3160

Table 1 Crystal data and structure refinement for 3160.
Identification code 3160
Empirical formula C17H27FeNO2Si
Formula weight 361.33
Temperature/K 173
Crystal system monoclinic
Space group P21/c
a/Å 12.2692(6)
b/Å 16.7258(6)
c/Å 18.2415(7)
α/° 90
β/° 101.842(4)
γ/° 90
Volume/Å3 3663.7(3)
Z 8
ρcalcg/cm3 1.310
μ/mm‑1 0.895
F(000) 1536.0
Crystal size/mm3 0.095 × 0.082 × 0.04
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.412 to 53.996
Index ranges -15 ≤ h ≤ 15, -21 ≤ k ≤ 21, -23 ≤ l ≤ 23
Reflections collected 74078
Independent reflections 7995 [Rint = 0.0712, Rsigma = 0.0434]
Data/restraints/parameters 7995/4/423
Goodness-of-fit on F2 1.037
Final R indexes [I>=2σ (I)] R1 = 0.0432, wR2 = 0.0861
Final R indexes [all data] R1 = 0.0671, wR2 = 0.0944
Largest diff. peak/hole / e Å-3 0.43/-0.27

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for 3160. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Fe1439.4(3)8174.3(2)3599.7(2)23.46(10)
Si11401.3(5)6179.6(4)3295.0(4)19.60(14)
O11170.2(13)5930.2(9)2404.6(9)21.5(4)
O22688.3(14)6466(1)3557.6(9)25.8(4)
N1-590.2(16)6640.9(13)1598.2(11)26.5(5)
C1342.3(19)6957.7(13)3389.7(13)21.4(5)
C2-342.6(19)7402.4(14)2790.8(13)23.0(5)
C3-1136(2)7851.5(15)3085.5(14)27.6(6)
C4-962(2)7708.3(15)3865.5(14)28.7(6)
C5-66(2)7163.1(14)4053.7(14)25.0(5)
C61442(2)8905.1(15)3135.0(16)34.8(6)
C7575(2)9353.4(15)3352.8(16)36.0(7)
C8670(2)9254.0(15)4131.1(15)35.4(6)
C91585(2)8750.0(15)4405.0(16)34.9(6)
C102065(2)8535.8(16)3790.0(17)36.7(7)
C11-270(2)7414.2(15)1975.1(13)27.6(6)
C12-1707(2)6380.6(18)1667.8(16)40.1(7)
C13-512(2)6695.3(18)809.3(14)39.7(7)
C141267(2)5264.7(14)3875.1(14)26.9(6)
C1549(2)5002.4(17)3759.2(16)39.8(7)
C161737(3)5407.1(16)4710.1(14)38.5(7)
C171958(2)4592.0(15)3612.7(16)37.1(7)
Fe24270.3(3)4867.1(2)1355.7(2)24.52(10)
Si23658.8(6)6911.3(4)1730.8(4)22.22(15)
O33940.7(14)7130.3(10)2626.9(9)25.7(4)
O42331.1(14)6724.7(10)1466.2(10)27.9(4)
N25605.3(17)6274.3(14)3380.6(12)31.8(5)
C184578.1(19)6062.0(14)1590.0(13)23.4(5)
C195232(2)5556.3(14)2157.9(14)25.6(5)
C205919(2)5056.4(16)1810.2(15)32.5(6)
C215696(2)5227.6(16)1030.9(15)32.1(6)
C224883(2)5838.6(15)897.3(14)28.4(6)
C232649(2)4633.8(16)1402.8(18)39.9(7)
C243365(2)4134.6(16)1893.2(17)36.9(7)
C253990(2)3675.5(15)1470.9(16)35.2(7)
C263654(2)3902.1(16)713.1(16)36.5(7)
C272822(2)4501.4(16)669.4(17)40.4(7)
C285194(2)5535.1(16)2979.4(14)31.9(6)
C295526(2)6208(2)4165.7(15)46.8(8)
C306747(2)6462(2)3315.0(18)54.4(9)
