Table 1 Crystal data and structure refinement for
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

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for . Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Zn19712.6(3)153.1(3)750.39(17)19.82(9)
Fe213418.2(3)-702.9(4)2494.5(2)22.77(11)
Si312322.7(6)274.3(7)671.7(4)19.17(17)
Cl48863.8(8)1856.1(8)1139.0(5)40.1(2)
O111031.0(15)353.3(17)269.4(10)20.1(4)
C211758(2)-574(3)2121.0(15)19.9(6)
C512359(2)283(2)1691.3(16)20.8(6)
C612742(2)874(3)2942.7(17)27.5(7)
C1214110(3)-2233(3)2034.3(18)33.9(8)
C1312008(2)-195(3)2889.6(16)25.7(6)
C1612961(2)1164(3)2218.2(16)25.1(6)
C1813864(3)-2573(3)2738(2)40.4(8)
C2814863(3)-1199(3)2139(2)43.1(9)
C3915081(3)-902(4)2901(2)48.7(10)
C4114471(3)-1744(4)3269.2(19)46.3(10)
N29857(2)-1329(2)1523.9(13)24.4(5)
C311052(2)-1685(3)1805.7(16)23.3(6)
C49304(3)-978(4)2168.3(18)38.3(8)
C19296(3)-2492(3)1149.8(18)37.0(8)
C712718(2)2999(3)414.9(15)21.8(6)
C811799(3)3336(3)758.6(17)28.2(7)
C913997(2)1458(3)24.9(17)29.5(7)
C1111408(3)4580(3)743(2)40.9(9)
C1013090(2)1693(3)371.1(15)21.7(6)
C1413254(3)4005(3)68.7(16)27.7(7)
C1514177(3)3686(3)-275.5(17)34.3(8)
C1711927(3)5552(3)385(2)46.9(10)
C1912827(3)5276(3)65.8(19)39.7(8)
C1A14554(3)2457(3)-289.0(18)36.0(8)
O212881.5(18)-1057.5(19)408.8(12)30.0(5)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for . The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+...+2hka×b×U12]
AtomU11U22U33U23U13U12
Zn122.74(18)20.33(17)15.84(17)0.49(12)1.58(13)0.35(13)
Fe224.9(2)22.9(2)18.4(2)0.80(16)-2.45(16)4.38(17)
Si320.9(4)16.7(4)19.0(4)1.8(3)0.8(3)1.4(3)
Cl454.4(5)32.1(4)34.0(5)-8.2(3)8.4(4)12.8(4)
O121.3(10)21.3(10)16.7(10)1.6(7)0.0(8)-0.8(8)
C221.0(14)20.7(14)17.1(14)2.3(11)-0.1(11)2.7(11)
C520.2(14)17.7(13)22.6(15)2.7(11)-1.5(11)2.3(11)
C631.0(16)24.5(15)23.0(16)-6.3(12)-6.9(13)5.9(13)
C1237.4(19)31.0(17)30.2(18)-5.9(13)-3.6(14)15.7(14)
C1327.3(16)29.4(15)19.3(15)2.6(12)0.5(12)6.3(13)
C1625.2(15)20.3(14)27.2(16)0.1(12)-3.1(13)-1.0(12)
C1845(2)25.2(17)53(2)10.8(15)11.4(18)13.8(15)
C2834.2(19)47(2)50(2)5.7(17)11.6(17)15.0(17)
C3929.9(19)41(2)68(3)-11.3(19)-14.1(18)12.0(16)
C4158(2)50(2)26.1(19)2.2(16)-8.0(17)36.7(19)
N225.6(13)28.0(13)19.1(13)5.6(10)2.1(10)-5(1)
C326.6(15)19.7(14)23.2(15)5.1(11)2.4(12)-2.2(12)
C429.5(18)59(2)28.1(18)13.9(16)10.9(14)2.8(16)
C138.8(19)31.5(17)36.0(19)8.9(14)-7.5(15)-16.0(15)
C723.9(15)21.6(14)18.5(14)2.3(11)-0.3(12)-3.0(12)
C834.0(17)21.7(15)30.2(17)0.0(12)8.7(14)-4.6(13)
C920.9(15)39.0(18)28.1(17)3.8(13)2.9(13)3.9(13)
C1156(2)25.6(17)45(2)0.8(14)21.8(18)8.7(16)
C1019.1(14)26.8(15)16.9(14)3.3(11)-3.8(11)-2.7(12)
C1431.4(17)29.3(16)20.9(15)2.9(12)-0.2(13)-10.2(13)
C1530.6(18)46(2)25.4(17)8.3(14)3.1(14)-16.3(15)
C1770(3)19.4(16)54(2)4.0(15)19(2)2.4(17)
C1956(2)25.4(16)37(2)6.1(14)5.7(17)-12.7(16)
C1A23.9(17)56(2)29.4(18)3.3(15)8.5(14)-3.8(15)
O236.8(13)24.0(11)28.2(12)0.8(9)2.8(10)10.7(9)

