mo_b0003_0m_a

Table 1 Crystal data and structure refinement for mo_b0003_0m_a.
Identification code mo_b0003_0m_a
Empirical formula C26H33FeNO2Si2
Formula weight 503.56
Temperature/K 100.0
Crystal system monoclinic
Space group P21/n
a/Å 14.5175(5)
b/Å 13.6757(5)
c/Å 14.6276(6)
α/° 90
β/° 116.7530(10)
γ/° 90
Volume/Å3 2593.25(17)
Z 4
ρcalcg/cm3 1.290
μ/mm‑1 0.696
F(000) 1064.0
Crystal size/mm3 0.1 × 0.083 × 0.071
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.312 to 54.368
Index ranges -18 ≤ h ≤ 18, -17 ≤ k ≤ 17, -18 ≤ l ≤ 18
Reflections collected 108395
Independent reflections 5760 [Rint = 0.0313, Rsigma = 0.0115]
Data/restraints/parameters 5760/0/302
Goodness-of-fit on F2 1.114
Final R indexes [I>=2σ (I)] R1 = 0.0334, wR2 = 0.0943
Final R indexes [all data] R1 = 0.0379, wR2 = 0.1033
Largest diff. peak/hole / e Å-3 0.83/-0.80

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for mo_b0003_0m_a. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Fe11791.2(2)3807.7(2)5416.8(2)16.06(9)
Si13546.1(3)5341.6(3)5032.5(3)12.22(11)
Si21973.8(4)3827.2(4)7892.9(4)27.61(14)
O13748.5(10)4375.5(9)4496.2(10)17.1(3)
O24634.4(9)5756.8(9)5940.3(9)15.4(2)
N14877.0(11)4831.0(11)7624.3(11)18.7(3)
C12714.8(12)5009.1(12)5642.9(12)13.0(3)
C23021.5(12)4459.8(12)6580.3(13)14.3(3)
C32166.2(13)4409.7(13)6833.3(13)15.5(3)
C41333.9(13)4937.8(13)6034.8(13)15.6(3)
C51666.1(13)5301.8(13)5324.5(13)15.0(3)
C61850.8(16)3000.5(14)4258.8(16)25.1(4)
C72255.1(16)2456.9(14)5176.2(17)26.5(4)
C81461(2)2368.5(16)5494(2)42.6(6)
C9581.3(19)2863(2)4776(2)51.1(8)
C10815.3(17)3256.5(19)4008(2)41.1(6)
C114091.7(13)4045.6(13)7170.8(14)18.1(3)
C125918.7(14)4400.7(16)8089.6(17)30.6(5)
C134707.1(17)5401.8(17)8381.3(16)31.2(5)
C142896(2)2824(3)8539(4)100.8(19)
C152096(3)4817(3)8835(2)69.6(11)
C16637.4(16)3335.0(17)7355.4(17)29.8(4)
C172955.7(13)6369.8(13)4106.0(12)14.1(3)
C183298.1(13)7307.1(13)4439.6(13)17.1(3)
