| Identification code | 3099 |
| Empirical formula | C38H56Br2Fe2N2O3Si2Zn |
| Formula weight | 981.91 |
| Temperature/K | 173 |
| Crystal system | monoclinic |
| Space group | C2/c |
| a/Å | 12.5345(7) |
| b/Å | 27.3803(19) |
| c/Å | 12.0501(9) |
| α/° | 90 |
| β/° | 100.600(7) |
| γ/° | 90 |
| Volume/Å3 | 4065.0(5) |
| Z | 4 |
| ρcalcg/cm3 | 1.604 |
| μ/mm‑1 | 3.352 |
| F(000) | 2008.0 |
| Crystal size/mm3 | 0.3 × 0.2 × 0.1 |
| Radiation | MoKα (λ = 0.71073) |
| 2Θ range for data collection/° | 4.548 to 53.998 |
| Index ranges | -15 ≤ h ≤ 15, -34 ≤ k ≤ 33, -14 ≤ l ≤ 15 |
| Reflections collected | 18217 |
| Independent reflections | 4399 [Rint = 0.0609, Rsigma = 0.0630] |
| Data/restraints/parameters | 4399/0/233 |
| Goodness-of-fit on F2 | 1.045 |
| Final R indexes [I>=2σ (I)] | R1 = 0.0406, wR2 = 0.0669 |
| Final R indexes [all data] | R1 = 0.0659, wR2 = 0.0745 |
| Largest diff. peak/hole / e Å-3 | 0.60/-0.39 |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| Br1 | 927.4(3) | 2054.1(2) | 1342.6(3) | 28.46(11) |
| Zn1 | 0 | 2557.1(2) | 2500 | 19.46(14) |
| Fe1 | 3281.9(4) | 4266.5(2) | 4758.8(4) | 20.61(13) |
| Si1 | 868.9(7) | 3570.3(4) | 3569.7(7) | 16.3(2) |
| O1 | 0 | 3788.8(12) | 2500 | 17.4(7) |
| O2 | 1075.1(15) | 2993.9(8) | 3406.7(17) | 18.2(5) |
| N1 | 3071(2) | 2809.4(11) | 3182(2) | 20.6(7) |
| C1 | 2184(2) | 3896.6(13) | 3550(3) | 19.3(8) |
| C2 | 3267(2) | 3687.0(13) | 3700(3) | 21.1(8) |
| C3 | 3992(3) | 4058.2(14) | 3452(3) | 26.3(9) |
| C4 | 3400(3) | 4490.2(14) | 3164(3) | 27.0(9) |
| C5 | 2299(3) | 4393.7(13) | 3225(3) | 22.9(8) |
| C6 | 3829(3) | 4025.4(16) | 6380(3) | 34.6(10) |
| C7 | 4536(3) | 4383.1(16) | 6078(3) | 34.4(10) |
| C8 | 3945(3) | 4818.7(15) | 5809(3) | 34.1(10) |
| C9 | 2859(3) | 4729.8(15) | 5935(3) | 33.7(10) |
| C10 | 2789(3) | 4240.3(15) | 6292(3) | 31.7(9) |
| C11 | 3581(2) | 3176.2(13) | 4052(3) | 23.7(8) |
| C12 | 3308(3) | 2903.9(15) | 2043(3) | 28.1(9) |
| C13 | 3398(3) | 2307.3(14) | 3567(3) | 29.7(9) |
| C14 | 241(2) | 3709.3(13) | 4824(3) | 19.0(8) |
| C15 | -801(3) | 3412.9(15) | 4820(3) | 29.0(9) |
| C16 | -1345(3) | 3537.8(17) | 5816(4) | 44.6(11) |
| C17 | -1586(4) | 4081.4(18) | 5855(4) | 53.5(13) |
