mo_B0167_0m

Table 1 Crystal data and structure refinement for mo_B0167_0m.
Identification code mo_B0167_0m
Empirical formula C38H60Fe2N2O4Si2
Formula weight 776.76
Temperature/K 100.01
Crystal system triclinic
Space group P-1
a/Å 7.622(8)
b/Å 9.880(8)
c/Å 14.226(12)
α/° 76.29(3)
β/° 85.20(3)
γ/° 70.52(3)
Volume/Å3 981.2(15)
Z 1
ρcalcg/cm3 1.315
μ/mm‑1 0.840
F(000) 414.0
Crystal size/mm3 0.345 × 0.172 × 0.08
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.788 to 57.612
Index ranges -10 ≤ h ≤ 10, -11 ≤ k ≤ 13, -19 ≤ l ≤ 19
Reflections collected 23027
Independent reflections 5104 [Rint = 0.0371, Rsigma = 0.0295]
Data/restraints/parameters 5104/0/224
Goodness-of-fit on F2 1.048
Final R indexes [I>=2σ (I)] R1 = 0.0373, wR2 = 0.0858
Final R indexes [all data] R1 = 0.0497, wR2 = 0.0913
Largest diff. peak/hole / e Å-3 0.72/-0.45

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for mo_B0167_0m. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Fe12000.8(4)6859.2(3)5423.0(2)20.46(8)
Si12707.8(7)7578.1(6)7634.1(4)21.41(11)
O12676(2)9267.8(16)7180.0(11)36.4(4)
O24825(2)6439.3(18)7699.4(11)35.4(3)
N12329(3)3420(2)8121.7(13)40.7(5)
C11453(2)6980(2)6846.5(13)21.1(3)
C21639(3)5534(2)6724.6(13)24.6(4)
C3292(3)5690(3)6043.6(15)37.0(5)
C4-737(3)7194(3)5739.5(17)42.7(6)
C5-26(3)7992(3)6231.1(15)33.4(5)
C64438(2)5758(2)4823.1(12)19.8(3)
C72968(3)6267(2)4142.5(12)23.2(4)
C82220(3)7816(2)3991.6(15)29.7(4)
C93223(3)8279(2)4578.2(15)29.5(4)
C104584(2)7012(2)5097.3(13)22.1(4)
C113016(3)4109(2)7201.8(15)31.8(5)
C12865(4)2874(3)7983.2(19)52.8(8)
C133865(5)2228(3)8633.3(19)61.3(8)
C141471(3)7694(2)8822.9(14)32.5(5)
C151231(5)6228(3)9320.6(18)56.8(8)
C16-478(4)8847(3)8625(2)50.9(7)
C172481(4)8217(4)9468.6(18)52.8(7)
C183980(4)9740(3)6538.6(17)45.7(6)
C196368(4)6517(4)8155(2)58.6(8)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for mo_B0167_0m. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Fe118.65(13)28.38(15)20.23(13)-9.36(10)2.37(9)-13.11(10)
Si128.0(3)23.8(3)19.5(2)-7.40(19)2.69(19)-16.5(2)
O156(1)28.3(8)35.5(8)-11.6(6)15.5(7)-28.1(7)
O225.3(7)45.0(9)40.0(8)-10.5(7)-6.6(6)-14.5(6)
N174.0(14)31.7(10)26.9(9)-12.2(8)20.5(9)-31.9(10)
C120.3(8)27.0(9)20.2(8)-10.4(7)4.3(6)-10.6(7)
C229.9(10)33.4(10)22.2(9)-14.1(8)12.9(7)-23.2(8)
C336.5(11)68.6(16)30.2(11)-27.6(11)16.4(9)-41.1(12)
C419(1)85(2)32.3(11)-23.1(12)3.9(8)-21.4(11)
C521.9(9)44.1(13)31.3(11)-15.5(9)1.2(8)-2.4(8)
C620.4(8)27.7(9)16.0(8)-5.8(7)4.9(6)-14.5(7)
C725.3(9)33.9(10)14.9(8)-5.5(7)2.6(7)-16.2(8)
C829.6(10)33.4(11)25.7(10)2.4(8)-4.3(8)-14.7(8)
C928.2(10)27.2(10)36.0(11)-2.9(8)-0.2(8)-15.4(8)
C1020.2(8)28.9(10)23.8(9)-8.3(7)4.0(7)-15.7(7)
C1147.0(12)26.5(10)28.5(10)-10.5(8)17.2(9)-21.4(9)
C1287(2)47.3(14)45.4(14)-22.4(12)39.1(14)-51.0(15)
C13107(3)45.6(16)34.5(13)3.3(11)3.8(15)-37.6(17)
C1452.5(13)35.4(11)23.1(9)-13.5(8)10.5(9)-29.5(10)
C15114(3)45.1(14)27.3(11)-13.8(10)22.6(14)-47.4(16)
C1657.4(16)63.2(17)43.9(14)-29.0(13)23.0(12)-28.6(14)
C1772.6(18)81(2)31.6(12)-33.9(13)13.7(12)-48.9(16)
C1878.0(18)43.6(13)34.2(12)-12.5(10)18.1(12)-45.7(13)
C1933.1(13)108(3)42.5(14)-20.1(15)-6.8(11)-28.9(15)