C192900.4(14)8131.3(14)3797.5(14)21.1(4)
C202176.9(14)8017.2(14)2800.5(14)20.4(4)
C211796.7(13)7073.2(13)2414.2(13)17.2(3)
C221040.1(14)6943.1(15)1381.7(14)22.5(4)
C23625.4(16)6038.0(16)1036.6(14)26.6(4)
C24944.9(15)5225.3(15)1700.0(15)24.4(4)
C251700.9(14)5323.4(13)2687.4(14)19.6(4)
C262161.3(13)6246.6(12)3074.8(13)15.0(3)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for mo_b0003_0m_a. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Fe111.39(14)15.29(14)21.93(15)-4.69(9)7.88(11)-2.96(8)
Si19.7(2)15.3(2)10.5(2)-0.66(16)3.55(17)-0.50(16)
Si217.6(3)38.7(3)25.6(3)15.3(2)8.8(2)-2.0(2)
O113.2(6)20.1(6)18.5(6)-4.0(5)7.6(5)-0.2(5)
O212.3(5)20.8(6)11.5(6)0.1(5)4.0(5)-2.3(5)
N111.6(7)22.5(7)17.3(7)5.2(6)2.4(6)-0.8(6)
C111.0(7)13.5(7)13.4(7)-1.9(6)4.5(6)-1.0(6)
C211.7(7)13.6(7)16.5(8)0.5(6)5.4(6)-1.2(6)
C312.2(7)16.6(8)17.6(8)1.2(6)6.6(6)-0.3(6)
C412.7(8)17.3(8)17.6(8)-0.5(6)7.5(6)0.8(6)
C512.9(8)16.1(8)14.6(8)-0.1(6)5.0(6)1.7(6)
C627.3(10)20.7(9)28.2(10)-12.2(8)13.2(8)-6.8(8)
C731(1)14.9(8)39.5(11)-6.7(8)21.1(9)-2.8(8)
C866.3(17)19.6(10)68.6(17)-17.0(11)54.1(15)-20.4(11)
C927.6(12)47.8(15)88(2)-46.8(15)35.5(14)-26.2(11)
C1023.5(10)40.4(13)42.4(13)-27.7(11)-0.3(9)-1.5(9)
C1112.6(8)16.3(8)22.8(9)5.8(7)5.7(7)0.9(6)
C1212.4(8)32.5(11)36.7(11)14.4(9)2.2(8)0.9(8)
C1328(1)39.5(12)22.1(9)-6.2(9)7.6(8)-6.7(9)
C1441.5(16)131(3)147(4)123(3)58(2)45(2)
C1584(2)106(3)31.9(13)-25.3(16)37.9(15)-61(2)
C1624.9(10)37.2(11)35.9(11)-1.8(9)21.3(9)-5.8(9)
C1712.2(7)19.4(8)11.6(7)0.4(6)6.1(6)-0.2(6)
C1816.0(8)20.6(9)13.1(7)0.1(6)5.3(6)-2.4(6)
C1923.3(9)18.0(8)21.3(9)0.9(7)9.3(7)-3.9(7)
C2020.2(8)21.4(9)18.9(8)6.3(7)8.2(7)1.4(7)
C2115.1(8)23.4(9)14.1(8)2.3(7)7.6(7)2.7(7)
C2221.6(9)28.6(10)14.9(8)4.1(7)6.2(7)6.3(7)
C2322.4(9)34.1(11)14.1(8)-3.3(7)0.1(7)7.3(8)
C2420.4(9)23.9(9)21.1(9)-7.8(7)2.6(7)3.2(7)
C2517.3(8)19.9(9)17.3(8)-2.1(7)4.1(7)3.7(7)
C2612.0(7)20.2(8)12.8(7)-0.6(6)5.7(6)1.7(6)

