| Identification code | |
| Empirical formula | C23H24ClFeNO2SiZn |
| Formula weight | 531.19 |
| Temperature/K | 150 |
| Crystal system | monoclinic |
| Space group | P21/c |
| a/Å | 12.1782(18) |
| b/Å | 10.3464(7) |
| c/Å | 18.1035(15) |
| α/° | 90.00 |
| β/° | 99.600(8) |
| γ/° | 90.00 |
| Volume/Å3 | 2249.1(4) |
| Z | 4 |
| ρcalcmg/mm3 | 1.569 |
| m/mm‑1 | 1.903 |
| F(000) | 1088.0 |
| Crystal size/mm3 | 0.106 × 0.094 × 0.056 |
| 2Θ range for data collection | 4.56 to 54° |
| Index ranges | -15 ≤ h ≤ 15, -13 ≤ k ≤ 13, -23 ≤ l ≤ 22 |
| Reflections collected | 20563 |
| Independent reflections | 4906[R(int) = 0.0476] |
| Data/restraints/parameters | 4906/1/277 |
| Goodness-of-fit on F2 | 1.036 |
| Final R indexes [I>=2σ (I)] | R1 = 0.0373, wR2 = 0.0791 |
| Final R indexes [all data] | R1 = 0.0536, wR2 = 0.0855 |
| Largest diff. peak/hole / e Å-3 | 0.81/-0.34 |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| Zn1 | 9712.6(3) | 153.1(3) | 750.39(17) | 19.82(9) |
| Fe2 | 13418.2(3) | -702.9(4) | 2494.5(2) | 22.77(11) |
| Si3 | 12322.7(6) | 274.3(7) | 671.7(4) | 19.17(17) |
| Cl4 | 8863.8(8) | 1856.1(8) | 1139.0(5) | 40.1(2) |
| O1 | 11031.0(15) | 353.3(17) | 269.4(10) | 20.1(4) |
| C2 | 11758(2) | -574(3) | 2121.0(15) | 19.9(6) |
| C5 | 12359(2) | 283(2) | 1691.3(16) | 20.8(6) |
| C6 | 12742(2) | 874(3) | 2942.7(17) | 27.5(7) |
| C12 | 14110(3) | -2233(3) | 2034.3(18) | 33.9(8) |
| C13 | 12008(2) | -195(3) | 2889.6(16) | 25.7(6) |
| C16 | 12961(2) | 1164(3) | 2218.2(16) | 25.1(6) |
| C18 | 13864(3) | -2573(3) | 2738(2) | 40.4(8) |
| C28 | 14863(3) | -1199(3) | 2139(2) | 43.1(9) |
| C39 | 15081(3) | -902(4) | 2901(2) | 48.7(10) |
| C41 | 14471(3) | -1744(4) | 3269.2(19) | 46.3(10) |
| N2 | 9857(2) | -1329(2) | 1523.9(13) | 24.4(5) |
| C3 | 11052(2) | -1685(3) | 1805.7(16) | 23.3(6) |
| C4 | 9304(3) | -978(4) | 2168.3(18) | 38.3(8) |
| C1 | 9296(3) | -2492(3) | 1149.8(18) | 37.0(8) |
| C7 | 12718(2) | 2999(3) | 414.9(15) | 21.8(6) |
| C8 | 11799(3) | 3336(3) | 758.6(17) | 28.2(7) |
| C9 | 13997(2) | 1458(3) | 24.9(17) | 29.5(7) |
| C11 | 11408(3) | 4580(3) | 743(2) | 40.9(9) |
| C10 | 13090(2) | 1693(3) | 371.1(15) | 21.7(6) |
| C14 | 13254(3) | 4005(3) | 68.7(16) | 27.7(7) |
| C15 | 14177(3) | 3686(3) | -275.5(17) | 34.3(8) |
