3260_twin1_hklf4

Table 1 Crystal data and structure refinement for 3260_twin1_hklf4.
Identification code 3260_twin1_hklf4
Empirical formula C37H59Fe2N2O5Si2
Formula weight 779.74
Temperature/K 173
Crystal system triclinic
Space group P-1
a/Å 12.4955(17)
b/Å 13.3231(18)
c/Å 14.0840(17)
α/° 64.660(12)
β/° 81.873(11)
γ/° 69.240(13)
Volume/Å3 1981.4(5)
Z 2
ρcalcg/cm3 1.307
μ/mm‑1 0.834
F(000) 830.0
Crystal size/mm3 0.1 × 0.1 × 0.01
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 5.696 to 51.998
Index ranges -15 ≤ h ≤ 15, -13 ≤ k ≤ 16, -12 ≤ l ≤ 17
Reflections collected 15878
Independent reflections 7620 [Rint = 0.1129, Rsigma = 0.3177]
Data/restraints/parameters 7620/6/466
Goodness-of-fit on F2 0.658
Final R indexes [I>=2σ (I)] R1 = 0.0499, wR2 = 0.0646
Final R indexes [all data] R1 = 0.1540, wR2 = 0.0769
Largest diff. peak/hole / e Å-3 0.48/-0.56

