3216_twin1_hklf4

Table 1 Crystal data and structure refinement for 3216_twin1_hklf4.
Identification code 3216_twin1_hklf4
Empirical formula C19H30FeLiNO2Si
Formula weight 395.32
Temperature/K 173.15
Crystal system triclinic
Space group P-1
a/Å 9.510(6)
b/Å 10.509(4)
c/Å 11.173(6)
α/° 81.19(4)
β/° 71.92(5)
γ/° 72.75(5)
Volume/Å3 1011.4(10)
Z 2
ρcalcg/cm3 1.298
μ/mm‑1 0.816
F(000) 420.0
Crystal size/mm3 0.18 × 0.06 × 0.06
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.672 to 51.998
Index ranges -11 ≤ h ≤ 11, -12 ≤ k ≤ 12, -13 ≤ l ≤ 13
Reflections collected 13640
Independent reflections 13640 [Rint = ?, Rsigma = 0.1906]
Data/restraints/parameters 13640/0/234
Goodness-of-fit on F2 0.846
Final R indexes [I>=2σ (I)] R1 = 0.0661, wR2 = 0.1534
Final R indexes [all data] R1 = 0.1586, wR2 = 0.1723
Largest diff. peak/hole / e Å-3 0.79/-0.75

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for 3216_twin1_hklf4. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Fe18764.6(11)3839.4(9)2873.1(10)51.6(4)
Si16860.9(19)1722.6(19)2389.0(17)39.3(5)
O15384(4)2623(4)3434(4)41.5(11)
O26813(5)179(4)2865(4)54.3(13)
N16772(5)2348(5)5840(5)37.0(13)
C18583(6)2029(5)2559(6)31.7(15)
C28864(6)1956(6)3754(6)36.1(16)
C310278(7)2272(6)3552(7)49.5(19)
C410877(8)2559(7)2238(8)61(2)
C59862(7)2395(6)1628(7)46.0(18)
C66802(7)5300(6)3879(6)43.3(18)
C78264(8)5485(6)3868(8)70(3)
C89179(11)5671(8)2603(11)100(4)
C98356(12)5590(8)1792(9)92(4)
C106942(9)5357(6)2555(7)63(2)
C117984(7)1382(6)5000(6)42.7(17)
C127477(7)3060(7)6436(7)59(2)
C135858(7)1591(7)6835(6)50.7(19)
C146648(8)2045(9)759(7)68(2)
C157944(8)1099(7)-138(6)64(2)
C165151(9)1855(14)725(8)171(7)
C176692(12)3491(10)197(8)122(4)
C188095(8)-953(6)2693(6)61(2)
C193949(7)2246(8)3950(7)77(3)
Li15518(11)3789(10)4781(9)38(3)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for 3216_twin1_hklf4. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Fe128.5(6)35.7(6)75.2(8)-13.9(5)15.3(5)-12.2(4)
Si123.7(10)52.3(12)37.4(12)-10.5(9)-3.4(8)-5.1(9)
O118(2)61(3)43(3)-17(2)-0.4(19)-9(2)
O243(3)50(3)66(3)-21(3)8(2)-22(2)
N132(3)40(3)37(3)-8(3)-5(3)-8(3)
C123(3)27(3)39(4)-5(3)-2(3)-3(3)
C217(3)35(4)54(5)-10(3)-10(3)-2(3)
C321(4)52(5)73(6)-20(4)-11(4)-1(3)
C429(4)55(5)90(7)-27(4)8(4)-13(4)
C532(4)34(4)54(5)-6(3)9(3)-2(3)
C627(4)29(4)57(5)-3(3)11(3)-6(3)
C744(5)43(4)110(7)-38(4)25(5)-23(4)
C863(6)41(5)152(11)-33(6)57(7)-25(5)
C9108(9)33(5)72(7)-1(4)53(6)-10(5)
C1061(5)23(4)66(6)8(4)11(4)9(3)
C1132(4)46(4)48(4)-4(4)-18(3)1(3)
C1235(4)79(6)64(5)-21(4)-9(4)-13(4)
C1349(4)55(5)38(4)-3(4)-9(4)-3(4)
C1444(5)94(7)52(5)-13(5)-17(4)12(4)
C1560(5)87(6)36(4)-18(4)-11(4)0(4)
C1641(6)410(20)60(7)-85(9)-14(5)-19(9)
C17145(10)124(9)53(6)-27(6)-44(6)57(7)
C1866(5)36(4)63(5)-8(4)7(4)-12(4)
C1928(4)123(7)84(6)-54(5)12(4)-30(5)
Li130(6)40(6)40(7)-1(5)-6(5)-9(5)

