mo_B0093_0m

Table 1 Crystal data and structure refinement for mo_B0093_0m.
Identification code mo_B0093_0m
Empirical formula C21H27FeNO2Si
Formula weight 409.37
Temperature/K 100.01
Crystal system orthorhombic
Space group P212121
a/Å 7.6971(9)
b/Å 10.4780(9)
c/Å 24.508(3)
α/° 90
β/° 90
γ/° 90
Volume/Å3 1976.6(4)
Z 4
ρcalcg/cm3 1.376
μ/mm‑1 0.838
F(000) 864.0
Crystal size/mm3 0.3 × 0.2 × 0.02
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 5.548 to 57.99
Index ranges -10 ≤ h ≤ 8, -10 ≤ k ≤ 14, -27 ≤ l ≤ 33
Reflections collected 15827
Independent reflections 5236 [Rint = 0.0171, Rsigma = 0.0185]
Data/restraints/parameters 5236/0/239
Goodness-of-fit on F2 1.105
Final R indexes [I>=2σ (I)] R1 = 0.0201, wR2 = 0.0523
Final R indexes [all data] R1 = 0.0207, wR2 = 0.0525
Largest diff. peak/hole / e Å-3 0.29/-0.44
Flack parameter-0.001(3)

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for mo_B0093_0m. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Fe12658.6(3)4014.3(2)7365.3(2)9.42(6)
Si15195.2(6)4475.7(4)6174.9(2)10.84(9)
O16299.4(17)3573.1(13)5755.3(5)16.9(3)
O26412.1(16)5617.0(13)6428.4(5)15.8(2)
N12989.3(19)1177.2(13)6021.8(6)12.4(3)
C14508(2)3577.9(15)6785.7(6)9.8(3)
C23242(2)2564.9(15)6836.5(7)10.1(3)
C33267(2)2117.7(15)7388.1(7)12.1(3)
C44520(2)2836.6(15)7684.0(7)12.4(3)
C55287(2)3732.2(15)7318.8(7)11.0(3)
C61518(3)5731.2(18)7186.5(8)21.9(4)
C7278(3)4729(2)7158.6(10)30.6(5)
C8207(2)4133.7(18)7678.7(10)29.2(5)
C91394(3)4766.1(17)8024.9(8)20.8(4)
C102201(2)5752.4(15)7722.5(7)16.2(3)
C112084(2)2054.2(15)6395.3(7)12.1(3)
C123615(2)51.8(17)6309.4(7)16.1(3)
C131802(3)797.1(18)5583.8(7)18.7(4)
C147627(3)2738(2)5937.6(8)32.0(5)
C157554(3)6364(2)6102.4(8)26.2(4)
C163471(2)5162.3(17)5731.9(7)13.3(3)
C172949(2)6434.9(17)5788.3(7)16.6(3)
C181663(3)6955.5(19)5456.9(8)19.6(4)
C19867(2)6208.3(19)5061.7(8)20.9(4)
C201360(3)4938(2)4995.8(8)21.0(4)
C212667(2)4430.7(17)5324.3(6)17.1(3)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for mo_B0093_0m. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Fe18.37(10)8.79(10)11.11(10)-1.31(8)1.27(8)0.92(8)
Si19.6(2)14.07(19)8.80(18)0.91(16)0.66(15)-0.61(16)
O114.6(6)23.7(6)12.5(6)-1.5(5)1.9(5)3.5(5)
O215.3(6)18.8(6)13.3(5)1.2(5)1.0(5)-6.9(5)
N114.2(7)12.6(6)10.4(6)-2.2(5)-0.4(5)0.1(5)
C18.8(7)11.3(6)9.3(7)-0.8(5)0.5(5)0.8(6)
C29.9(7)9.2(6)11.2(7)-1.9(5)1.1(5)1.3(5)
C313.7(7)10.1(6)12.5(7)0.6(6)2.8(6)2.2(5)
C413.8(7)12.7(6)10.8(7)1.1(6)-0.1(6)3.6(6)
C59.0(6)13.0(6)10.9(7)-1.1(5)-0.1(6)1.8(5)
C626.7(10)18.7(9)20.5(8)0.4(7)3.6(7)13.6(7)
C716.4(9)32.6(11)42.9(12)-21.9(9)-11.4(8)15.4(8)
C812.9(8)16.3(8)58.4(14)-9.9(9)16.8(9)-1.3(7)
C925.1(10)16.9(8)20.5(8)-0.1(7)12.3(7)7.5(7)
C1014.8(7)11.9(7)22.0(8)-5.6(6)4.0(6)1.7(6)
C1110.9(7)11.8(7)13.7(7)-1.1(6)-0.2(6)0.1(6)
C1219.5(8)13.1(8)15.7(8)-1.5(6)1.1(6)2.3(7)
C1322.2(9)19.4(8)14.3(7)-3.7(6)-4.2(6)-1.1(7)
C1428.9(11)42.2(12)24.8(9)-11.3(9)-6.1(9)19.5(10)
C1524.6(10)29.8(9)24.2(9)5.2(7)3.5(8)-14.2(9)
C1611.9(7)17.7(8)10.4(7)3.4(6)0.6(6)-1.2(6)
C1716.6(9)15.2(7)17.8(8)3.0(6)-0.5(6)-3.7(6)
C1817.9(9)17.8(8)23.2(9)7.3(7)1.1(7)1.3(7)
C1916.6(8)28.3(10)17.9(8)7.0(7)-1.6(7)4.4(7)
C2020.3(9)29.0(9)13.7(7)-1.7(7)-5.0(7)1.7(7)
C2118.5(8)19.3(7)13.5(7)-0.6(6)-1.3(7)1.5(7)

