3214

Table 1 Crystal data and structure refinement for 3214.
Identification code 3214
Empirical formula C28H39Fe2NO2Si2
Formula weight 589.48
Temperature/K 173.15
Crystal system triclinic
Space group P-1
a/Å 6.5034(3)
b/Å 14.1336(6)
c/Å 15.1720(7)
α/° 91.897(4)
β/° 96.259(4)
γ/° 93.728(4)
Volume/Å3 1382.17(11)
Z 2
ρcalcg/cm3 1.416
μ/mm‑1 1.162
F(000) 620.0
Crystal size/mm3 0.096 × 0.072 × 0.043
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 5.406 to 51.996
Index ranges -8 ≤ h ≤ 8, -17 ≤ k ≤ 17, -18 ≤ l ≤ 18
Reflections collected 18465
Independent reflections 5406 [Rint = 0.0357, Rsigma = 0.0370]
Data/restraints/parameters 5406/0/323
Goodness-of-fit on F2 1.026
Final R indexes [I>=2σ (I)] R1 = 0.0343, wR2 = 0.0798
Final R indexes [all data] R1 = 0.0459, wR2 = 0.0857
Largest diff. peak/hole / e Å-3 0.74/-0.48

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for 3214. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Fe12265.4(5)1430.8(2)7114.0(2)20.78(10)
Fe22940.0(7)2057.4(3)11064.1(2)42.24(13)
Si12037.7(9)2969.6(5)8934.0(4)21.32(15)
Si22976.9(10)2446.3(5)5068.9(4)23.81(15)
O13207(2)3957.2(11)9365.7(10)25.3(4)
O2-476(2)3016.4(13)8842.8(11)33.6(4)
N1157(3)4325.6(15)7019.7(13)30.2(5)
C12894(3)2694.3(16)7835.9(14)20.0(5)
C21957(3)2844.3(15)6950.5(14)18.5(4)
C33221(3)2485.1(16)6310.2(14)20.7(5)
C44943(3)2108.2(18)6816.7(15)25.7(5)
C54743(3)2232.9(17)7733.1(15)24.9(5)
C6-285(4)721.3(18)7515.8(19)37.9(6)
C7-331(4)617.7(19)6588.5(19)39.3(7)
C81455(5)179.5(18)6400.7(17)41.2(7)
C92623(5)4.6(19)7209.7(19)41.4(7)
C101532(5)343.2(18)7899.3(17)38.9(7)
C114389(5)3525(2)4695.2(17)40.1(7)
C12242(4)2369(2)4542.4(17)47.1(8)
C134274(4)1383.3(19)4694.3(16)34.5(6)
C14-44(4)3316.2(17)6761.5(15)24.3(5)
C151567(5)4854(2)6509.0(19)45.9(7)
C16-1880(5)4699(2)6908(2)54.4(9)
C173532(4)4796.6(18)8895.5(16)31.8(6)
C18-1480(5)3742(3)9236(3)64.7(11)
C192771(4)2039.2(18)9706.9(15)31.1(6)
C201406(6)1316(2)10001.9(17)51.7(9)
C212595(9)712(2)10547(2)77.6(14)
C224664(8)1040(3)10598(2)74.6(14)
C234813(5)1862(2)10090.3(17)47.6(8)
C242214(6)3350(2)11504.7(18)48.5(8)
C25782(6)2633(3)11748(2)63(1)
C261927(7)1997(2)12277.2(19)70.3(12)
C274021(7)2328(2)12365.8(19)63.7(11)
C284186(6)3159(2)11895.3(18)49.6(8)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for 3214. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Fe126.49(19)19.70(18)16.71(16)-0.82(12)2.91(13)5.70(13)
Fe287.2(4)24.7(2)16.55(19)-1.58(15)14.13(19)3.7(2)
Si122.1(3)24.8(4)16.9(3)-4.3(2)3.6(2)0.9(3)
Si226.6(4)29.9(4)15.3(3)-0.9(3)3.5(2)3.8(3)
O128.6(9)27.0(9)19.2(8)-3.9(7)1.8(7)-1.9(7)
O222.3(9)44.2(11)33.9(10)-12.2(8)6.0(7)0.6(8)
N139.5(12)26.2(12)24.6(10)-5.7(8)-2.6(9)13.8(9)
C120.9(12)20.4(12)18.1(11)-3.2(9)2.3(9)-0.6(9)
C220.3(11)15.7(11)19.0(11)-1.8(8)2.5(8)-1.5(9)
C320.7(12)22.8(12)18.9(11)0.0(9)4.6(9)-0.7(9)
C419.4(12)37.0(15)21.5(12)-2.4(10)4.7(9)5.1(10)
C521.3(12)33.8(14)19.1(11)-2.4(10)-1.5(9)4.7(10)
C645.1(17)20.8(14)50.6(17)3.4(12)20.7(13)-2.0(12)
C742.6(17)25.9(14)45.8(16)2.2(12)-5.3(13)-7.5(12)
C872(2)22.6(14)28.9(14)-8.2(11)13.8(13)-6.0(13)
C956.3(19)22.4(14)48.6(17)3.5(12)11.2(14)16.3(13)
C1070(2)22.0(14)25.5(13)3.5(10)7.3(13)3.9(13)
C1158.8(19)37.4(16)26.5(14)5.7(12)14.4(13)2.4(14)
C1236.3(16)82(2)21.6(13)-11.9(14)-2.8(11)7.7(15)
C1347.7(16)34.8(15)22.7(12)-2.0(11)10.4(11)6.6(12)
C1425.7(12)27.5(13)19.1(11)-4.9(9)-0.3(9)5.6(10)
C1568(2)25.8(15)43.6(17)4.3(12)4.1(15)4.6(14)
C1663(2)50(2)49.5(18)-18.7(15)-9.1(15)35.3(17)
C1738.9(15)28.7(14)26.6(13)-2.4(10)3.0(11)-5.1(11)
C1829.9(16)78(3)86(3)-41(2)14.9(16)8.1(16)
C1949.8(16)28.1(14)16.6(11)-3.4(10)8.7(11)5.0(12)
C2097(3)34.2(17)23.6(14)-9.5(12)20.9(15)-15.6(16)
C21185(5)26.2(18)24.3(16)-4.0(13)26(2)4(2)
C22150(4)54(2)25.2(16)3.6(15)5(2)59(3)
C2373(2)51.7(19)22.0(13)0.3(12)6.9(13)31.7(17)
C2486(2)32.0(16)30.2(15)-9.0(12)18.2(15)7.6(16)
C2582(3)68(3)40.7(18)-23.3(17)29.7(17)-5(2)
C26146(4)43(2)23.2(15)-8.9(14)36(2)-20(2)
C27134(4)33.0(18)22.4(15)-3.4(12)5.1(18)4(2)
C2890(3)30.8(16)26.7(14)-5.4(12)6.0(15)-0.1(16)