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for 3260_twin1_hklf4. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Fe19763.0(5)2585.1(5)9996.1(5)26.9(2)
Si19800.1(10)4340.8(10)7252.7(10)23.9(3)
O110840(2)3178(2)7239(2)30.3(8)
O28791(2)4782(2)6399(2)24.1(8)
N17780(3)2979(3)7422(3)25.7(10)
C19115(3)3892(3)8563(3)20.6(11)
C28559(3)3016(3)8929(3)20.4(11)
C38031(3)2951(3)9919(4)28.9(13)
C48262(3)3771(3)10175(3)28.8(12)
C58915(3)4346(3)9352(4)29.9(13)
C611459(4)1859(4)9775(4)39.9(14)
C711321(4)2260(4)10572(4)41.0(14)
C810680(4)1682(4)11380(4)44.9(15)
C910418(4)905(4)11092(4)42.6(15)
C1010895(4)1014(4)10102(4)33.7(13)
C118561(3)2292(3)8358(4)26.8(12)
C126572(3)3209(3)7740(4)35.6(14)
C138013(4)2296(3)6773(3)35.7(13)
C1410338(4)5610(4)6912(4)26.9(12)
C1511282(4)5253(4)7682(4)47.6(15)
C169361(4)6691(3)6947(3)38.7(14)
C1710825(3)5941(3)5795(3)34.5(13)
Fe24497.8(5)10023.4(5)8123.9(5)27.8(2)
Si23473.9(10)9713.2(10)6055(1)23.1(3)
O34514(2)8727(2)5753(2)24.2(8)
O43484(2)11033(2)5243(2)25.8(8)
N25396(3)6882(3)7486(3)27.4(10)
C183683(3)9374(3)7456(3)23.4(11)
C194596(3)8449(3)8175(4)23.4(12)
C204380(4)8441(4)9196(4)34.5(13)
C213340(4)9364(3)9137(4)30.9(13)
C222900(4)9924(4)8086(4)28.4(13)
C235211(4)11133(4)6928(4)39.0(13)
C246039(4)10279(4)7682(4)40.9(14)
C255716(5)10360(5)8661(4)49.6(15)
C264664(5)11270(5)8503(5)46.5(15)
C274346(4)11768(4)7435(5)49.7(16)
C285660(3)7607(3)7920(3)32.0(13)
C294763(4)6145(3)8241(4)44.2(15)
C306467(3)6166(3)7192(3)36.9(13)
C312078(3)9632(3)5855(4)25.4(12)
C321050(3)10615(3)6015(4)41.4(14)
C332017(4)9758(4)4723(4)49.0(15)
C341938(4)8447(3)6610(4)48.7(16)
O57915(3)6810(3)4525(3)33.9(9)
C355846(5)5504(5)4680(5)60.2(18)
C365932(4)4543(5)4511(4)57.5(17)
C375085(6)4032(4)4817(5)57.7(18)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for 3260_twin1_hklf4. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Fe132.0(4)21.9(4)23.4(5)-7.9(4)2.2(4)-7.5(3)
Si129.8(8)20.6(7)21.3(9)-7.4(7)4.0(7)-11.1(6)
O134.0(18)25.7(17)28(2)-11.9(17)8.9(16)-8.1(15)
O227.6(18)20.3(16)25(2)-5.5(16)4.4(16)-15.0(15)
N125(2)24(2)28(3)-12(2)3(2)-7.8(18)
C115(2)18(3)32(3)-17(2)-3(2)1(2)
C221(3)14(2)22(3)-3(2)0(2)-6(2)
C329(3)30(3)36(3)-16(3)13(2)-19(2)
C433(3)32(3)24(3)-14(3)8(2)-12(2)
C531(3)19(3)36(3)-10(3)5(2)-7(2)
C634(3)34(3)40(4)-13(3)-6(3)1(3)
C742(3)32(3)51(4)-19(3)-14(3)-7(3)
C854(4)38(3)33(4)-13(3)-9(3)-3(3)
C949(3)29(3)29(4)-1(3)-3(3)-2(3)
C1044(3)22(3)26(3)-11(3)-5(3)3(2)
C1128(3)18(3)36(3)-11(3)5(3)-12(2)
C1236(3)35(3)41(4)-16(3)3(3)-18(2)
C1347(3)30(3)35(3)-17(3)2(3)-14(2)
C1433(3)33(3)24(3)-15(3)6(2)-20(2)
C1557(4)54(3)48(4)-23(3)10(3)-37(3)
C1668(4)25(3)31(3)-10(3)14(3)-32(3)
C1739(3)32(3)36(4)-9(3)8(3)-25(2)
Fe233.9(4)28.2(4)25.0(5)-9.0(4)1.6(4)-17.2(3)
Si222.3(7)21.1(7)27.3(9)-9.8(7)1.3(6)-8.9(6)
O320.1(17)20.6(17)26(2)-5.0(17)2.3(15)-6.8(14)
O426.3(18)17.7(16)26(2)-3.2(16)4.1(16)-7.2(14)
N223(2)20(2)32(3)-9(2)6.7(19)-3.7(18)
C1828(3)19(3)23(3)-6(2)1(2)-10(2)
C1920(3)24(3)24(3)-7(3)8(2)-11(2)
C2039(3)30(3)24(3)1(3)3(3)-16(2)
C2135(3)30(3)32(3)-17(3)15(3)-17(2)
C2226(3)26(3)39(4)-17(3)2(3)-13(2)
C2351(3)56(4)26(3)-12(3)6(3)-43(3)
C2433(3)37(3)53(4)-16(3)4(3)-16(3)
C2568(4)63(4)31(4)-9(3)-10(3)-44(3)
C2659(4)60(4)48(4)-31(4)16(3)-46(3)
C2756(4)26(3)62(5)-6(3)2(4)-23(3)
C2831(3)30(3)28(3)-8(3)5(2)-8(2)
C2949(3)29(3)45(4)-7(3)11(3)-16(3)
C3037(3)31(3)38(4)-16(3)-1(3)-2(2)
C3116(3)21(3)44(4)-16(3)9(2)-12(2)
C3227(3)43(3)51(4)-15(3)3(3)-14(2)
C3336(3)64(4)59(4)-34(4)-11(3)-14(3)
C3437(3)35(3)74(5)-18(3)3(3)-19(2)
O544(2)30(2)21(2)-10.2(19)2.5(18)-4.9(17)
C3549(4)50(4)77(5)-5(4)-1(4)-36(3)
C3641(4)58(4)51(4)-8(4)-11(3)-4(3)
C3763(4)34(3)72(5)-7(4)-41(4)-15(3)

 

