3074

Table 1 Crystal data and structure refinement for 3074.
Identification code 3074
Empirical formula C25H29FeNO2Si
Formula weight 459.43
Temperature/K 173
Crystal system orthorhombic
Space group P212121
a/Å 7.8104(5)
b/Å 12.1050(9)
c/Å 23.811(2)
α/° 90
β/° 90
γ/° 90
Volume/Å3 2251.2(3)
Z 4
ρcalcg/cm3 1.356
μ/mm‑1 0.745
F(000) 968.0
Crystal size/mm3 0.2 × 0.05 × 0.05
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.798 to 53.996
Index ranges -9 ≤ h ≤ 9, -15 ≤ k ≤ 15, -30 ≤ l ≤ 30
Reflections collected 17819
Independent reflections 4885 [Rint = 0.0658, Rsigma = 0.0771]
Data/restraints/parameters 4885/0/275
Goodness-of-fit on F2 1.043
Final R indexes [I>=2σ (I)] R1 = 0.0522, wR2 = 0.0875
Final R indexes [all data] R1 = 0.0728, wR2 = 0.0948
Largest diff. peak/hole / e Å-3 0.43/-0.35
Flack parameter-0.004(15)

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for 3074. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Fe17647.8(8)10623.1(5)7448.8(3)26.13(18)
Si110120.6(16)10331.4(11)6186.1(5)24.1(3)
O111283(4)11143(3)5792.8(14)33.9(8)
O211279(4)9308(3)6419.4(13)32.1(8)
N17926(5)13153(3)6106.2(16)28.1(10)
C19429(5)11017(4)6837.3(19)22.9(11)
C28217(6)11905(4)6920.3(19)26.2(11)
C38317(6)12252(4)7493(2)32.3(11)
C49539(6)11599(4)7774(2)34.8(13)
C510227(5)10850(4)7373.8(19)26.8(11)
C117043(6)12379(4)6485(2)29.3(12)
C126747(7)13529(4)5671(2)41.0(14)
C138603(7)14085(4)6424(2)37.2(14)
C148400(6)9920(4)5678.8(19)25.0(11)
C157940(6)10673(4)5271.4(19)30.9(11)
C166647(7)10470(4)4870(2)38.5(13)
C175850(7)9465(4)4867(2)38.8(13)
C186287(6)8632(4)5261(2)27.5(11)
C197561(6)8875(3)5675.1(18)22.8(9)
C207938(6)8023(4)6070(2)28.9(12)
C217134(7)7028(4)6046(2)34.7(13)
C225906(7)6810(4)5634(2)39.4(14)
C235482(7)7594(4)5254(2)34.0(13)
C2412671(9)11760(5)6002(3)63.7(19)
C2512364(7)8668(4)6065(2)42.4(13)
C66008(7)9403(5)7188(2)51.5(17)
C75094(6)10310(5)7395(3)55.1(17)
C85603(7)10459(5)7959(2)49.3(16)
C96797(7)9659(5)8089(2)49.0(16)
C107061(7)9009(4)7613(3)53.5(17)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for 3074. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Fe120.7(3)33.3(3)24.4(3)0.6(3)1.4(3)0.9(3)
Si117.1(7)31.5(7)23.7(7)-0.3(6)0.6(5)-1.9(6)
O124.5(18)48(2)29(2)4.6(17)1.0(15)-8.6(17)
O226.9(18)38.5(19)31.0(18)-4.1(17)3.0(15)7.3(18)
N129(3)27(2)28(2)3.8(17)-5.6(19)3(2)
C115(2)28(2)26(3)2(2)-1.3(19)-6(2)
C226(3)29(2)23(3)4(2)2(2)-6(2)
C332(3)32(2)33(3)-7(2)-2(3)-2(2)
C431(3)47(3)27(3)-4(2)-6(2)-7(3)
C517(2)38(3)25(3)3(2)-1.9(19)-3(2)
C1124(3)30(3)34(3)-4(2)-3(2)6(2)
C1243(3)44(3)36(3)6(3)-7(3)4(3)
C1340(3)30(3)41(3)3(2)-2(3)-2(3)
C1422(3)31(3)22(3)0(2)6(2)2(2)
C1536(3)26(2)30(3)6(2)-2(2)-4(3)
C1648(3)36(3)31(3)10(3)-12(2)-2(3)
C1738(3)43(3)35(3)3(3)-8(2)-1(3)
C1823(3)31(3)29(3)-5(2)3(2)-1(2)
C1917(2)21(2)30(2)0.6(18)6(2)5(2)
C2023(3)30(3)34(3)1(2)3(2)0(2)
C2128(3)28(3)48(3)5(2)9(3)6(3)
C2235(3)28(3)55(4)0(3)10(3)-3(3)
C2326(3)39(3)38(3)-9(3)0(2)-5(3)
C2453(4)76(4)62(4)23(3)-13(4)-33(4)
C2532(3)51(3)45(3)-11(3)-2(3)16(3)
C638(3)75(4)41(3)-13(4)14(3)-35(4)
C720(3)79(4)67(5)31(4)1(3)-8(3)
C843(3)53(4)52(4)-9(3)32(3)-3(3)
C943(3)68(4)36(3)26(3)0(3)-13(3)
C1038(3)33(3)89(5)5(3)18(4)-6(3)

