3116

Table 1 Crystal data and structure refinement for 3116.
Identification code 3116
Empirical formula C46H52Fe4N2O3Si2
Formula weight 960.47
Temperature/K 150
Crystal system monoclinic
Space group P21/n
a/Å 12.8025(4)
b/Å 18.1923(6)
c/Å 17.9925(7)
α/° 90
β/° 90.855(3)
γ/° 90
Volume/Å3 4190.1(2)
Z 4
ρcalcg/cm3 1.523
μ/mm‑1 1.458
F(000) 1992.0
Crystal size/mm3 0.2 × 0.1 × 0.05
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.478 to 54
Index ranges -16 ≤ h ≤ 16, -23 ≤ k ≤ 23, -22 ≤ l ≤ 22
Reflections collected 31598
Independent reflections 9116 [Rint = 0.0358, Rsigma = 0.0398]
Data/restraints/parameters 9116/0/526
Goodness-of-fit on F2 1.028
Final R indexes [I>=2σ (I)] R1 = 0.0431, wR2 = 0.0946
Final R indexes [all data] R1 = 0.0611, wR2 = 0.1035
Largest diff. peak/hole / e Å-3 0.96/-0.50

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for 3116. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Fe12922.8(4)748.9(2)933.5(3)28.67(11)
Fe2-495.8(3)2297.3(2)-917.7(2)22.57(10)
Fe33517.5(4)4272.7(2)-2583.3(3)29.95(12)
Fe42220.9(4)4702.9(2)637.0(3)30.41(12)
Si12103.4(6)2053.6(4)-348.7(5)21.58(17)
Si23016.0(6)3579.1(4)-849.1(5)21.79(17)
O12339.5(15)2918.2(10)-496.0(11)24.5(4)
O22512.6(17)1536.9(12)-1008.5(13)31.0(5)
O34246.6(17)3459.5(13)-694.4(14)32.2(5)
N15173.6(19)2431.7(14)192.3(16)31.7(6)
N23603(2)1869.8(14)-2251.4(15)34.1(6)
C12725(2)1796.1(15)555.2(16)23.1(6)
C23802(2)1657.8(16)766.6(17)27.7(7)
C33829(3)1468.7(18)1538.8(19)37.4(8)
C42795(3)1471.5(18)1808.6(19)36.5(8)
C52126(3)1679.7(16)1213.3(17)28.4(7)
C62972(8)44(2)83(3)102(3)
C73707(4)-163(2)619(3)68.8(15)
C83193(3)-309.8(18)1269(2)46.8(9)
C92147(3)-201.9(18)1159(3)53.3(11)
C101973(5)16(2)440(4)92(2)
C114723(2)1685.6(17)277.4(19)32.0(7)
C125429(3)2777(2)901(2)51.4(10)
C136122(3)2353(2)-253(3)53.5(11)
C14691(2)2003.1(15)-201.3(16)22.5(6)
C15-46(2)1417.9(16)-293.8(16)24.1(6)
C16-1050(2)1664.2(17)-76.3(17)27.7(7)
C17-955(2)2403.7(17)158.5(17)28.0(7)
C18105(2)2614.3(16)83.0(16)25.2(6)
C19168(3)2532(2)-1913.8(19)45.1(9)
C20-584(3)1976(2)-2003.8(19)43.5(9)
C21-1559(3)2250(2)-1773(2)40.4(8)
C22-1397(3)2984(2)-1537(2)42.3(9)
C23-328(3)3152(2)-1631.4(19)42.3(9)
C242738(2)3611.9(15)-1861.0(16)23.6(6)
C253193(2)3193.0(17)-2457.2(17)29.0(7)
C262769(3)3454.4(19)-3145.9(18)35.5(8)
C272060(3)4032.2(19)-2995.9(18)35.2(8)
C282038(2)4126.4(17)-2214.6(18)29.4(7)
C294794(3)4665(2)-2024(2)42.4(9)
C305095(3)4322(2)-2687(2)47(1)
C314594(3)4693(2)-3285(2)55.3(11)
C323992(3)5268(2)-2993(2)51(1)
C334108(3)5248.1(19)-2206(2)44.5(9)
C344021(3)2612.9(18)-2372.9(18)33.6(7)
C353027(3)1604(2)-2901(2)53.4(10)
C364470(3)1364(2)-2080(2)46.4(9)
C372587(2)4462.1(16)-449.0(18)29.1(7)
C381547(3)4750(2)-393(2)43.5(9)
C391588(5)5457(2)-73(3)68.9(15)
C402628(5)5624(2)68(3)78.0(19)
C413254(4)5016(2)-155(2)55.3(12)
C422224(4)3757(2)1236(2)56.4(12)
