mo_B0610_0m

Table 1 Crystal data and structure refinement for mo_B0610_0m.
Identification code mo_B0610_0m
Empirical formula C23H25FeNO2Si
Formula weight 431.38
Temperature/K 145.55
Crystal system monoclinic
Space group P21/n
a/Å 13.173(4)
b/Å 11.838(5)
c/Å 13.877(5)
α/° 90
β/° 97.130(7)
γ/° 90
Volume/Å3 2147.3(13)
Z 4
ρcalcg/cm3 1.334
μ/mm‑1 0.776
F(000) 904.0
Crystal size/mm3 0.626 × 0.48 × 0.307
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 5.71 to 54
Index ranges -16 ≤ h ≤ 12, -15 ≤ k ≤ 15, -17 ≤ l ≤ 17
Reflections collected 20907
Independent reflections 4644 [Rint = 0.0306, Rsigma = 0.0284]
Data/restraints/parameters 4644/0/355
Goodness-of-fit on F2 1.180
Final R indexes [I>=2σ (I)] R1 = 0.0654, wR2 = 0.1304
Final R indexes [all data] R1 = 0.0731, wR2 = 0.1343
Largest diff. peak/hole / e Å-3 0.74/-0.74

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for mo_B0610_0m. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Fe16093.0(5)3796.4(4)3707.8(3)49.3(2)
Si18401.3(10)4858.6(8)5109.6(7)46.9(3)
O19263(3)4026(2)5709.5(17)52.3(8)
O28751(3)5271(2)4070.6(19)46.0(7)
N18907(2)1971(2)4880.0(19)38.0(7)
C17217(3)3987(3)4868(2)39.9(9)
C27210(3)2849(3)4466(2)37.2(8)
C36226(3)2364(3)4535(2)43.8(9)
C45612(3)3179(3)4955(2)40.7(9)
C56229(3)4171(3)5165(2)40.5(9)
C66434(5)4827(5)2610(3)93(2)
C76294(7)3670(6)2275(3)113(3)
C85310(7)3320(5)2408(3)100(3)
C94801(5)4231(4)2807(3)73.4(17)
C105481(5)5161(4)2931(3)75.8(18)
C118114(3)2315(3)4080(2)42.2(9)
C129853(3)1643(3)4490(3)47.4(10)
C138525(3)1016(3)5425(3)46.3(10)
C14A8366(9)5988(8)6043(7)36(2)
C14B7942(13)6224(11)5757(11)33(3)
C15A8815(10)5897(7)6982(5)48(2)
C15B8281(12)6278(14)6713(11)48(4)
C16A8694(14)6736(8)7702(7)77(4)
C16B8030(19)7220(20)7305(18)78(10)
C17A8107(15)7665(12)7483(10)82(6)
C17B7480(20)8080(20)6910(20)80(10)
C18A7614(12)7840(9)6520(14)70(5)
C18B7059(17)8084(15)5931(17)67(6)
C19A6991(13)8806(10)6240(19)102(7)
C19B6590(20)8906(16)5663(16)49(6)
C20A6456(14)9038(12)5238(13)70(5)
C20B6072(13)8995(9)4536(17)65(6)
C21A6726(7)8180(7)4583(13)82(4)
C21B6317(14)8095(9)3952(13)58(5)
C22A7285(8)7222(7)4844(12)49(3)
C22B6923(13)7197(8)4334(12)39(4)
C23A7746(8)6994(9)5798(9)44(2)
C23B7347(19)7146(12)5343(13)40(5)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for mo_B0610_0m. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Fe197.3(5)31.9(3)18.2(2)2.49(19)5.4(2)24.0(3)
Si190.9(9)24.8(4)32.2(5)-11.3(4)35.6(5)-24.4(5)
O195(2)38.4(14)22.9(11)-3(1)5.8(12)-39.5(15)
O274(2)30.2(13)40.3(14)2.9(10)34.5(15)-0.8(14)
N153(2)29.9(14)26.7(13)1.1(11)-11.5(13)-15.7(13)
C180(3)22.1(15)20.4(14)-1.3(12)16.5(16)-10.6(16)
C268(3)21.4(14)19.6(14)-0.5(11)-6.5(15)-3.5(15)
C367(3)22.2(15)35.2(17)1.0(13)-21.2(17)-3.1(16)
C459(2)32.5(17)27.1(16)6.0(13)-7.3(15)-9.7(16)
C574(3)26.9(16)22.9(15)-1.4(12)13.9(16)-11.4(16)
C6140(5)101(4)45(2)49(3)44(3)67(4)
C7197(8)125(5)17.3(19)12(2)17(3)126(6)
C8175(7)89(4)26(2)-18(2)-24(3)84(5)
C9124(5)70(3)23.0(18)-2.3(19)-6(2)54(3)
C10138(5)60(3)35(2)25(2)32(3)58(3)
C1175(3)23.5(15)23.1(15)-4.4(12)-11.8(16)2.2(16)
C1256(3)45(2)37.7(19)-0.9(16)-9.5(17)-13.6(18)
C1350(2)36.9(18)44(2)15.3(15)-22.8(17)-16.5(16)
C14A52(6)21(4)41(5)-5(3)25(4)-12(4)
C14B51(9)12(6)43(8)-12(5)35(6)-12(5)
C15A85(7)34(4)30(4)-12(3)30(4)-28(4)
C15B54(9)51(8)47(8)-24(7)33(7)-33(6)
C16A148(13)47(5)47(5)-24(4)54(6)-49(6)
C16B94(15)85(19)70(15)-65(16)63(12)-69(15)
C17A146(14)46(6)73(8)-40(6)81(9)-54(8)
C17B101(17)68(17)86(17)-70(14)67(14)-61(13)
C18A90(10)32(5)103(12)-35(8)77(9)-38(6)
C18B83(13)44(10)88(12)-47(9)66(10)-48(9)
C19A93(11)23(5)210(20)-29(11)98(12)-20(7)
C19B65(15)8(7)78(15)2(9)30(12)4(7)
C20A67(7)20(4)120(15)15(8)4(10)-7(4)
C20B58(10)23(5)126(15)0(7)61(10)2(5)
C21A38(5)36(4)171(14)3(6)10(6)-2(3)
C21B68(11)21(5)95(11)19(6)54(9)8(6)
C22A30(5)27(3)89(10)-9(6)2(6)-6(3)
C22B54(9)15(4)56(9)-3(5)40(7)-5(5)
C23A48(5)34(5)57(6)-7(4)34(4)-18(4)
C23B73(13)18(5)37(9)-12(7)41(9)-19(7)

