3245

Table 1 Crystal data and structure refinement for 3245.
Identification code 3245
Empirical formula C26H35Fe2NO2Si2
Formula weight 561.43
Temperature/K 173.15
Crystal system monoclinic
Space group P21/n
a/Å 8.3578(5)
b/Å 33.5505(17)
c/Å 9.6944(5)
α/° 90
β/° 98.012(5)
γ/° 90
Volume/Å3 2691.8(3)
Z 4
ρcalcg/cm3 1.385
μ/mm‑1 1.190
F(000) 1176.0
Crystal size/mm3 0.3 × 0.3 × 0.1
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.414 to 52
Index ranges -10 ≤ h ≤ 10, -41 ≤ k ≤ 41, -11 ≤ l ≤ 11
Reflections collected 22659
Independent reflections 5294 [Rint = 0.0551, Rsigma = 0.0526]
Data/restraints/parameters 5294/0/311
Goodness-of-fit on F2 1.043
Final R indexes [I>=2σ (I)] R1 = 0.0371, wR2 = 0.0722
Final R indexes [all data] R1 = 0.0573, wR2 = 0.0807
Largest diff. peak/hole / e Å-3 0.39/-0.33

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for 3245. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Fe12990.0(5)1480.5(2)7528.3(4)19.53(11)
Fe27793.2(4)171.0(2)6820.8(4)17.87(11)
Si14874.6(8)555.7(2)8742.6(7)16.51(16)
Si22058.4(10)2118.6(2)10202.7(8)25.34(19)
O15983(2)510.5(6)10268(2)23.3(5)
O23614(2)191.9(6)8389(2)22.6(5)
N16250(3)1249.2(7)11421(2)24.8(5)
C13585(3)1004.3(7)8855(2)17.0(6)
C23967(3)1381.0(7)9547(2)17.3(6)
C32512(3)1617.5(7)9503(2)19.3(6)
C41241(3)1377.3(7)8764(3)19.8(6)
C51892(3)1008.1(7)8385(3)18.3(6)
C64500(4)1472(1)6039(3)40.3(8)
C74517(4)1848.8(9)6663(3)38.0(8)
C82933(5)2002.0(9)6434(3)40.6(9)
C91933(4)1718.4(10)5678(3)43.6(9)
C102909(5)1390.4(9)5432(3)41.9(9)
C115657(3)1491.8(8)10174(3)23.1(6)
C127975(4)1322.4(10)11857(3)41.0(8)
C135320(4)1338.9(9)12563(3)33.3(7)
C141816(4)2070.2(9)12082(3)31.8(7)
C153644(4)2501.7(9)10019(3)48.7(9)
C1687(4)2286.8(10)9226(3)46.8(9)
C176161(3)585.5(7)7346(3)17.5(6)
C185693(3)438.7(8)5954(3)20.4(6)
C196941(3)520.0(8)5140(3)25.7(7)
C208206(3)719.3(8)6008(3)26.0(6)
C217732(3)760.2(7)7357(3)21.6(6)
C228064(3)-258.2(8)8347(3)24.6(6)
C237337(3)-422.4(8)7059(3)24.3(6)
C248428(3)-365.5(8)6068(3)26.2(6)
C259813(3)-170.6(8)6753(3)25.3(6)
C269591(3)-104.4(8)8153(3)26.2(6)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for 3245. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Fe125.8(2)17.2(2)16.05(19)0.80(16)4.55(16)2.31(17)
Fe214.3(2)22.7(2)16.91(19)-1.89(16)3.30(15)1.91(16)
Si114.6(4)16.5(4)18.6(4)-0.2(3)3.2(3)0.6(3)
Si235.3(5)18.5(4)22.9(4)-3.5(3)6.8(4)3.4(3)
O127.8(12)18.3(11)22.5(11)-1.1(10)-0.7(9)1.3(9)
O220.7(11)16.1(11)29.8(11)4.3(9)-0.4(8)-0.7(9)
N120.1(13)29.1(13)23.5(12)-2.1(11)-3.1(10)-0.9(10)
C117.8(14)18.4(14)15.5(12)2.6(11)5.0(11)0.0(11)
C219.2(14)18.7(14)14.6(12)2.4(11)4.7(11)-1.9(11)
C321.8(15)19.5(14)17.6(13)1.7(11)6.4(11)-2.1(11)
C414.1(14)22.5(14)23.6(14)-0.8(12)5.3(11)2.3(11)
C517.5(14)16.4(13)21.5(13)-2.3(11)4.6(11)-0.8(11)
C654(2)38(2)33.8(18)16.0(15)26.4(17)16.0(17)
C749(2)37.6(19)28.6(16)13.7(15)11.1(15)-12.1(17)
C876(3)22.9(16)26.2(16)10.1(14)18.8(17)11.3(17)
C952(2)56(2)20.9(15)12.7(16)0.9(15)13.0(19)
C1081(3)29.2(18)16.7(15)-1.3(13)10.3(16)-2.5(18)
C1123.0(15)23.5(15)23.0(14)-0.6(12)4.1(12)-3.1(12)
C1229.3(19)51(2)39.5(18)-3.3(16)-8.7(15)-2.5(16)
C1342(2)35.7(18)21.2(15)0.9(13)2.6(14)0.7(15)
C1437.4(19)31.0(17)28.0(15)-6.4(13)7.6(14)4.6(14)
C1575(3)26.4(18)49(2)-9.1(16)24.7(19)-12.9(18)
C1663(2)38(2)36.3(18)-10.4(15)-2.4(17)29.3(18)
C1713.4(14)17.0(13)21.8(13)-2.2(11)1.7(11)1.4(11)
C1815.2(14)22.8(15)22.7(14)-1.0(12)1.1(11)5.7(11)
C1926.9(16)31.1(16)19.6(14)4.1(12)4.4(12)11.2(13)
C2022.4(16)26.2(15)31.6(16)6.1(13)11.6(13)0.5(12)
C2117.4(15)18.9(14)28.8(15)-2.4(12)3.8(12)1.7(11)
C2223.9(16)28.9(16)21.7(14)3.2(12)6.3(12)4.4(12)
C2321.4(15)21.4(15)29.6(15)1.6(12)1.6(12)2.0(12)
C2431.4(17)24.5(15)23.3(14)-3.7(12)5.6(13)7.9(13)
C2517.4(15)30.9(16)29.0(15)4.3(13)7.6(12)10.2(12)
C2620.3(16)32.5(17)24.6(14)2.2(13)-1.0(12)3.4(13)

