, Dcalc = 1.470 g/cm3, 45279 reflections measured (2.904° ≤ 2Θ ≤ 58.166°), 6334 unique (Rint = 0.0586, Rsigma = 0.0352) which were used in all calculations. The final R1 was 0.0622 (I > 2σ(I)) and wR2 was 0.1746 (all data).
Refinement model description
Number of restraints - 19, number of constraints - unknown.
Details:
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All N(H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Rigid bond restraints
C21, C22
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C9) ≈ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
Uanis(C20) ≈ Ueq, Uanis(C20) ≈ Ueq, Uanis(C20) ≈ Ueq, Uanis(C23)
≈ Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C23) = Uanis(C23) = Uanis(C23)
Uanis(C20) = Uanis(C20) = Uanis(C20)
Uanis(C22) = Uanis(C22) = Uanis(C22) = Uanis(C24) = Uanis(C24) = Uanis(C24)
Uanis(C21) = Uanis(C21) = Uanis(C21) = Uanis(C25) = Uanis(C25) = Uanis(C25)
4. Others
Fixed Sof: C20(0.33333) C21(0.33333) H21(0.33333) C22(0.33333) H22(0.33333)
C23(0.33333) H23(0.33333) C24(0.33333) H24(0.33333) C25(0.33333) H25(0.33333)
Br2(0.5) Br3(0.16667) Zn2(0.08333)
5.a Ternary CH refined with riding coordinates:
N1(H1), C9(H9)
5.b Secondary CH2 refined with riding coordinates:
C11(H11A,H11B)
5.c Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C15(H15), C16(H16),
C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25)
5.d Fitted hexagon refined as free rotating group:
C20(C21,C22,C23,C24,C25)
5.e Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)
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.