 

Table 4 Bond Lengths for .
AtomAtomLength/Å AtomAtomLength/Å
Zn1Zn112.9337(7) C5C161.430(4)
Zn1Cl42.2160(8) C6C131.416(4)
Zn1O11.9610(19) C6C161.413(4)
Zn1O111.9863(19) C12C181.402(5)
Zn1N22.065(2) C12C281.401(5)
Fe2C22.026(3) C18C411.403(5)
Fe2C52.048(3) C28C391.395(5)
Fe2C62.055(3) C39C411.386(5)
Fe2C122.036(3) N2C31.506(4)
Fe2C132.037(3) N2C41.486(4)
Fe2C162.049(3) N2C11.489(4)
Fe2C182.038(3) C7C81.411(4)
Fe2C282.038(3) C7C101.432(4)
Fe2C392.046(3) C7C141.428(4)
Fe2C412.043(3) C8C111.371(4)
Si3O11.622(2) C9C101.379(4)
Si3C51.839(3) C9C1A1.407(4)
Si3C101.869(3) C11C171.403(5)
Si3O21.642(2) C14C151.412(4)
O1Zn111.9864(19) C14C191.414(4)
C2C51.454(4) C15C1A1.354(5)
C2C131.429(4) C17C191.352(5)
C2C31.491(4)    

12-X,-Y,-Z

 