 

Table 4 Bond Lengths for mo_B0093_0m.
AtomAtomLength/Å AtomAtomLength/Å
Fe1C12.0624(16) N1C131.465(2)
Fe1C22.0465(16) C1C21.447(2)
Fe1C32.0424(16) C1C51.447(2)
Fe1C42.0458(16) C2C31.431(2)
Fe1C52.0482(16) C2C111.500(2)
Fe1C62.0492(18) C3C41.422(2)
Fe1C72.044(2) C4C51.425(2)
Fe1C82.0413(18) C6C71.420(3)
Fe1C92.0447(18) C6C101.415(3)
Fe1C102.0511(15) C7C81.420(4)
Si1O11.6352(13) C8C91.412(3)
Si1O21.6412(13) C9C101.415(3)
Si1C11.8454(17) C16C171.400(2)
Si1C161.8593(18) C16C211.403(2)
O1C141.418(2) C17C181.392(3)
O2C151.423(2) C18C191.388(3)
N1C111.472(2) C19C201.393(3)
N1C121.456(2) C20C211.394(3)

 

Table 5 Bond Angles for mo_B0093_0m.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C2Fe1C141.22(6) C14O1Si1122.24(12)
C2Fe1C568.96(6) C15O2Si1122.76(12)
C2Fe1C6127.59(7) C12N1C11111.16(13)
C2Fe1C10165.22(7) C12N1C13109.93(14)
C3Fe1C169.20(6) C13N1C11109.26(13)
C3Fe1C240.97(6) Si1C1Fe1130.06(9)
C3Fe1C440.72(6) C2C1Fe168.80(9)
C3Fe1C568.57(6) C2C1Si1129.56(12)
C3Fe1C6163.38(8) C2C1C5106.49(14)
C3Fe1C7124.69(8) C5C1Fe168.87(9)
C3Fe1C9117.54(7) C5C1Si1123.83(12)
C3Fe1C10153.08(7) C1C2Fe169.98(9)
C4Fe1C169.26(6) C1C2C11126.89(15)
C4Fe1C268.93(7) C3C2Fe169.36(9)
C4Fe1C540.74(6) C3C2C1108.20(14)
C4Fe1C6155.68(8) C3C2C11124.91(15)
C4Fe1C10119.54(7) C11C2Fe1126.23(11)
C5Fe1C141.21(6) C2C3Fe169.67(9)
C5Fe1C6122.56(8) C4C3Fe169.77(9)
C5Fe1C10108.77(7) C4C3C2108.52(14)
C6Fe1C1110.07(7) C3C4Fe169.51(9)
C6Fe1C1040.37(7) C3C4C5108.03(14)
C7Fe1C1121.97(8) C5C4Fe169.72(9)
C7Fe1C2108.17(7) C1C5Fe169.92(9)
C7Fe1C4160.69(9) C4C5Fe169.54(9)
C7Fe1C5157.68(9) C4C5C1108.76(14)
C7Fe1C640.61(9) C7C6Fe169.49(11)
C7Fe1C968.15(9) C10C6Fe169.89(10)
C7Fe1C1068.04(7) C10C6C7107.82(18)
C8Fe1C1155.62(8) C6C7Fe169.90(11)
C8Fe1C2119.11(8) C8C7Fe169.56(11)
C8Fe1C3105.15(7) C8C7C6107.90(18)
C8Fe1C4122.73(8) C7C8Fe169.75(12)
C8Fe1C5160.59(9) C9C8Fe169.91(10)
C8Fe1C668.31(8) C9C8C7107.95(17)
C8Fe1C740.69(10) C8C9Fe169.65(11)
C8Fe1C940.44(9) C8C9C10108.17(17)
C8Fe1C1068.04(7) C10C9Fe170.03(10)
C9Fe1C1163.43(8) C6C10Fe169.74(10)
C9Fe1C2153.00(7) C6C10C9108.17(17)
C9Fe1C4105.30(8) C9C10Fe169.54(10)
C9Fe1C5124.74(8) N1C11C2112.92(13)
C9Fe1C668.09(8) C17C16Si1121.06(13)
C9Fe1C1040.43(7) C17C16C21117.65(16)
C10Fe1C1127.55(7) C21C16Si1121.29(13)
O1Si1O2111.28(7) C18C17C16121.34(17)
O1Si1C1111.36(7) C19C18C17119.99(18)
O1Si1C16103.15(7) C18C19C20119.99(17)
O2Si1C1103.17(7) C19C20C21119.61(18)
O2Si1C16110.27(8) C20C21C16121.41(17)
C1Si1C16117.80(8)     

