3161

Table 1 Crystal data and structure refinement for 3161.
Identification code 3161
Empirical formula C46H48Cl2Fe2N2O4Si2Zn2
Formula weight 1062.38
Temperature/K 173
Crystal system monoclinic
Space group P21/c
a/Å 12.1868(6)
b/Å 10.3523(4)
c/Å 18.1265(8)
α/° 90
β/° 99.579(4)
γ/° 90
Volume/Å3 2254.98(18)
Z 2
ρcalcg/cm3 1.565
μ/mm‑1 1.898
F(000) 1088.0
Crystal size/mm3 0.106 × 0.094 × 0.056
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.546 to 53.996
Index ranges -15 ≤ h ≤ 15, -13 ≤ k ≤ 13, -23 ≤ l ≤ 22
Reflections collected 20568
Independent reflections 4909 [Rint = 0.0476, Rsigma = 0.0446]
Data/restraints/parameters 4909/1/277
Goodness-of-fit on F2 1.032
Final R indexes [I>=2σ (I)] R1 = 0.0373, wR2 = 0.0793
Final R indexes [all data] R1 = 0.0536, wR2 = 0.0857
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 3161. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Zn19712.6(3)153.1(3)750.4(2)19.86(9)
Fe113418.2(3)-702.9(4)2494.5(2)22.81(11)
Cl18863.8(8)1856.1(8)1139.0(5)40.1(2)
Si112322.7(6)274.3(7)671.7(4)19.20(17)
O111031.0(15)353.4(17)269.4(10)20.2(4)
O212881.5(18)-1057.4(19)408.8(12)30.1(5)
N19857(2)-1329(2)1523.9(13)24.5(5)
C112359(2)283(2)1691.4(16)20.8(6)
C211758(2)-574(3)2121.1(15)20.0(6)
C312008(2)-195(3)2889.7(16)25.8(6)
C412742(2)874(3)2942.7(17)27.5(7)
C512961(2)1164(3)2218.2(16)25.1(6)
C614110(3)-2233(3)2034.4(18)34.0(8)
C713864(3)-2573(3)2738(2)40.5(8)
C814471(3)-1744(4)3269.3(19)46.3(10)
C915081(3)-902(4)2901(2)48.8(10)
C1014863(3)-1199(3)2139(2)43.2(9)
C1111052(2)-1685(3)1805.7(16)23.4(6)
C129296(3)-2492(3)1149.8(18)37.1(8)
C139304(3)-978(4)2168.3(18)38.4(8)
C1413090(2)1693(3)371.1(15)21.8(6)
C1513997(2)1458(3)24.9(17)29.5(7)
C1614554(3)2457(3)-289.0(18)36.0(8)
C1714177(3)3686(3)-275.5(17)34.4(8)
C1813254(3)4004(3)68.7(16)27.8(7)
C1912827(3)5276(3)65.7(19)39.9(8)
C2011927(3)5552(3)385(2)47(1)
C2111408(3)4580(3)743(2)40.9(9)
C2211799(3)3336(3)758.6(17)28.3(7)
C2312718(2)2999(3)414.9(15)21.8(6)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for 3161. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Zn122.77(18)20.35(17)15.91(17)0.49(12)1.59(13)0.35(13)
Fe125.0(2)22.9(2)18.5(2)0.80(16)-2.44(16)4.38(17)
Cl154.5(5)32.2(4)34.1(5)-8.2(3)8.4(4)12.8(4)
Si120.9(4)16.7(4)19.1(4)1.8(3)0.8(3)1.4(3)
O121.3(10)21.3(10)16.8(10)1.6(7)0.0(8)-0.8(8)
O236.9(13)24.1(11)28.4(12)0.8(9)2.8(10)10.7(9)
N125.7(13)28.1(13)19.2(13)5.7(10)2.1(10)-4.9(10)
C120.3(14)17.7(13)22.7(15)2.7(11)-1.4(11)2.3(11)
C221.0(14)20.7(14)17.1(14)2.3(11)-0.1(11)2.8(11)
C327.3(16)29.5(15)19.4(15)2.6(12)0.5(12)6.3(13)
C431.0(16)24.6(15)23.1(16)-6.3(12)-6.9(13)6.0(13)
C525.2(15)20.3(14)27.3(16)0.1(12)-3.1(13)-0.9(12)
C637.4(19)31.0(17)30.3(18)-5.9(13)-3.6(14)15.6(14)
C745(2)25.2(17)53(2)10.8(15)11.4(18)13.8(15)
C858(2)50(2)26.2(19)2.2(16)-8.0(17)36.7(19)
C930.0(19)41(2)68(3)-11.4(19)-14.0(18)12.0(16)
C1034.3(19)47(2)50(2)5.8(17)11.5(17)15.1(17)
C1126.6(15)19.7(14)23.3(15)5.1(11)2.4(12)-2.2(12)
C1238.8(19)31.5(17)36.1(19)9.0(14)-7.6(15)-16.0(15)
C1329.6(18)59(2)28.2(18)13.9(16)11.0(14)2.8(16)
C1419.2(14)26.9(15)17.0(14)3.3(11)-3.8(11)-2.7(12)
C1521.0(15)39.1(18)28.2(17)3.8(13)2.9(13)3.9(13)
C1623.9(17)56(2)29.5(18)3.3(15)8.4(14)-3.8(15)
C1730.7(18)46(2)25.6(17)8.4(14)3.1(14)-16.2(15)
C1831.4(17)29.3(16)21.0(15)2.9(12)-0.2(13)-10.3(13)
C1956(2)25.5(16)37(2)6.1(14)5.8(17)-12.8(16)
C2070(3)19.4(16)54(2)4.1(15)19(2)2.4(17)
C2156(2)25.7(17)46(2)0.8(15)21.9(18)8.7(16)
C2234.1(17)21.7(15)30.3(17)0.0(12)8.8(14)-4.5(13)
C2323.9(15)21.6(14)18.6(14)2.3(11)-0.3(12)-3.1(12)