C431263(4)4118(2)1304(2)53.8(11)
C441455(3)4817(2)1619(2)46.1(9)
C452539(3)4878(2)1737(2)47.4(10)
C463019(4)4228(2)1502(2)57.2(11)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for 3116. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Fe136.5(3)19.7(2)29.7(3)0.69(18)-3.15(19)-2.79(18)
Fe221.4(2)25.8(2)20.4(2)-0.90(17)-0.71(16)0.99(17)
Fe331.7(2)32.3(2)25.9(2)8.87(19)2.96(18)-4.51(19)
Fe437.1(3)23.9(2)30.4(3)-5.59(18)6.3(2)-3.63(19)
Si119.9(4)20.4(4)24.5(4)-0.1(3)0.2(3)-1.2(3)
Si224.0(4)20.1(4)21.3(4)1.6(3)3.2(3)-1.6(3)
O129.2(11)22.7(10)21.7(11)3.0(8)2.2(8)-3.1(8)
O238.4(12)29.6(11)25.1(12)-2.6(9)3.8(10)-0.4(10)
O327.8(12)35.1(13)33.7(14)9.3(11)-0.4(10)-0.7(10)
N121.3(13)32.5(14)41.1(17)2.6(12)-4.9(11)-4.5(11)
N242.5(16)31.5(14)28.6(15)-1.5(11)6.4(12)6.8(12)
C127.8(15)19.9(13)21.7(15)-1.9(11)0.0(12)-1.2(12)
C233.3(16)21.7(14)27.8(17)-0.9(12)-6.6(13)-1.6(12)
C347(2)33.4(17)30.9(19)0.3(14)-14.6(15)-5.1(15)
C453(2)35.1(18)21.6(17)1.4(14)-2.2(15)-4.6(16)
C534.4(17)27.0(15)23.7(16)-3.0(12)2.6(13)-4.6(13)
C6253(9)23(2)29(3)-5.3(18)9(4)-25(4)
C774(3)35(2)98(4)-18(2)42(3)-4(2)
C864(3)26.3(17)50(2)6.7(16)-5(2)7.7(17)
C948(2)22.0(17)90(4)3.9(19)14(2)-2.1(16)
C10117(5)18.2(19)139(6)-5(3)-85(4)-7(2)
C1126.2(16)28.9(16)41(2)-1.4(14)-6.3(14)1.1(13)
C1251(2)45(2)58(3)-4.7(19)-16.5(19)-10.4(18)
C1326.3(18)48(2)86(3)-2(2)8.0(19)-2.4(17)
C1423.1(14)23.9(14)20.4(15)-0.5(11)-2.5(11)-0.5(11)
C1524.8(15)23.4(14)24.1(16)1.1(12)0.6(12)0.2(12)
C1623.1(15)31.1(16)28.8(17)3.3(13)2.0(12)-3.1(12)
C1727.4(15)33.3(16)23.3(16)-1.1(13)5.6(12)3.7(13)
C1830.2(15)24.3(14)21.0(15)-2.3(12)-1.4(12)-1.2(12)
C1938.4(19)75(3)21.7(18)8.7(18)3.4(14)4.6(19)
C2060(2)48(2)22.3(18)-4.5(15)-7.1(16)15.8(19)
C2135.9(18)53(2)32.0(19)2.5(16)-13.2(15)-1.5(17)
C2250(2)47(2)29.2(19)4.9(16)-9.0(16)19.9(17)
C2356(2)42(2)28.2(19)15.2(15)-5.9(16)-9.6(17)
C2424.1(14)23.8(14)22.9(16)5.9(12)1.8(12)-2.3(12)
C2530.8(16)31.3(16)25.1(16)1.2(13)3.5(13)-6.9(13)
C2642.2(19)44.0(19)20.5(17)0.5(14)3.1(14)-7.1(16)
C2735.4(18)44.0(19)26.1(18)11.5(15)-4.9(14)-6.2(15)
C2826.4(15)32.2(16)29.5(17)7.3(13)0.1(13)-1.9(13)
C2929.8(17)46(2)51(2)12.3(18)-4.2(16)-13.6(16)
C3029.9(18)52(2)60(3)5.5(19)14.0(17)-6.5(17)
C3152(2)70(3)45(2)13(2)15.5(19)-24(2)
C3254(2)42(2)57(3)24.3(19)-4(2)-14.5(18)
C3343(2)32.7(18)57(3)4.4(17)3.6(18)-10.9(16)
C3434.3(17)41.2(18)25.4(17)-2.6(14)8.1(13)2.9(15)
C3571(3)43(2)46(2)-8.7(18)-4(2)-7(2)
C3652(2)43(2)45(2)0.5(17)14.8(18)17.6(18)
C3737.0(17)23.0(14)27.4(17)1.6(12)10.3(13)-2.0(13)
C3851(2)50(2)30(2)7.0(16)5.4(16)19.8(18)
C39112(4)41(2)54(3)15(2)39(3)35(3)
C40139(5)20.7(18)77(4)-7.9(19)64(4)-18(2)
C4166(3)38(2)63(3)-15.8(19)35(2)-26.1(19)
C42119(4)28.4(18)22.3(19)1.2(14)0(2)-4(2)
C4371(3)64(3)27(2)-5.2(18)11.8(19)-31(2)
C4453(2)55(2)30(2)-8.8(17)9.5(17)-0.9(19)
C4561(2)45(2)37(2)-21.9(17)-4.6(18)-4.5(18)
C4668(3)60(3)43(2)-14(2)-15(2)19(2)