 

Table 4 Bond Lengths for 3245.
AtomAtomLength/Å AtomAtomLength/Å
Fe1C12.068(2) Si2C151.873(3)
Fe1C22.040(2) Si2C161.869(3)
Fe1C32.062(2) N1C111.484(3)
Fe1C42.045(3) N1C121.466(3)
Fe1C52.063(3) N1C131.470(3)
Fe1C62.047(3) C1C21.446(3)
Fe1C72.039(3) C1C51.425(3)
Fe1C82.043(3) C2C31.448(4)
Fe1C92.048(3) C2C111.504(3)
Fe1C102.047(3) C3C41.442(3)
Fe2C172.061(2) C4C51.422(3)
Fe2C182.046(2) C6C71.401(4)
Fe2C192.052(3) C6C101.404(5)
Fe2C202.049(3) C7C81.409(4)
Fe2C212.047(3) C8C91.403(4)
Fe2C222.055(3) C9C101.410(4)
Fe2C232.046(3) C17C181.438(3)
Fe2C242.040(3) C17C211.437(3)
Fe2C252.049(3) C18C191.420(4)
Fe2C262.059(3) C19C201.423(4)
Si1O11.639(2) C20C211.425(4)
Si1O21.618(2) C22C231.421(4)
Si1C11.863(3) C22C261.413(4)
Si1C171.845(3) C23C241.427(4)
Si2C31.871(3) C24C251.412(4)
Si2C141.868(3) C25C261.413(4)

 