 

Table 6 Torsion Angles for mo_B0093_0m.
ABCDAngle/˚ ABCDAngle/˚
Fe1C1C2C3-59.02(11) C1C2C11N178.4(2)
Fe1C1C2C11120.86(16) C2C1C5Fe1-58.75(11)
Fe1C1C5C458.85(11) C2C1C5C40.10(18)
Fe1C2C3C4-59.13(11) C2C3C4Fe159.07(11)
Fe1C2C11N1169.49(11) C2C3C4C5-0.21(17)
Fe1C3C4C5-59.28(11) C3C2C11N1-101.74(18)
Fe1C4C5C1-59.09(11) C3C4C5Fe159.15(11)
Fe1C6C7C859.41(13) C3C4C5C10.06(18)
Fe1C6C10C9-59.12(12) C5C1C2Fe158.79(11)
Fe1C7C8C959.71(13) C5C1C2C3-0.23(18)
Fe1C8C9C1059.67(12) C5C1C2C11179.65(14)
Fe1C9C10C659.25(12) C6C7C8Fe1-59.62(13)
Si1C1C2Fe1-125.09(14) C6C7C8C90.1(2)
Si1C1C2C3175.88(12) C7C6C10Fe159.36(13)
Si1C1C2C11-4.2(3) C7C6C10C90.2(2)
Si1C1C5Fe1124.86(12) C7C8C9Fe1-59.61(13)
Si1C1C5C4-176.29(11) C7C8C9C100.1(2)
Si1C16C17C18179.82(14) C8C9C10Fe1-59.43(12)
Si1C16C21C20179.25(15) C8C9C10C6-0.2(2)
O1Si1O2C1545.22(17) C10C6C7Fe1-59.61(12)
O1Si1C1Fe1-164.13(10) C10C6C7C8-0.2(2)
O1Si1C1C2-69.44(16) C11C2C3Fe1-120.48(15)
O1Si1C1C5106.07(14) C11C2C3C4-179.61(14)
O1Si1C16C17-140.64(14) C12N1C11C262.45(18)
O1Si1C16C2138.38(16) C13N1C11C2-176.05(14)
O2Si1O1C1469.61(18) C16Si1O1C14-172.18(16)
O2Si1C1Fe176.42(12) C16Si1O2C15-68.62(16)
O2Si1C1C2171.11(15) C16Si1C1Fe1-45.29(14)
O2Si1C1C5-13.38(15) C16Si1C1C249.40(18)
O2Si1C16C17-21.73(16) C16Si1C1C5-135.09(13)
O2Si1C16C21157.30(13) C16C17C18C190.1(3)
C1Si1O1C14-44.90(18) C17C16C21C20-1.7(3)
C1Si1O2C15164.73(15) C17C18C19C20-0.1(3)
C1Si1C16C1796.26(15) C18C19C20C21-0.8(3)
C1Si1C16C21-84.72(16) C19C20C21C161.7(3)
C1C2C3Fe159.41(11) C21C16C17C180.8(3)
C1C2C3C40.27(18)      

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for mo_B0093_0m.
AtomxyzU(eq)
H325651453753215
H447962737805915
H561664332741013
H618336288689726
H7-3874499684737
H8-5123433777635
H916144564839625
H1030536329785619
H11A10941600656515
H11B16092778618315
H12A2629-399647424
H12B4428312659624
H12C4209-515605224
H13A2407226533128
H13B14061558538728
H13C798354574128
H14A85302672565748
H14B71331891600748
H14C81373073627548
H15A68946772580839
H15B84545814594539
H15C80997022632939
H1734846954605820
H1813297822550124
H19-136563483625
H208084421472925
H2130203571527121

Experimental

Single crystals of C21H27FeNO2Si [mo_B0093_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_B0093_0m]

Crystal Data for C21H27FeNO2Si (=409.37 g/mol): orthorhombic, space group P212121 (no. 19), a = 7.6971(9) Å, b = 10.4780(9) Å, c = 24.508(3) Å, = 1976.6(4) Å3, Z = 4, T = 100.01 K, μ(MoKα) = 0.838 mm-1, Dcalc = 1.376 g/cm3, 15827 reflections measured (5.548° ≤ 2Θ ≤ 57.99°), 5236 unique (Rint = 0.0171, Rsigma = 0.0185) which were used in all calculations. The final R1 was 0.0201 (I > 2σ(I)) and wR2 was 0.0525 (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), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C17(H17),
C18(H18), C19(H19), C20(H20), C21(H21)
2.c Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,
H15C)

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