 

Table 4 Bond Lengths for 3214.
AtomAtomLength/Å AtomAtomLength/Å
Fe1C12.058(2) Si2C131.872(3)
Fe1C22.041(2) O1C171.420(3)
Fe1C32.064(2) O2C181.402(3)
Fe1C42.033(2) N1C141.461(3)
Fe1C52.031(2) N1C151.450(4)
Fe1C62.043(3) N1C161.453(3)
Fe1C72.050(3) C1C21.441(3)
Fe1C82.050(3) C1C51.426(3)
Fe1C92.052(3) C2C31.440(3)
Fe1C102.040(3) C2C141.505(3)
Fe2C192.049(2) C3C41.430(3)
Fe2C202.023(3) C4C51.417(3)
Fe2C212.023(3) C6C71.407(4)
Fe2C222.034(3) C6C101.404(4)
Fe2C232.037(3) C7C81.403(4)
Fe2C242.026(3) C8C91.409(4)
Fe2C252.030(3) C9C101.414(4)
Fe2C262.024(3) C19C201.426(4)
Fe2C272.038(3) C19C231.431(4)
Fe2C282.039(3) C20C211.415(5)
Si1O11.6274(17) C21C221.388(6)
Si1O21.6316(17) C22C231.420(5)
Si1C11.851(2) C24C251.416(5)
Si1C191.842(3) C24C281.399(5)
Si2C31.871(2) C25C261.419(5)
Si2C111.865(3) C26C271.402(6)
Si2C121.863(3) C27C281.399(4)

 