 

Table 4 Bond Lengths for mo_b0003_0m_a.
AtomAtomLength/Å AtomAtomLength/Å
Fe1C12.0511(16) C1C51.434(2)
Fe1C22.0360(17) C2C31.448(2)
Fe1C32.0620(18) C2C111.507(2)
Fe1C42.0461(17) C3C41.441(2)
Fe1C52.0504(18) C4C51.418(2)
Fe1C62.0560(19) C6C71.410(3)
Fe1C72.0502(19) C6C101.421(3)
Fe1C82.041(2) C7C81.428(3)
Fe1C92.037(2) C8C91.409(4)
Fe1C102.048(2) C9C101.419(4)
Si1O11.6294(13) C17C181.382(2)
Si1O21.6411(12) C17C261.438(2)
Si1C11.8523(17) C18C191.413(3)
Si1C171.8715(18) C19C201.369(3)
Si2C31.8721(18) C20C211.418(3)
Si2C141.852(3) C21C221.423(2)
Si2C151.883(3) C21C261.425(2)
Si2C161.861(2) C22C231.370(3)
N1C111.488(2) C23C241.410(3)
N1C121.473(2) C24C251.372(2)
N1C131.464(3) C25C261.422(2)
C1C21.447(2)    

 

Table 5 Bond Angles for mo_b0003_0m_a.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C1Fe1C370.15(6) C13N1C11111.48(15)
C1Fe1C6107.22(7) C13N1C12110.55(16)
C2Fe1C141.46(6) Si1C1Fe1129.75(9)
C2Fe1C341.38(6) C2C1Fe168.71(9)
C2Fe1C468.71(7) C2C1Si1126.51(12)
C2Fe1C568.71(7) C5C1Fe169.51(9)
C2Fe1C6125.27(7) C5C1Si1127.00(13)
C2Fe1C7107.80(8) C5C1C2106.35(14)
C2Fe1C8121.04(10) C1C2Fe169.83(9)
C2Fe1C9155.86(11) C1C2C3109.47(14)
C2Fe1C10162.10(9) C1C2C11122.43(15)
C4Fe1C169.04(7) C3C2Fe170.27(9)
C4Fe1C341.05(7) C3C2C11128.09(15)
C4Fe1C540.51(7) C11C2Fe1127.19(12)
C4Fe1C6155.77(8) Si2C3Fe1126.28(9)
C4Fe1C7162.44(8) C2C3Fe168.35(9)
C4Fe1C10120.51(8) C2C3Si2134.13(13)
C5Fe1C140.93(6) C4C3Fe168.88(10)
C5Fe1C369.13(7) C4C3Si2120.09(12)
C5Fe1C6121.07(8) C4C3C2105.77(14)
C6Fe1C3162.22(8) C3C4Fe170.06(10)
C7Fe1C1120.53(7) C5C4Fe169.91(10)
C7Fe1C3125.01(8) C5C4C3109.41(14)
C7Fe1C5155.90(7) C1C5Fe169.56(9)
C7Fe1C640.17(8) C4C5Fe169.59(10)
C8Fe1C1156.39(10) C4C5C1109.00(15)
C8Fe1C3106.98(9) C7C6Fe169.69(11)
C8Fe1C4124.98(8) C7C6C10108.3(2)
C8Fe1C5161.57(9) C10C6Fe169.44(12)
C8Fe1C668.01(9) C6C7Fe170.14(11)
C8Fe1C740.87(9) C6C7C8107.6(2)
C8Fe1C1068.12(12) C8C7Fe169.21(12)
C9Fe1C1161.39(11) C7C8Fe169.92(11)
C9Fe1C3119.89(10) C9C8Fe169.64(14)
C9Fe1C4107.34(8) C9C8C7108.1(2)
C9Fe1C5124.68(10) C8C9Fe169.94(13)
C9Fe1C668.16(9) C8C9C10108.2(2)
C9Fe1C768.39(9) C10C9Fe170.11(12)
C9Fe1C840.42(13) C6C10Fe170.04(11)
C9Fe1C1040.64(12) C9C10Fe169.25(13)
C10Fe1C1124.25(10) C9C10C6107.7(2)
C10Fe1C3155.28(9) N1C11C2111.69(14)
C10Fe1C5107.45(9) C18C17Si1117.80(12)
C10Fe1C640.52(9) C18C17C26118.05(15)
C10Fe1C768.13(9) C26C17Si1124.14(13)
O1Si1O2110.71(7) C17C18C19122.04(16)
O1Si1C1109.32(7) C20C19C18120.33(17)
O1Si1C17112.56(7) C19C20C21120.16(17)
O2Si1C1107.08(7) C20C21C22120.85(17)
O2Si1C17106.64(7) C20C21C26119.53(15)
C1Si1C17110.37(7) C22C21C26119.60(17)
C3Si2C15107.48(11) C23C22C21120.35(17)
C14Si2C3113.25(12) C22C23C24120.33(17)
C14Si2C15110.5(2) C25C24C23120.48(18)
C14Si2C16108.93(15) C24C25C26121.09(17)
C16Si2C3108.66(9) C21C26C17119.74(16)
C16Si2C15107.81(13) C25C26C17122.24(16)
C12N1C11109.81(15) C25C26C21118.01(16)

 

Table 6 Hydrogen Bonds for mo_b0003_0m_a.
DHAd(D-H)/Åd(H-A)/Åd(D-A)/ÅD-H-A/°
O1H1O210.76(3)1.95(3)2.7021(18)179(3)
O2H2N10.80(3)1.86(3)2.648(2)171(3)

11-X,1-Y,1-Z

 