 

Table 4 Bond Lengths for 3116.
AtomAtomLength/Å AtomAtomLength/Å
Fe1C12.038(3) N1C111.484(4)
Fe1C22.025(3) N1C121.454(5)
Fe1C32.052(3) N1C131.472(4)
Fe1C42.060(3) N2C341.472(4)
Fe1C52.044(3) N2C351.456(5)
Fe1C61.998(4) N2C361.471(4)
Fe1C72.024(4) C1C21.446(4)
Fe1C82.046(3) C1C51.437(4)
Fe1C92.038(4) C2C31.431(4)
Fe1C102.002(4) C2C111.483(4)
Fe2C142.048(3) C3C41.418(5)
Fe2C152.033(3) C4C51.413(5)
Fe2C162.038(3) C6C71.389(8)
Fe2C172.041(3) C6C101.440(9)
Fe2C182.031(3) C7C81.377(6)
Fe2C192.040(3) C8C91.364(5)
Fe2C202.041(3) C9C101.368(7)
Fe2C212.042(3) C14C151.430(4)
Fe2C222.024(3) C14C181.439(4)
Fe2C232.030(3) C15C161.422(4)
Fe3C242.042(3) C16C171.415(4)
Fe3C252.021(3) C17C181.418(4)
Fe3C262.032(3) C19C201.404(5)
Fe3C272.045(3) C19C231.394(5)
Fe3C282.034(3) C20C211.412(5)
Fe3C292.036(4) C21C221.417(5)
Fe3C302.033(3) C22C231.414(5)
Fe3C312.033(3) C24C251.445(4)
Fe3C322.050(3) C24C281.438(4)
Fe3C332.041(4) C25C261.427(5)
Fe4C372.063(3) C25C341.502(4)
Fe4C382.035(4) C26C271.417(5)
Fe4C392.035(4) C27C281.417(5)
Fe4C402.035(4) C29C301.405(5)
Fe4C412.040(4) C29C331.412(5)
Fe4C422.031(4) C30C311.416(6)
Fe4C432.029(4) C31C321.406(6)
Fe4C442.043(3) C32C331.422(6)
Fe4C452.039(4) C37C381.436(5)
Fe4C462.040(4) C37C411.418(5)
Si1O11.624(2) C38C391.410(6)
Si1O21.608(2) C39C401.386(8)
Si1C11.860(3) C40C411.427(6)
Si1C141.834(3) C42C431.401(6)
Si2O11.617(2) C42C461.409(6)
Si2O31.611(2) C43C441.412(5)
Si2C241.851(3) C44C451.406(5)
Si2C371.847(3) C45C461.401(5)

 