Table 5 Bond Angles for .
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
Cl4Zn1Zn11125.16(3) Si3O1Zn11131.45(11)
O1Zn1Zn1142.33(5) Si3O1Zn1126.87(11)
O11Zn1Zn1141.66(5) C5C2Fe269.89(15)
O11Zn1Cl4109.90(6) C5C2C3125.1(2)
O1Zn1Cl4121.12(6) C13C2Fe269.80(16)
O1Zn1O1183.99(8) C13C2C5108.0(2)
O11Zn1N2114.11(8) C13C2C3126.9(2)
O1Zn1N2113.35(9) C3C2Fe2123.83(19)
N2Zn1Zn11122.79(7) Si3C5Fe2128.10(15)
N2Zn1Cl4111.52(7) C2C5Fe268.29(15)
C2Fe2C541.83(11) C2C5Si3127.2(2)
C2Fe2C668.68(11) C16C5Fe269.60(16)
C2Fe2C12111.87(12) C16C5Si3126.6(2)
C2Fe2C1341.18(11) C16C5C2106.2(2)
C2Fe2C1668.96(11) C13C6Fe269.06(16)
C2Fe2C18110.45(13) C16C6Fe269.63(16)
C2Fe2C28141.00(14) C16C6C13108.5(3)
C2Fe2C39177.43(14) C18C12Fe269.97(18)
C2Fe2C41137.81(15) C28C12Fe269.97(18)
C5Fe2C668.80(11) C28C12C18107.7(3)
C5Fe2C1640.86(11) C2C13Fe269.02(16)
C12Fe2C5110.57(12) C6C13Fe270.44(17)
C12Fe2C6178.46(13) C6C13C2108.1(3)
C12Fe2C13140.82(13) C5C16Fe269.54(15)
C12Fe2C16138.36(13) C6C16Fe270.09(16)
C12Fe2C1840.26(13) C6C16C5109.2(3)
C12Fe2C2840.24(14) C12C18Fe269.78(18)
C12Fe2C3967.47(14) C12C18C41107.5(3)
C12Fe2C4167.39(13) C41C18Fe270.07(18)
C13Fe2C569.66(11) C12C28Fe269.79(19)
C13Fe2C640.50(11) C39C28Fe270.3(2)
C13Fe2C1668.38(12) C39C28C12108.3(3)
C13Fe2C18112.25(13) C28C39Fe269.7(2)
C13Fe2C28177.82(14) C41C39Fe270.1(2)
C13Fe2C39137.87(14) C41C39C28107.9(3)
C13Fe2C41111.38(14) C18C41Fe269.70(18)
C16Fe2C640.29(11) C39C41Fe270.3(2)
C18Fe2C5137.73(13) C39C41C18108.6(3)
C18Fe2C6141.11(13) C3N2Zn1112.29(16)
C18Fe2C16178.39(13) C4N2Zn1110.63(19)
C18Fe2C3967.35(15) C4N2C3109.5(2)
C18Fe2C4140.23(14) C4N2C1108.7(2)
C28Fe2C5112.10(13) C1N2Zn1108.12(17)
C28Fe2C6138.48(14) C1N2C3107.5(2)
C28Fe2C16111.99(13) C2C3N2113.9(2)
C28Fe2C1867.45(14) C8C7C10122.6(2)
C28Fe2C3939.95(15) C8C7C14117.9(3)
C28Fe2C4166.90(15) C14C7C10119.4(3)
C39Fe2C5140.71(15) C11C8C7121.5(3)
C39Fe2C6112.05(13) C10C9C1A122.1(3)
C39Fe2C16113.27(14) C8C11C17120.0(3)
C41Fe2C5177.85(13) C7C10Si3123.2(2)
C41Fe2C6113.26(13) C9C10Si3118.1(2)
C41Fe2C16141.16(14) C9C10C7118.4(3)
C41Fe2C3939.63(15) C15C14C7118.7(3)
O1Si3C5108.03(11) C15C14C19122.3(3)
O1Si3C10108.92(11) C19C14C7119.0(3)
O1Si3O2109.27(11) C1AC15C14121.6(3)
C5Si3C10111.05(12) C19C17C11120.4(3)
O2Si3C5110.68(12) C17C19C14121.3(3)
O2Si3C10108.85(12) C15C1AC9119.7(3)
Zn1O1Zn1196.01(8)     

12-X,-Y,-Z

 

Table 6 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for .
AtomxyzU(eq)
H6130381322339033
H1213818-2631157041
H1311730-591329431
H16134331837210030
H1813375-3243283848
H2815173-774175652
H3915562-238312858
H4114466-1759379356
H3A11073-2356219828
H3B11374-2065138828
H4A9665-213241957
H4B9365-1700252357
H4C8516-790198857
H1A8501-231399555
H1B9389-3222150055
H1C9630-270770955
H8114452688100634
H914253595-235
H1110784478397449
H15145434351-50341
H1711644641036756
H19131795949-16548
H1AA151912269-50943
H212610(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.

  1. O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341.
  2. SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122
  3. SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122

Crystal structure determination of []

Crystal Data. C23H24ClFeNO2SiZn, =531.19, monoclinic, a = 12.1782(18) Å, b = 10.3464(7) Å, c = 18.1035(15) Å, β = 99.600(8)°, = 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.