| C18 | -558(3) | 4382.4(17) | 5878(3) | 44.6(11) |
| C19 | -21(3) | 4258.6(14) | 4879(3) | 26.9(8) |
| Atom | U11 | U22 | U33 | U23 | U13 | U12 |
|---|---|---|---|---|---|---|
| Br1 | 21.43(18) | 24.8(2) | 37.6(2) | -8.73(17) | 1.42(15) | 4.15(15) |
| Zn1 | 14.5(3) | 15.0(3) | 27.2(3) | 0 | -0.5(2) | 0 |
| Fe1 | 19.8(2) | 21.8(3) | 18.6(3) | -0.6(2) | -1.0(2) | -5.5(2) |
| Si1 | 13.0(4) | 16.9(5) | 17.9(5) | -1.0(4) | -0.3(4) | -0.8(4) |
| O1 | 13.9(15) | 18(2) | 18.9(17) | 0 | 0.6(13) | 0 |
| O2 | 13.7(10) | 16.7(14) | 22.5(13) | -1.4(10) | -1.1(9) | 0.5(9) |
| N1 | 14.3(14) | 22.1(18) | 24.8(16) | -1.6(13) | 2.1(13) | 2.7(12) |
| C1 | 19.1(16) | 22(2) | 15.8(17) | -2.2(14) | 0.0(14) | -2.8(14) |
| C2 | 20.4(17) | 24(2) | 17.7(18) | -3.4(15) | 0.6(14) | -2.5(14) |
| C3 | 18.2(17) | 39(3) | 21(2) | -1.7(17) | 3.3(15) | -9.0(16) |
| C4 | 31.7(19) | 26(2) | 21.9(19) | 5.6(16) | 2.1(16) | -10.4(17) |
| C5 | 22.7(17) | 22(2) | 20.7(18) | 1.1(16) | -3.1(15) | -3.2(15) |
| C6 | 44(2) | 34(3) | 20(2) | 2.1(17) | -7.7(18) | -7.2(19) |
| C7 | 25.8(19) | 49(3) | 24(2) | -6.7(19) | -7.7(16) | -7.9(19) |
| C8 | 41(2) | 33(3) | 26(2) | -8.9(18) | -0.2(18) | -17.0(19) |
| C9 | 37(2) | 36(3) | 25(2) | -15.7(18) | -3.1(17) | 0.8(19) |
| C10 | 31(2) | 40(3) | 24(2) | -5.4(18) | 4.2(16) | -13.9(18) |
| C11 | 15.2(16) | 29(2) | 25.0(19) | -1.2(16) | -0.9(14) | 2.1(15) |
| C12 | 18.7(17) | 38(3) | 27(2) | -4.3(18) | 2.5(15) | 0.3(16) |
| C13 | 25.4(19) | 23(2) | 39(2) | -1.8(18) | 0.0(17) | 7.1(16) |
| C14 | 18.4(16) | 19(2) | 18.3(17) | -0.7(14) | 0.8(14) | 0.8(14) |
| C15 | 20.7(18) | 35(3) | 32(2) | 2.1(18) | 6.6(16) | -1.9(16) |
| C16 | 36(2) | 57(3) | 46(3) | 9(2) | 22(2) | -2(2) |
| C17 | 56(3) | 65(4) | 49(3) | 7(3) | 37(2) | 18(2) |
| C18 | 63(3) | 39(3) | 34(2) | -5(2) | 16(2) | 16(2) |
| C19 | 28.1(19) | 27(2) | 27(2) | -2.6(17) | 6.3(16) | 4.7(16) |
| Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
|---|---|---|---|---|---|---|
| Br1 | Zn1 | 2.4061(5) | N1 | C12 | 1.480(4) | |
| Zn1 | Br11 | 2.4061(5) | N1 | C13 | 1.484(4) | |
| Zn1 | O2 | 1.974(2) | C1 | C2 | 1.455(4) | |
| Zn1 | O21 | 1.975(2) | C1 | C5 | 1.431(5) | |
| Fe1 | C1 | 2.075(3) | C2 | C3 | 1.431(5) | |
