mo_B0673_0m

Table 1 Crystal data and structure refinement for mo_B0673_0m.
Identification code mo_B0673_0m
Empirical formula C29H35FeNO2Si2
Formula weight 541.61
Temperature/K 100.01
Crystal system triclinic
Space group P-1
a/Å 8.4627(9)
b/Å 12.9654(13)
c/Å 13.1700(10)
α/° 73.895(2)
β/° 73.944(3)
γ/° 84.816(3)
Volume/Å3 1334.0(2)
Z 2
ρcalcg/cm3 1.348
μ/mm‑1 0.682
F(000) 572.0
Crystal size/mm3 0.356 × 0.246 × 0.17
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 5.01 to 66.456
Index ranges -13 ≤ h ≤ 13, -19 ≤ k ≤ 19, -16 ≤ l ≤ 20
Reflections collected 36672
Independent reflections 10182 [Rint = 0.0326, Rsigma = 0.0368]
Data/restraints/parameters 10182/0/325
Goodness-of-fit on F2 1.032
Final R indexes [I>=2σ (I)] R1 = 0.0351, wR2 = 0.0781
Final R indexes [all data] R1 = 0.0487, wR2 = 0.0831
Largest diff. peak/hole / e Å-3 0.81/-0.40

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for mo_B0673_0m. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Fe13078.4(2)2618.6(2)3652.9(2)9.29(4)
Si16767.6(4)1873.1(3)2128.9(3)10.73(6)
Si26904.6(4)3304.8(2)3597.8(3)9.79(6)
O17471.4(10)2369.7(7)2937.4(7)12.17(15)
O27148.8(12)2702.0(8)911.7(7)17.55(18)
N14454.3(14)2737.0(9)196.2(8)16.2(2)
C14502.1(14)1702.0(9)2688.5(9)11.05(19)
C23194.1(15)2249.9(9)2220.4(10)13.0(2)
C31657.5(15)1928.9(10)2996(1)15.3(2)
C41961.8(16)1197.6(10)3950(1)15.7(2)
C53698.7(15)1050.6(9)3762(1)13.5(2)
C64648.0(14)3549.8(9)3948.8(9)11.7(2)
C73644.6(15)4194.6(9)3279(1)14.1(2)
C81954.8(16)4039.5(10)3860.5(11)16.6(2)
C91879.6(16)3298.7(11)4897.9(11)17.4(2)
C103520.4(15)3001.6(10)4953.6(10)14.9(2)
C113349.4(17)3071.1(11)1131.4(10)18.9(2)
C123840.1(19)1792.8(12)33.0(12)24.3(3)
C134628(2)3637.0(13)-791.6(11)27.0(3)
C147860.2(15)551.5(10)2055.6(10)14.4(2)
C156994.1(19)-26.0(12)1488.3(15)28.1(3)
C169647.9(17)755.5(12)1368.7(12)22.2(3)
C177867(2)-173.6(11)3194.1(12)27.6(3)
C187988.9(15)4569.4(9)2730.1(9)12.1(2)
C197618.7(17)5539.3(10)3024.5(10)16.8(2)
C208496.6(19)6465.5(11)2407.5(11)22.1(3)
C219758.8(19)6441.4(11)1475.5(11)22.8(3)
C2210130.5(17)5493.8(11)1158.8(11)20.7(3)
C239250.1(16)4569.1(10)1778.5(10)16.6(2)
C247427.7(14)2809.1(9)4944.7(9)11.8(2)
C257597.0(17)1710.4(10)5420.6(10)17.4(2)
C267823.3(19)1333.2(10)6472.5(11)21.4(3)
C277891.9(17)2052.8(10)7068.5(10)18.0(2)
C287731.0(16)3146(1)6612.4(10)16.6(2)
C297495.1(16)3516.7(10)5566.1(10)15.3(2)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for mo_B0673_0m. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Fe19.05(8)9.86(7)9.13(7)-3.20(5)-1.68(6)-1.00(5)
Si110.82(15)10.91(13)10.36(13)-3.42(11)-1.62(11)-1.44(11)
Si29.51(14)10.48(13)10.28(13)-4.19(10)-2.36(11)-0.95(11)
O111.0(4)13.8(4)14.2(4)-7.7(3)-3.6(3)0.7(3)
O216.5(4)20.5(4)12.4(4)1.1(3)-2.5(3)-5.9(3)
N117.8(5)20.8(5)10.1(4)-3.8(4)-3.5(4)-1.7(4)
C112.2(5)10.3(4)11.5(5)-4.4(4)-2.7(4)-0.8(4)
C214.8(5)14.0(5)11.6(5)-5.1(4)-4.3(4)0.7(4)
C311.8(5)18.4(5)18.8(5)-8.8(4)-5.2(4)-0.7(4)
C414.2(6)12.8(5)18.3(5)-3.6(4)-0.5(4)-5.0(4)
C514.3(5)10.5(5)14.0(5)-1.8(4)-1.9(4)-1.4(4)
C611.3(5)12.4(5)12.8(5)-6.2(4)-2.2(4)-1.0(4)
C714.3(5)10.4(5)18.7(5)-4.7(4)-5.1(4)-0.3(4)
C812.7(5)15.9(5)24.3(6)-10.7(5)-5.6(5)3.4(4)
C912.3(5)25.0(6)16.7(5)-11.9(5)0.0(4)-1.8(5)
C1014.0(5)20.7(6)11.2(5)-6.7(4)-2.3(4)-2.1(4)
C1123.6(7)20.2(6)12.1(5)-4.0(4)-5.8(5)5.8(5)
C1226.1(7)30.7(7)20.0(6)-12.5(5)-5.4(5)-4.6(6)
C1334.8(8)30.7(7)12.2(6)0.1(5)-6.1(6)-2.5(6)
C1413.3(5)14.5(5)16.7(5)-7.8(4)-2.3(4)-0.1(4)
C1523.2(7)26.3(7)45.6(9)-25.1(7)-11.6(7)2.3(6)
C1614.5(6)25.7(6)25.6(7)-11.0(5)-0.7(5)2.3(5)
C1733.7(8)17.6(6)23.6(7)-1.5(5)-1.6(6)8.8(6)
C1811.9(5)13.5(5)11.4(5)-2.4(4)-4.2(4)-1.7(4)
C1923.2(6)14.8(5)12.4(5)-4.1(4)-3.0(5)-3.4(5)
C2035.3(8)15.5(5)16.1(6)-4.0(4)-6.0(5)-7.3(5)
C2128.9(7)21.4(6)16.6(6)1.1(5)-6.0(5)-12.1(5)
C2217.8(6)25.2(6)15.1(5)-1.1(5)-0.4(5)-5.5(5)
C2314.7(6)18.5(5)15.4(5)-4.4(4)-1.8(4)-0.9(4)
C2410.1(5)13.6(5)12.1(5)-4.3(4)-2.6(4)-0.2(4)
C2524.0(6)13.0(5)17.1(5)-4.7(4)-7.3(5)-1.2(5)
C2630.6(7)14.2(5)19.6(6)-1.1(4)-10.1(5)-0.3(5)
C2722.1(6)19.0(6)12.8(5)-2.9(4)-5.8(5)0.4(5)
C2820.3(6)17.6(5)13.7(5)-7.1(4)-5.2(5)2.2(5)
C2918.5(6)13.5(5)14.8(5)-4.6(4)-5.6(5)1.6(4)

