3207_twin1_hklf4

Table 1 Crystal data and structure refinement for 3207_twin1_hklf4.
Identification code 3207_twin1_hklf4
Empirical formula C36H58Fe2Li2N2OSi2
Formula weight 716.60
Temperature/K 173.15
Crystal system triclinic
Space group P-1
a/Å 9.3542(8)
b/Å 9.9397(8)
c/Å 22.1527(17)
α/° 79.942(7)
β/° 78.411(7)
γ/° 70.771(7)
Volume/Å3 1892.0(3)
Z 2
ρcalcg/cm3 1.258
μ/mm‑1 0.859
F(000) 764.0
Crystal size/mm3 0.14 × 0.06 × 0.045
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.37 to 51.998
Index ranges -11 ≤ h ≤ 11, -12 ≤ k ≤ 12, -27 ≤ l ≤ 27
Reflections collected 8461
Independent reflections 8461 [Rint = 0.1294, Rsigma = 0.1020]
Data/restraints/parameters 8461/6/431
Goodness-of-fit on F2 1.034
Final R indexes [I>=2σ (I)] R1 = 0.0506, wR2 = 0.1223
Final R indexes [all data] R1 = 0.0805, wR2 = 0.1391
Largest diff. peak/hole / e Å-3 0.48/-0.48