C313936(2)7814.4(15)1187.9(14)31.9(6)
C323290(3)8514.3(17)1454.0(17)54.0(9)
C333517(3)7730.4(16)341.9(14)37.6(7)
C345195(3)7989(2)1348.9(18)57.8(10)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for 3160. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Fe123.86(19)20.52(18)25.3(2)-3.21(14)3.47(15)1.66(14)
Si120.1(3)21.3(3)18.7(3)-0.3(3)6.9(3)0.4(3)
O121.8(9)25.4(9)18.3(9)-2.8(7)6.7(7)1.5(7)
O221.3(9)32.5(10)23.9(9)1.4(8)5.2(7)-2.5(7)
N121.6(11)37.2(12)20.4(11)-7.3(9)4.2(9)1.5(9)
C121.7(12)21.1(12)23.5(13)-5.6(10)9.5(10)-3.5(9)
C222.0(13)24.0(12)23.5(13)-4.8(10)6.2(10)0.1(10)
C323.3(13)28.4(13)31.1(14)-5.3(11)5.6(11)3.1(10)
C423.7(13)32.5(14)32.9(15)-11.2(11)13.3(11)0.1(11)
C530.3(14)23.1(12)22.8(13)-1.7(10)8.6(11)-3.1(10)
C636.7(16)28.0(14)40.6(17)0.6(12)9.9(13)-9.0(12)
C740.2(17)21.2(13)43.5(17)2.9(12)1.5(13)-0.4(12)
C844.0(17)22.7(13)37.6(16)-7.4(12)3.9(13)-0.6(12)
C940.6(17)24.9(14)33.8(15)-3.7(11)-5.1(13)-5.1(12)
C1024.5(14)25.6(14)56.7(19)-0.9(13)0.8(13)-4.9(11)
C1129.6(14)28.2(14)25.2(13)2.3(10)6.2(11)3.9(11)
C1225.0(15)53.4(19)41.2(17)-15.6(14)5.4(13)-3.4(13)
C1341.6(17)55.4(19)20.4(14)-3.1(13)2.3(12)7.9(14)
C1434.1(15)25.0(13)24.5(13)0(1)12.6(11)-2.4(11)
C1545.2(18)38.9(17)39.1(17)5.1(13)17.9(14)-9.9(13)
C1652.6(19)37.2(16)25.7(15)7.6(12)8.0(13)2.1(13)
C1748.3(18)25.6(14)40.3(17)5.3(12)16.0(14)5.6(12)
Fe223.9(2)22.78(19)29.1(2)-1.18(15)10.75(15)-1.96(14)
Si224.4(4)22.5(3)20.7(3)1.5(3)6.9(3)-2.7(3)
O329.4(10)27.4(9)21.4(9)0.1(7)7.9(8)0.1(8)
O422.8(9)31.7(10)28.7(10)2.4(8)4.5(8)-1.2(7)
N221.0(11)50.0(14)24.2(12)-3.6(10)3.9(9)0.1(10)
C1822.4(13)23.9(13)25.9(13)-2.3(10)9.3(10)-7.4(10)
C1921.2(13)28.5(13)28.2(14)-2.3(11)7.7(11)-2.1(10)
C2021.5(13)35.9(15)40.9(16)-2.4(12)8.6(12)2.5(11)
C2128.6(14)36.4(15)36.4(16)-8.4(12)18.8(12)-5.2(12)
C2231.9(15)30.5(14)25.6(14)-3.3(11)12.5(11)-10.7(11)
C2324.8(15)26.5(14)72(2)-8.5(14)19.6(15)-7.7(11)
C2443.7(17)29.9(15)42.3(17)-2.7(12)21.0(14)-11.8(13)
C2538.9(16)20.0(13)49.7(18)2.1(12)16.4(14)-1.1(11)
C2644.3(17)31.0(15)38.7(17)-9.9(12)19.0(14)-13.3(13)
C2734.8(16)34.3(16)48.0(19)3.9(13)-1.0(14)-12.7(13)
C2830.8(15)37.6(15)28.2(14)6.7(12)8.1(12)8.3(12)
C2936.5(17)77(2)25.0(15)-1.7(15)1.7(13)12.2(16)
C3028.4(17)86(3)48(2)-22.2(18)8.0(14)-9.3(16)
C3145.5(17)27.2(14)22.7(14)1.6(11)6.6(12)-11.8(12)
C32100(3)25.3(15)36.2(18)2.0(13)12.8(18)1.5(16)
C3354.1(19)31.9(15)26.3(15)5.2(12)7.0(13)-3.4(13)
C3459(2)64(2)45.5(19)15.1(16)-0.6(16)-37.9(18)