 

Table 4 Bond Lengths for mo_B0673_0m.
AtomAtomLength/Å AtomAtomLength/Å
Fe1C12.0517(11) C2C111.5104(17)
Fe1C22.0463(12) C3C41.4206(18)
Fe1C32.0477(12) C4C51.4257(18)
Fe1C42.0373(12) C6C71.4406(17)
Fe1C52.0288(12) C6C101.4384(17)
Fe1C62.0521(11) C7C81.4257(18)
Fe1C72.0336(12) C8C91.4241(19)
Fe1C82.0474(12) C9C101.4233(18)
Fe1C92.0532(12) C14C151.5390(18)
Fe1C102.0447(12) C14C161.5361(18)
Si1O11.6442(9) C14C171.5342(19)
Si1O21.6277(10) C18C191.4006(17)
Si1C11.8635(12) C18C231.4037(17)
Si1C141.8858(12) C19C201.3929(18)
Si2O11.6449(9) C20C211.392(2)
Si2C61.8561(12) C21C221.387(2)
Si2C181.8678(12) C22C231.3930(18)
Si2C241.8725(12) C24C251.4000(17)
N1C111.4713(17) C24C291.4023(16)
N1C121.4622(18) C25C261.3960(18)
N1C131.4692(17) C26C271.3897(18)
C1C21.4501(16) C27C281.3878(18)
C1C51.4436(16) C28C291.3918(17)
C2C31.4264(18)    

 