| Fe1 | C2 | 2.034(3) | C2 | C11 | 1.493(5) | |
| Fe1 | C3 | 2.028(4) | C3 | C4 | 1.406(5) | |
| Fe1 | C4 | 2.048(3) | C4 | C5 | 1.420(4) | |
| Fe1 | C5 | 2.054(3) | C6 | C7 | 1.413(5) | |
| Fe1 | C6 | 2.057(3) | C6 | C10 | 1.416(5) | |
| Fe1 | C7 | 2.045(3) | C7 | C8 | 1.410(5) | |
| Fe1 | C8 | 2.047(4) | C8 | C9 | 1.418(5) | |
| Fe1 | C9 | 2.043(4) | C9 | C10 | 1.415(5) | |
| Fe1 | C10 | 2.055(4) | C14 | C15 | 1.538(4) | |
| Si1 | O1 | 1.6398(14) | C14 | C19 | 1.543(5) | |
| Si1 | O2 | 1.617(2) | C15 | C16 | 1.524(5) | |
| Si1 | C1 | 1.878(3) | C16 | C17 | 1.521(6) | |
| Si1 | C14 | 1.867(3) | C17 | C18 | 1.526(6) | |
| O1 | Si11 | 1.6398(14) | C18 | C19 | 1.522(5) | |
| N1 | C11 | 1.506(4) |
| Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|
| Br11 | Zn1 | Br1 | 110.17(3) | O2 | Si1 | C1 | 107.61(14) | |
| O2 | Zn1 | Br11 | 112.29(6) | O2 | Si1 | C14 | 113.45(14) | |
| O21 | Zn1 | Br11 | 108.31(6) | C14 | Si1 | C1 | 114.48(15) | |
| O21 | Zn1 | Br1 | 112.29(6) | Si11 | O1 | Si1 | 137.2(2) | |
| O2 | Zn1 | Br1 | 108.31(6) | Si1 | O2 | Zn1 | 123.40(11) | |
| O2 | Zn1 | O21 | 105.43(13) | C12 | N1 | C11 | 113.4(3) | |
| C2 | Fe1 | C1 | 41.45(12) | C12 | N1 | C13 | 111.1(3) | |
| C2 | Fe1 | C4 | 68.81(14) | C13 | N1 | C11 | 110.1(3) | |
| C2 | Fe1 | C5 | 68.45(14) | Si1 | C1 | Fe1 | 133.92(17) | |
| C2 | Fe1 | C6 | 107.97(15) | C2 | C1 | Fe1 | 67.78(17) | |
| C2 | Fe1 | C7 | 121.78(15) | C2 | C1 | Si1 | 127.7(3) | |
| C2 | Fe1 | C8 | 156.87(14) | C5 | C1 | Fe1 | 68.94(18) | |
| C2 | Fe1 | C9 | 161.06(15) | C5 | C1 | Si1 | 126.1(2) | |
| C2 | Fe1 | C10 | 124.58(15) | C5 | C1 | C2 | 105.7(3) | |
| C3 | Fe1 | C1 | 69.34(13) | C1 | C2 | Fe1 | 70.77(19) | |
| C3 | Fe1 | C2 | 41.25(13) | C1 | C2 | C11 | 126.6(3) | |
| C3 | Fe1 | C4 | 40.35(14) | C3 | C2 | Fe1 | 69.1(2) | |
| C3 | Fe1 | C5 | 67.99(14) | C3 | C2 | C1 | 108.0(3) | |
| C3 | Fe1 | C6 | 121.98(15) | C3 | C2 | C11 | 125.5(3) | |
| C3 | Fe1 | C7 | 105.25(14) | C11 | C2 | Fe1 | 125.5(2) | |
| C3 | Fe1 | C8 | 120.08(15) | C2 | C3 | Fe1 | 69.6(2) | |
| C3 | Fe1 | C9 | 156.93(16) | C4 | C3 | Fe1 | 70.6(2) | |
| C3 | Fe1 | C10 | 159.38(16) | C4 | C3 | C2 | 108.8(3) | |