Table 5 Bond Angles for 3116.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C1Fe1C369.33(13) C43Fe4C4440.57(15)
C1Fe1C469.37(12) C43Fe4C4567.83(16)
C1Fe1C541.22(11) C43Fe4C4668.11(19)
C1Fe1C8176.53(14) C44Fe4C37163.52(15)
C1Fe1C9143.29(15) C45Fe4C37155.09(15)
C2Fe1C141.70(12) C45Fe4C41120.77(17)
C2Fe1C341.10(13) C45Fe4C4440.28(15)
C2Fe1C469.08(13) C45Fe4C4640.17(15)
C2Fe1C568.94(12) C46Fe4C37120.93(15)
C2Fe1C8136.10(15) C46Fe4C4467.97(17)
C2Fe1C9174.80(16) O1Si1C1107.95(12)
C3Fe1C440.34(14) O1Si1C14104.97(12)
C5Fe1C367.74(13) O2Si1O1112.47(12)
C5Fe1C440.29(13) O2Si1C1110.99(13)
C5Fe1C8142.19(14) O2Si1C14114.22(13)
C6Fe1C1110.46(17) C14Si1C1105.74(13)
C6Fe1C2112.8(2) O1Si2C24108.32(12)
C6Fe1C3142.4(3) O1Si2C37109.24(12)
C6Fe1C4177.2(3) O3Si2O1111.09(12)
C6Fe1C5137.9(3) O3Si2C24110.33(13)
C6Fe1C740.4(2) O3Si2C37110.22(14)
C6Fe1C867.32(19) C37Si2C24107.55(14)
C6Fe1C968.2(2) Si2O1Si1152.38(14)
C6Fe1C1042.2(3) C12N1C11112.8(3)
C7Fe1C1137.07(17) C12N1C13110.0(3)
C7Fe1C2110.39(15) C13N1C11107.0(3)
C7Fe1C3113.09(19) C35N2C34111.5(3)
C7Fe1C4141.5(2) C35N2C36109.4(3)
C7Fe1C5178.0(2) C36N2C34109.3(3)
C7Fe1C839.55(17) Si1C1Fe1125.23(15)
C7Fe1C966.78(17) C2C1Fe168.68(16)
C8Fe1C3110.64(15) C2C1Si1131.9(2)
C8Fe1C4112.99(15) C5C1Fe169.63(17)
C9Fe1C3135.17(18) C5C1Si1122.0(2)
C9Fe1C4110.17(16) C5C1C2106.1(3)
C9Fe1C5114.05(14) C1C2Fe169.62(16)
C9Fe1C839.03(16) C1C2C11126.9(3)
C10Fe1C1113.75(16) C3C2Fe170.46(18)
C10Fe1C2144.4(2) C3C2C1107.9(3)
C10Fe1C3174.2(3) C3C2C11125.2(3)
C10Fe1C4135.2(3) C11C2Fe1124.4(2)
C10Fe1C5111.0(2) C2C3Fe168.44(18)
C10Fe1C768.4(2) C4C3Fe170.13(19)
C10Fe1C866.60(18) C4C3C2108.8(3)
C10Fe1C939.6(2) C3C4Fe169.54(19)
C15Fe2C1441.02(11) C5C4Fe169.26(18)
C15Fe2C1640.89(11) C5C4C3107.5(3)
C15Fe2C1768.53(12) C1C5Fe169.15(16)
C15Fe2C19122.10(14) C4C5Fe170.45(19)
C15Fe2C20108.32(13) C4C5C1109.8(3)
C15Fe2C21124.28(14) C7C6Fe170.8(3)
C16Fe2C1469.39(12) C7C6C10106.2(4)
C16Fe2C1740.59(12) C10C6Fe169.1(3)
C16Fe2C19157.67(15) C6C7Fe168.8(3)
C16Fe2C20122.30(15) C8C7Fe171.1(2)
C16Fe2C21107.49(14) C8C7C6108.3(5)
C17Fe2C1469.46(12) C7C8Fe169.4(2)
C17Fe2C21121.43(14) C9C8Fe170.2(2)
C18Fe2C1441.31(11) C9C8C7109.3(4)
C18Fe2C1568.49(12) C8C9Fe170.8(2)
C18Fe2C1668.49(12) C8C9C10108.9(4)
C18Fe2C1740.77(12) C10C9Fe168.8(2)
C18Fe2C19124.21(14) C6C10Fe168.7(3)
C18Fe2C20160.87(14) C9C10Fe171.6(3)
C18Fe2C21156.94(13) C9C10C6107.4(5)
C19Fe2C14107.02(13) C2C11N1114.0(3)
C19Fe2C17160.59(15) Si1C14Fe2128.27(16)
C19Fe2C2040.24(15) C15C14Fe268.90(16)
C19Fe2C2168.17(15) C15C14Si1132.1(2)
C20Fe2C14123.87(13) C15C14C18105.7(2)
C20Fe2C17157.35(15) C18C14Fe268.69(16)
C20Fe2C2140.47(14) C18C14Si1122.2(2)
C21Fe2C14160.58(13) C14C15Fe270.08(16)
C22Fe2C14156.78(14) C16C15Fe269.76(17)
C22Fe2C15160.84(14) C16C15C14109.3(3)
C22Fe2C16123.80(14) C15C16Fe269.35(16)
C22Fe2C17107.12(14) C17C16Fe269.82(17)
C22Fe2C18121.21(14) C17C16C15107.9(3)
C22Fe2C1968.18(15) C16C17Fe269.59(17)
C22Fe2C2068.08(15) C16C17C18107.8(3)
C22Fe2C2140.79(15) C18C17Fe269.23(17)
C22Fe2C2340.83(15) C14C18Fe270.00(17)
C23Fe2C14120.92(13) C17C18Fe270.01(17)
C23Fe2C15156.97(14) C17C18C14109.2(3)
C23Fe2C16160.74(14) C20C19Fe269.9(2)