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for 3207_twin1_hklf4. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Fe14141.6(9)4453.4(9)8892.7(4)26.5(2)
Fe24920.7(9)6107.2(9)6258.3(4)24.9(2)
Si27760.5(18)7404.1(18)5268.9(8)28.4(4)
Si12171(2)1983.6(19)9573.3(8)33.1(4)
N14571(5)1633(5)7522(2)24.8(11)
O18473(4)689(4)7389(2)39.4(11)
C13894(6)2442(6)9120(3)23.1(13)
C72388(7)6204(6)8630(3)33.0(15)
N27974(5)5436(5)7450(2)27.6(12)
C143525(7)2645(7)7948(3)24.9(13)
C196539(6)4308(6)6675(3)25.7(14)
C163809(7)1737(7)6990(3)36.8(16)
C154910(7)164(6)7828(3)34.2(15)
C206135(6)4036(6)6124(3)27.6(15)
C187138(6)5516(6)6447(3)24.5(14)
C307717(7)6270(7)6849(3)30.7(15)
C12349(6)3070(7)9259(3)39.6(17)
C177093(6)5986(6)5793(3)24.8(13)
C62177(7)5867(6)9278(3)34.3(16)
C35822(6)3009(6)8312(3)27.9(14)
C216455(6)5027(6)5593(3)25.5(14)
C132054(7)2297(8)10407(3)49.5(19)
C83815(7)6510(6)8448(3)37.4(16)
C262991(6)7211(7)5862(3)37.6(16)
C233538(7)7772(6)6728(3)39.7(18)
C55106(6)2563(6)9397(3)27.0(14)
C24339(6)2721(5)8463(3)21.5(13)
C296977(8)9218(7)5567(3)52(2)
C328205(7)6297(7)7874(3)42.8(18)
C103448(7)5959(6)9502(3)37.5(17)
C252664(6)6246(7)6363(3)38.7(17)
C319318(6)4169(6)7382(3)37.8(17)
C46211(6)2916(6)8914(3)32.0(15)
C223535(6)8167(7)6095(4)42.4(19)
C242997(6)6559(6)6913(3)34.3(16)
C279890(7)6928(7)5187(4)51(2)
C338776(7)-69(7)7995(4)48(2)
C94452(7)6347(6)8995(3)38.3(17)
C3410176(9)64(8)8172(5)77(3)
C287194(8)7534(7)4499(3)49.3(19)
Li16572(11)2339(10)7364(5)30(2)
C369378(9)720(9)6329(4)74(2)
C112377(8)59(7)9548(4)59(2)
C359446(11)-91(10)6917(5)95(3)
Li26131(10)4682(11)7632(5)32(3)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for 3207_twin1_hklf4. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Fe126.2(5)31.3(5)23.7(5)-8.8(4)-4.8(4)-7.8(4)
Fe221.8(4)26.7(5)25.6(5)-4.6(4)-4.7(4)-5.3(4)
Si228.5(9)32(1)24.8(10)-1.8(8)-4.8(8)-9.9(8)
Si131.4(10)39.5(11)26.7(11)1.5(9)-6.4(9)-10.0(8)
N126(3)23(3)27(3)-9(2)-7(2)-6(2)
O127(2)32(3)50(3)-11(2)-4(2)5(2)
C124(3)23(3)23(3)-7(3)-6(3)-5(3)
C736(4)33(4)24(4)-9(3)-8(3)3(3)
N237(3)24(3)25(3)4(2)-12(2)-13(2)
C1421(3)35(4)20(3)-1(3)-9(3)-8(3)
C1921(3)18(3)35(4)-5(3)-7(3)0(2)
C1642(4)42(4)28(4)-12(3)-7(3)-11(3)