| C4 | Fe1 | C1 | 68.93(13) | C3 | C4 | Fe1 | 69.1(2) | |
| C4 | Fe1 | C5 | 40.51(12) | C3 | C4 | C5 | 107.7(3) | |
| C4 | Fe1 | C6 | 156.67(15) | C5 | C4 | Fe1 | 69.97(19) | |
| C4 | Fe1 | C10 | 160.05(16) | C1 | C5 | Fe1 | 70.51(18) | |
| C5 | Fe1 | C1 | 40.55(13) | C4 | C5 | Fe1 | 69.52(18) | |
| C5 | Fe1 | C6 | 161.69(14) | C4 | C5 | C1 | 109.8(3) | |
| C5 | Fe1 | C10 | 125.86(14) | C7 | C6 | Fe1 | 69.4(2) | |
| C6 | Fe1 | C1 | 124.92(15) | C7 | C6 | C10 | 107.8(4) | |
| C7 | Fe1 | C1 | 159.71(16) | C10 | C6 | Fe1 | 69.8(2) | |
| C7 | Fe1 | C4 | 120.33(14) | C6 | C7 | Fe1 | 70.29(19) | |
| C7 | Fe1 | C5 | 157.13(15) | C8 | C7 | Fe1 | 69.93(19) | |
| C7 | Fe1 | C6 | 40.29(14) | C8 | C7 | C6 | 108.5(3) | |
| C7 | Fe1 | C8 | 40.30(15) | C7 | C8 | Fe1 | 69.8(2) | |
| C7 | Fe1 | C10 | 67.75(14) | C7 | C8 | C9 | 107.7(4) | |
| C8 | Fe1 | C1 | 159.39(15) | C9 | C8 | Fe1 | 69.6(2) | |
| C8 | Fe1 | C4 | 105.54(15) | C8 | C9 | Fe1 | 69.9(2) | |
| C8 | Fe1 | C5 | 122.64(15) | C10 | C9 | Fe1 | 70.2(2) | |
| C8 | Fe1 | C6 | 67.87(16) | C10 | C9 | C8 | 108.0(3) | |
| C8 | Fe1 | C10 | 67.97(15) | C6 | C10 | Fe1 | 69.9(2) | |
| C9 | Fe1 | C1 | 124.53(14) | C9 | C10 | Fe1 | 69.4(2) | |
| C9 | Fe1 | C4 | 122.55(16) | C9 | C10 | C6 | 108.0(3) | |
| C9 | Fe1 | C5 | 109.28(15) | C2 | C11 | N1 | 111.8(3) | |
| C9 | Fe1 | C6 | 67.92(16) | C15 | C14 | Si1 | 112.0(2) | |
| C9 | Fe1 | C7 | 67.91(15) | C15 | C14 | C19 | 109.1(3) | |
| C9 | Fe1 | C8 | 40.57(14) | C19 | C14 | Si1 | 111.0(2) | |
| C9 | Fe1 | C10 | 40.41(15) | C16 | C15 | C14 | 112.5(3) | |
| C10 | Fe1 | C1 | 110.12(14) | C17 | C16 | C15 | 111.3(3) | |
| C10 | Fe1 | C6 | 40.30(14) | C16 | C17 | C18 | 110.9(3) | |
| O1 | Si1 | C1 | 105.90(13) | C19 | C18 | C17 | 111.1(3) | |
| O1 | Si1 | C14 | 104.13(11) | C18 | C19 | C14 | 112.3(3) | |
| O2 | Si1 | O1 | 111.01(13) |
| D | H | A | d(D-H)/Å | d(H-A)/Å | d(D-A)/Å | D-H-A/° |
|---|---|---|---|---|---|---|
| N1 | H1 | O2 | 0.90(3) | 1.73(4) | 2.615(3) | 169(4) |
| A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|---|---|
| Fe1 | C1 | C2 | C3 | -59.4(2) | C1 | C2 | C11 | N1 | 65.3(4) | |
| Fe1 | C1 | C2 | C11 | 120.5(3) | C2 | C1 | C5 | Fe1 | -58.1(2) | |