Table 4 Bond Lengths for 3260_twin1_hklf4.
AtomAtomLength/Å AtomAtomLength/Å
Fe1C12.053(4) Fe2C202.044(4)
Fe1C22.035(4) Fe2C212.036(4)
Fe1C32.051(4) Fe2C222.056(4)
Fe1C42.045(4) Fe2C232.049(4)
Fe1C52.035(4) Fe2C242.039(5)
Fe1C62.035(4) Fe2C252.047(5)
Fe1C72.046(5) Fe2C262.030(5)
Fe1C82.051(5) Fe2C272.047(4)
Fe1C92.041(4) Si2O31.645(3)
Fe1C102.025(4) Si2O41.640(3)
Si1O11.638(3) Si2C181.861(5)
Si1O21.637(3) Si2C311.852(4)
Si1C11.862(4) N2C281.486(5)
Si1C141.888(4) N2C291.463(4)
N1C111.491(5) N2C301.466(4)
N1C121.473(5) C18C191.452(5)
N1C131.484(5) C18C221.444(5)
C1C21.439(5) C19C201.421(6)
C1C51.433(5) C19C281.519(5)
C2C31.436(5) C20C211.421(5)
C2C111.496(5) C21C221.430(6)
C3C41.413(6) C23C241.391(6)
C4C51.419(5) C23C271.430(6)
C6C71.403(6) C24C251.419(6)
C6C101.416(6) C25C261.403(6)
C7C81.400(6) C26C271.411(6)
C8C91.408(6) C31C321.547(5)
C9C101.405(6) C31C331.540(6)
C14C151.521(6) C31C341.537(5)
C14C161.537(5) C35C361.366(6)
C14C171.539(5) C35C3711.368(7)
Fe2C182.065(4) C36C371.377(7)
Fe2C192.027(4) C37C3511.368(7)

11-X,1-Y,1-Z

 

