3202

Table 1 Crystal data and structure refinement for 3202.
Identification code 3202
Empirical formula C89H119Fe4N4O6Si8
Formula weight 1788.99
Temperature/K 173
Crystal system monoclinic
Space group P21/n
a/Å 10.9706(5)
b/Å 23.7261(9)
c/Å 17.2222(7)
α/° 90.0
β/° 91.143(4)
γ/° 90.0
Volume/Å3 4481.8(3)
Z 2
ρcalcg/cm3 1.326
μ/mm‑1 0.795
F(000) 1890.0
Crystal size/mm3 0.2 × 0.2 × 0.02
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.362 to 51.994
Index ranges -13 ≤ h ≤ 13, -29 ≤ k ≤ 29, -20 ≤ l ≤ 21
Reflections collected 36392
Independent reflections 8814 [Rint = 0.0490, Rsigma = 0.0475]
Data/restraints/parameters 8814/0/514
Goodness-of-fit on F2 1.040
Final R indexes [I>=2σ (I)] R1 = 0.0387, wR2 = 0.0783
Final R indexes [all data] R1 = 0.0556, wR2 = 0.0855
Largest diff. peak/hole / e Å-3 0.41/-0.29

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for 3202. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Fe15563.2(3)5609.5(2)8671.3(2)21.17(9)
Fe27224.8(3)2854.8(2)6656.3(2)21.44(9)
Si15213.9(6)4610.4(3)7174.7(4)16.97(14)
Si25457.7(6)3508.1(3)8094.1(4)17.89(15)
Si32683.8(6)3443.9(3)7904.3(4)22.10(16)
Si42620.8(6)4106.7(3)6871.0(4)20.81(15)
O15783.2(15)4140.9(6)7781.5(9)20.4(4)
O24023.3(15)4341.7(6)6728.6(9)20.1(4)
O34035.2(15)3492.8(7)8347.4(9)22.0(4)
N14887(2)6107.4(9)6215.8(12)28.1(5)
N25233(2)1854.6(10)8414.8(15)42.6(7)
C14717(2)5229.7(9)7738.5(13)18.2(5)
C24853(2)5830.7(9)7603.9(13)19.2(5)
C34227(2)6121.2(10)8200.6(14)25.3(6)
C43712(2)5721.8(11)8707.3(15)28.1(6)
C54003(2)5176.3(10)8429.7(14)24.1(6)
C67169(2)5186.7(11)8850.6(15)27.6(6)
C77391(2)5760.6(11)8666.1(15)29.2(6)
C86840(3)6098.3(11)9239.3(15)31.9(6)
C96262(3)5736.0(11)9773.0(15)32.0(6)
C106467(3)5171.9(11)9531.6(15)30.5(6)
C115543(2)6104.7(10)6962.7(13)22.0(5)
C125701(3)6307.8(12)5613.1(15)39.7(7)
C133820(3)6467.2(15)6240.5(19)53.8(9)
C146385(2)4750.3(9)6425.1(13)18.4(5)
C157584(2)4901.3(10)6628.4(15)23.5(5)
C168455(2)4983.8(11)6061.7(16)28.7(6)
C178148(2)4913.7(11)5286.2(16)31.1(6)
C186967(2)4768.5(11)5067.7(15)30.3(6)
C196103(2)4689.3(10)5636.5(14)25.0(6)
C205686(2)3000.7(9)7288.2(14)20.3(5)
C216019(2)2409.8(10)7312.7(15)22.6(5)
C226011(2)2201.5(10)6537.5(15)26.0(6)
C235693(2)2646.3(10)6023.5(15)25.2(6)
C245485(2)3136.1(10)6480.9(14)21.4(5)
C258521(2)3441.1(11)6965.0(16)30.1(6)