 

Table 4 Bond Lengths for 3216_twin1_hklf4.
AtomAtomLength/Å AtomAtomLength/Å
Fe1C12.051(6) N1Li12.091(11)
Fe1C22.060(6) C1C21.428(8)
Fe1C32.062(7) C1C51.442(8)
Fe1C42.038(7) C2C31.423(8)
Fe1C52.033(6) C2C111.523(8)
Fe1C62.152(6) C3C41.421(9)
Fe1C72.056(7) C4C51.403(9)
Fe1C82.037(8) C6C71.456(9)
Fe1C92.045(9) C6C101.437(9)
Fe1C102.060(7) C6Li112.272(11)
Si1O11.662(4) C6Li12.218(11)
Si1O21.637(5) C7C81.430(11)
Si1C11.829(6) C8C91.395(13)
Si1C141.864(8) C9C101.420(10)
O1C191.454(7) C14C151.524(9)
O1Li12.136(10) C14C161.507(11)
O2C181.415(7) C14C171.560(11)
N1C111.472(7) Li1C612.272(11)
N1C121.476(7) Li1Li112.51(2)
N1C131.470(7)    

11-X,1-Y,1-Z

 

Table 5 Bond Angles for 3216_twin1_hklf4.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C1Fe1C240.6(2) Si1C1Fe1125.2(3)
C1Fe1C368.3(2) C2C1Fe170.0(3)
C1Fe1C6121.2(2) C2C1Si1122.8(4)
C1Fe1C7155.7(3) C2C1C5106.4(5)
C1Fe1C10110.6(3) C5C1Fe168.6(3)
C2Fe1C340.4(2) C5C1Si1130.8(5)
C2Fe1C6111.4(2) C1C2Fe169.4(3)
C3Fe1C6129.8(3) C1C2C11126.1(5)
C4Fe1C169.0(2) C3C2Fe169.9(4)
C4Fe1C268.5(3) C3C2C1108.3(6)
C4Fe1C340.6(3) C3C2C11124.6(6)
C4Fe1C6165.2(3) C11C2Fe1135.3(4)
C4Fe1C7126.1(3) C2C3Fe169.8(4)
C4Fe1C9115.1(3) C4C3Fe168.8(4)
C4Fe1C10151.1(3) C4C3C2108.3(6)
C5Fe1C141.3(2) C3C4Fe170.6(4)
C5Fe1C268.3(3) C5C4Fe169.7(4)
C5Fe1C367.7(3) C5C4C3107.8(6)
C5Fe1C440.3(3) C1C5Fe170.0(3)
C5Fe1C6154.4(3) C4C5Fe170.0(4)
C5Fe1C7162.2(2) C4C5C1109.1(6)
C5Fe1C8123.4(3) Fe1C6Li193.0(3)
C5Fe1C9105.5(3) Fe1C6Li11160.8(4)
C5Fe1C10119.9(3) C7C6Fe166.2(3)
C7Fe1C2121.9(3) C7C6Li1134.7(6)
C7Fe1C3109.5(3) C7C6Li11125.8(5)
C7Fe1C640.4(2) C10C6Fe166.6(4)
C7Fe1C1066.2(3) C10C6C7102.0(6)
C8Fe1C1162.6(4) C10C6Li11119.0(5)
C8Fe1C2153.4(4) C10C6Li1105.7(5)
C8Fe1C3117.6(4) Li1C6Li1167.8(4)
C8Fe1C4104.2(3) C6C7Fe173.3(4)
C8Fe1C669.1(3) C8C7Fe168.9(4)
C8Fe1C740.9(3) C8C7C6110.9(8)
C8Fe1C940.0(4) C7C8Fe170.2(4)
C8Fe1C1067.1(4) C9C8Fe170.3(5)
C9Fe1C1127.0(4) C9C8C7107.7(8)
C9Fe1C2166.6(4) C8C9Fe169.7(6)
C9Fe1C3149.8(3) C8C9C10107.2(8)
C9Fe1C668.8(3) C10C9Fe170.3(4)
C9Fe1C767.6(4) C6C10Fe173.5(4)
C9Fe1C1040.5(3) C9C10Fe169.2(5)
C10Fe1C2131.3(3) C9C10C6112.3(8)
C10Fe1C3168.1(3) N1C11C2116.5(5)
C10Fe1C639.8(3) C15C14Si1110.9(5)
O1Si1C1106.3(2) C15C14C17106.6(7)
O1Si1C14112.8(3) C16C14Si1111.3(6)
O2Si1O1103.8(2) C16C14C15107.9(7)
O2Si1C1110.3(3) C16C14C17107.2(8)
O2Si1C14108.1(3) C17C14Si1112.7(6)
C1Si1C14115.0(3) O1Li1C6112.3(5)
Si1O1Li1126.1(3) O1Li1C61113.2(5)
C19O1Si1121.5(4) O1Li1Li11133.8(7)
C19O1Li1106.9(4) N1Li1O1102.0(5)
C18O2Si1125.8(4) N1Li1C6109.3(5)
C11N1C12109.5(5) N1Li1C61107.2(5)
C11N1Li1109.6(4) N1Li1Li11124.1(7)
C12N1Li1106.8(5) C6Li1C61112.2(4)
C13N1C11107.7(5) C6Li1Li1157.1(4)
C13N1C12108.6(5) C61Li1Li1155.1(4)
C13N1Li1114.7(5)     