 

Table 4 Bond Lengths for 3160.
AtomAtomLength/Å AtomAtomLength/Å
Fe1C12.069(2) Fe2C182.062(2)
Fe1C22.045(2) Fe2C192.038(2)
Fe1C32.040(3) Fe2C202.047(3)
Fe1C42.035(2) Fe2C212.049(2)
Fe1C52.035(2) Fe2C222.040(2)
Fe1C62.038(3) Fe2C232.046(3)
Fe1C72.037(3) Fe2C242.035(3)
Fe1C82.042(3) Fe2C252.041(2)
Fe1C92.053(3) Fe2C262.046(3)
Fe1C102.045(3) Fe2C272.046(3)
Si1O11.6442(16) Si2O31.6414(17)
Si1O21.6253(17) Si2O41.6313(18)
Si1C11.872(2) Si2C181.864(2)
Si1C141.887(2) Si2C311.875(2)
N1C111.479(3) N2C281.472(3)
N1C121.468(3) N2C291.460(3)
N1C131.464(3) N2C301.464(3)
C1C21.441(3) C18C191.446(3)
C1C51.444(3) C18C221.439(3)
C2C31.420(3) C19C201.426(3)
C2C111.509(3) C19C281.509(3)
C3C41.415(4) C20C211.421(4)
C4C51.416(3) C21C221.414(4)
C6C71.423(4) C23C241.395(4)
C6C101.421(4) C23C271.415(4)
C7C81.410(4) C24C251.419(4)
C8C91.411(4) C25C261.411(4)
C9C101.416(4) C26C271.421(4)
C14C151.530(4) C31C321.547(4)
C14C161.533(4) C31C331.530(4)
C14C171.543(3) C31C341.540(4)

 