Table 5 Bond Angles for 3245.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C2Fe1C141.20(9) C26Fe2C17126.75(10)
C2Fe1C341.34(10) O1Si1C1106.33(11)
C2Fe1C468.50(10) O1Si1C17110.67(11)
C2Fe1C568.24(10) O2Si1O1113.03(11)
C2Fe1C6118.08(12) O2Si1C1104.89(11)
C2Fe1C8127.99(12) O2Si1C17108.31(11)
C2Fe1C9165.95(12) C17Si1C1113.57(11)
C2Fe1C10151.85(13) C3Si2C15113.60(14)
C3Fe1C169.86(10) C14Si2C3109.29(12)
C3Fe1C569.06(10) C14Si2C15109.08(14)
C4Fe1C168.56(10) C14Si2C16108.22(14)
C4Fe1C341.10(10) C16Si2C3107.24(13)
C4Fe1C540.49(9) C16Si2C15109.27(17)
C4Fe1C6166.63(12) C12N1C11110.3(2)
C4Fe1C9108.83(13) C12N1C13110.5(2)
C4Fe1C10129.03(13) C13N1C11110.5(2)
C5Fe1C140.36(9) Si1C1Fe1132.76(13)
C6Fe1C1108.03(11) C2C1Fe168.39(14)
C6Fe1C3151.28(13) C2C1Si1129.88(19)
C6Fe1C5128.78(12) C5C1Fe169.65(14)
C6Fe1C967.71(13) C5C1Si1123.06(19)
C6Fe1C1040.12(13) C5C1C2106.6(2)
C7Fe1C1127.88(12) C1C2Fe170.41(13)
C7Fe1C2107.69(11) C1C2C3109.6(2)
C7Fe1C3117.41(12) C1C2C11122.5(2)
C7Fe1C4152.03(12) C3C2Fe170.12(14)
C7Fe1C5165.99(12) C3C2C11127.9(2)
C7Fe1C640.10(12) C11C2Fe1125.08(17)
C7Fe1C840.37(13) Si2C3Fe1127.74(13)
C7Fe1C967.78(13) C2C3Fe168.54(14)
C7Fe1C1067.47(13) C2C3Si2133.9(2)
C8Fe1C1166.11(13) C4C3Fe168.81(14)
C8Fe1C3107.33(11) C4C3Si2120.65(19)
C8Fe1C4118.84(12) C4C3C2105.4(2)
C8Fe1C5152.53(13) C3C4Fe170.08(14)
C8Fe1C667.51(13) C5C4Fe170.45(14)
C8Fe1C940.12(13) C5C4C3109.5(2)
C8Fe1C1067.39(12) C1C5Fe169.98(14)
C9Fe1C1152.01(12) C4C5Fe169.05(14)
C9Fe1C3127.63(12) C4C5C1108.9(2)
C9Fe1C5119.36(13) C7C6Fe169.65(17)
C10Fe1C1118.37(11) C7C6C10108.0(3)
C10Fe1C3166.27(13) C10C6Fe169.94(18)
C10Fe1C5109.36(12) C6C7Fe170.24(17)
C10Fe1C940.30(12) C6C7C8108.0(3)
C18Fe2C1741.00(9) C8C7Fe169.99(18)
C18Fe2C1940.55(10) C7C8Fe169.64(17)
C18Fe2C2068.19(11) C9C8Fe170.10(17)
C18Fe2C2168.26(10) C9C8C7108.3(3)
C18Fe2C22127.29(11) C8C9Fe169.78(16)
C18Fe2C23108.11(11) C8C9C10107.5(3)
C18Fe2C25153.66(10) C10C9Fe169.81(17)
C18Fe2C26164.67(10) C6C10Fe169.94(17)
C19Fe2C1769.06(10) C6C10C9108.3(3)
C19Fe2C22164.40(11) C9C10Fe169.89(17)
C19Fe2C26153.70(11) N1C11C2112.4(2)
C20Fe2C1769.01(10) Si1C17Fe2128.17(13)
C20Fe2C1940.60(11) C18C17Fe268.92(14)
C20Fe2C22153.97(11) C18C17Si1124.03(19)
C20Fe2C26119.80(11) C21C17Fe268.99(14)
C21Fe2C1740.94(10) C21C17Si1129.94(19)
C21Fe2C1968.42(11) C21C17C18106.0(2)
C21Fe2C2040.71(10) C17C18Fe270.08(14)
C21Fe2C22119.90(11) C19C18Fe269.97(15)
C21Fe2C25126.76(11) C19C18C17109.3(2)
C21Fe2C26108.44(11) C18C19Fe269.48(14)
C22Fe2C17107.78(10) C18C19C20107.7(2)
C22Fe2C2640.19(11) C20C19Fe269.59(15)
C23Fe2C17119.23(10) C19C20Fe269.80(15)
C23Fe2C19126.54(11) C19C20C21108.0(2)
C23Fe2C20163.91(11) C21C20Fe269.54(15)
C23Fe2C21154.09(11) C17C21Fe270.07(14)
C23Fe2C2240.56(10) C20C21Fe269.75(15)
C23Fe2C2568.10(11) C20C21C17108.9(2)
C23Fe2C2667.90(11) C23C22Fe269.41(15)
C24Fe2C17153.87(11) C26C22Fe270.06(15)
C24Fe2C18119.44(11) C26C22C23107.9(2)
C24Fe2C19107.33(11) C22C23Fe270.03(15)
C24Fe2C20126.04(11) C22C23C24107.7(2)
C24Fe2C21163.76(11) C24C23Fe269.33(15)
C24Fe2C2268.37(11) C23C24Fe269.79(15)
C24Fe2C2340.89(11) C25C24Fe270.13(15)
C24Fe2C2540.41(11) C25C24C23107.7(2)
C24Fe2C2667.98(11) C24C25Fe269.46(15)
C25Fe2C17164.16(10) C24C25C26108.4(2)
C25Fe2C19119.33(11) C26C25Fe270.24(15)
C25Fe2C20107.83(11) C22C26Fe269.75(15)
C25Fe2C2267.82(11) C25C26Fe269.52(15)
C25Fe2C2640.23(10) C25C26C22108.2(2)