 

Table 4 Bond Lengths for mo_B0610_0m.
AtomAtomLength/Å AtomAtomLength/Å
Fe1C12.060(4) C7C81.395(11)
Fe1C22.036(4) C8C91.418(6)
Fe1C32.043(3) C9C101.416(8)
Fe1C42.050(4) C14AC15A1.366(12)
Fe1C52.056(3) C14AC23A1.460(12)
Fe1C62.045(5) C14BC15B1.348(19)
Fe1C72.043(4) C14BC23B1.42(2)
Fe1C82.043(5) C15AC16A1.432(11)
Fe1C92.048(5) C15BC16B1.45(2)
Fe1C102.051(4) C16AC17A1.36(2)
Si1O11.649(4) C16BC17B1.33(4)
Si1O21.641(3) C17AC18A1.43(2)
Si1C11.866(4) C17BC18B1.41(4)
Si1C14A1.866(9) C18AC19A1.43(2)
Si1C14B1.980(13) C18AC23A1.442(16)
N1C111.484(4) C18BC19B1.19(3)
N1C121.472(5) C18BC23B1.455(19)
N1C131.483(4) C19AC20A1.50(2)
C1C21.457(4) C19BC20B1.63(3)
C1C51.430(6) C20AC21A1.44(2)
C2C31.432(6) C20BC21B1.400(18)
C2C111.504(5) C21AC22A1.377(13)
C3C41.429(5) C21BC22B1.395(18)
C4C51.438(5) C22AC23A1.412(13)
C6C71.450(9) C22BC23B1.442(19)
C6C101.439(7)    

 