Table 7 Torsion Angles for mo_b0003_0m_a.
ABCDAngle/˚ ABCDAngle/˚
Fe1C1C2C3-59.25(12) C5C1C2C30.35(19)
Fe1C1C2C11121.97(16) C5C1C2C11-178.42(15)
Fe1C1C5C458.54(12) C6C7C8Fe1-59.86(14)
Fe1C2C3Si2120.12(17) C6C7C8C9-0.5(2)
Fe1C2C3C4-59.00(12) C7C6C10Fe159.02(14)
Fe1C2C11N1155.49(12) C7C6C10C9-0.2(2)
Fe1C3C4C5-58.99(12) C7C8C9Fe1-59.56(14)
Fe1C4C5C1-58.52(12) C7C8C9C100.4(2)
Fe1C6C7C859.28(14) C8C9C10Fe1-59.81(15)
Fe1C6C10C9-59.21(15) C8C9C10C6-0.1(2)
Fe1C7C8C959.39(15) C10C6C7Fe1-58.86(14)
Fe1C8C9C1059.91(15) C10C6C7C80.4(2)
Fe1C9C10C659.71(14) C11C2C3Fe1-122.33(18)
Si1C1C2Fe1-124.43(13) C11C2C3Si2-2.2(3)
Si1C1C2C3176.32(12) C11C2C3C4178.67(16)
Si1C1C2C11-2.5(2) C12N1C11C2-173.45(16)
Si1C1C5Fe1124.97(13) C13N1C11C263.7(2)
Si1C1C5C4-176.50(12) C14Si2C3Fe173.3(2)
Si1C17C18C19179.97(14) C14Si2C3C2-21.0(3)
Si1C17C26C21-177.07(12) C14Si2C3C4158.0(2)
Si1C17C26C254.4(2) C15Si2C3Fe1-164.34(15)
Si2C3C4Fe1-120.62(12) C15Si2C3C2101.4(2)
Si2C3C4C5-179.61(12) C15Si2C3C4-79.58(19)
O1Si1C1Fe1-17.43(13) C16Si2C3Fe1-47.92(14)
O1Si1C1C274.18(16) C16Si2C3C2-142.19(18)
O1Si1C1C5-110.67(15) C16Si2C3C436.84(17)
O1Si1C17C18-140.36(13) C17Si1C1Fe1106.89(11)
O1Si1C17C2640.39(16) C17Si1C1C2-161.50(14)
O2Si1C1Fe1-137.42(10) C17Si1C1C513.65(17)
O2Si1C1C2-45.81(16) C17C18C19C20-2.2(3)
O2Si1C1C5129.34(15) C18C17C26C213.7(2)
O2Si1C17C18-18.77(15) C18C17C26C25-174.87(16)
O2Si1C17C26161.98(14) C18C19C20C212.0(3)
C1Si1C17C1897.20(14) C19C20C21C22179.60(17)
C1Si1C17C26-82.04(15) C19C20C21C260.9(3)
C1C2C3Fe158.98(12) C20C21C22C23-175.42(18)
C1C2C3Si2179.11(14) C20C21C26C17-3.8(2)
C1C2C3C4-0.02(19) C20C21C26C25174.79(16)
C1C2C11N167.3(2) C21C22C23C24-0.1(3)
C2C1C5Fe1-59.09(11) C22C21C26C17177.49(16)
C2C1C5C4-0.56(19) C22C21C26C25-3.9(2)
C2C3C4Fe158.66(11) C22C23C24C25-2.4(3)
C2C3C4C5-0.33(19) C23C24C25C261.6(3)
C3C2C11N1-111.28(19) C24C25C26C17-179.93(17)
C3C4C5Fe159.08(12) C24C25C26C211.5(3)
C3C4C5C10.6(2) C26C17C18C19-0.7(3)
C5C1C2Fe159.61(11) C26C21C22C233.2(3)

 

Table 8 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for mo_b0003_0m_a.
AtomxyzU(eq)
H14200(20)4350(20)4380(20)40(8)
H24760(30)5520(20)6480(30)53(9)
H46665028599119
H512605679473318
H622093167387430
H729332197552132
H815172034608651
H9-582924480361
H103613625342949
H11A41093618772422
H11B42643641670722
H12A59953968865346
H12B64344924835346
H12C60214024757246
H13A40185696805547
H13B52285919865547
H13C47624972894047
H14A288323568026151
H14B270024919019151
H14C359330948914151
H15A280950559169104
H15B191045539353104
H15C163253588474104
H16A1443877711845
H16B5502968788645
H16C5152901677945
H1838177400512220
H1931368767405925
H2019298572236724
H22821748793027
H23120595734732
H246344605146229
H2519204765311923

Experimental

Single crystals of C26H33FeNO2Si2 [mo_b0003_0m_a] were []. A suitable crystal was selected and [] on a Bruker D8 Venture diffractometer. The crystal was kept at 100.0 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 [mo_b0003_0m_a]

Crystal Data for C26H33FeNO2Si2 (=503.56 g/mol): monoclinic, space group P21/n (no. 14), a = 14.5175(5) Å, b = 13.6757(5) Å, c = 14.6276(6) Å, β = 116.7530(10)°, = 2593.25(17) Å3, Z = 4, T = 100.0 K, μ(MoKα) = 0.696 mm-1, Dcalc = 1.290 g/cm3, 108395 reflections measured (4.312° ≤ 2Θ ≤ 54.368°), 5760 unique (Rint = 0.0313, Rsigma = 0.0115) which were used in all calculations. The final R1 was 0.0334 (I > 2σ(I)) and wR2 was 0.1033 (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), C22(H22), C23(H23), C24(H24), C25(H25)
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)

This report has been created with Olex2, compiled on 2017.01.04 svn.r3372 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.