 

Table 4 Bond Lengths for 3074.
AtomAtomLength/Å AtomAtomLength/Å
Fe1C12.070(4) C2C31.429(6)
Fe1C22.047(4) C2C111.498(6)
Fe1C32.043(5) C3C41.409(7)
Fe1C42.044(5) C4C51.422(6)
Fe1C52.041(4) C14C151.379(6)
Fe1C62.052(5) C14C191.425(6)
Fe1C72.034(5) C15C161.412(6)
Fe1C82.016(5) C16C171.367(7)
Fe1C92.032(5) C17C181.420(7)
Fe1C102.045(5) C18C191.431(6)
Si1O11.633(3) C18C231.405(7)
Si1O21.631(3) C19C201.427(6)
Si1C11.840(5) C20C211.360(6)
Si1C141.874(5) C21C221.397(7)
O1C241.407(7) C22C231.352(7)
O2C251.425(5) C6C71.400(8)
N1C111.472(6) C6C101.389(8)
N1C121.460(6) C7C81.411(8)
N1C131.458(6) C8C91.379(8)
C1C21.446(6) C9C101.397(8)
C1C51.436(6)    

 

Table 5 Bond Angles for 3074.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C2Fe1C141.13(18) C13N1C12110.9(4)
C2Fe1C6119.7(2) Si1C1Fe1133.3(2)
C3Fe1C168.99(19) C2C1Fe168.6(2)
C3Fe1C240.89(18) C2C1Si1130.0(3)
C3Fe1C440.34(18) C5C1Fe168.5(2)
C3Fe1C6150.5(2) C5C1Si1124.0(3)
C3Fe1C10166.0(2) C5C1C2105.5(4)
C4Fe1C169.38(19) C1C2Fe170.3(2)
C4Fe1C268.8(2) C1C2C11126.2(4)
C4Fe1C6169.2(2) C3C2Fe169.4(3)
C4Fe1C10129.9(2) C3C2C1108.2(4)
C5Fe1C140.88(17) C3C2C11125.5(4)
C5Fe1C268.29(19) C11C2Fe1125.7(3)
C5Fe1C367.80(19) C2C3Fe169.7(3)
C5Fe1C440.73(18) C4C3Fe169.9(3)
C5Fe1C6133.4(2) C4C3C2109.0(4)
C5Fe1C10111.5(2) C3C4Fe169.8(3)
C6Fe1C1111.87(19) C3C4C5107.1(4)
C7Fe1C1131.2(2) C5C4Fe169.5(3)
C7Fe1C2108.4(2) C1C5Fe170.6(2)
C7Fe1C3115.7(2) C4C5Fe169.8(3)
C7Fe1C4147.1(3) C4C5C1110.1(4)
C7Fe1C5170.9(2) N1C11C2112.4(4)
C7Fe1C640.1(2) C15C14Si1117.7(3)
C7Fe1C1067.3(2) C15C14C19117.6(4)
C8Fe1C1168.3(2) C19C14Si1124.7(3)
C8Fe1C2128.1(2) C14C15C16123.2(5)
C8Fe1C3105.5(2) C17C16C15119.0(5)
C8Fe1C4113.6(2) C16C17C18121.3(5)
C8Fe1C5148.0(2) C17C18C19118.5(4)
C8Fe1C667.5(2) C23C18C17121.3(5)
C8Fe1C740.8(2) C23C18C19120.2(4)
C8Fe1C939.8(2) C14C19C18120.4(4)
C8Fe1C1067.3(2) C14C19C20122.9(4)
C9Fe1C1151.7(2) C20C19C18116.7(4)
C9Fe1C2165.4(2) C21C20C19121.1(5)
C9Fe1C3126.8(2) C20C21C22120.9(5)
C9Fe1C4106.5(2) C23C22C21120.4(5)
C9Fe1C5117.8(2) C22C23C18120.7(5)
C9Fe1C667.0(2) C7C6Fe169.3(3)
C9Fe1C767.6(2) C10C6Fe169.9(3)
C9Fe1C1040.1(2) C10C6C7108.3(5)
C10Fe1C1120.3(2) C6C7Fe170.7(3)
C10Fe1C2152.9(2) C6C7C8107.0(5)
C10Fe1C639.6(2) C8C7Fe168.9(3)
O1Si1C1112.04(19) C7C8Fe170.3(3)
O1Si1C14100.89(19) C9C8Fe170.7(3)
O2Si1O1110.09(18) C9C8C7108.3(5)
O2Si1C1102.61(19) C8C9Fe169.5(3)
O2Si1C14114.54(19) C8C9C10108.2(5)
C1Si1C14116.9(2) C10C9Fe170.4(3)
C24O1Si1123.0(3) C6C10Fe170.4(3)
C25O2Si1122.7(3) C6C10C9108.1(5)
C12N1C11109.7(4) C9C10Fe169.5(3)
C13N1C11110.1(4)     

 