 

Table 6 Hydrogen Bonds for 3245.
DHAd(D-H)/Åd(H-A)/Åd(D-A)/ÅD-H-A/°
O1H1N10.65(3)2.07(3)2.715(3)168(3)
O2H2O110.71(3)1.99(3)2.691(3)170(3)

11-X,-Y,2-Z

 

Table 7 Torsion Angles for 3245.
ABCDAngle/˚ ABCDAngle/˚
Fe1C1C2C359.35(17) C2C3C4Fe1-59.07(16)
Fe1C1C2C11-119.8(2) C2C3C4C50.5(3)
Fe1C1C5C4-58.20(17) C3C2C11N1112.0(3)
Fe1C2C3Si2-122.3(2) C3C4C5Fe1-59.39(17)
Fe1C2C3C459.25(16) C3C4C5C1-0.6(3)
Fe1C2C11N1-156.82(18) C5C1C2Fe1-59.45(16)
Fe1C3C4C559.62(17) C5C1C2C3-0.1(3)
Fe1C4C5C158.77(17) C5C1C2C11-179.2(2)
Fe1C6C7C8-60.1(2) C6C7C8Fe160.2(2)
Fe1C6C10C959.6(2) C6C7C8C90.6(3)
Fe1C7C8C9-59.7(2) C7C6C10Fe1-59.49(19)
Fe1C8C9C10-59.9(2) C7C6C10C90.1(3)
Fe1C9C10C6-59.6(2) C7C8C9Fe159.4(2)
Fe2C17C18C19-59.13(18) C7C8C9C10-0.5(3)
Fe2C17C21C2059.09(18) C8C9C10Fe159.9(2)
Fe2C18C19C20-59.32(18) C8C9C10C60.2(3)
Fe2C19C20C21-59.24(18) C10C6C7Fe159.7(2)
Fe2C20C21C17-59.29(18) C10C6C7C8-0.4(3)
Fe2C22C23C2459.30(18) C11C2C3Fe1119.5(2)
Fe2C22C26C25-59.07(19) C11C2C3Si2-2.8(4)
Fe2C23C24C2560.16(18) C11C2C3C4178.8(2)
Fe2C24C25C2659.66(19) C12N1C11C2170.9(2)
Fe2C25C26C2259.21(19) C13N1C11C2-66.6(3)
Si1C1C2Fe1128.4(2) C14Si2C3Fe1-177.43(16)
Si1C1C2C3-172.28(18) C14Si2C3C2-81.5(3)
Si1C1C2C118.6(4) C14Si2C3C496.7(2)
Si1C1C5Fe1-128.51(18) C15Si2C3Fe1-55.4(2)
Si1C1C5C4173.29(17) C15Si2C3C240.5(3)
Si1C17C18Fe2-122.60(19) C15Si2C3C4-141.2(2)
Si1C17C18C19178.27(18) C16Si2C3Fe165.5(2)
Si1C17C21Fe2122.8(2) C16Si2C3C2161.4(3)
Si1C17C21C20-178.1(2) C16Si2C3C4-20.4(2)
Si2C3C4Fe1122.24(17) C17Si1C1Fe113.1(2)
Si2C3C4C5-178.14(17) C17Si1C1C2-83.7(2)
O1Si1C1Fe1135.03(17) C17Si1C1C5105.2(2)
O1Si1C1C238.2(3) C17C18C19Fe259.19(18)
O1Si1C1C5-132.9(2) C17C18C19C20-0.1(3)
O1Si1C17Fe259.95(19) C18C17C21Fe2-59.28(16)
O1Si1C17C18148.7(2) C18C17C21C20-0.2(3)
O1Si1C17C21-33.7(3) C18C19C20Fe259.25(18)
O2Si1C1Fe1-104.99(18) C18C19C20C210.0(3)
O2Si1C1C2158.2(2) C19C20C21Fe259.40(18)
O2Si1C1C5-12.9(2) C19C20C21C170.1(3)
O2Si1C17Fe2-64.47(18) C21C17C18Fe259.32(17)
O2Si1C17C1824.3(2) C21C17C18C190.2(3)