Table 5 Bond Angles for 3214.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C1Fe1C369.81(9) O1Si1O2111.26(9)
C2Fe1C141.17(8) O1Si1C1110.58(9)
C2Fe1C341.06(9) O1Si1C19106.27(10)
C2Fe1C6114.06(10) O2Si1C1110.07(9)
C2Fe1C7112.11(10) O2Si1C19108.69(11)
C2Fe1C8137.67(10) C19Si1C1109.88(11)
C2Fe1C9176.87(10) C3Si2C13107.86(11)
C4Fe1C168.93(9) C11Si2C3108.89(11)
C4Fe1C268.27(9) C11Si2C13107.98(13)
C4Fe1C340.84(9) C12Si2C3113.65(11)
C4Fe1C6174.96(10) C12Si2C11109.44(14)
C4Fe1C7143.93(11) C12Si2C13108.86(14)
C4Fe1C8114.10(11) C17O1Si1124.91(14)
C4Fe1C9110.00(11) C18O2Si1123.56(18)
C4Fe1C10135.27(11) C15N1C14111.9(2)
C5Fe1C140.81(9) C15N1C16110.4(2)
C5Fe1C268.41(9) C16N1C14109.0(2)
C5Fe1C369.12(9) Si1C1Fe1125.77(12)
C5Fe1C440.79(9) C2C1Fe168.81(12)
C5Fe1C6135.09(10) C2C1Si1131.25(17)
C5Fe1C7175.27(11) C5C1Fe168.61(13)
C5Fe1C8142.56(11) C5C1Si1122.75(16)
C5Fe1C9112.15(11) C5C1C2105.99(19)
C5Fe1C10109.07(11) C1C2Fe170.02(12)
C6Fe1C1109.61(10) C1C2C14123.14(19)
C6Fe1C3143.76(10) C3C2Fe170.31(13)
C6Fe1C740.21(11) C3C2C1109.86(19)
C6Fe1C867.51(12) C3C2C14127.00(19)
C6Fe1C967.88(12) C14C2Fe1126.45(16)
C7Fe1C1136.58(11) Si2C3Fe1127.13(12)
C7Fe1C3114.55(10) C2C3Fe168.63(12)
C7Fe1C840.01(12) C2C3Si2133.15(17)
C7Fe1C967.60(12) C4C3Fe168.44(13)
C8Fe1C1176.58(11) C4C3Si2121.21(17)
C8Fe1C3111.27(10) C4C3C2105.64(18)
C8Fe1C940.18(11) C3C4Fe170.73(13)
C9Fe1C1141.16(10) C5C4Fe169.53(13)
C9Fe1C3135.95(10) C5C4C3109.4(2)
C10Fe1C1111.67(10) C1C5Fe170.58(13)
C10Fe1C2142.60(10) C4C5Fe169.68(13)
C10Fe1C3175.57(11) C4C5C1109.09(19)
C10Fe1C640.25(11) C7C6Fe170.17(15)
C10Fe1C767.49(11) C10C6Fe169.76(16)
C10Fe1C867.51(11) C10C6C7107.8(2)
C10Fe1C940.44(11) C6C7Fe169.62(15)
C20Fe2C1940.99(11) C8C7Fe170.03(16)
C20Fe2C2268.19(16) C8C7C6108.1(2)
C20Fe2C2368.55(13) C7C8Fe169.96(15)
C20Fe2C24124.54(14) C7C8C9108.5(2)
C20Fe2C25107.32(15) C9C8Fe169.98(15)
C20Fe2C26121.29(15) C8C9Fe169.84(15)
C20Fe2C27156.65(13) C8C9C10107.2(3)
C20Fe2C28161.49(13) C10C9Fe169.30(15)
C21Fe2C1968.99(11) C6C10Fe169.99(15)
C21Fe2C2040.95(15) C6C10C9108.4(2)
C21Fe2C2240.00(17) C9C10Fe170.26(15)
C21Fe2C2368.27(16) N1C14C2112.69(19)
C21Fe2C24160.31(19) Si1C19Fe2129.66(13)
C21Fe2C25122.70(19) C20C19Fe268.52(14)
C21Fe2C26105.82(14) C20C19Si1126.2(2)
C21Fe2C27120.64(14) C20C19C23106.3(3)
C21Fe2C28156.84(17) C23C19Fe269.06(14)
C22Fe2C1968.85(11) C23C19Si1127.4(2)
C22Fe2C2340.81(14) C19C20Fe270.49(16)
C22Fe2C27106.87(15) C21C20Fe269.51(19)
C22Fe2C28122.93(18) C21C20C19108.5(3)
C23Fe2C1941.00(11) C20C21Fe269.54(18)
C23Fe2C27123.58(16) C22C21Fe270.4(2)
C23Fe2C28109.17(14) C22C21C20108.5(3)
C24Fe2C19108.71(11) C21C22Fe269.6(2)
C24Fe2C22159.00(19) C21C22C23108.5(3)
C24Fe2C23123.67(13) C23C22Fe269.72(18)
C24Fe2C2540.88(13) C19C23Fe269.95(16)
C24Fe2C2768.14(13) C22C23Fe269.5(2)
C24Fe2C2840.27(13) C22C23C19108.1(3)
C25Fe2C19122.68(13) C25C24Fe269.70(18)
C25Fe2C22158.22(18) C28C24Fe270.34(17)
C25Fe2C23159.41(14) C28C24C25107.7(3)
C25Fe2C2768.33(16) C24C25Fe269.43(18)
C25Fe2C2867.97(15) C24C25C26107.3(3)
C26Fe2C19158.06(16) C26C25Fe269.3(2)
C26Fe2C22121.67(15) C25C26Fe269.73(17)
C26Fe2C23158.67(16) C27C26Fe270.36(18)
C26Fe2C2468.62(13) C27C26C25108.2(3)
C26Fe2C2540.97(15) C26C27Fe269.27(18)
C26Fe2C2740.37(15) C28C27Fe269.95(17)
C26Fe2C2867.74(14) C28C27C26107.9(3)
C27Fe2C19160.65(15) C24C28Fe269.39(17)
C27Fe2C2840.14(12) C27C28Fe269.91(18)
C28Fe2C19125.22(11) C27C28C24108.9(3)