 

Table 4 Bond Lengths for 3161.
AtomAtomLength/Å AtomAtomLength/Å
Zn1Zn112.9371(6) C1C21.455(4)
Zn1Cl12.2174(8) C1C51.431(4)
Zn1O111.9888(19) C2C31.431(4)
Zn1O11.9624(19) C2C111.492(4)
Zn1N12.066(2) C3C41.417(4)
Fe1C12.050(3) C4C51.415(4)
Fe1C22.028(3) C6C71.403(5)
Fe1C32.038(3) C6C101.402(5)
Fe1C42.056(3) C7C81.405(5)
Fe1C52.050(3) C8C91.387(5)
Fe1C62.037(3) C9C101.397(5)
Fe1C72.039(3) C14C151.380(4)
Fe1C82.045(3) C14C231.433(4)
Fe1C92.048(3) C15C161.408(4)
Fe1C102.039(3) C16C171.355(5)
Si1O11.623(2) C17C181.413(4)
Si1O21.643(2) C18C191.415(4)
Si1C11.841(3) C18C231.429(4)
Si1C141.870(3) C19C201.353(5)
O1Zn111.9889(19) C20C211.404(5)
N1C111.507(4) C21C221.371(4)
N1C121.490(4) C22C231.413(4)
N1C131.487(4)    

12-X,-Y,-Z

 