C1547(4)27(3)36(4)-4(3)-20(3)-11(3)
C2021(3)19(3)45(4)-13(3)-7(3)-4(2)
C1818(3)23(3)30(4)-9(3)-1(3)-1(2)
C3031(4)35(4)33(4)1(3)-14(3)-17(3)
C1230(4)60(5)32(4)-7(3)0(3)-20(3)
C1720(3)26(3)28(4)-10(3)-6(3)-1(2)
C630(4)28(3)42(4)-20(3)3(3)-3(3)
C323(3)37(4)26(4)-12(3)-2(3)-10(3)
C2125(3)31(3)22(3)-6(3)-8(3)-6(3)
C1340(4)79(5)25(4)9(4)-12(3)-15(4)
C851(4)25(3)31(4)-2(3)-4(4)-8(3)
C2625(3)48(4)36(4)-5(4)-14(3)-1(3)
C2338(4)27(4)46(5)-16(3)-12(4)9(3)
C529(3)35(3)18(3)-3(2)-16(2)-2(2)
C227(3)16(3)22(3)-3(3)-14(3)1(2)
C2953(5)53(5)50(5)-11(4)4(4)-22(4)
C3255(4)41(4)41(5)-17(3)-5(4)-21(3)
C1052(4)34(4)31(4)-20(3)-9(4)-9(3)
C2516(3)38(4)62(5)-10(4)-9(3)-4(3)
C3133(4)29(3)51(5)-5(3)-21(3)0(3)
C427(3)37(4)33(4)-11(3)-12(3)-3(3)
C2217(3)28(4)69(6)1(4)-2(4)5(3)
C2425(3)31(4)35(4)-7(3)8(3)1(3)
C2734(4)55(5)66(6)1(4)-7(4)-21(3)
C3338(4)28(4)70(6)3(4)-13(4)-1(3)
C944(4)26(3)49(5)-17(3)-3(4)-12(3)
C3474(6)64(6)103(8)0(6)-23(6)-33(5)
C2867(5)54(5)32(4)11(4)-16(4)-28(4)
Li128(5)34(6)34(6)-17(5)-9(5)-8(5)
C3666(6)70(6)64(6)-6(5)1(5)-1(4)
C1162(5)44(4)67(6)19(4)-12(5)-22(4)
C3588(7)78(7)80(8)2(6)5(6)12(6)
Li222(5)30(6)43(7)-7(5)6(5)-15(5)

 

Table 4 Bond Lengths for 3207_twin1_hklf4.
AtomAtomLength/Å AtomAtomLength/Å
Fe1C12.052(5) O1C351.400(9)
Fe1C72.051(6) C1C51.439(7)
Fe1C62.042(6) C1C21.437(7)
Fe1C32.130(6) C7C61.405(8)
Fe1C82.061(6) C7C81.430(8)
Fe1C52.036(6) N2C301.459(7)
Fe1C22.050(5) N2C321.466(7)
Fe1C102.049(6) N2C311.462(7)
Fe1C42.037(6) N2Li22.040(10)
Fe1C92.053(6) C14C21.517(7)
Fe2C192.132(6) C19C201.441(8)
Fe2C202.039(5) C19C181.459(7)
Fe2C182.069(5) C19Li12.257(12)
Fe2C172.061(5) C19Li22.151(12)
Fe2C212.019(6) C20C211.447(8)
Fe2C262.056(6) C18C301.530(7)
Fe2C232.036(6) C18C171.446(8)
Fe2C252.037(6) C17C211.446(7)
Fe2C222.045(6) C6C101.411(8)
Fe2C242.047(6) C3C21.469(7)
Si2C171.855(6) C3C41.431(8)
Si2C291.891(6) C3Li12.220(11)
Si2C271.868(6) C3Li22.094(12)
Si2C281.858(7) C8C91.417(9)
Si1C11.868(6) C26C251.389(9)
Si1C121.886(6) C26C221.422(8)
Si1C131.901(7) C23C221.390(9)
Si1C111.869(7) C23C241.423(8)
N1C141.473(7) C5C41.414(8)
N1C161.469(7) C10C91.399(9)
N1C151.459(7) C25C241.423(9)
N1Li12.153(10) C33C341.493(9)
O1C331.451(8) C36C351.410(11)
O1Li11.985(10)    