 

Table 4 Bond Lengths for mo_B0167_0m.
AtomAtomLength/Å AtomAtomLength/Å
Fe1C12.057(2) N1C121.436(3)
Fe1C22.055(2) N1C131.450(4)
Fe1C32.034(2) C1C21.439(3)
Fe1C42.030(3) C1C51.427(3)
Fe1C52.030(2) C2C31.417(3)
Fe1C62.047(2) C2C111.492(3)
Fe1C72.048(2) C3C41.409(4)
Fe1C82.050(3) C4C51.419(3)
Fe1C92.041(2) C6C611.445(4)
Fe1C102.031(3) C6C71.422(3)
Si1O11.634(2) C6C101.424(3)
Si1O21.626(2) C7C81.412(3)
Si1C11.841(2) C8C91.419(3)
Si1C141.875(2) C9C101.418(3)
O1C181.412(3) C14C151.517(3)
O2C191.421(3) C14C161.541(4)
N1C111.466(3) C14C171.521(3)

11-X,1-Y,1-Z

 

Table 5 Bond Angles for mo_B0167_0m.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C2Fe1C140.96(8) C18O1Si1127.68(16)
C3Fe1C168.69(8) C19O2Si1127.22(19)
C3Fe1C240.53(8) C12N1C11112.1(2)
C3Fe1C6117.51(11) C12N1C13110.0(2)
C3Fe1C7108.08(9) C13N1C11109.1(2)
C3Fe1C8128.43(9) Si1C1Fe1128.09(10)
C3Fe1C9166.73(9) C2C1Fe169.47(10)
C4Fe1C169.02(8) C2C1Si1130.93(15)
C4Fe1C268.51(10) C5C1Fe168.55(12)
C4Fe1C340.57(11) C5C1Si1122.37(16)
C4Fe1C6150.69(9) C5C1C2106.68(18)
C4Fe1C7117.54(9) C1C2Fe169.57(11)
C4Fe1C8108.04(10) C1C2C11127.19(18)
C4Fe1C9128.77(11) C3C2Fe168.92(13)
C4Fe1C10167.18(10) C3C2C1107.84(19)
C5Fe1C140.86(8) C3C2C11124.96(19)
C5Fe1C268.48(10) C11C2Fe1125.97(14)
C5Fe1C368.34(11) C2C3Fe170.54(12)
C5Fe1C440.92(10) C4C3Fe169.55(14)
C5Fe1C6167.01(8) C4C3C2108.95(19)
C5Fe1C7151.29(8) C3C4Fe169.87(12)
C5Fe1C8118.25(10) C3C4C5107.6(2)
C5Fe1C9108.55(11) C5C4Fe169.53(12)
C5Fe1C10128.75(9) C1C5Fe170.59(12)
C6Fe1C1128.31(8) C4C5Fe169.55(14)
C6Fe1C2107.77(9) C4C5C1108.9(2)
C6Fe1C740.63(7) C61C6Fe1126.08(17)
C6Fe1C868.32(9) C7C6Fe169.73(12)
C7Fe1C1166.69(8) C7C6C61126.1(2)
C7Fe1C2128.38(9) C7C6C10107.41(17)
C7Fe1C840.30(9) C10C6Fe168.96(11)
C8Fe1C1151.62(9) C10C6C61126.5(2)
C8Fe1C2166.29(8) C6C7Fe169.63(12)
C9Fe1C1118.04(9) C8C7Fe169.92(12)
C9Fe1C2151.70(8) C8C7C6108.56(17)
C9Fe1C668.46(10) C7C8Fe169.78(11)
C9Fe1C768.04(9) C7C8C9107.86(18)
C9Fe1C840.58(8) C9C8Fe169.36(13)
C10Fe1C1107.76(8) C8C9Fe170.07(13)
C10Fe1C2117.78(8) C10C9Fe169.24(13)
C10Fe1C3151.10(10) C10C9C8108.16(19)
C10Fe1C640.87(8) C6C10Fe170.17(10)
C10Fe1C768.42(8) C9C10Fe169.99(12)
C10Fe1C868.52(8) C9C10C6108.00(17)
C10Fe1C940.77(8) N1C11C2112.70(18)
O1Si1C1110.75(10) C15C14Si1110.79(16)
O1Si1C14103.32(9) C15C14C16108.1(2)
O2Si1O1110.90(10) C15C14C17111.3(2)
O2Si1C1105.80(10) C16C14Si1108.18(16)
O2Si1C14115.34(11) C17C14Si1111.02(17)
C1Si1C14110.81(11) C17C14C16107.3(2)

11-X,1-Y,1-Z

 