 

Table 6 Torsion Angles for 3214.
ABCDAngle/˚ ABCDAngle/˚
Fe1C1C2C3-59.17(15) C2C1C5C40.3(3)
Fe1C1C2C14121.2(2) C2C3C4Fe158.83(15)
Fe1C1C5C459.23(17) C2C3C4C5-0.1(3)
Fe1C2C3Si2121.4(2) C3C2C14N1-110.8(2)
Fe1C2C3C4-58.71(16) C3C4C5Fe159.65(17)
Fe1C2C14N1157.39(16) C3C4C5C1-0.1(3)
Fe1C3C4C5-58.93(17) C5C1C2Fe158.81(16)
Fe1C4C5C1-59.78(17) C5C1C2C3-0.4(3)
Fe1C6C7C859.68(19) C5C1C2C14180.0(2)
Fe1C6C10C9-60.00(19) C6C7C8Fe1-59.43(18)
Fe1C7C8C959.60(19) C6C7C8C90.2(3)
Fe1C8C9C1059.49(19) C7C6C10Fe160.11(18)
Fe1C9C10C659.83(19) C7C6C10C90.1(3)
Fe2C19C20C21-59.3(2) C7C8C9Fe1-59.59(19)
Fe2C19C23C2259.2(2) C7C8C9C10-0.1(3)
Fe2C20C21C22-59.9(2) C8C9C10Fe1-59.84(19)
Fe2C21C22C23-59.0(2) C8C9C10C60.0(3)
Fe2C22C23C19-59.47(19) C10C6C7Fe1-59.85(18)
Fe2C24C25C2659.2(2) C10C6C7C8-0.2(3)
Fe2C24C28C27-58.9(2) C11Si2C3Fe1-172.95(15)
Fe2C25C26C2760.1(2) C11Si2C3C292.3(2)
Fe2C26C27C2859.5(2) C11Si2C3C4-87.6(2)
Fe2C27C28C2458.6(2) C12Si2C3Fe164.78(19)
Si1C1C2Fe1-119.6(2) C12Si2C3C2-30.0(3)
Si1C1C2C3-178.76(17) C12Si2C3C4150.2(2)
Si1C1C2C141.6(3) C13Si2C3Fe1-56.01(17)
Si1C1C5Fe1119.64(17) C13Si2C3C2-150.8(2)
Si1C1C5C4178.87(17) C13Si2C3C429.4(2)
Si1C19C20Fe2-124.2(2) C14C2C3Fe1-121.4(2)
Si1C19C20C21176.5(2) C14C2C3Si20.1(4)
Si1C19C23Fe2124.6(2) C14C2C3C4179.9(2)
Si1C19C23C22-176.2(2) C15N1C14C264.0(3)
Si2C3C4Fe1-121.29(16) C16N1C14C2-173.7(2)
Si2C3C4C5179.78(17) C19Si1O1C17162.29(19)
O1Si1O2C18-11.0(3) C19Si1O2C18105.7(3)
O1Si1C1Fe1169.17(12) C19Si1C1Fe152.17(17)
O1Si1C1C2-98.6(2) C19Si1C1C2144.4(2)
O1Si1C1C583.2(2) C19Si1C1C5-33.8(2)
O1Si1C19Fe243.8(2) C19C20C21Fe259.9(2)
O1Si1C19C20134.8(2) C19C20C21C220.0(3)
O1Si1C19C23-49.0(2) C20C19C23Fe2-58.62(17)
O2Si1O1C17-79.6(2) C20C19C23C220.6(3)
O2Si1C1Fe1-67.49(16) C20C21C22Fe259.3(2)
O2Si1C1C224.8(2) C20C21C22C230.3(4)
O2Si1C1C5-153.42(19) C21C22C23Fe258.9(2)
O2Si1C19Fe2-76.05(19) C21C22C23C19-0.6(3)
O2Si1C19C2014.9(2) C23C19C20Fe258.96(18)
O2Si1C19C23-168.9(2) C23C19C20C21-0.4(3)
C1Si1O1C1743.1(2) C24C25C26Fe2-59.3(2)
C1Si1O2C18-133.9(3) C24C25C26C270.8(3)
C1Si1C19Fe2163.45(16) C25C24C28Fe259.9(2)
C1Si1C19C20-105.5(2) C25C24C28C271.0(3)
C1Si1C19C2370.6(2) C25C26C27Fe2-59.7(2)
C1C2C3Fe158.99(15) C25C26C27C28-0.2(3)
C1C2C3Si2-179.58(18) C26C27C28Fe2-59.1(2)
C1C2C3C40.3(3) C26C27C28C24-0.5(3)
C1C2C14N168.8(3) C28C24C25Fe2-60.3(2)
C2C1C5Fe1-58.93(15) C28C24C25C26-1.1(3)