Table 5 Bond Angles for 3160.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C2Fe1C140.99(9) C19Fe2C1841.29(9)
C2Fe1C9164.44(10) C19Fe2C2040.85(10)
C3Fe1C169.00(10) C19Fe2C2168.82(10)
C3Fe1C240.66(9) C19Fe2C2268.67(10)
C3Fe1C8118.57(11) C19Fe2C23120.13(11)
C3Fe1C9153.91(10) C19Fe2C25124.29(11)
C3Fe1C10162.83(11) C19Fe2C26161.60(11)
C4Fe1C169.40(9) C19Fe2C27155.57(11)
C4Fe1C268.65(9) C20Fe2C1869.05(10)
C4Fe1C340.64(10) C20Fe2C2140.58(11)
C4Fe1C6160.12(11) C21Fe2C1869.14(10)
C4Fe1C7122.33(11) C22Fe2C1841.06(9)
C4Fe1C8105.50(11) C22Fe2C2068.05(11)
C4Fe1C9119.81(11) C22Fe2C2140.45(10)
C4Fe1C10156.26(11) C22Fe2C23127.75(11)
C5Fe1C141.18(9) C22Fe2C25154.71(10)
C5Fe1C268.41(10) C22Fe2C26121.15(10)
C5Fe1C368.18(10) C22Fe2C27109.52(11)
C5Fe1C440.71(10) C23Fe2C18108.32(10)
C5Fe1C6158.11(10) C23Fe2C20154.26(12)
C5Fe1C7160.06(11) C23Fe2C21164.39(12)
C5Fe1C8124.48(10) C24Fe2C18125.33(10)
C5Fe1C9108.64(11) C24Fe2C19106.69(11)
C5Fe1C10123.00(11) C24Fe2C20119.31(12)
C6Fe1C1121.97(10) C24Fe2C21154.01(12)
C6Fe1C2108.20(10) C24Fe2C22163.78(11)
C6Fe1C3124.28(11) C24Fe2C2339.98(11)
C6Fe1C868.30(11) C24Fe2C2540.74(10)
C6Fe1C968.48(11) C24Fe2C2668.11(11)
C6Fe1C1040.73(11) C24Fe2C2767.89(12)
C7Fe1C1156.22(10) C25Fe2C18162.30(11)
C7Fe1C2119.94(11) C25Fe2C20106.43(11)
C7Fe1C3105.50(11) C25Fe2C21119.28(11)
C7Fe1C640.87(11) C25Fe2C2367.89(11)
C7Fe1C840.45(11) C25Fe2C2640.39(11)
C7Fe1C968.23(11) C25Fe2C2768.13(12)
C7Fe1C1068.29(11) C26Fe2C18156.00(11)
C8Fe1C1162.69(10) C26Fe2C20124.90(11)
C8Fe1C2154.11(10) C26Fe2C21107.66(11)
C8Fe1C940.31(10) C26Fe2C2368.02(11)
C8Fe1C1067.82(11) C27Fe2C18121.04(11)
C9Fe1C1126.78(10) C27Fe2C20162.93(11)
C10Fe1C1109.83(10) C27Fe2C21126.64(12)
C10Fe1C2127.30(11) C27Fe2C2340.44(12)
C10Fe1C940.44(11) C27Fe2C2640.65(11)
O1Si1C1106.58(10) O3Si2C18107.31(10)
O1Si1C14109.34(10) O3Si2C31108.80(10)
O2Si1O1109.04(9) O4Si2O3109.32(9)
O2Si1C1114.74(10) O4Si2C18114.15(10)
O2Si1C14105.37(11) O4Si2C31106.03(11)
C1Si1C14111.72(11) C18Si2C31111.14(12)
C12N1C11112.48(19) C29N2C28109.8(2)
C13N1C11109.7(2) C29N2C30110.8(2)
C13N1C12110.7(2) C30N2C28112.0(2)
Si1C1Fe1133.32(12) Si2C18Fe2132.59(12)
C2C1Fe168.61(13) C19C18Fe268.44(13)
C2C1Si1126.64(17) C19C18Si2127.54(18)
C2C1C5105.3(2) C22C18Fe268.65(13)
C5C1Fe168.13(13) C22C18Si2126.35(19)
C5C1Si1127.55(18) C22C18C19105.7(2)
C1C2Fe170.40(13) C18C19Fe270.26(13)
C1C2C11127.7(2) C18C19C28126.9(2)
C3C2Fe169.48(14) C20C19Fe269.93(14)
C3C2C1108.9(2) C20C19C18108.4(2)
C3C2C11123.4(2) C20C19C28124.7(2)
C11C2Fe1126.11(17) C28C19Fe2124.67(17)
C2C3Fe169.86(14) C19C20Fe269.22(14)
C4C3Fe169.48(14) C21C20Fe269.78(15)
C4C3C2108.5(2) C21C20C19108.5(2)
C3C4Fe169.88(14) C20C21Fe269.64(14)
C3C4C5107.6(2) C22C21Fe269.43(14)
C5C4Fe169.64(14) C22C21C20107.6(2)
C1C5Fe170.69(13) C18C22Fe270.30(13)
C4C5Fe169.65(14) C21C22Fe270.12(14)
C4C5C1109.6(2) C21C22C18109.7(2)
C7C6Fe169.54(15) C24C23Fe269.59(15)
C10C6Fe169.90(15) C24C23C27108.4(2)
C10C6C7107.4(3) C27C23Fe269.76(15)
C6C7Fe169.59(15) C23C24Fe270.43(15)
C8C7Fe169.94(15) C23C24C25108.4(3)
C8C7C6107.9(2) C25C24Fe269.83(14)
C7C8Fe169.61(15) C24C25Fe269.43(14)
C7C8C9108.8(3) C26C25Fe270.01(15)
C9C8Fe170.26(14) C26C25C24107.7(3)
C8C9Fe169.43(15) C25C26Fe269.60(15)
C8C9C10107.5(2) C25C26C27107.8(2)
C10C9Fe169.49(15) C27C26Fe269.67(15)
C6C10Fe169.37(15) C23C27Fe269.79(16)
C9C10Fe170.07(15) C23C27C26107.6(3)
C9C10C6108.5(2) C26C27Fe269.68(16)
N1C11C2112.5(2) N2C28C19113.4(2)
C15C14Si1110.50(18) C32C31Si2106.50(18)
C15C14C16109.8(2) C33C31Si2113.51(18)
C15C14C17109.4(2) C33C31C32107.4(2)
C16C14Si1111.91(17) C33C31C34109.0(2)
C16C14C17107.6(2) C34C31Si2109.6(2)
C17C14Si1107.50(16) C34C31C32110.8(2)