| C17 | 11927(3) | 5552(3) | 385(2) | 46.9(10) |
| C19 | 12827(3) | 5276(3) | 65.8(19) | 39.7(8) |
| C1A | 14554(3) | 2457(3) | -289.0(18) | 36.0(8) |
| O2 | 12881.5(18) | -1057.5(19) | 408.8(12) | 30.0(5) |
| Atom | U11 | U22 | U33 | U23 | U13 | U12 |
|---|---|---|---|---|---|---|
| Zn1 | 22.74(18) | 20.33(17) | 15.84(17) | 0.49(12) | 1.58(13) | 0.35(13) |
| Fe2 | 24.9(2) | 22.9(2) | 18.4(2) | 0.80(16) | -2.45(16) | 4.38(17) |
| Si3 | 20.9(4) | 16.7(4) | 19.0(4) | 1.8(3) | 0.8(3) | 1.4(3) |
| Cl4 | 54.4(5) | 32.1(4) | 34.0(5) | -8.2(3) | 8.4(4) | 12.8(4) |
| O1 | 21.3(10) | 21.3(10) | 16.7(10) | 1.6(7) | 0.0(8) | -0.8(8) |
| C2 | 21.0(14) | 20.7(14) | 17.1(14) | 2.3(11) | -0.1(11) | 2.7(11) |
| C5 | 20.2(14) | 17.7(13) | 22.6(15) | 2.7(11) | -1.5(11) | 2.3(11) |
| C6 | 31.0(16) | 24.5(15) | 23.0(16) | -6.3(12) | -6.9(13) | 5.9(13) |
| C12 | 37.4(19) | 31.0(17) | 30.2(18) | -5.9(13) | -3.6(14) | 15.7(14) |
| C13 | 27.3(16) | 29.4(15) | 19.3(15) | 2.6(12) | 0.5(12) | 6.3(13) |
| C16 | 25.2(15) | 20.3(14) | 27.2(16) | 0.1(12) | -3.1(13) | -1.0(12) |
| C18 | 45(2) | 25.2(17) | 53(2) | 10.8(15) | 11.4(18) | 13.8(15) |
| C28 | 34.2(19) | 47(2) | 50(2) | 5.7(17) | 11.6(17) | 15.0(17) |
| C39 | 29.9(19) | 41(2) | 68(3) | -11.3(19) | -14.1(18) | 12.0(16) |
| C41 | 58(2) | 50(2) | 26.1(19) | 2.2(16) | -8.0(17) | 36.7(19) |
| N2 | 25.6(13) | 28.0(13) | 19.1(13) | 5.6(10) | 2.1(10) | -5(1) |
| C3 | 26.6(15) | 19.7(14) | 23.2(15) | 5.1(11) | 2.4(12) | -2.2(12) |
| C4 | 29.5(18) | 59(2) | 28.1(18) | 13.9(16) | 10.9(14) | 2.8(16) |
| C1 | 38.8(19) | 31.5(17) | 36.0(19) | 8.9(14) | -7.5(15) | -16.0(15) |
| C7 | 23.9(15) | 21.6(14) | 18.5(14) | 2.3(11) | -0.3(12) | -3.0(12) |
| C8 | 34.0(17) | 21.7(15) | 30.2(17) | 0.0(12) | 8.7(14) | -4.6(13) |
| C9 | 20.9(15) | 39.0(18) | 28.1(17) | 3.8(13) | 2.9(13) | 3.9(13) |
| C11 | 56(2) | 25.6(17) | 45(2) | 0.8(14) | 21.8(18) | 8.7(16) |
| C10 | 19.1(14) | 26.8(15) | 16.9(14) | 3.3(11) | -3.8(11) | -2.7(12) |
| C14 | 31.4(17) | 29.3(16) | 20.9(15) | 2.9(12) | -0.2(13) | -10.2(13) |
| C15 | 30.6(18) | 46(2) | 25.4(17) | 8.3(14) | 3.1(14) | -16.3(15) |
| C17 | 70(3) | 19.4(16) | 54(2) | 4.0(15) | 19(2) | 2.4(17) |
| C19 | 56(2) | 25.4(16) | 37(2) | 6.1(14) | 5.7(17) | -12.7(16) |