Table 6 Torsion Angles for mo_B0167_0m.
ABCDAngle/˚ ABCDAngle/˚
Fe1C1C2C3-58.46(14) C1C2C3Fe158.87(13)
Fe1C1C2C11120.27(19) C1C2C3C4-0.3(2)
Fe1C1C5C459.18(15) C1C2C11N190.2(2)
Fe1C2C3C4-59.13(15) C2C1C5Fe1-59.26(13)
Fe1C2C11N1-179.31(14) C2C1C5C4-0.1(2)
Fe1C3C4C5-59.53(16) C2C3C4Fe159.74(14)
Fe1C4C5C1-59.82(15) C2C3C4C50.2(2)
Fe1C6C7C859.27(13) C3C2C11N1-91.3(2)
Fe1C6C10C9-60.02(14) C3C4C5Fe159.74(15)
Fe1C7C8C959.11(15) C3C4C5C1-0.1(2)
Fe1C8C9C1058.95(14) C5C1C2Fe158.68(14)
Fe1C9C10C660.13(13) C5C1C2C30.2(2)
Si1C1C2Fe1-123.17(17) C5C1C2C11178.95(18)
Si1C1C2C3178.36(14) C61C6C7Fe1120.5(2)
Si1C1C2C11-2.9(3) C61C6C7C8179.8(2)
Si1C1C5Fe1122.39(14) C61C6C10Fe1-120.0(2)
Si1C1C5C4-178.42(14) C61C6C10C9180.0(2)
O1Si1O2C1954.0(2) C6C7C8Fe1-59.10(13)
O1Si1C1Fe159.25(15) C6C7C8C90.0(2)
O1Si1C1C2154.41(17) C7C6C10Fe159.36(13)
O1Si1C1C5-27.70(18) C7C6C10C9-0.7(2)
O1Si1C14C15175.54(19) C7C8C9Fe1-59.37(14)
O1Si1C14C1657.25(17) C7C8C9C10-0.4(2)
O1Si1C14C17-60.2(2) C8C9C10Fe1-59.47(15)
O2Si1O1C1827.1(2) C8C9C10C60.7(2)
O2Si1C1Fe1-61.00(15) C10C6C7Fe1-58.88(12)
O2Si1C1C234.16(19) C10C6C7C80.4(2)
O2Si1C1C5-147.94(16) C11C2C3Fe1-119.90(18)
O2Si1C14C15-63.3(2) C11C2C3C4-179.04(18)
O2Si1C14C16178.43(14) C12N1C11C270.2(2)
O2Si1C14C1761.0(2) C13N1C11C2-167.79(19)
C1Si1O1C18-90.0(2) C14Si1O1C18151.3(2)
C1Si1O2C19174.2(2) C14Si1O2C19-63.0(2)
C1Si1C14C1556.9(2) C14Si1C1Fe1173.31(12)
C1Si1C14C16-61.41(18) C14Si1C1C2-91.54(19)
C1Si1C14C17-178.86(18) C14Si1C1C586.36(19)

11-X,1-Y,1-Z

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for mo_B0167_0m.
AtomxyzU(eq)
H31124907582744
H4-17287601528751
H5-4639030616240
H725575667384028
H812228436357236
H930199267461735
H1054417002554927
H11A33193424676038
H11B41764282732038
H12A-1803690765379
H12B4482423861379
H12C13292136758979
H13A43841492824192
H13B34181770925292
H13C48312618875292
H15A6085906888185
H15B4756338990785
H15C24545492949585
H16A-3569812832376
H16B-11658900923776
H16C-11548562819076
H17A36767456966879
H17B171984051004379
H17C26989126911179
H18A335010378594269
H18B49568882638569
H18C453810290684369
H19A74446374771788
H19B66715746875088
H19C60537484831388

Experimental

Single crystals of C38H60Fe2N2O4Si2 [mo_B0167_0m] were []. A suitable crystal was selected and [] on a 'Bruker APEX-II CCD' diffractometer. The crystal was kept at 100.01 K during data collection. Using Olex2 [1], the structure was solved with the XT [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. (2015). Acta Cryst. A71, 3-8.
  3. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Crystal structure determination of [mo_B0167_0m]

Crystal Data for C38H60Fe2N2O4Si2 (=776.76 g/mol): triclinic, space group P-1 (no. 2), a = 7.622(8) Å, b = 9.880(8) Å, c = 14.226(12) Å, α = 76.29(3)°, β = 85.20(3)°, γ = 70.52(3)°, = 981.2(15) Å3, Z = 1, T = 100.01 K, μ(MoKα) = 0.840 mm-1, Dcalc = 1.315 g/cm3, 23027 reflections measured (4.788° ≤ 2Θ ≤ 57.612°), 5104 unique (Rint = 0.0371, Rsigma = 0.0295) which were used in all calculations. The final R1 was 0.0373 (I > 2σ(I)) and wR2 was 0.0913 (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), C7(H7), C8(H8), C9(H9), C10(H10)
2.c Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C)

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