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for 3214.
AtomxyzU(eq)
H460481819657631
H556912040820430
H6-1301998782745
H7-1388811616347
H8181627582549
H93904-286727950
H101956319851747
H11A37594093489860
H11B43043502404660
H11C58473547494660
H12A-5591866481271
H12B2112222390571
H12C-3642976463371
H13A57561456490852
H13B40981326404552
H13C3649812493552
H14A-5193240611929
H14B-11142995708629
H15A10114816588169
H15B29234583657869
H15C17225519672369
H16A-17645371710082
H16B-28064345726782
H16C-24454632628282
H17A42854655838748
H17B43455279929048
H17C21905034868548
H18A-10354353900797
H18B-11233756988197
H18C-29843625909597
H20-561250985762
H2120661721082993
H2257917621092089
H23605222311001757
H24189338671114158
H25-67625871158776
H26137114431252884
H27513220391268876
H28543435341184960

Experimental

Single crystals of C28H39Fe2NO2Si2 [3214] were []. A suitable crystal was selected and [] on a Xcalibur, Sapphire3 diffractometer. The crystal was kept at 173.15 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 [3214]

Crystal Data for C28H39Fe2NO2Si2 (=589.48 g/mol): triclinic, space group P-1 (no. 2), a = 6.5034(3) Å, b = 14.1336(6) Å, c = 15.1720(7) Å, α = 91.897(4)°, β = 96.259(4)°, γ = 93.728(4)°, = 1382.17(11) Å3, Z = 2, T = 173.15 K, μ(MoKα) = 1.162 mm-1, Dcalc = 1.416 g/cm3, 18465 reflections measured (5.406° ≤ 2Θ ≤ 51.996°), 5406 unique (Rint = 0.0357, Rsigma = 0.0370) which were used in all calculations. The final R1 was 0.0343 (I > 2σ(I)) and wR2 was 0.0857 (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:
C14(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21),
C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28)
2.c Idealised Me refined as rotating group:
C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,
H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)

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