O2Si1C17C21-158.1(2) C22C23C24Fe2-59.75(18)
C1Si1C17Fe2179.45(14) C22C23C24C250.4(3)
C1Si1C17C18-91.8(2) C23C22C26Fe259.29(18)
C1Si1C17C2185.8(3) C23C22C26C250.2(3)
C1C2C3Fe1-59.53(17) C23C24C25Fe2-59.94(18)
C1C2C3Si2178.16(19) C23C24C25C26-0.3(3)
C1C2C3C4-0.3(3) C24C25C26Fe2-59.17(18)
C1C2C11N1-69.0(3) C24C25C26C220.0(3)
C2C1C5Fe158.64(16) C26C22C23Fe2-59.69(19)
C2C1C5C40.4(3) C26C22C23C24-0.4(3)

 

Table 8 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for 3245.
AtomxyzU(eq)
H16100(40)674(8)10630(30)21(10)
H23760(30)-2(8)8660(30)22(9)
H41391454856224
H51295798789822
H654071302602748
H754351978715546
H825992254673849
H98041743538652
H1025521155494050
H11A63921455946628
H11B568217771043728
H12A857812591108862
H12B836011541266162
H12C814116031211462
H13A545016211281650
H13B571511741337350
H13C417412821226350
H14A104118571219348
H14B141623221241448
H14C286220061262648
H15A328727621032173
H15B38212518904273
H15C465524261059773
H16A-7792112944970
H16B1402276822370
H16C-1322561949370
H184703308563124
H196933453418631
H209193809573631
H218354883813726
H227605-253919029
H236308-548688929
H248254-445511731
H2510737-97634230
H261033922884431

Experimental

Single crystals of C26H35Fe2NO2Si2 [3245] 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 [3245]

Crystal Data for C26H35Fe2NO2Si2 (=561.43 g/mol): monoclinic, space group P21/n (no. 14), a = 8.3578(5) Å, b = 33.5505(17) Å, c = 9.6944(5) Å, β = 98.012(5)°, = 2691.8(3) Å3, Z = 4, T = 173.15 K, μ(MoKα) = 1.190 mm-1, Dcalc = 1.385 g/cm3, 22659 reflections measured (4.414° ≤ 2Θ ≤ 52°), 5294 unique (Rint = 0.0551, Rsigma = 0.0526) which were used in all calculations. The final R1 was 0.0371 (I > 2σ(I)) and wR2 was 0.0807 (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:
C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C18(H18), C19(H19),
C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26)
2.c Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,
H15C), C16(H16A,H16B,H16C)

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