| C1A | 23.9(17) | 56(2) | 29.4(18) | 3.3(15) | 8.5(14) | -3.8(15) |
| O2 | 36.8(13) | 24.0(11) | 28.2(12) | 0.8(9) | 2.8(10) | 10.7(9) |
| Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
|---|---|---|---|---|---|---|
| Zn1 | Zn11 | 2.9337(7) | C5 | C16 | 1.430(4) | |
| Zn1 | Cl4 | 2.2160(8) | C6 | C13 | 1.416(4) | |
| Zn1 | O1 | 1.9610(19) | C6 | C16 | 1.413(4) | |
| Zn1 | O11 | 1.9863(19) | C12 | C18 | 1.402(5) | |
| Zn1 | N2 | 2.065(2) | C12 | C28 | 1.401(5) | |
| Fe2 | C2 | 2.026(3) | C18 | C41 | 1.403(5) | |
| Fe2 | C5 | 2.048(3) | C28 | C39 | 1.395(5) | |
| Fe2 | C6 | 2.055(3) | C39 | C41 | 1.386(5) | |
| Fe2 | C12 | 2.036(3) | N2 | C3 | 1.506(4) | |
| Fe2 | C13 | 2.037(3) | N2 | C4 | 1.486(4) | |
| Fe2 | C16 | 2.049(3) | N2 | C1 | 1.489(4) | |
| Fe2 | C18 | 2.038(3) | C7 | C8 | 1.411(4) | |
| Fe2 | C28 | 2.038(3) | C7 | C10 | 1.432(4) | |
| Fe2 | C39 | 2.046(3) | C7 | C14 | 1.428(4) | |
| Fe2 | C41 | 2.043(3) | C8 | C11 | 1.371(4) | |
| Si3 | O1 | 1.622(2) | C9 | C10 | 1.379(4) | |
| Si3 | C5 | 1.839(3) | C9 | C1A | 1.407(4) | |
| Si3 | C10 | 1.869(3) | C11 | C17 | 1.403(5) | |
| Si3 | O2 | 1.642(2) | C14 | C15 | 1.412(4) | |
| O1 | Zn11 | 1.9864(19) | C14 | C19 | 1.414(4) | |
| C2 | C5 | 1.454(4) | C15 | C1A | 1.354(5) | |
| C2 | C13 | 1.429(4) | C17 | C19 | 1.352(5) | |
| C2 | C3 | 1.491(4) |
| Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
|---|---|---|---|---|---|---|---|---|
| Cl4 | Zn1 | Zn11 | 125.16(3) | Si3 | O1 | Zn11 | 131.45(11) | |
| O1 | Zn1 | Zn11 | 42.33(5) | Si3 | O1 | Zn1 | 126.87(11) | |
| O11 | Zn1 | Zn11 | 41.66(5) | C5 | C2 | Fe2 | 69.89(15) | |
| O11 | Zn1 | Cl4 | 109.90(6) | C5 | C2 | C3 | 125.1(2) | |
| O1 | Zn1 | Cl4 | 121.12(6) | C13 | C2 | Fe2 | 69.80(16) | |
| O1 | Zn1 | O11 | 83.99(8) | C13 | C2 | C5 | 108.0(2) | |
| O11 | Zn1 | N2 | 114.11(8) | C13 | C2 | C3 | 126.9(2) | |
| O1 | Zn1 | N2 | 113.35(9) | C3 | C2 | Fe2 | 123.83(19) | |
| N2 | Zn1 | Zn11 | 122.79(7) | Si3 | C5 | Fe2 | 128.10(15) | |
| N2 | Zn1 | Cl4 | 111.52(7) | C2 | C5 | Fe2 | 68.29(15) | |
| C2 | Fe2 | C5 | 41.83(11) | C2 | C5 | Si3 | 127.2(2) | |
| C2 | Fe2 | C6 | 68.68(11) | C16 | C5 | Fe2 | 69.60(16) | |
| C2 | Fe2 | C12 | 111.87(12) | C16 | C5 | Si3 | 126.6(2) | |
| C2 | Fe2 | C13 | 41.18(11) | C16 | C5 | C2 | 106.2(2) | |