 

Table 6 Hydrogen Bonds for 3160.
DHAd(D-H)/Åd(H-A)/Åd(D-A)/ÅD-H-A/°
O1H1N10.931(17)1.716(18)2.634(3)168(3)
O2H2O30.927(17)1.845(18)2.747(2)164(3)
O3H3AN20.944(17)1.697(18)2.638(3)174(3)
O4H4AO10.958(18)1.826(19)2.779(2)173(3)

 

Table 7 Torsion Angles for 3160.
ABCDAngle/˚ ABCDAngle/˚
Fe1C1C2C3-58.96(17) Fe2C18C19C2059.76(17)
Fe1C1C2C11121.0(2) Fe2C18C19C28-119.1(3)
Fe1C1C5C458.94(17) Fe2C18C22C21-59.18(17)
Fe1C2C3C4-58.90(17) Fe2C19C20C2158.90(18)
Fe1C2C11N1160.10(16) Fe2C19C28N2-157.04(17)
Fe1C3C4C5-59.68(17) Fe2C20C21C2259.27(17)
Fe1C4C5C1-59.57(16) Fe2C21C22C1859.29(16)
Fe1C6C7C859.70(18) Fe2C23C24C25-59.75(18)
Fe1C6C10C9-59.37(18) Fe2C23C27C2659.65(18)
Fe1C7C8C959.52(18) Fe2C24C25C26-59.76(18)
Fe1C8C9C1059.28(18) Fe2C25C26C27-59.40(18)
Fe1C9C10C658.94(18) Fe2C26C27C23-59.72(18)
Si1C1C2Fe1-128.82(18) Si2C18C19Fe2127.89(18)
Si1C1C2C3172.21(17) Si2C18C19C20-172.35(18)
Si1C1C2C11-7.8(4) Si2C18C19C288.8(4)
Si1C1C5Fe1128.60(19) Si2C18C22Fe2-127.92(18)
Si1C1C5C4-172.46(17) Si2C18C22C21172.90(18)
O1Si1C1Fe1-109.11(16) O3Si2C18Fe2107.68(17)
O1Si1C1C2-14.7(2) O3Si2C18C1913.3(2)
O1Si1C1C5156.4(2) O3Si2C18C22-158.7(2)
O1Si1C14C15-70.79(19) O3Si2C31C32-52.2(2)
O1Si1C14C16166.45(17) O3Si2C31C33-170.12(19)
O1Si1C14C1748.5(2) O3Si2C31C3467.7(2)
O2Si1C1Fe111.7(2) O4Si2C18Fe2-13.6(2)
O2Si1C1C2106.1(2) O4Si2C18C19-108.0(2)
O2Si1C1C5-82.9(2) O4Si2C18C2280.0(2)
O2Si1C14C15172.15(17) O4Si2C31C3265.3(2)
O2Si1C14C1649.4(2) O4Si2C31C33-52.6(2)
O2Si1C14C17-68.59(19) O4Si2C31C34-174.82(19)
C1Si1C14C1546.9(2) C18Si2C31C32-170.15(19)
C1Si1C14C16-75.8(2) C18Si2C31C3371.9(2)
C1Si1C14C17166.19(17) C18Si2C31C34-50.2(2)
C1C2C3Fe159.53(16) C18C19C20Fe2-59.96(16)
C1C2C3C40.6(3) C18C19C20C21-1.1(3)
C1C2C11N167.9(3) C18C19C28N2-66.7(3)
C2C1C5Fe1-58.82(15) C19C18C22Fe258.66(16)
C2C1C5C40.1(3) C19C18C22C21-0.5(3)
C2C3C4Fe159.13(17) C19C20C21Fe2-58.55(17)
C2C3C4C5-0.5(3) C19C20C21C220.7(3)
C3C2C11N1-112.1(3) C20C19C28N2114.6(3)
C3C4C5Fe159.83(17) C20C21C22Fe2-59.41(17)
C3C4C5C10.3(3) C20C21C22C18-0.1(3)
C5C1C2Fe158.51(15) C22C18C19Fe2-58.79(16)
C5C1C2C3-0.5(3) C22C18C19C201.0(3)
C5C1C2C11179.5(2) C22C18C19C28-177.9(2)
C6C7C8Fe1-59.48(18) C23C24C25Fe260.13(18)
C6C7C8C90.0(3) C23C24C25C260.4(3)
C7C6C10Fe159.70(18) C24C23C27Fe2-59.05(18)
C7C6C10C90.3(3) C24C23C27C260.6(3)
C7C8C9Fe1-59.12(19) C24C25C26Fe259.40(18)
C7C8C9C100.2(3) C24C25C26C270.0(3)
C8C9C10Fe1-59.24(18) C25C26C27Fe259.35(18)
C8C9C10C6-0.3(3) C25C26C27C23-0.4(3)
C10C6C7Fe1-59.93(17) C27C23C24Fe259.16(18)
C10C6C7C8-0.2(3) C27C23C24C25-0.6(3)
C11C2C3Fe1-120.5(2) C28C19C20Fe2118.9(2)
C11C2C3C4-179.4(2) C28C19C20C21177.8(2)
C12N1C11C255.7(3) C29N2C28C19179.2(2)
C13N1C11C2179.5(2) C30N2C28C19-57.3(3)
C14Si1C1Fe1131.52(16) C31Si2C18Fe2-133.48(17)
C14Si1C1C2-134.1(2) C31Si2C18C19132.1(2)
C14Si1C1C537.0(2) C31Si2C18C22-39.9(2)