Table 6 Torsion Angles for 3074.
ABCDAngle/˚ ABCDAngle/˚
Fe1C1C2C359.2(3) C3C2C11N1101.6(5)
Fe1C1C2C11-120.3(5) C3C4C5Fe1-59.9(3)
Fe1C1C5C4-58.7(3) C3C4C5C1-0.6(5)
Fe1C2C3C458.9(3) C5C1C2Fe1-58.8(3)
Fe1C2C11N1-169.6(3) C5C1C2C30.4(5)
Fe1C3C4C559.8(3) C5C1C2C11-179.1(4)
Fe1C4C5C159.3(3) C11C2C3Fe1119.8(5)
Fe1C6C7C8-59.6(4) C11C2C3C4178.7(4)
Fe1C6C10C959.5(4) C12N1C11C2176.3(4)
Fe1C7C8C9-60.8(4) C13N1C11C2-61.4(5)
Fe1C8C9C10-60.0(4) C14Si1O1C24173.5(4)
Fe1C9C10C6-60.1(4) C14Si1O2C2564.9(4)
Si1C1C2Fe1129.3(4) C14Si1C1Fe151.9(4)
Si1C1C2C3-171.5(3) C14Si1C1C2-46.0(5)
Si1C1C2C118.9(7) C14Si1C1C5143.5(4)
Si1C1C5Fe1-128.6(3) C14C15C16C17-2.7(8)
Si1C1C5C4172.7(3) C14C19C20C21-178.7(4)
Si1C14C15C16-179.1(4) C15C14C19C18-0.2(6)
Si1C14C19C18-178.6(3) C15C14C19C20179.3(4)
Si1C14C19C200.9(6) C15C16C17C180.7(8)
O1Si1O2C25-47.9(4) C16C17C18C191.4(8)
O1Si1C1Fe1167.6(3) C16C17C18C23-179.3(5)
O1Si1C1C269.8(4) C17C18C19C14-1.7(7)
O1Si1C1C5-100.8(4) C17C18C19C20178.8(4)
O1Si1C14C15-31.2(4) C17C18C23C22-179.8(5)
O1Si1C14C19147.2(4) C18C19C20C210.8(7)
O2Si1O1C24-65.1(4) C19C14C15C162.4(7)
O2Si1C1Fe1-74.3(3) C19C18C23C22-0.5(8)
O2Si1C1C2-172.2(4) C19C20C21C22-0.2(8)
O2Si1C1C517.2(4) C20C21C22C23-0.8(8)
O2Si1C14C15-149.4(3) C21C22C23C181.1(8)
O2Si1C14C1929.0(4) C23C18C19C14179.0(4)
C1Si1O1C2448.4(5) C23C18C19C20-0.5(7)
C1Si1O2C25-167.3(4) C6C7C8Fe160.7(4)
C1Si1C14C1590.6(4) C6C7C8C90.0(6)
C1Si1C14C19-91.0(4) C7C6C10Fe1-58.8(4)
C1C2C3Fe1-59.8(3) C7C6C10C90.7(6)
C1C2C3C4-0.8(5) C7C8C9Fe160.5(4)
C1C2C11N1-78.9(6) C7C8C9C100.5(6)
C2C1C5Fe158.9(3) C8C9C10Fe159.4(4)
C2C1C5C40.1(5) C8C9C10C6-0.7(6)
C2C3C4Fe1-58.8(3) C10C6C7Fe159.2(4)
C2C3C4C50.9(5) C10C6C7C8-0.4(6)

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for 3074.
AtomxyzU(eq)
H3766612831765739
H4984511649816042
H51108810316745032
H11A654511770626135
H11B609112770667535