| Fe1 | C1 | C5 | C4 | 58.5(2) | C2 | C1 | C5 | C4 | 0.4(4) | |
| Fe1 | C2 | C3 | C4 | -59.9(2) | C2 | C3 | C4 | Fe1 | 59.3(2) | |
| Fe1 | C2 | C11 | N1 | 156.8(2) | C2 | C3 | C4 | C5 | -0.2(4) | |
| Fe1 | C3 | C4 | C5 | -59.5(2) | C3 | C2 | C11 | N1 | -114.9(3) | |
| Fe1 | C4 | C5 | C1 | -59.1(2) | C3 | C4 | C5 | Fe1 | 58.9(2) | |
| Fe1 | C6 | C7 | C8 | 59.7(2) | C3 | C4 | C5 | C1 | -0.2(4) | |
| Fe1 | C6 | C10 | C9 | -59.1(2) | C5 | C1 | C2 | Fe1 | 58.8(2) | |
| Fe1 | C7 | C8 | C9 | 59.5(2) | C5 | C1 | C2 | C3 | -0.5(4) | |
| Fe1 | C8 | C9 | C10 | 60.1(2) | C5 | C1 | C2 | C11 | 179.3(3) | |
| Fe1 | C9 | C10 | C6 | 59.5(2) | C6 | C7 | C8 | Fe1 | -59.9(3) | |
| Si1 | C1 | C2 | Fe1 | -129.2(3) | C6 | C7 | C8 | C9 | -0.5(4) | |
| Si1 | C1 | C2 | C3 | 171.5(2) | C7 | C6 | C10 | Fe1 | 59.2(3) | |
| Si1 | C1 | C2 | C11 | -8.7(5) | C7 | C6 | C10 | C9 | 0.1(4) | |
| Si1 | C1 | C5 | Fe1 | 129.7(3) | C7 | C8 | C9 | Fe1 | -59.6(3) | |
| Si1 | C1 | C5 | C4 | -171.8(2) | C7 | C8 | C9 | C10 | 0.5(4) | |
| Si1 | C14 | C15 | C16 | -177.8(3) | C8 | C9 | C10 | Fe1 | -59.9(2) | |
| Si1 | C14 | C19 | C18 | 178.7(2) | C8 | C9 | C10 | C6 | -0.4(4) | |
| O1 | Si1 | O2 | Zn1 | -26.39(17) | C10 | C6 | C7 | Fe1 | -59.5(2) | |
| O1 | Si1 | C1 | Fe1 | 129.7(2) | C10 | C6 | C7 | C8 | 0.2(4) | |
| O1 | Si1 | C1 | C2 | -135.6(3) | C11 | C2 | C3 | Fe1 | -119.4(3) | |
| O1 | Si1 | C1 | C5 | 34.9(3) | C11 | C2 | C3 | C4 | -179.4(3) | |
| O1 | Si1 | C14 | C15 | 67.6(3) | C12 | N1 | C11 | C2 | 55.1(4) | |
| O1 | Si1 | C14 | C19 | -54.6(2) | C13 | N1 | C11 | C2 | -179.7(3) | |
| O2 | Si1 | O1 | Si11 | 13.49(9) | C14 | Si1 | O1 | Si11 | -108.94(12) | |
| O2 | Si1 | C1 | Fe1 | -111.5(2) | C14 | Si1 | O2 | Zn1 | 90.46(17) | |
| O2 | Si1 | C1 | C2 | -16.8(3) | C14 | Si1 | C1 | Fe1 | 15.6(3) | |
| O2 | Si1 | C1 | C5 | 153.6(3) | C14 | Si1 | C1 | C2 | 110.3(3) | |
| O2 | Si1 | C14 | C15 | -53.2(3) | C14 | Si1 | C1 | C5 | -79.2(3) | |
| O2 | Si1 | C14 | C19 | -175.36(19) | C14 | C15 | C16 | C17 | 55.9(4) | |
| C1 | Si1 | O1 | Si11 | 130.00(12) | C15 | C14 | C19 | C18 | 54.8(4) | |
| C1 | Si1 | O2 | Zn1 | -141.84(15) | C15 | C16 | C17 | C18 | -55.5(5) | |
| C1 | Si1 | C14 | C15 | -177.2(2) | C16 | C17 | C18 | C19 | 55.8(5) | |