Table 5 Bond Angles for 3260_twin1_hklf4.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C2Fe1C141.22(14) C19Fe2C2168.61(15)
C2Fe1C341.16(15) C19Fe2C2268.48(15)
C2Fe1C468.63(17) C19Fe2C23121.56(18)
C2Fe1C7158.72(19) C19Fe2C24109.20(17)
C2Fe1C8158.18(19) C19Fe2C25126.1(2)
C2Fe1C9121.3(2) C19Fe2C26162.2(2)
C3Fe1C169.54(16) C19Fe2C27156.4(2)
C3Fe1C8123.3(2) C20Fe2C1869.89(18)
C4Fe1C169.38(16) C20Fe2C2268.66(17)
C4Fe1C340.36(15) C20Fe2C23156.31(18)
C4Fe1C7124.94(19) C20Fe2C25107.7(2)
C4Fe1C8109.57(19) C20Fe2C27161.2(2)
C5Fe1C141.05(15) C21Fe2C1869.66(18)
C5Fe1C268.43(17) C21Fe2C2040.75(14)
C5Fe1C368.24(16) C21Fe2C2240.90(16)
C5Fe1C440.70(14) C21Fe2C23162.04(19)
C5Fe1C6123.21(18) C21Fe2C24155.9(2)
C5Fe1C7109.95(18) C21Fe2C25119.9(2)
C5Fe1C8125.4(2) C21Fe2C27124.18(19)
C5Fe1C9160.61(19) C22Fe2C1841.03(14)
C6Fe1C1105.99(17) C23Fe2C18107.28(18)
C6Fe1C2121.57(19) C23Fe2C22125.5(2)
C6Fe1C3158.1(2) C24Fe2C18125.68(19)
C6Fe1C4159.85(19) C24Fe2C20121.73(19)
C6Fe1C740.21(17) C24Fe2C22162.5(2)
C6Fe1C867.82(19) C24Fe2C2339.80(16)
C6Fe1C968.18(18) C24Fe2C2540.66(18)
C7Fe1C1123.38(18) C24Fe2C2767.66(18)
C7Fe1C3159.6(2) C25Fe2C18163.4(2)
C7Fe1C839.96(16) C25Fe2C22154.7(2)
C8Fe1C1160.21(19) C25Fe2C2367.95(19)
C9Fe1C1156.91(19) C25Fe2C2767.8(2)
C9Fe1C3107.10(18) C26Fe2C18154.6(2)
C9Fe1C4123.69(18) C26Fe2C20124.4(2)
C9Fe1C767.47(19) C26Fe2C21106.39(19)
C9Fe1C840.25(17) C26Fe2C22119.71(19)
C10Fe1C1120.63(17) C26Fe2C2368.37(19)
C10Fe1C2105.46(18) C26Fe2C2467.95(19)
C10Fe1C3121.77(19) C26Fe2C2540.26(17)
C10Fe1C4158.51(18) C26Fe2C2740.48(18)
C10Fe1C5158.21(18) C27Fe2C18119.8(2)
C10Fe1C640.82(16) C27Fe2C22107.10(19)
C10Fe1C767.76(19) C27Fe2C2340.86(17)
C10Fe1C867.83(18) O3Si2C18107.39(17)
C10Fe1C940.43(16) O3Si2C31109.38(17)
O1Si1C1107.24(16) O4Si2O3109.28(15)
O1Si1C14111.11(17) O4Si2C18113.54(18)
O2Si1O1111.61(17) O4Si2C31106.34(17)
O2Si1C1105.47(17) C31Si2C18110.9(2)
O2Si1C14107.21(18) C29N2C28111.0(3)
C1Si1C14114.1(2) C29N2C30111.1(3)
C12N1C11111.1(3) C30N2C28109.0(3)
C12N1C13108.4(3) Si2C18Fe2130.9(2)
C13N1C11109.1(3) C19C18Fe267.8(2)
Si1C1Fe1130.95(19) C19C18Si2128.3(3)
C2C1Fe168.7(2) C22C18Fe269.2(2)
C2C1Si1122.7(3) C22C18Si2126.4(3)
C5C1Fe168.8(2) C22C18C19105.0(4)
C5C1Si1131.4(3) C18C19Fe270.6(2)
C5C1C2105.6(4) C18C19C28127.3(4)
C1C2Fe170.1(2) C20C19Fe270.2(3)
C1C2C11124.3(4) C20C19C18110.0(3)
C3C2Fe170.0(3) C20C19C28122.7(4)
C3C2C1109.0(4) C28C19Fe2124.6(3)
C3C2C11126.7(4) C19C20Fe268.9(2)
C11C2Fe1125.3(3) C21C20Fe269.3(2)
C2C3Fe168.8(2) C21C20C19107.4(4)
C4C3Fe169.6(2) C20C21Fe269.9(2)
C4C3C2107.7(4) C20C21C22108.5(4)
C3C4Fe170.0(2) C22C21Fe270.3(2)
C3C4C5108.0(4) C18C22Fe269.8(2)
C5C4Fe169.2(2) C21C22Fe268.8(2)
C1C5Fe170.2(2) C21C22C18109.1(4)
C4C5Fe170.1(2) C24C23Fe269.7(3)
C4C5C1109.7(4) C24C23C27107.5(5)
C7C6Fe170.3(3) C27C23Fe269.5(3)
C7C6C10107.2(4) C23C24Fe270.5(3)
C10C6Fe169.2(2) C23C24C25109.0(4)
C6C7Fe169.5(3) C25C24Fe270.0(3)
C8C7Fe170.2(3) C24C25Fe269.4(3)
C8C7C6108.8(4) C26C25Fe269.3(3)
C7C8Fe169.8(3) C26C25C24107.4(5)
C7C8C9107.9(4) C25C26Fe270.5(3)
C9C8Fe169.5(3) C25C26C27108.5(5)
C8C9Fe170.3(3) C27C26Fe270.4(3)
C10C9Fe169.2(3) C23C27Fe269.6(2)
C10C9C8107.9(5) C26C27Fe269.1(3)
C6C10Fe170.0(2) C26C27C23107.6(4)
C9C10Fe170.4(3) N2C28C19113.1(4)
C9C10C6108.2(5) C32C31Si2112.6(3)
N1C11C2112.3(3) C33C31Si2108.7(3)
C15C14Si1109.7(3) C33C31C32108.2(4)
C15C14C16109.6(4) C34C31Si2111.5(3)
C15C14C17109.0(4) C34C31C32107.6(3)
C16C14Si1110.8(3) C34C31C33108.0(4)
C16C14C17108.5(4) C36C35C371120.0(5)
C17C14Si1109.3(3) C35C36C37121.6(5)
C19Fe2C1841.55(15) C351C37C36118.4(5)
C19Fe2C2040.86(16)     

11-X,1-Y,1-Z

 

Table 6 Hydrogen Bonds for 3260_twin1_hklf4.
DHAd(D-H)/Åd(H-A)/Åd(D-A)/ÅD-H-A/°
O2H2N10.939(18)1.96(2)2.848(4)158(3)
O3H3AN20.991(19)1.67(3)2.630(4)161(5)
O4H4AO310.938(18)1.807(19)2.742(4)175(4)
O5H5AO20.971(19)1.92(2)2.843(4)157(4)
O1H1O520.996(19)1.79(3)2.735(4)158(4)