 

Table 5 Bond Angles for 3207_twin1_hklf4.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C1Fe1C370.3(2) C33O1Li1117.1(5)
C1Fe1C8158.3(2) C35O1C33110.7(6)
C1Fe1C9159.5(2) C35O1Li1130.8(6)
C7Fe1C1122.0(2) Si1C1Fe1126.6(3)
C7Fe1C3127.5(2) C5C1Fe168.8(3)
C7Fe1C840.7(2) C5C1Si1123.9(4)
C7Fe1C967.9(3) C2C1Fe169.4(3)
C6Fe1C1107.4(2) C2C1Si1130.7(4)
C6Fe1C740.2(2) C2C1C5105.4(5)
C6Fe1C3164.7(2) C6C7Fe169.6(3)
C6Fe1C867.8(3) C6C7C8107.7(6)
C6Fe1C2127.6(2) C8C7Fe170.0(3)
C6Fe1C1040.4(2) C30N2C32111.0(5)
C6Fe1C967.5(2) C30N2C31111.0(5)
C8Fe1C3108.5(2) C30N2Li299.3(5)
C5Fe1C141.2(2) C32N2Li2121.2(5)
C5Fe1C7155.8(2) C31N2C32108.5(5)
C5Fe1C6119.6(3) C31N2Li2105.5(4)
C5Fe1C369.2(2) N1C14C2110.0(5)
C5Fe1C8160.0(2) Fe2C19Li1139.2(4)
C5Fe1C268.1(2) Fe2C19Li2103.8(3)
C5Fe1C10105.2(2) C20C19Fe266.3(3)
C5Fe1C440.6(2) C20C19C18102.3(5)
C5Fe1C9122.4(3) C20C19Li1105.8(4)
C2Fe1C141.0(2) C20C19Li2154.7(5)
C2Fe1C7111.4(2) C18C19Fe267.4(3)
C2Fe1C341.1(2) C18C19Li1148.0(5)
C2Fe1C8124.0(2) C18C19Li294.2(4)
C2Fe1C9157.4(3) Li2C19Li165.5(4)
C10Fe1C1123.4(3) C19C20Fe273.3(3)
C10Fe1C767.7(2) C19C20C21111.7(5)
C10Fe1C3153.5(2) C21C20Fe268.4(3)
C10Fe1C867.6(3) C19C18Fe272.0(3)
C10Fe1C2162.5(2) C19C18C30124.7(5)
C10Fe1C939.9(2) C30C18Fe2125.6(4)
C4Fe1C168.7(2) C17C18Fe269.2(3)
C4Fe1C7163.2(3) C17C18C19113.3(5)
C4Fe1C6154.3(3) C17C18C30121.9(5)
C4Fe1C340.1(2) N2C30C18112.0(5)
C4Fe1C8125.1(3) Si2C17Fe2128.5(3)
C4Fe1C267.1(2) C18C17Fe269.8(3)
C4Fe1C10119.1(3) C18C17Si2131.2(4)
C4Fe1C9106.8(2) C21C17Fe267.7(3)
C9Fe1C3120.0(2) C21C17Si2124.1(4)
C9Fe1C840.3(2) C21C17C18104.6(5)
C20Fe2C1940.4(2) C7C6Fe170.3(3)
C20Fe2C1866.7(2) C7C6C10108.4(6)
C20Fe2C1769.7(2) C10C6Fe170.1(3)
C20Fe2C26122.4(2) Fe1C3Li1145.9(4)
C20Fe2C22159.9(3) C2C3Fe166.5(3)
C20Fe2C24120.5(2) C2C3Li199.7(4)
C18Fe2C1940.6(2) C2C3Li2120.4(5)
C17Fe2C1970.7(2) C4C3Fe166.4(3)
C17Fe2C1841.0(2) C4C3C2102.2(5)
C21Fe2C1970.2(2) C4C3Li1147.1(5)
C21Fe2C2041.8(2) C4C3Li2119.8(5)
C21Fe2C1868.1(2) Li2C3Fe192.4(4)
C21Fe2C1741.5(2) Li2C3Li167.1(4)
C21Fe2C26106.1(2) C20C21Fe269.8(3)
C21Fe2C23160.2(3) C17C21Fe270.8(3)
C21Fe2C25120.7(2) C17C21C20108.0(5)
C21Fe2C22123.5(3) C7C8Fe169.3(3)
C21Fe2C24156.6(2) C9C8Fe169.5(3)
C26Fe2C19157.4(2) C9C8C7107.2(6)
C26Fe2C18160.2(2) C25C26Fe269.4(4)
C26Fe2C17122.2(2) C25C26C22106.8(6)
C23Fe2C19122.8(2) C22C26Fe269.3(3)
C23Fe2C20157.5(3) C22C23Fe270.4(4)
C23Fe2C18110.8(2) C22C23C24109.0(6)
C23Fe2C17124.3(2) C24C23Fe270.0(3)
C23Fe2C2667.8(3) C1C5Fe170.0(3)
C23Fe2C2567.6(3) C4C5Fe169.7(3)
C23Fe2C2239.8(3) C4C5C1108.0(5)
C23Fe2C2440.8(2) C1C2Fe169.6(3)
C25Fe2C19121.8(3) C1C2C14127.8(5)
C25Fe2C20106.5(2) C1C2C3111.9(5)
C25Fe2C18159.7(3) C14C2Fe1129.1(4)
C25Fe2C17157.1(3) C3C2Fe172.4(3)
C25Fe2C2639.7(2) C3C2C14120.2(5)
C25Fe2C2267.1(3) C6C10Fe169.5(3)
C25Fe2C2440.8(2) C9C10Fe170.2(3)
C22Fe2C19159.4(3) C9C10C6108.2(6)
C22Fe2C18125.6(2) C26C25Fe270.9(3)
C22Fe2C17108.4(2) C26C25C24110.1(6)
C22Fe2C2640.6(2) C24C25Fe270.0(3)
C22Fe2C2468.0(3) C3C4Fe173.4(3)
C24Fe2C19105.6(2) C5C4Fe169.7(3)
C24Fe2C18124.5(2) C5C4C3112.6(5)
C24Fe2C17160.6(2) C26C22Fe270.1(3)
C24Fe2C2668.4(3) C23C22Fe269.8(4)
C17Si2C29113.5(3) C23C22C26108.6(6)
C17Si2C27109.9(3) C23C24Fe269.2(3)
C17Si2C28108.2(3) C25C24Fe269.3(3)
C27Si2C29105.7(3) C25C24C23105.5(6)
C28Si2C29109.9(3) O1C33C34112.8(6)
C28Si2C27109.7(3) C8C9Fe170.2(3)
C1Si1C12112.8(3) C10C9Fe169.9(3)
C1Si1C13106.8(3) C10C9C8108.5(6)
C1Si1C11110.4(3) N1Li1C19116.5(5)
C12Si1C13111.0(3) N1Li1C386.7(4)
C11Si1C12106.5(3) O1Li1N1111.4(5)
C11Si1C13109.4(3) O1Li1C19120.5(5)
C14N1Li1100.7(4) O1Li1C3107.2(5)
C16N1C14108.2(4) C3Li1C19108.5(4)
C16N1Li1118.2(5) O1C35C36112.1(7)
C15N1C14110.7(5) N2Li2C1988.7(4)
C15N1C16108.5(4) N2Li2C3126.0(6)
C15N1Li1110.3(4) C3Li2C19117.8(5)

 