Table 5 Bond Angles for mo_B0673_0m.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C1Fe1C6107.00(5) C2C1Fe169.08(6)
C1Fe1C9166.51(5) C2C1Si1128.82(9)
C2Fe1C141.45(5) C5C1Fe168.43(6)
C2Fe1C340.78(5) C5C1Si1125.05(9)
C2Fe1C6128.17(5) C5C1C2105.86(10)
C2Fe1C8117.42(5) C1C2Fe169.48(6)
C2Fe1C9150.81(5) C1C2C11128.02(11)
C3Fe1C169.39(5) C3C2Fe169.66(7)
C3Fe1C6166.53(5) C3C2C1108.42(10)
C3Fe1C9117.20(5) C3C2C11123.49(11)
C4Fe1C169.89(5) C11C2Fe1124.24(8)
C4Fe1C269.05(5) C2C3Fe169.56(7)
C4Fe1C340.70(5) C4C3Fe169.26(7)
C4Fe1C6151.60(5) C4C3C2108.77(11)
C4Fe1C8126.85(5) C3C4Fe170.05(7)
C4Fe1C9106.83(5) C3C4C5107.52(11)
C4Fe1C10117.62(5) C5C4Fe169.16(7)
C5Fe1C141.43(5) C1C5Fe170.13(6)
C5Fe1C269.02(5) C4C5Fe169.79(7)
C5Fe1C368.54(5) C4C5C1109.42(10)
C5Fe1C441.05(5) Si2C6Fe1121.50(6)
C5Fe1C6117.93(5) C7C6Fe168.67(6)
C5Fe1C7152.44(5) C7C6Si2129.41(9)
C5Fe1C8165.52(5) C10C6Fe169.17(7)
C5Fe1C9127.80(5) C10C6Si2124.39(9)
C5Fe1C10108.19(5) C10C6C7105.85(10)
C6Fe1C969.31(5) C6C7Fe170.04(6)
C7Fe1C1117.78(5) C8C7Fe170.07(7)
C7Fe1C2107.78(5) C8C7C6109.15(11)
C7Fe1C3127.88(5) C7C8Fe169.03(7)
C7Fe1C4165.46(5) C9C8Fe169.90(7)
C7Fe1C641.29(5) C9C8C7107.83(11)
C7Fe1C840.89(5) C8C9Fe169.46(7)
C7Fe1C968.60(5) C10C9Fe169.36(7)
C7Fe1C1068.56(5) C10C9C8107.85(11)
C8Fe1C1151.56(5) C6C10Fe169.72(6)
C8Fe1C3107.16(5) C9C10Fe170.00(7)
C8Fe1C669.47(5) C9C10C6109.31(11)
C8Fe1C940.64(5) N1C11C2114.06(10)
C10Fe1C1128.33(5) C15C14Si1108.73(9)
C10Fe1C2167.21(5) C16C14Si1109.60(9)
C10Fe1C3151.04(5) C16C14C15108.42(11)
C10Fe1C641.11(5) C17C14Si1112.09(9)
C10Fe1C868.45(5) C17C14C15109.30(12)
C10Fe1C940.65(5) C17C14C16108.63(11)
O1Si1C1109.06(5) C19C18Si2121.43(9)
O1Si1C14108.05(5) C19C18C23117.70(11)
O2Si1O1109.29(5) C23C18Si2120.83(9)
O2Si1C1109.19(5) C20C19C18121.13(12)
O2Si1C14109.69(5) C21C20C19120.12(12)
C1Si1C14111.53(5) C22C21C20119.76(12)
O1Si2C6112.97(5) C21C22C23119.93(12)
O1Si2C18108.34(5) C22C23C18121.35(12)
O1Si2C24107.78(5) C25C24Si2121.25(9)
C6Si2C18110.01(5) C25C24C29117.38(11)
C6Si2C24105.22(5) C29C24Si2121.05(9)
C18Si2C24112.55(5) C26C25C24121.35(11)
Si1O1Si2136.87(6) C27C26C25120.06(12)
C12N1C11111.58(11) C28C27C26119.61(12)
C12N1C13110.33(11) C27C28C29120.07(11)
C13N1C11108.85(11) C28C29C24121.53(11)
Si1C1Fe1122.36(6)     

 

Table 6 Hydrogen Bonds for mo_B0673_0m.
DHAd(D-H)/Åd(H-A)/Åd(D-A)/ÅD-H-A/°
O2H2N10.83(2)1.87(2)2.6900(15)169(2)

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for mo_B0673_0m.
AtomxyzU(eq)
H26400(30)2705(17)610(18)42(6)
H36042165289218
H41155867459619
H54243595426516
H740454651256417
H810424371360220
H99073047545421
H1038232517555918
H11A22443223100123
H11B37593747117023
H12A3735119869636
H12B46111586-58736
H12C27631962-11936
H13A35393869-90141
H13B53003407-142841
H13C51624235-70441
H15A5861-185193042
H15B7585-697141242
H15C698443776242
H16A9661121063533
H16B1020269131033
H16C102211117172333
H17A8429189355441
H17B8444-850312041
H17C6732-323363641
H1967545566365620
H2082347115262326
H21103637072105827
H2210985547552025
H2395093925155220
H2575571211502021
H267931584678126
H2780481798778422
H2877823642701520
H2973774267526618

Experimental

Single crystals of C29H35FeNO2Si2 [mo_B0673_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 Intrinsic Phasing 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_B0673_0m]

Crystal Data for C29H35FeNO2Si2 (=541.61 g/mol): triclinic, space group P-1 (no. 2), a = 8.4627(9) Å, b = 12.9654(13) Å, c = 13.1700(10) Å, α = 73.895(2)°, β = 73.944(3)°, γ = 84.816(3)°, = 1334.0(2) Å3, Z = 2, T = 100.01 K, μ(MoKα) = 0.682 mm-1, Dcalc = 1.348 g/cm3, 36672 reflections measured (5.01° ≤ 2Θ ≤ 66.456°), 10182 unique (Rint = 0.0326, Rsigma = 0.0368) which were used in all calculations. The final R1 was 0.0351 (I > 2σ(I)) and wR2 was 0.0831 (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), C19(H19), C20(H20),
C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29)
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)

This report has been created with Olex2, compiled on 2017.03.02 svn.r3394 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.