C23Fe2C17124.21(14) C23C19Fe269.6(2)
C23Fe2C18107.53(14) C23C19C20108.0(3)
C23Fe2C1940.05(15) C19C20Fe269.8(2)
C23Fe2C2067.57(16) C19C20C21108.6(3)
C23Fe2C2168.35(15) C21C20Fe269.8(2)
C24Fe3C2769.71(12) C20C21Fe269.75(19)
C24Fe3C32154.04(15) C20C21C22107.1(3)
C25Fe3C2441.68(12) C22C21Fe268.95(19)
C25Fe3C2641.22(13) C21C22Fe270.26(19)
C25Fe3C2769.20(13) C23C22Fe269.78(19)
C25Fe3C2869.03(12) C23C22C21107.8(3)
C25Fe3C29116.77(14) C19C23Fe270.4(2)
C25Fe3C30105.02(15) C19C23C22108.5(3)
C25Fe3C31125.27(16) C22C23Fe269.38(19)
C25Fe3C32163.94(16) Si2C24Fe3123.83(15)
C25Fe3C33152.04(15) C25C24Fe368.41(16)
C26Fe3C2469.79(12) C25C24Si2129.8(2)
C26Fe3C2740.68(14) C28C24Fe369.06(16)
C26Fe3C2868.42(13) C28C24Si2124.4(2)
C26Fe3C29150.71(15) C28C24C25105.7(3)
C26Fe3C30116.62(15) C24C25Fe369.92(17)
C26Fe3C31106.55(16) C24C25C34125.9(3)
C26Fe3C32127.42(16) C26C25Fe369.80(19)
C26Fe3C33166.44(15) C26C25C24108.5(3)
C27Fe3C32109.38(15) C26C25C34125.5(3)
C28Fe3C2441.32(11) C34C25Fe3123.2(2)
C28Fe3C2740.65(13) C25C26Fe368.98(18)
C28Fe3C29129.02(15) C27C26Fe370.1(2)
C28Fe3C32121.01(15) C27C26C25108.6(3)
C28Fe3C33110.35(14) C26C27Fe369.17(19)
C29Fe3C24106.76(14) C28C27Fe369.25(18)
C29Fe3C27167.38(15) C28C27C26107.5(3)
C29Fe3C3268.16(16) C24C28Fe369.62(16)
C29Fe3C3340.52(15) C27C28Fe370.10(18)
C30Fe3C24125.43(14) C27C28C24109.8(3)
C30Fe3C27151.44(16) C30C29Fe369.7(2)
C30Fe3C28165.24(15) C30C29C33108.3(4)
C30Fe3C2940.41(16) C33C29Fe369.9(2)
C30Fe3C3268.18(16) C29C30Fe369.9(2)
C30Fe3C3368.19(16) C29C30C31107.9(4)
C31Fe3C24163.59(16) C31C30Fe369.6(2)
C31Fe3C27118.58(16) C30C31Fe369.6(2)
C31Fe3C28153.58(16) C32C31Fe370.5(2)
C31Fe3C2968.17(17) C32C31C30108.3(4)
C31Fe3C3040.76(17) C31C32Fe369.2(2)
C31Fe3C3240.30(17) C31C32C33107.7(4)
C31Fe3C3368.19(17) C33C32Fe369.3(2)
C33Fe3C24118.84(14) C29C33Fe369.6(2)
C33Fe3C27129.67(15) C29C33C32107.8(4)
C33Fe3C3240.69(16) C32C33Fe370.0(2)
C38Fe4C3741.03(13) N2C34C25113.7(3)
C38Fe4C3940.54(17) Si2C37Fe4128.82(16)
C38Fe4C4167.81(18) C38C37Fe468.42(19)
C38Fe4C44125.51(16) C38C37Si2128.8(3)
C38Fe4C45162.39(15) C41C37Fe468.9(2)
C38Fe4C46155.97(15) C41C37Si2125.6(3)
C39Fe4C3769.08(14) C41C37C38105.6(3)
C39Fe4C4168.3(2) C37C38Fe470.6(2)
C39Fe4C44106.40(17) C39C38Fe469.7(3)
C39Fe4C45125.12(17) C39C38C37109.4(4)
C39Fe4C46162.6(2) C38C39Fe469.7(2)
C40Fe4C3768.60(15) C40C39Fe470.1(3)
C40Fe4C3867.4(2) C40C39C38107.7(4)
C40Fe4C3939.8(2) C39C40Fe470.1(2)
C40Fe4C4141.00(17) C39C40C41108.8(4)
C40Fe4C44118.75(16) C41C40Fe469.7(2)
C40Fe4C45108.05(19) C37C41Fe470.68(19)
C40Fe4C46127.1(2) C37C41C40108.5(4)
C41Fe4C3740.42(14) C40C41Fe469.3(2)
C41Fe4C44154.17(15) C43C42Fe469.8(2)
C41Fe4C46109.2(2) C43C42C46108.4(3)
C42Fe4C37108.89(14) C46C42Fe470.1(2)
C42Fe4C38121.11(16) C42C43Fe469.9(2)
C42Fe4C39154.5(2) C42C43C44108.0(4)
C42Fe4C40165.0(2) C44C43Fe470.2(2)
C42Fe4C41127.67(19) C43C44Fe469.2(2)
C42Fe4C4467.94(16) C45C44Fe469.7(2)
C42Fe4C4567.62(16) C45C44C43107.3(4)
C42Fe4C4640.50(17) C44C45Fe470.0(2)
C43Fe4C37126.60(14) C46C45Fe470.0(2)
C43Fe4C38108.00(17) C46C45C44108.8(3)
C43Fe4C39119.1(2) C42C46Fe469.4(2)
C43Fe4C40152.9(2) C45C46Fe469.9(2)
C43Fe4C41164.37(16) C45C46C42107.4(4)
C43Fe4C4240.38(18)     