Table 5 Bond Angles for 3161.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
Cl1Zn1Zn11125.16(3) Si1O1Zn1126.84(11)
O1Zn1Zn1142.33(5) Si1O1Zn11131.46(11)
O11Zn1Zn1141.64(5) C11N1Zn1112.30(16)
O1Zn1Cl1121.12(6) C12N1Zn1108.08(17)
O11Zn1Cl1109.90(6) C12N1C11107.5(2)
O1Zn1O1183.97(8) C13N1Zn1110.66(19)
O11Zn1N1114.14(8) C13N1C11109.4(2)
O1Zn1N1113.36(8) C13N1C12108.8(2)
N1Zn1Zn11122.81(7) Si1C1Fe1128.13(15)
N1Zn1Cl1111.49(7) C2C1Fe168.28(15)
C1Fe1C468.83(11) C2C1Si1127.2(2)
C2Fe1C141.82(11) C5C1Fe169.57(16)
C2Fe1C341.20(11) C5C1Si1126.6(2)
C2Fe1C468.70(11) C5C1C2106.2(2)
C2Fe1C568.95(11) C1C2Fe169.90(15)
C2Fe1C6111.85(12) C1C2C11125.0(2)
C2Fe1C7110.46(13) C3C2Fe169.78(16)
C2Fe1C8137.83(15) C3C2C1108.0(2)
C2Fe1C9177.43(14) C3C2C11126.9(2)
C2Fe1C10140.99(14) C11C2Fe1123.84(19)
C3Fe1C169.69(11) C2C3Fe169.02(16)
C3Fe1C440.49(11) C4C3Fe170.45(17)
C3Fe1C568.39(12) C4C3C2108.1(3)
C3Fe1C7112.24(13) C3C4Fe169.06(16)
C3Fe1C8111.36(14) C5C4Fe169.62(16)
C3Fe1C9137.84(14) C5C4C3108.5(3)
C3Fe1C10177.81(14) C1C5Fe169.56(15)
C5Fe1C140.86(11) C4C5Fe170.08(16)
C5Fe1C440.31(11) C4C5C1109.3(3)
C6Fe1C1110.54(12) C7C6Fe169.95(18)
C6Fe1C3140.82(13) C10C6Fe169.97(18)
C6Fe1C4178.46(13) C10C6C7107.6(3)
C6Fe1C5138.34(13) C6C7Fe169.77(17)
C6Fe1C740.27(13) C6C7C8107.6(3)
C6Fe1C867.42(13) C8C7Fe170.10(18)
C6Fe1C967.49(14) C7C8Fe169.66(18)
C6Fe1C1040.24(14) C9C8Fe170.3(2)
C7Fe1C1137.72(13) C9C8C7108.5(3)
C7Fe1C4141.09(13) C8C9Fe170.1(2)
C7Fe1C5178.38(13) C8C9C10108.0(3)
C7Fe1C840.24(14) C10C9Fe169.7(2)
C7Fe1C967.35(15) C6C10Fe169.79(19)
C7Fe1C1067.45(14) C9C10Fe170.4(2)
C8Fe1C1177.85(13) C9C10C6108.3(3)
C8Fe1C4113.22(13) C2C11N1113.9(2)
C8Fe1C5141.16(14) C15C14Si1118.1(2)
C8Fe1C939.62(15) C15C14C23118.4(3)
C9Fe1C1140.72(15) C23C14Si1123.2(2)
C9Fe1C4112.03(13) C14C15C16122.1(3)
C9Fe1C5113.28(14) C17C16C15119.7(3)
C10Fe1C1112.08(13) C16C17C18121.6(3)
C10Fe1C4138.49(14) C17C18C19122.3(3)
C10Fe1C5111.98(13) C17C18C23118.7(3)
C10Fe1C866.91(15) C19C18C23119.0(3)
C10Fe1C939.97(15) C20C19C18121.3(3)
O1Si1O2109.25(11) C19C20C21120.4(3)
O1Si1C1108.07(11) C22C21C20120.0(3)
O1Si1C14108.90(11) C21C22C23121.4(3)
O2Si1C1110.69(12) C18C23C14119.4(3)
O2Si1C14108.84(12) C22C23C14122.6(2)
C1Si1C14111.05(12) C22C23C18117.9(3)
Zn1O1Zn1196.03(8)     

12-X,-Y,-Z

 

Table 6 Hydrogen Bonds for 3161.
DHAd(D-H)/Åd(H-A)/Åd(D-A)/ÅD-H-A/°
O2H2Cl110.970(19)2.44(3)3.331(2)153(4)

12-X,-Y,-Z

 