Table 5 Bond Angles for mo_B0610_0m.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C2Fe1C141.69(12) C1C2Fe170.0(2)
C2Fe1C341.12(15) C1C2C11123.9(3)
C2Fe1C469.32(15) C3C2Fe169.7(2)
C2Fe1C568.98(14) C3C2C1108.0(3)
C2Fe1C6120.1(2) C3C2C11128.2(3)
C2Fe1C7106.85(19) C11C2Fe1126.9(2)
C2Fe1C8123.87(17) C2C3Fe169.16(19)
C2Fe1C9161.10(18) C4C3Fe169.84(19)
C2Fe1C10156.5(2) C4C3C2108.6(3)
C3Fe1C169.45(13) C3C4Fe169.3(2)
C3Fe1C440.86(15) C3C4C5107.4(3)
C3Fe1C568.64(13) C5C4Fe169.72(19)
C3Fe1C6154.47(19) C1C5Fe169.81(19)
C3Fe1C7118.3(2) C1C5C4109.2(3)
C3Fe1C8105.4(2) C4C5Fe169.28(19)
C3Fe1C9123.9(2) C7C6Fe169.2(3)
C3Fe1C10161.8(2) C10C6Fe169.6(3)
C4Fe1C169.34(14) C10C6C7106.1(7)
C4Fe1C540.99(13) C6C7Fe169.3(2)
C4Fe1C10125.58(17) C8C7Fe170.0(3)
C5Fe1C140.65(15) C8C7C6108.8(5)
C6Fe1C1108.3(2) C7C8Fe170.0(3)
C6Fe1C4163.99(18) C7C8C9108.5(6)
C6Fe1C5127.1(2) C9C8Fe169.9(3)
C6Fe1C968.8(3) C8C9Fe169.5(3)
C6Fe1C1041.1(2) C10C9Fe169.9(3)
C7Fe1C1126.9(3) C10C9C8108.5(6)
C7Fe1C4152.4(3) C6C10Fe169.2(2)
C7Fe1C5165.1(3) C9C10Fe169.7(2)
C7Fe1C641.6(3) C9C10C6108.1(5)
C7Fe1C967.8(2) N1C11C2111.3(3)
C7Fe1C1068.68(18) C15AC14ASi1124.1(7)
C8Fe1C1162.8(2) C15AC14AC23A116.8(8)
C8Fe1C4118.1(3) C23AC14ASi1118.9(7)
C8Fe1C5154.3(3) C15BC14BSi1113.7(11)
C8Fe1C668.9(3) C15BC14BC23B117.4(12)
C8Fe1C739.9(3) C23BC14BSi1128.8(10)
C8Fe1C940.57(19) C14AC15AC16A122.5(10)
C8Fe1C1068.4(2) C14BC15BC16B121.6(18)
C9Fe1C1155.74(16) C17AC16AC15A121.1(11)
C9Fe1C4106.5(2) C17BC16BC15B121(2)
C9Fe1C5120.70(17) C16AC17AC18A120.5(11)
C9Fe1C1040.4(2) C16BC17BC18B122(2)
C10Fe1C1121.5(2) C17AC18AC19A123.3(17)
C10Fe1C5109.12(17) C17AC18AC23A118.1(13)
O1Si1C1105.56(15) C19AC18AC23A118.7(19)
O1Si1C14A98.8(4) C17BC18BC23B117(2)
O1Si1C14B119.3(6) C19BC18BC17B115.4(17)
O2Si1O1111.77(17) C19BC18BC23B128(2)
O2Si1C1109.03(17) C18AC19AC20A125.7(18)
O2Si1C14A115.5(3) C18BC19BC20B119.4(18)
O2Si1C14B106.9(4) C21AC20AC19A109.3(14)
C1Si1C14A115.4(3) C21BC20BC19B114.1(14)
C1Si1C14B103.7(5) C22AC21AC20A125.6(14)
C12N1C11110.3(3) C22BC21BC20B121.5(15)
C12N1C13110.0(3) C21AC22AC23A123.9(12)
C13N1C11109.8(3) C21BC22BC23B122.4(13)
Si1C1Fe1134.82(16) C18AC23AC14A121.1(11)
C2C1Fe168.27(19) C22AC23AC14A122.5(9)
C2C1Si1123.0(3) C22AC23AC18A116.4(12)
C5C1Fe169.5(2) C14BC23BC18B121.8(17)
C5C1Si1129.4(2) C14BC23BC22B123.5(12)
C5C1C2106.8(3) C22BC23BC18B114.6(18)