 

Table 6 Hydrogen Bonds for 3116.
DHAd(D-H)/Åd(H-A)/Åd(D-A)/ÅD-H-A/°
O2H2N20.95(5)2.10(5)2.722(3)122(4)
O3H3N10.73(4)2.01(4)2.719(4)167(4)

 

Table 7 Torsion Angles for 3116.
ABCDAngle/˚ ABCDAngle/˚
Fe1C1C2C3-60.3(2) C3C2C11N1-96.3(4)
Fe1C1C2C11118.3(3) C3C4C5Fe159.3(2)
Fe1C1C5C458.8(2) C3C4C5C11.2(4)
Fe1C2C3C4-58.6(2) C5C1C2Fe159.93(19)
Fe1C2C11N1174.5(2) C5C1C2C3-0.4(3)
Fe1C3C4C5-59.1(2) C5C1C2C11178.2(3)
Fe1C4C5C1-58.0(2) C6C7C8Fe1-58.9(3)
Fe1C6C7C860.4(3) C6C7C8C90.0(5)
Fe1C6C10C9-61.6(3) C7C6C10Fe161.5(3)
Fe1C7C8C959.0(3) C7C6C10C9-0.1(5)
Fe1C8C9C1058.4(3) C7C8C9Fe1-58.5(3)
Fe1C9C10C659.7(3) C7C8C9C10-0.1(4)
Fe2C14C15C16-58.9(2) C8C9C10Fe1-59.6(3)
Fe2C14C18C1759.2(2) C8C9C10C60.1(5)
Fe2C15C16C17-59.4(2) C10C6C7Fe1-60.4(3)
Fe2C16C17C18-58.8(2) C10C6C7C80.0(5)
Fe2C17C18C14-59.2(2) C11C2C3Fe1-118.9(3)
Fe2C19C20C2159.2(2) C11C2C3C4-177.5(3)
Fe2C19C23C22-59.1(2) C12N1C11C254.2(4)
Fe2C20C21C2259.1(2) C13N1C11C2175.4(3)
Fe2C21C22C2360.0(2) C14Si1O1Si2-153.3(3)
Fe2C22C23C1959.8(2) C14Si1C1Fe180.19(19)
Fe3C24C25C26-59.4(2) C14Si1C1C2172.2(3)
Fe3C24C25C34117.1(3) C14Si1C1C5-6.3(3)
Fe3C24C28C2758.7(2) C14C15C16Fe259.1(2)
Fe3C25C26C27-59.2(2) C14C15C16C17-0.3(3)
Fe3C25C34N2177.1(2) C15C14C18Fe2-59.3(2)
Fe3C26C27C28-58.8(2) C15C14C18C17-0.1(3)
Fe3C27C28C24-58.4(2) C15C16C17Fe259.1(2)
Fe3C29C30C3159.5(3) C15C16C17C180.2(3)
Fe3C29C33C32-59.8(2) C16C17C18Fe259.1(2)
Fe3C30C31C3260.1(3) C16C17C18C14-0.1(4)
Fe3C31C32C3358.8(3) C18C14C15Fe259.1(2)
Fe3C32C33C2959.5(2) C18C14C15C160.2(3)
Fe4C37C38C3959.1(3) C19C20C21Fe2-59.2(2)
Fe4C37C41C40-59.2(3) C19C20C21C22-0.2(4)
Fe4C38C39C4060.1(3) C20C19C23Fe259.6(2)
Fe4C39C40C4159.2(3) C20C19C23C220.4(4)
Fe4C40C41C3760.0(3) C20C21C22Fe2-59.6(2)
Fe4C42C43C44-60.1(3) C20C21C22C230.4(4)
Fe4C42C46C4559.8(3) C21C22C23Fe2-60.3(2)
Fe4C43C44C45-59.5(3) C21C22C23C19-0.5(4)
Fe4C44C45C46-59.4(3) C23C19C20Fe2-59.3(2)
Fe4C45C46C42-59.5(3) C23C19C20C21-0.2(4)
Si1C1C2Fe1-118.8(3) C24Si2O1Si174.1(3)
Si1C1C2C3-179.1(2) C24Si2C37Fe4158.80(19)
Si1C1C2C11-0.5(5) C24Si2C37C3866.5(3)
Si1C1C5Fe1119.6(2) C24Si2C37C41-110.7(3)