 

Table 8 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for 3160.
AtomxyzU(eq)
H1513(18)6112(18)2101(15)58(10)
H23010(20)6765(15)3229(14)46(9)
H3-16908191280633
H4-13737937420234
H52236963454230
H615798861264342
H7299664303143
H81969488442342
H918348584491042
H1026988202381244
H11A-7657839171533
H11B5027546193533
H12A-17246303219860
H12B-18905876139760
H12C-22546789145560
H13A-691617556860
H13B246685077560
H13C-1040709855860
H15A-3835415395460
H15B24499402660
H15C-2524926322360
H16A25245558478358
H16B16684916499158
H16C13205838489158
H17A16564472308456
H17B19234112391456
H17C27354765367356
H3A4567(19)6850(16)2892(15)53(9)
H4A1980(30)6420(18)1797(17)78(12)
H2064394674205839
H216032497766638
H224583606742234
H2321335000153948
H2434244107242044
H2545373285166442
H263935369230544
H272449476522748
H28A44175442303138
H28B56495080321738
H29A59815757439770
H29B47486118419870
H29C57956703442970
H30A72406018351782
H30B69946950359782
H30C67726543278782
H32A24968381136781
H32B33938999117481
H32C35728606199081
H33A3899728315656
H33B367182259356
H33C2713763023556
H34A54748027189187
H34B53308495111287
H34C55837556114687

Experimental

Single crystals of C17H27FeNO2Si [3160] were []. A suitable crystal was selected and [] on a Xcalibur, Sapphire3 diffractometer. The crystal was kept at 173 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 [3160]

Crystal Data for C17H27FeNO2Si (=361.33 g/mol): monoclinic, space group P21/c (no. 14), a = 12.2692(6) Å, b = 16.7258(6) Å, c = 18.2415(7) Å, β = 101.842(4)°, = 3663.7(3) Å3, Z = 8, T = 173 K, μ(MoKα) = 0.895 mm-1, Dcalc = 1.310 g/cm3, 74078 reflections measured (4.412° ≤ 2Θ ≤ 53.996°), 7995 unique (Rint = 0.0712, Rsigma = 0.0434) which were used in all calculations. The final R1 was 0.0432 (I > 2σ(I)) and wR2 was 0.0944 (all data).

Refinement model description

Number of restraints - 4, 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. Restrained distances
O4-H4A = O3-H3A = O2-H2 = O1-H1
1 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
C11(H11A,H11B), C28(H28A,H28B)
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), C20(H20),
C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27)
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), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,
H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)

This report has been created with Olex2, compiled on 2017.01.04 svn.r3372 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.