11-X,2-Y,1-Z; 22-X,1-Y,1-Z

 

Table 7 Torsion Angles for 3260_twin1_hklf4.
ABCDAngle/˚ ABCDAngle/˚
Fe1C1C2C359.4(3) Fe2C18C19C28-119.3(4)
Fe1C1C2C11-119.8(4) Fe2C18C22C21-57.6(3)
Fe1C1C5C4-59.0(3) Fe2C19C20C2158.8(3)
Fe1C2C3C459.0(3) Fe2C19C28N2-150.3(3)
Fe1C2C11N1-163.5(3) Fe2C20C21C2260.0(3)
Fe1C3C4C559.0(3) Fe2C21C22C1858.2(3)
Fe1C4C5C159.1(3) Fe2C23C24C25-59.6(3)
Fe1C6C7C859.4(3) Fe2C23C27C2658.9(3)
Fe1C6C10C9-60.3(3) Fe2C24C25C26-59.1(3)
Fe1C7C8C959.3(3) Fe2C25C26C27-60.4(3)
Fe1C8C9C1059.1(3) Fe2C26C27C23-59.2(3)
Fe1C9C10C660.0(3) Si2C18C19Fe2125.4(3)
Si1C1C2Fe1125.9(3) Si2C18C19C20-175.2(3)
Si1C1C2C3-174.8(3) Si2C18C19C286.2(6)
Si1C1C2C116.1(5) Si2C18C22Fe2-126.2(3)
Si1C1C5Fe1-126.5(3) Si2C18C22C21176.2(3)
Si1C1C5C4174.5(3) O3Si2C18Fe294.7(3)
O1Si1C1Fe127.0(3) O3Si2C18C191.9(4)
O1Si1C1C2-62.3(4) O3Si2C18C22-172.2(3)
O1Si1C1C5124.2(4) O3Si2C31C32-174.3(3)
O1Si1C14C15-57.9(3) O3Si2C31C33-54.4(3)
O1Si1C14C16-179.0(3) O3Si2C31C3464.6(3)
O1Si1C14C1761.6(3) O4Si2C18Fe2-26.2(3)
O2Si1C1Fe1146.0(3) O4Si2C18C19-119.1(4)
O2Si1C1C256.8(3) O4Si2C18C2266.9(4)
O2Si1C1C5-116.7(4) O4Si2C31C32-56.4(4)
O2Si1C14C15179.9(3) O4Si2C31C3363.5(3)
O2Si1C14C1658.8(4) O4Si2C31C34-177.5(3)
O2Si1C14C17-60.6(3) C18Si2C31C3267.5(3)
C1Si1C14C1563.5(3) C18Si2C31C33-172.6(3)
C1Si1C14C16-57.6(4) C18Si2C31C34-53.7(3)
C1Si1C14C17-177.0(3) C18C19C20Fe2-59.6(3)
C1C2C3Fe1-59.4(3) C18C19C20C21-0.7(5)
C1C2C3C4-0.4(5) C18C19C28N2-59.2(5)
C1C2C11N1-74.8(5) C19C18C22Fe258.7(3)
C2C1C5Fe159.2(3) C19C18C22C211.1(4)
C2C1C5C40.1(4) C19C20C21Fe2-58.6(3)
C2C3C4Fe1-58.5(3) C19C20C21C221.4(5)
C2C3C4C50.5(5) C20C19C28N2122.4(4)
C3C2C11N1106.2(5) C20C21C22Fe2-59.8(3)
C3C4C5Fe1-59.5(3) C20C21C22C18-1.6(5)
C3C4C5C1-0.4(5) C22C18C19Fe2-59.6(3)
C5C1C2Fe1-59.2(3) C22C18C19C20-0.2(5)
C5C1C2C30.2(4) C22C18C19C28-178.8(4)
C5C1C2C11-178.9(4) C23C24C25Fe259.9(3)
C6C7C8Fe1-58.9(3) C23C24C25C260.8(6)
C6C7C8C90.4(5) C24C23C27Fe2-59.6(3)
C7C6C10Fe160.3(3) C24C23C27C26-0.7(5)
C7C6C10C90.0(5) C24C25C26Fe259.1(3)
C7C8C9Fe1-59.5(3) C24C25C26C27-1.3(6)
C7C8C9C10-0.4(5) C25C26C27Fe260.5(3)
C8C9C10Fe1-59.8(3) C25C26C27C231.2(6)
C8C9C10C60.2(5) C27C23C24Fe259.5(3)
C10C6C7Fe1-59.6(3) C27C23C24C25-0.1(5)
C10C6C7C8-0.3(5) C28C19C20Fe2119.1(4)
C11C2C3Fe1119.7(4) C28C19C20C21177.9(4)
C11C2C3C4178.7(4) C29N2C28C19-61.4(4)
C12N1C11C2-72.7(4) C30N2C28C19175.8(3)
C13N1C11C2167.8(3) C31Si2C18Fe2-145.9(2)
C14Si1C1Fe1-96.6(3) C31Si2C18C19121.3(4)
C14Si1C1C2174.2(3) C31Si2C18C22-52.7(4)
C14Si1C1C50.7(4) C35C36C37C351-1.4(9)
Fe2C18C19C2059.3(3) C371C35C36C371.4(9)