Si1C1C5C4178.4(2) C24C25C26Fe359.4(2)
Si1C14C15Fe2-123.1(3) C24C25C26C270.3(4)
Si1C14C15C16178.0(2) C24C25C34N288.9(4)
Si1C14C18Fe2122.7(2) C25C24C28Fe3-58.89(19)
Si1C14C18C17-178.1(2) C25C24C28C27-0.2(3)
Si2C24C25Fe3-116.7(2) C25C26C27Fe358.4(2)
Si2C24C25C26-176.1(2) C25C26C27C28-0.4(4)
Si2C24C25C340.4(5) C26C25C34N2-95.2(4)
Si2C24C28Fe3117.4(2) C26C27C28Fe358.8(2)
Si2C24C28C27176.1(2) C26C27C28C240.4(4)
Si2C37C38Fe4123.2(3) C28C24C25Fe359.31(19)
Si2C37C38C39-177.8(3) C28C24C25C260.0(3)
Si2C37C41Fe4-123.4(3) C28C24C25C34176.4(3)
Si2C37C41C40177.5(3) C29C30C31Fe3-59.7(2)
O1Si1C1Fe1-167.88(15) C29C30C31C320.4(4)
O1Si1C1C2-75.8(3) C30C29C33Fe359.3(2)
O1Si1C1C5105.6(2) C30C29C33C32-0.5(4)
O1Si1C14Fe260.1(2) C30C31C32Fe3-59.6(3)
O1Si1C14C15155.6(3) C30C31C32C33-0.7(4)
O1Si1C14C18-27.0(3) C31C32C33Fe3-58.8(3)
O1Si2C24Fe3-172.83(15) C31C32C33C290.8(4)
O1Si2C24C25-83.9(3) C33C29C30Fe3-59.5(2)
O1Si2C24C28100.7(3) C33C29C30C310.0(4)
O1Si2C37Fe441.4(2) C34C25C26Fe3-117.1(3)
O1Si2C37C38-50.9(3) C34C25C26C27-176.2(3)
O1Si2C37C41131.9(3) C35N2C34C2566.2(4)
O2Si1O1Si2-28.5(4) C36N2C34C25-172.7(3)
O2Si1C1Fe1-44.2(2) C37Si2O1Si1-169.0(3)
O2Si1C1C247.8(3) C37Si2C24Fe369.2(2)
O2Si1C1C5-130.7(2) C37Si2C24C25158.1(3)
O2Si1C14Fe2-63.5(2) C37Si2C24C28-17.2(3)
O2Si1C14C1531.9(3) C37C38C39Fe4-59.6(2)
O2Si1C14C18-150.6(2) C37C38C39C400.5(5)
O3Si2O1Si1-47.2(4) C38C37C41Fe458.9(2)
O3Si2C24Fe3-51.0(2) C38C37C41C40-0.3(4)
O3Si2C24C2537.9(3) C38C39C40Fe4-59.8(3)
O3Si2C24C28-137.5(2) C38C39C40C41-0.7(5)
O3Si2C37Fe4-80.9(2) C39C40C41Fe4-59.4(3)
O3Si2C37C38-173.2(3) C39C40C41C370.6(5)
O3Si2C37C419.6(4) C41C37C38Fe4-59.2(3)
C1Si1O1Si294.3(3) C41C37C38C39-0.1(4)
C1Si1C14Fe2174.14(17) C42C43C44Fe459.9(3)
C1Si1C14C15-90.4(3) C42C43C44C450.4(4)
C1Si1C14C1887.0(3) C43C42C46Fe4-59.5(3)
C1C2C3Fe159.8(2) C43C42C46C450.3(5)
C1C2C3C41.2(4) C43C44C45Fe459.2(3)
C1C2C11N185.3(4) C43C44C45C46-0.2(5)
C2C1C5Fe1-59.31(19) C44C45C46Fe459.4(3)
C2C1C5C4-0.5(3) C44C45C46C42-0.1(5)
C2C3C4Fe157.6(2) C46C42C43Fe459.7(3)
C2C3C4C5-1.5(4) C46C42C43C44-0.4(4)