| C2 | Fe2 | C16 | 68.96(11) | C13 | C6 | Fe2 | 69.06(16) | |
| C2 | Fe2 | C18 | 110.45(13) | C16 | C6 | Fe2 | 69.63(16) | |
| C2 | Fe2 | C28 | 141.00(14) | C16 | C6 | C13 | 108.5(3) | |
| C2 | Fe2 | C39 | 177.43(14) | C18 | C12 | Fe2 | 69.97(18) | |
| C2 | Fe2 | C41 | 137.81(15) | C28 | C12 | Fe2 | 69.97(18) | |
| C5 | Fe2 | C6 | 68.80(11) | C28 | C12 | C18 | 107.7(3) | |
| C5 | Fe2 | C16 | 40.86(11) | C2 | C13 | Fe2 | 69.02(16) | |
| C12 | Fe2 | C5 | 110.57(12) | C6 | C13 | Fe2 | 70.44(17) | |
| C12 | Fe2 | C6 | 178.46(13) | C6 | C13 | C2 | 108.1(3) | |
| C12 | Fe2 | C13 | 140.82(13) | C5 | C16 | Fe2 | 69.54(15) | |
| C12 | Fe2 | C16 | 138.36(13) | C6 | C16 | Fe2 | 70.09(16) | |
| C12 | Fe2 | C18 | 40.26(13) | C6 | C16 | C5 | 109.2(3) | |
| C12 | Fe2 | C28 | 40.24(14) | C12 | C18 | Fe2 | 69.78(18) | |
| C12 | Fe2 | C39 | 67.47(14) | C12 | C18 | C41 | 107.5(3) | |
| C12 | Fe2 | C41 | 67.39(13) | C41 | C18 | Fe2 | 70.07(18) | |
| C13 | Fe2 | C5 | 69.66(11) | C12 | C28 | Fe2 | 69.79(19) | |
| C13 | Fe2 | C6 | 40.50(11) | C39 | C28 | Fe2 | 70.3(2) | |
| C13 | Fe2 | C16 | 68.38(12) | C39 | C28 | C12 | 108.3(3) | |
| C13 | Fe2 | C18 | 112.25(13) | C28 | C39 | Fe2 | 69.7(2) | |
| C13 | Fe2 | C28 | 177.82(14) | C41 | C39 | Fe2 | 70.1(2) | |
| C13 | Fe2 | C39 | 137.87(14) | C41 | C39 | C28 | 107.9(3) | |
| C13 | Fe2 | C41 | 111.38(14) | C18 | C41 | Fe2 | 69.70(18) | |
| C16 | Fe2 | C6 | 40.29(11) | C39 | C41 | Fe2 | 70.3(2) | |
| C18 | Fe2 | C5 | 137.73(13) | C39 | C41 | C18 | 108.6(3) | |
| C18 | Fe2 | C6 | 141.11(13) | C3 | N2 | Zn1 | 112.29(16) | |
| C18 | Fe2 | C16 | 178.39(13) | C4 | N2 | Zn1 | 110.63(19) | |
| C18 | Fe2 | C39 | 67.35(15) | C4 | N2 | C3 | 109.5(2) | |
| C18 | Fe2 | C41 | 40.23(14) | C4 | N2 | C1 | 108.7(2) | |
| C28 | Fe2 | C5 | 112.10(13) | C1 | N2 | Zn1 | 108.12(17) | |
| C28 | Fe2 | C6 | 138.48(14) | C1 | N2 | C3 | 107.5(2) | |
| C28 | Fe2 | C16 | 111.99(13) | C2 | C3 | N2 | 113.9(2) | |
| C28 | Fe2 | C18 | 67.45(14) | C8 | C7 | C10 | 122.6(2) | |
| C28 | Fe2 | C39 | 39.95(15) | C8 | C7 | C14 | 117.9(3) | |
| C28 | Fe2 | C41 | 66.90(15) | C14 | C7 | C10 | 119.4(3) | |
| C39 | Fe2 | C5 | 140.71(15) | C11 | C8 | C7 | 121.5(3) | |
| C39 | Fe2 | C6 | 112.05(13) | C10 | C9 | C1A | 122.1(3) | |