Table 7 Torsion Angles for 3161.
ABCDAngle/˚ ABCDAngle/˚
Zn1N1C11C254.8(3) C3C2C11N194.5(3)
Fe1C1C2C359.58(19) C3C4C5Fe1-58.3(2)
Fe1C1C2C11-117.9(3) C3C4C5C10.4(3)
Fe1C1C5C4-59.0(2) C5C1C2Fe1-59.55(18)
Fe1C2C3C459.9(2) C5C1C2C30.0(3)
Fe1C2C11N1-176.53(17) C5C1C2C11-177.4(3)
Fe1C3C4C558.6(2) C6C7C8Fe160.0(2)
Fe1C4C5C158.66(19) C6C7C8C90.2(4)
Fe1C6C7C8-60.2(2) C7C6C10Fe1-60.1(2)
Fe1C6C10C960.0(2) C7C6C10C90.0(4)
Fe1C7C8C9-59.8(2) C7C8C9Fe159.4(2)
Fe1C8C9C10-59.6(2) C7C8C9C10-0.2(4)
Fe1C9C10C6-59.7(2) C8C9C10Fe159.9(2)
Si1C1C2Fe1122.1(2) C8C9C10C60.2(4)
Si1C1C2C3-178.3(2) C10C6C7Fe160.1(2)
Si1C1C2C114.3(4) C10C6C7C8-0.1(3)
Si1C1C5Fe1-123.0(2) C11C2C3Fe1117.8(3)
Si1C1C5C4178.1(2) C11C2C3C4177.6(3)
Si1C14C15C16173.3(2) C12N1C11C2173.5(2)
Si1C14C23C18-170.4(2) C13N1C11C2-68.5(3)
Si1C14C23C226.5(4) C14Si1O1Zn1181.42(16)
O1Si1C1Fe1143.60(16) C14Si1O1Zn1-131.75(14)
O1Si1C1C253.3(3) C14Si1C1Fe1-97.02(19)
O1Si1C1C5-124.6(2) C14Si1C1C2172.7(2)
O1Si1C14C15-122.0(2) C14Si1C1C5-5.3(3)
O1Si1C14C2351.6(3) C14C15C16C17-2.1(5)
O2Si1O1Zn1109.49(14) C15C14C23C183.2(4)
O2Si1O1Zn11-37.35(17) C15C14C23C22-179.9(3)
O2Si1C1Fe124.0(2) C15C16C17C182.1(5)
O2Si1C1C2-66.3(3) C16C17C18C19-177.8(3)
O2Si1C1C5115.8(2) C16C17C18C230.5(5)
O2Si1C14C15-3.0(3) C17C18C19C20178.5(3)
O2Si1C14C23170.6(2) C17C18C23C14-3.2(4)
C1Si1O1Zn11-157.85(14) C17C18C23C22179.8(3)
C1Si1O1Zn1-11.01(16) C18C19C20C211.3(6)
C1Si1C14C15119.1(2) C19C18C23C14175.2(3)
C1Si1C14C23-67.3(3) C19C18C23C22-1.8(4)
C1C2C3Fe1-59.66(19) C19C20C21C22-1.2(6)
C1C2C3C40.2(3) C20C21C22C23-0.5(5)
C1C2C11N1-88.5(3) C21C22C23C14-174.9(3)
C2C1C5Fe158.71(18) C21C22C23C182.0(5)
C2C1C5C4-0.3(3) C23C14C15C16-0.6(4)
C2C3C4Fe1-58.98(19) C23C18C19C200.2(5)
C2C3C4C5-0.4(3)      

12-X,-Y,-Z

 

Table 8 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for 3161.
AtomxyzU(eq)
H212610(40)-1300(40)-107(13)87(16)
H311730-591329431
H4130381322338933
H5134321836210030
H613819-2631157141
H713375-3242283849
H814466-1759379356
H915562-239312759
H1015173-774175752
H11A11073-2356219728
H11B11374-2065138828
H12A8502-231399556
H12B9389-3222149956
H12C9630-270770956
H13A9665-213241958
H13B9365-1700252358
H13C8517-790198858
H1514253596-235
H16151912269-50943
H17145434351-50341
H19131795948-16548
H2011645640936756
H2110785478397449
H22114452688100634

Experimental

Single crystals of C46H48Cl2Fe2N2O4Si2Zn2 [3161] 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.

  1. Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341.
  2. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.
  3. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Crystal structure determination of [3161]

Crystal Data for C46H48Cl2Fe2N2O4Si2Zn2 (=1062.38 g/mol): monoclinic, space group P21/c (no. 14), a = 12.1868(6) Å, b = 10.3523(4) Å, c = 18.1265(8) Å, β = 99.579(4)°, = 2254.98(18) Å3, Z = 2, T = 173 K, μ(MoKα) = 1.898 mm-1, Dcalc = 1.565 g/cm3, 20568 reflections measured (4.546° ≤ 2Θ ≤ 53.996°), 4909 unique (Rint = 0.0476, Rsigma = 0.0446) which were used in all calculations. The final R1 was 0.0373 (I > 2σ(I)) and wR2 was 0.0857 (all data).

Refinement model description

Number of restraints - 1, 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. Restrained distances
O2-H2
1 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
C11(H11A,H11B)
3.b Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C15(H15),
C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22)
3.c Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)

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