| C1 | Si1 | C14 | C19 | 60.6(3) | C17 | C18 | C19 | C14 | -56.3(4) | |
| C1 | C2 | C3 | Fe1 | 60.4(2) | C19 | C14 | C15 | C16 | -54.5(4) | |
| C1 | C2 | C3 | C4 | 0.4(4) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| H1 | 2370(30) | 2835(14) | 3230(30) | 36(11) |
| H3 | 4750 | 4019 | 3479 | 32 |
| H4 | 3685 | 4793 | 2965 | 32 |
| H5 | 1725 | 4625 | 3072 | 27 |
| H6 | 4017 | 3699 | 6602 | 41 |
| H7 | 5284 | 4338 | 6060 | 41 |
| H8 | 4225 | 5118 | 5584 | 41 |
| H9 | 2280 | 4959 | 5803 | 40 |
| H10 | 2156 | 4084 | 6446 | 38 |
| H11A | 3351 | 3106 | 4779 | 28 |
| H11B | 4381 | 3144 | 4169 | 28 |
| H12A | 3056 | 3232 | 1796 | 42 |
| H12B | 2933 | 2661 | 1512 | 42 |
| H12C | 4092 | 2881 | 2067 | 42 |
| H13A | 4175 | 2264 | 3574 | 45 |
| H13B | 2985 | 2070 | 3050 | 45 |
| H13C | 3250 | 2257 | 4329 | 45 |
| H14 | 775 | 3622 | 5519 | 23 |
| H15A | -1316 | 3477 | 4109 | 35 |
| H15B | -623 | 3060 | 4844 | 35 |
| H16A | -2030 | 3352 | 5753 | 54 |
| H16B | -863 | 3440 | 6528 | 54 |
| H17A | -1894 | 4154 | 6536 | 64 |
| H17B | -2131 | 4172 | 5184 | 64 |
| H18A | -743 | 4734 | 5857 | 54 |
| H18B | -43 | 4317 | 6589 | 54 |
| H19A | 659 | 4449 | 4936 | 32 |
| H19B | -509 | 4356 | 4171 | 32 |
Experimental
Single crystals of C38H56Br2Fe2N2O3Si2Zn [3099] 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 [3099]
Crystal Data for C38H56Br2Fe2N2O3Si2Zn (M =981.91 g/mol): monoclinic, space group C2/c (no. 15), a = 12.5345(7) Å, b = 27.3803(19) Å, c = 12.0501(9) Å, β = 100.600(7)°, V = 4065.0(5) Å3, Z = 4, T = 173 K, μ(MoKα) = 3.352 mm-1, Dcalc = 1.604 g/cm3, 18217 reflections measured (4.548° ≤ 2Θ ≤ 53.998°), 4399 unique (Rint = 0.0609, Rsigma = 0.0630) which were used in all calculations. The final R1 was 0.0406 (I > 2σ(I)) and wR2 was 0.0745 (all data).
Refinement model description
Number of restraints - 0, 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.a Ternary CH refined with riding coordinates:
C14(H14)
2.b Secondary CH2 refined with riding coordinates:
C11(H11A,H11B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,
H18B), C19(H19A,H19B)
2.c Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10)
2.d 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.