| C39 | Fe2 | C16 | 113.27(14) | C8 | C11 | C17 | 120.0(3) | |
| C41 | Fe2 | C5 | 177.85(13) | C7 | C10 | Si3 | 123.2(2) | |
| C41 | Fe2 | C6 | 113.26(13) | C9 | C10 | Si3 | 118.1(2) | |
| C41 | Fe2 | C16 | 141.16(14) | C9 | C10 | C7 | 118.4(3) | |
| C41 | Fe2 | C39 | 39.63(15) | C15 | C14 | C7 | 118.7(3) | |
| O1 | Si3 | C5 | 108.03(11) | C15 | C14 | C19 | 122.3(3) | |
| O1 | Si3 | C10 | 108.92(11) | C19 | C14 | C7 | 119.0(3) | |
| O1 | Si3 | O2 | 109.27(11) | C1A | C15 | C14 | 121.6(3) | |
| C5 | Si3 | C10 | 111.05(12) | C19 | C17 | C11 | 120.4(3) | |
| O2 | Si3 | C5 | 110.68(12) | C17 | C19 | C14 | 121.3(3) | |
| O2 | Si3 | C10 | 108.85(12) | C15 | C1A | C9 | 119.7(3) | |
| Zn1 | O1 | Zn11 | 96.01(8) |
| Atom | x | y | z | U(eq) |
|---|---|---|---|---|
| H6 | 13038 | 1322 | 3390 | 33 |
| H12 | 13818 | -2631 | 1570 | 41 |
| H13 | 11730 | -591 | 3294 | 31 |
| H16 | 13433 | 1837 | 2100 | 30 |
| H18 | 13375 | -3243 | 2838 | 48 |
| H28 | 15173 | -774 | 1756 | 52 |
| H39 | 15562 | -238 | 3128 | 58 |
| H41 | 14466 | -1759 | 3793 | 56 |
| H3A | 11073 | -2356 | 2198 | 28 |
| H3B | 11374 | -2065 | 1388 | 28 |
| H4A | 9665 | -213 | 2419 | 57 |
| H4B | 9365 | -1700 | 2523 | 57 |
| H4C | 8516 | -790 | 1988 | 57 |
| H1A | 8501 | -2313 | 995 | 55 |
| H1B | 9389 | -3222 | 1500 | 55 |
| H1C | 9630 | -2707 | 709 | 55 |
| H8 | 11445 | 2688 | 1006 | 34 |
| H9 | 14253 | 595 | -2 | 35 |
| H11 | 10784 | 4783 | 974 | 49 |
| H15 | 14543 | 4351 | -503 | 41 |
| H17 | 11644 | 6410 | 367 | 56 |
| H19 | 13179 | 5949 | -165 | 48 |
| H1AA | 15191 | 2269 | -509 | 43 |
| H2 | 12610(40) | -1300(40) | -107(13) | 87(16) |
Experimental
Single crystals of C23H24ClFeNO2SiZn [] 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 []
Crystal Data. C23H24ClFeNO2SiZn, M =531.19, monoclinic, a = 12.1782(18) Å, b = 10.3464(7) Å, c = 18.1035(15) Å, β = 99.600(8)°, V = 2249.1(4) Å3, T = 150, space group P21/c (no. 14), Z = 4, μ(Mo Kα) = 1.903, 20563 reflections measured, 4906 unique (Rint = 0.0476) which were used in all calculations. The final wR2 was 0.0855 (all data) and R1 was 0.0373 (>2sigma(I)).
This report has been created with Olex2, compiled on 2012.03.27 svn.r2268. Please let us know if there are any errors or if you would like to have additional featrues.