H12A634712893545261
H12B733614049542261
H12C576413896584661
H13A766714452662556
H13B914314611616656
H13C945413819669556
H15852111362526037
H16633511024460646
H1749899320459547
H2087658153635535
H2174106473631442
H2253676107562047
H2346317442498041
H24A1311312243570595
H24B1357811257612695
H24C1228812210632095
H25A125579065571264
H25B118187956598664
H25C134638544625364
H659219107681962
H7428510744719566
H8519411015820759
H973449566844359
H1078288402758464

Experimental

Single crystals of C25H29FeNO2Si [3074] 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 Superflip [2] structure solution program using Charge Flipping 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. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst., 40, 786-790; Palatinus, L. & van der Lee, A. (2008). J. Appl. Cryst. 41, 975-984; Palatinus, L., Prathapa, S. J. & van Smaalen, S. (2012). J. Appl. Cryst. 45, 575-580.
  3. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Crystal structure determination of [3074]

Crystal Data for C25H29FeNO2Si (=459.43 g/mol): orthorhombic, space group P212121 (no. 19), a = 7.8104(5) Å, b = 12.1050(9) Å, c = 23.811(2) Å, = 2251.2(3) Å3, Z = 4, T = 173 K, μ(MoKα) = 0.745 mm-1, Dcalc = 1.356 g/cm3, 17819 reflections measured (4.798° ≤ 2Θ ≤ 53.996°), 4885 unique (Rint = 0.0658, Rsigma = 0.0771) which were used in all calculations. The final R1 was 0.0522 (I > 2σ(I)) and wR2 was 0.0948 (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 Secondary CH2 refined with riding coordinates:
C11(H11A,H11B)
2.b Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21),
C22(H22), C23(H23), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10)
2.c Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C24(H24A,H24B,H24C), C25(H25A,H25B,
H25C)

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