Table 6 Torsion Angles for 3207_twin1_hklf4.
ABCDAngle/˚ ABCDAngle/˚
Fe1C1C5C4-59.6(4) C6C10C9C80.4(7)
Fe1C1C2C14-124.2(6) C13Si1C1Fe1-70.4(4)
Fe1C1C2C360.1(4) C13Si1C1C517.2(5)
Fe1C7C6C1060.0(4) C13Si1C1C2-163.9(5)
Fe1C7C8C9-59.5(4) C8C7C6Fe1-59.9(4)
Fe1C6C10C959.8(4) C8C7C6C100.1(7)
Fe1C3C2C1-58.5(4) C26C25C24Fe2-59.7(4)
Fe1C3C2C14125.5(5) C26C25C24C230.3(7)
Fe1C3C4C559.0(4) C5C1C2Fe1-59.8(4)
Fe1C8C9C10-59.6(4) C5C1C2C14176.0(5)
Fe1C5C4C3-61.1(4) C5C1C2C30.4(6)
Fe1C10C9C859.7(4) C2C1C5Fe160.2(4)
Fe2C19C20C2157.8(4) C2C1C5C40.6(6)
Fe2C19C18C30121.3(5) C2C3C4Fe1-57.4(4)
Fe2C19C18C17-56.8(4) C2C3C4C51.5(6)
Fe2C20C21C1760.8(4) C29Si2C17Fe243.3(5)
Fe2C18C30N2106.5(5) C29Si2C17C18-53.0(6)
Fe2C18C17Si2124.1(5) C29Si2C17C21130.6(5)
Fe2C18C17C21-59.1(3) C32N2C30C18-167.8(5)
Fe2C17C21C20-60.2(4) C25C26C22Fe259.6(4)
Fe2C26C25C2459.1(4) C25C26C22C230.2(7)
Fe2C26C22C23-59.4(4) C31N2C30C1871.5(6)
Fe2C23C22C2659.6(4) C4C3C2Fe157.4(4)
Fe2C23C24C25-60.1(4) C4C3C2C1-1.1(6)
Fe2C25C24C2360.0(4) C4C3C2C14-177.1(5)
Si2C17C21Fe2-122.4(4) C22C26C25Fe2-59.5(4)
Si2C17C21C20177.5(4) C22C26C25C24-0.4(7)
Si1C1C5Fe1-120.7(4) C22C23C24Fe259.9(4)
Si1C1C5C4179.7(4) C22C23C24C25-0.2(7)
Si1C1C2Fe1121.2(5) C24C23C22Fe2-59.6(4)
Si1C1C2C14-3.1(9) C24C23C22C260.0(7)
Si1C1C2C3-178.7(4) C27Si2C17Fe2161.4(4)
N1C14C2Fe1143.6(4) C27Si2C17C1865.0(6)
N1C14C2C1-123.0(6) C27Si2C17C21-111.3(5)
N1C14C2C352.3(7) C33O1C35C36-169.3(7)
C1C5C4Fe159.7(4) C28Si2C17Fe2-78.9(4)
C1C5C4C3-1.4(7) C28Si2C17C18-175.3(5)
C7C6C10Fe1-60.1(4) C28Si2C17C218.4(5)
C7C6C10C9-0.3(7) Li1N1C14C2-48.0(6)
C7C8C9Fe159.3(4) Li1O1C33C34-114.9(6)
C7C8C9C10-0.3(7) Li1O1C35C3625.4(12)
C19C20C21Fe2-60.6(4) Li1C19C20Fe2137.3(4)
C19C20C21C170.1(6) Li1C19C20C21-165.0(4)
C19C18C30N214.6(8) Li1C19C18Fe2-151.5(8)
C19C18C17Fe258.4(4) Li1C19C18C30-30.2(11)
C19C18C17Si2-177.5(4) Li1C19C18C17151.6(7)
C19C18C17C21-0.7(6) Li1C3C2Fe1-147.4(4)
C16N1C14C2-172.6(5) Li1C3C2C1154.1(5)
C15N1C14C268.7(6) Li1C3C2C14-21.9(6)
C20C19C18Fe257.6(3) Li1C3C4Fe1172.0(9)
C20C19C18C30178.9(5) Li1C3C4C5-129.0(8)
C20C19C18C170.7(6) C11Si1C1Fe1170.7(4)
C18C19C20Fe2-58.3(3) C11Si1C1C5-101.7(5)
C18C19C20C21-0.5(6) C11Si1C1C277.2(6)
C18C17C21Fe260.5(4) C35O1C33C3477.5(8)
C18C17C21C200.3(6) Li2N2C30C18-39.1(6)
C30C18C17Fe2-119.8(5) Li2C19C20Fe271.6(11)
C30C18C17Si24.3(8) Li2C19C20C21129.3(11)
C30C18C17C21-178.9(5) Li2C19C18Fe2-103.2(3)
C12Si1C1Fe151.7(4) Li2C19C18C3018.1(6)
C12Si1C1C5139.3(5) Li2C19C18C17-160.1(5)
C12Si1C1C2-41.8(6) Li2C3C2Fe1-78.3(5)
C17C18C30N2-167.4(5) Li2C3C2C1-136.8(5)
C6C7C8Fe159.6(4) Li2C3C2C1447.2(7)
C6C7C8C90.1(7) Li2C3C4Fe178.6(5)
C6C10C9Fe1-59.4(4) Li2C3C4C5137.6(5)