11-X,1-Y,1-Z

 

Table 6 Torsion Angles for 3216_twin1_hklf4.
ABCDAngle/˚ ABCDAngle/˚
Fe1C1C2C3-59.2(4) C1C2C11N1-98.3(7)
Fe1C1C2C11131.7(6) C2C1C5Fe1-60.1(4)
Fe1C1C5C459.3(4) C2C1C5C4-0.8(7)
Fe1C2C3C4-58.2(5) C2C3C4Fe158.7(4)
Fe1C2C11N1-1.6(9) C2C3C4C5-1.2(7)
Fe1C3C4C5-60.0(5) C3C2C11N194.4(7)
Fe1C4C5C1-59.3(4) C3C4C5Fe160.6(5)
Fe1C6C7C858.9(5) C3C4C5C11.3(7)
Fe1C6C10C9-58.6(5) C5C1C2Fe159.3(4)
Fe1C7C8C960.6(6) C5C1C2C30.1(7)
Fe1C8C9C1060.7(5) C5C1C2C11-169.0(5)
Fe1C9C10C661.1(5) C6C7C8Fe1-61.6(5)
Si1C1C2Fe1-119.7(4) C6C7C8C9-0.9(9)
Si1C1C2C3-178.9(4) C7C6C10Fe157.3(4)
Si1C1C2C1112.0(8) C7C6C10C9-1.3(7)
Si1C1C5Fe1118.7(5) C7C8C9Fe1-60.6(6)
Si1C1C5C4178.0(5) C7C8C9C100.1(9)
O1Si1O2C18-150.5(5) C8C9C10Fe1-60.3(6)
O1Si1C1Fe1-39.1(4) C8C9C10C60.8(9)
O1Si1C1C248.4(5) C10C6C7Fe1-57.6(4)
O1Si1C1C5-130.3(5) C10C6C7C81.3(7)
O1Si1C14C15-174.2(5) C11C2C3Fe1-131.8(6)
O1Si1C14C16-54.1(8) C11C2C3C4170.0(6)
O1Si1C14C1766.4(6) C12N1C11C2-74.3(7)
O2Si1O1C19-37.6(6) C13N1C11C2167.8(5)
O2Si1O1Li1112.6(4) C14Si1O1C1979.1(6)
O2Si1C1Fe1-151.0(3) C14Si1O1Li1-130.7(5)
O2Si1C1C2-63.5(5) C14Si1O2C1889.5(6)
O2Si1C1C5117.8(5) C14Si1C1Fe186.5(5)
O2Si1C14C15-60.1(6) C14Si1C1C2174.0(5)
O2Si1C14C1660.0(8) C14Si1C1C5-4.7(7)
O2Si1C14C17-179.5(5) Li1N1C11C242.5(7)
C1Si1O1C19-154.0(5) Li11C6C7Fe1162.7(6)
C1Si1O1Li1-3.8(5) Li1C6C7Fe169.2(7)
C1Si1O2C18-37.0(6) Li1C6C7C8128.1(8)
C1Si1C14C1563.7(7) Li11C6C7C8-138.5(6)
C1Si1C14C16-176.2(7) Li11C6C10Fe1-159.5(4)
C1Si1C14C17-55.8(6) Li1C6C10Fe1-86.5(4)
C1C2C3Fe158.9(4) Li1C6C10C9-145.1(6)
C1C2C3C40.7(7) Li11C6C10C9141.9(6)