11-X,1-Y,1-Z

 

Table 8 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for 3260_twin1_hklf4.
AtomxyzU(eq)
H28310(20)4330(20)6600(30)19(12)
H3760424471032835
H4802239121079035
H591804943932736
H6118562109913648
H71161528311056549
H81046017941201154
H999943961149551
H1010847593971840
H11A93491983812832
H11B83241612884432
H12A64143625820153
H12B64222462811753
H12C60773695711553
H13A78971537719453
H13B88062162653153
H13C74912736616453
H15A119104573765071
H15B109775046839671
H15C115665910749871
H16A90846515766858
H16B87346889648458
H16C96437358671058
H17A102216176529352
H17B114545261576152
H17C111116595561752
H3A4850(40)7940(20)6320(30)110(20)
H4A4150(20)11160(30)4880(30)55(16)
H2048457915980541
H2129969574970137
H22220410556784234
H23521911270620847
H2467129729756149
H2561349886930459
H26423811510902856
H27367912409711160
H28A61218065740538
H28B61307080856838
H29A40706641844866
H29B52455580886366
H29C45515719791866
H30A69535634781955
H30B68686680667955
H30C62985704688455
H32A110911384553362
H32B105510530674162
H32C33610553587462
H33A26399118461774
H33B209310515422774
H33C12799721460674
H34A19828344733773
H34B25507809649173
H34C11948432648473
H5A8210(30)6270(30)5230(18)55(17)
H5B7350(30)7470(30)4640(30)78(18)
H3564345851444872
H3665914218417469
H3751473374468169
H111140(40)3130(40)6560(20)87

Experimental

Single crystals of C37H59Fe2N2O5Si2 [3260_twin1_hklf4] 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 [3260_twin1_hklf4]

Crystal Data for C37H59Fe2N2O5Si2 (=779.74 g/mol): triclinic, space group P-1 (no. 2), a = 12.4955(17) Å, b = 13.3231(18) Å, c = 14.0840(17) Å, α = 64.660(12)°, β = 81.873(11)°, γ = 69.240(13)°, = 1981.4(5) Å3, Z = 2, T = 173 K, μ(MoKα) = 0.834 mm-1, Dcalc = 1.307 g/cm3, 15878 reflections measured (5.696° ≤ 2Θ ≤ 51.998°), 7620 unique (Rint = 0.1129, Rsigma = 0.3177) which were used in all calculations. The final R1 was 0.0499 (I > 2σ(I)) and wR2 was 0.0769 (all data).

Refinement model description

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

Details:

1. Fixed Uiso
At 1.2 times of:
All C(H,H) groups, H35 of C35, H7 of C7, H6 of C6, H5 of C5, H4 of C4, H3
of C3, H9 of C9, H8 of C8, H10 of C10, H21 of C21, H20 of C20, H25 of C25,
H24 of C24, H23 of C23, H22 of C22, H26 of C26, H27 of C27, H36 of C36, H37
of C37
At 1.5 times of:
All C(H,H,H) groups, H1 of C37
2. Restrained distances
O4-H4A = O5_$1-H5B_$1
1 with sigma of 0.02
O3-H3A
1 with sigma of 0.02
O2-H2 = O5_$1-H5A_$1 = 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), C35(H35),
C36(H36), C37(H37)
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)

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