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for 3207_twin1_hklf4.
AtomxyzU(eq)
H717056225836240
H14A3150(60)3570(60)7660(30)30
H14B2600(60)2440(50)8160(30)30
H16A35452726678755
H16B28731458713355
H16C45001094669355
H15A3967-110793551
H15B5329100820751
H15C5661-484754851
H2057113296611133
H30A7050(60)7320(60)6950(30)37
H30B8800(60)6310(60)6630(30)37
H12A3762791885359
H12B2564093921559
H12C-5322892954659
H613245618952441
H2162775046518331
H13A212032581041374
H13B290415771058974
H13C107822171064774
H842546773803745
H2628747228544545
H2338528238699548
H551562429982832
H29A70779105600778
H29B58949637552078
H29C75559852533078
H32A73077146792864
H32B91176599770164
H32C83475722827764
H1035955788992445
H2522755488634246
H31A102484465727957
H31B92593664705057
H31C93503529777357
H471123073898138
H2238448944585751
H2428826062731841
H27A103676064497577
H27B101956747559977
H27C102257723494377
H33A8899-1097799457
H33B7882314831057
H954026479901546
H34A999010538249116
H34B11037-1877835116
H34C10422-5888549116
H28A60947657455074
H28B77716654430874
H28C74178359423174
H36A981315026309111
H36B830811226260111
H36C99661016008111
H11A3283-554972889
H11B2492-116911689
H11C1463-164978589
H35A9155-9626914114
H35B10512-4037004114

Experimental

Single crystals of C36H58Fe2Li2N2OSi2 [3207_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 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 [3207_twin1_hklf4]

Crystal Data for C36H58Fe2Li2N2OSi2 (=716.60 g/mol): triclinic, space group P-1 (no. 2), a = 9.3542(8) Å, b = 9.9397(8) Å, c = 22.1527(17) Å, α = 79.942(7)°, β = 78.411(7)°, γ = 70.771(7)°, = 1892.0(3) Å3, Z = 2, T = 173.15 K, μ(MoKα) = 0.859 mm-1, Dcalc = 1.258 g/cm3, 8461 reflections measured (4.37° ≤ 2Θ ≤ 51.998°), 8461 unique (Rint = 0.1294, Rsigma = 0.1020) which were used in all calculations. The final R1 was 0.0506 (I > 2σ(I)) and wR2 was 0.1391 (all data).

Refinement model description

Number of restraints - 6, number of constraints - unknown.

Details:

1. Twinned data refinement
Scales: 0.6675(10) 0.3325(10)
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. Uiso/Uaniso restraints and constraints
Uanis(C5) ≈ Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
C33(H33A,H33B), C35(H35A,H35B)
4.b Aromatic/amide H refined with riding coordinates:
C7(H7), C20(H20), C6(H6), C21(H21), C8(H8), C26(H26), C23(H23), C5(H5),
C10(H10), C25(H25), C4(H4), C22(H22), C24(H24), C9(H9)
4.c Idealised Me refined as rotating group:
C16(H16A,H16B,H16C), C15(H15A,H15B,H15C), C12(H12A,H12B,H12C), C13(H13A,H13B,
H13C), C29(H29A,H29B,H29C), C32(H32A,H32B,H32C), C31(H31A,H31B,H31C), C27(H27A,
H27B,H27C), C34(H34A,H34B,H34C), C28(H28A,H28B,H28C), C36(H36A,H36B,H36C),
C11(H11A,H11B,H11C)

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