 

Table 8 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for 3116.
AtomxyzU(eq)
H22430(30)1820(20)-1450(30)73(15)
H34410(30)3160(20)-450(20)37(12)
H3A44411359182445
H425891355230044
H513891734124434
H63101177-417122
H74440-19654883
H83515-462172256
H91625-268152364
H101315129218111
H11A45181497-22038
H11B5269135548238
H12A47982812120077
H12B5707327181477
H12C59542481116677
H13A663920602380
H13B64132841-35580
H13C59462108-72380
H15111940-47329
H16-16741382-8733
H17-1503270633534
H18384308420130
H198892493-202654
H20-4571496-218952
H21-22031990-177649
H22-19133307-135051
H23-33609-152151
H2629353272-362543
H2716714306-335442
H2816224477-196235
H2950154529-153751
H3055533913-272656
H3146554573-379766
H3235815608-327161
H3337835570-186453
H34A44512608-282640
H34B44852744-194840
H35A34831611-333480
H35B24211921-299680
H35C27901100-281280
H36A49431344-250370
H36B4192872-198470
H36C48531540-163970
H389274503-54852
H39100757652883
H402883606927994
H4139944987-11466
H4223223276104368
H435993926116265
H449465178173055
H4528905293194257
H4637464124151969

Experimental

Single crystals of C46H52Fe4N2O3Si2 [3116] were []. A suitable crystal was selected and [] on a Xcalibur, Sapphire3 diffractometer. The crystal was kept at 150 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 [3116]

Crystal Data for C46H52Fe4N2O3Si2 (=960.47 g/mol): monoclinic, space group P21/n (no. 14), a = 12.8025(4) Å, b = 18.1923(6) Å, c = 17.9925(7) Å, β = 90.855(3)°, = 4190.1(2) Å3, Z = 4, T = 150 K, μ(MoKα) = 1.458 mm-1, Dcalc = 1.523 g/cm3, 31598 reflections measured (4.478° ≤ 2Θ ≤ 54°), 9116 unique (Rint = 0.0358, Rsigma = 0.0398) which were used in all calculations. The final R1 was 0.0431 (I > 2σ(I)) and wR2 was 0.1035 (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.a Secondary CH2 refined with riding coordinates:
C11(H11A,H11B), C34(H34A,H34B)
2.b Aromatic/amide H refined with riding coordinates:
C3(H3A), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C15(H15),
C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23),
C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
C33(H33), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44),
C45(H45), C46(H46)
2.c Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C35(H35A,H35B,H35C), C36(H36A,H36B,
H36C)

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.