 

Table 6 Hydrogen Bonds for mo_B0610_0m.
DHAd(D-H)/Åd(H-A)/Åd(D-A)/ÅD-H-A/°
O1H1N10.91(6)1.82(6)2.707(4)167(5)
O2H2O110.74(4)1.99(4)2.726(5)178(5)

12-X,1-Y,1-Z

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for mo_B0610_0m.
AtomxyzU(eq)
H19210(40)3300(50)5510(40)89(18)
H29290(30)5460(40)4120(30)40(14)
H360161623433453
H449223082507349
H560144842545549
H6703452742615111
H7679132252010136
H8502925932256120
H941204219296588
H1053335881318391
H11A78831643368751
H11B84122858365251
H12A9716996405471
H12B103751436502771
H12C101002279413171
H13A79381265573969
H13B9070753591969
H13C8315396497569
H15A92235252716457
H15B86955683700558
H16A90306641834393
H16B82647220798194
H17A80248204797599
H17B73588712731096
H19A690893466730123
H19B65119506610358
H20A60099655506684
H20B56449604429678
H21A65008284391298
H21B60648096328069
H22A73666681435459
H22B70636598391546

 

Table 8 Atomic Occupancy for mo_B0610_0m.
AtomOccupancy AtomOccupancy AtomOccupancy
C14A0.615(15) C14B0.385(15) C15A0.615(15)
H15A0.615(15) C15B0.385(15) H15B0.385(15)
C16A0.615(15) H16A0.615(15) C16B0.385(15)
H16B0.385(15) C17A0.615(15) H17A0.615(15)
C17B0.385(15) H17B0.385(15) C18A0.615(15)
C18B0.385(15) C19A0.615(15) H19A0.615(15)
C19B0.385(15) H19B0.385(15) C20A0.615(15)
H20A0.615(15) C20B0.385(15) H20B0.385(15)
C21A0.615(15) H21A0.615(15) C21B0.385(15)
H21B0.385(15) C22A0.615(15) H22A0.615(15)
C22B0.385(15) H22B0.385(15) C23A0.615(15)
C23B0.385(15)     

Experimental

Single crystals of C23H25FeNO2Si [mo_B0610_0m] were [The material was recrystallised from a mixture of acetone and water by slow evaporation]. A suitable crystal was selected and [The crystal was mounted on a MITIGEN holder oil] on a 'Bruker APEX-II CCD' diffractometer. The crystal was kept at 145.55 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_B0610_0m]

Crystal Data for C23H25FeNO2Si (=431.38 g/mol): monoclinic, space group P21/n (no. 14), a = 13.173(4) Å, b = 11.838(5) Å, c = 13.877(5) Å, β = 97.130(7)°, = 2147.3(13) Å3, Z = 4, T = 145.55 K, μ(MoKα) = 0.776 mm-1, Dcalc = 1.334 g/cm3, 20907 reflections measured (5.71° ≤ 2Θ ≤ 54°), 4644 unique (Rint = 0.0306, Rsigma = 0.0284) which were used in all calculations. The final R1 was 0.0654 (I > 2σ(I)) and wR2 was 0.1343 (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. Others
Sof(C14B)=Sof(C15B)=Sof(H15B)=Sof(C16B)=Sof(H16B)=Sof(C17B)=Sof(H17B)=
Sof(C18B)=Sof(C19B)=Sof(H19B)=Sof(C20B)=Sof(H20B)=Sof(C21B)=Sof(H21B)=
Sof(C22B)=Sof(H22B)=Sof(C23B)=1-FVAR(1)
Sof(C14A)=Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17A)=
Sof(C18A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21A)=
Sof(C22A)=Sof(H22A)=Sof(C23A)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
C11(H11A,H11B)
3.b Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C15A(H15A),
C15B(H15B), C16A(H16A), C16B(H16B), C17A(H17A), C17B(H17B), C19A(H19A),
C19B(H19B), C20A(H20A), C20B(H20B), C21A(H21A), C21B(H21B), C22A(H22A),
C22B(H22B)
3.c Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)

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