11-X,1-Y,1-Z

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for 3216_twin1_hklf4.
AtomxyzU(eq)
H3107432289418859
H4118002817184273
H59996250874355
H785695483460184
H81016958232360120
H986815675896110
H1061765251222875
H11A7513743480951
H11B8730870546551
H12A81752410686089
H12B66723640705589
H12C80513602578889
H13A52991186646476
H13B51252195747076
H13C6540888723476
H15A89311211-14097
H15B78241303-99397
H15C790917614197
H16A50389881148257
H16B51431886-154257
H16C430025681159257
H17A58584137734183
H17B65673611-655183
H17C76783633158183
H18A8006-1544213791
H18B8128-1434351291
H18C9037-666231291
H19A314828923626116
H19B364822374872116
H19C408313553698116

Experimental

Single crystals of C19H30FeLiNO2Si [3216_twin1_hklf4] were []. A suitable crystal was selected and [] on a Xcalibur, Sapphire3 diffractometer. The crystal was kept at 173.15 K during data collection. Using Olex2 [1], the structure was solved with the Superflip [2] structure solution program using Charge Flipping 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. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst., 40, 786-790; Palatinus, L. & van der Lee, A. (2008). J. Appl. Cryst. 41, 975-984; Palatinus, L., Prathapa, S. J. & van Smaalen, S. (2012). J. Appl. Cryst. 45, 575-580.
  3. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Crystal structure determination of [3216_twin1_hklf4]

Crystal Data for C19H30FeLiNO2Si (=395.32 g/mol): triclinic, space group P-1 (no. 2), a = 9.510(6) Å, b = 10.509(4) Å, c = 11.173(6) Å, α = 81.19(4)°, β = 71.92(5)°, γ = 72.75(5)°, = 1011.4(10) Å3, Z = 2, T = 173.15 K, μ(MoKα) = 0.816 mm-1, Dcalc = 1.298 g/cm3, 13640 reflections measured (4.672° ≤ 2Θ ≤ 51.998°), 13640 unique (Rint = ?, Rsigma = 0.1906) which were used in all calculations. The final R1 was 0.0661 (I > 2σ(I)) and wR2 was 0.1723 (all data).

Refinement model description

Number of restraints - 0, number of constraints - unknown.

Details:

1. Twinned data refinement
Scales: 0.6728(14) 0.3272(14)
2. 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
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), C7(H7), C8(H8), C9(H9), C10(H10)
3.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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