C268869(2)2898.6(11)7237.2(17)32.9(6)
C278949(2)2539.5(12)6583.5(18)35.1(7)
C288648(3)2857.5(11)5907.6(17)35.2(7)
C298387(3)3420.1(11)6146.2(16)32.5(7)
C306321(2)2063.6(10)8022.0(15)29.5(6)
C314577(3)1452.6(14)7922(2)57.3(10)
C325600(4)1581.6(13)9145.5(19)58.6(11)
C336387(2)3351.1(10)8987.4(13)20.5(5)
C347632(2)3473.6(11)9052.9(15)27.9(6)
C358325(3)3303.6(12)9692.4(16)34.9(7)
C367783(3)3010.1(11)10289.2(15)32.3(6)
C376555(3)2892.9(11)10247.0(15)29.2(6)
C385866(2)3061.1(10)9604.5(14)24.8(6)
C392488(3)2717.6(11)7504.1(17)35.6(7)
C401524(3)3573.5(13)8659.7(16)38.5(7)
C412087(2)3740.6(11)5969.5(14)30.6(6)
C421609(3)4723.8(12)7057.6(16)35.6(7)
C43704(6)5743(3)8712(4)46.2(16)
C44568(4)5246(2)8999(3)85.7(15)
C46130(4)5282.8(16)9830(2)75.4(13)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for 3202. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Fe124.8(2)21.33(18)17.36(19)-0.67(14)0.63(15)-4.24(15)
Fe221.3(2)19.67(18)23.4(2)1.10(14)3.53(15)2.83(15)
Si117.6(3)15.8(3)17.5(3)0.9(3)0.0(3)-0.9(3)
Si218.3(3)18.7(3)16.6(3)2.8(3)1.0(3)0.7(3)
Si318.5(4)26.3(4)21.6(4)0.5(3)3.1(3)-3.1(3)
Si418.3(4)25.2(4)18.9(4)-1.3(3)-0.9(3)-0.7(3)
O121.4(9)18.8(8)20.9(9)3.1(7)-1.8(7)-2.3(7)
O221.2(9)18.7(8)20.4(9)-0.3(7)-0.3(7)-2.5(7)
O319.3(9)26.5(9)20.2(9)2.1(7)1.8(7)0.0(7)
N132.0(13)30.8(12)21.4(11)1.2(9)-3.5(10)2.5(10)
N247.8(16)34.5(13)46.3(16)19.2(12)21.0(13)14.0(12)
C116.5(12)19.5(12)18.5(12)-2.2(10)-2.2(10)-2.1(10)
C218.5(13)20.6(12)18.3(12)0.7(10)-3.1(10)-0.6(10)
C327.2(15)20.5(12)28.1(14)-6.1(11)0.4(11)0.6(11)
C425.6(15)33.0(14)25.9(14)-4.9(11)8.1(12)0.3(12)
C525.6(14)25.1(13)21.8(13)0.6(10)2.0(11)-4.6(11)
C627.4(15)30.4(14)24.8(14)-1.5(11)-4.8(11)1.6(12)
C725.0(15)37.6(15)25.0(14)4.7(12)-2.2(11)-8.9(12)
C839.5(17)27.3(14)28.5(15)0.8(12)-12.1(13)-9.7(13)
C940.0(17)38.1(15)17.9(13)-1.3(12)-1.9(12)-4.0(13)
C1038.3(17)30.7(14)22.4(14)8.3(11)-3.9(12)-7.3(13)
C1125.3(14)19.5(12)21.2(13)-0.4(10)-1.2(11)-0.1(10)
C1257(2)40.0(16)22.0(15)6.2(12)1.4(14)-2.7(15)
C1347(2)72(2)41.9(19)8.7(17)-8.2(16)26.0(18)
C1420.5(13)13.8(11)20.7(13)1.1(9)0.6(10)2.4(10)
C1524.3(14)23.6(13)22.4(13)1.4(10)-3.1(11)-1.9(11)
C1617.4(13)30.8(14)38.0(16)9.3(12)1.6(12)0.1(11)
C1727.3(15)36.9(15)29.4(15)11.9(12)11.4(12)5.1(12)
C1831.4(16)40.1(16)19.3(13)4.8(12)1.9(12)5.2(13)
C1921.0(14)28.9(14)25.0(14)4.8(11)-2.1(11)3.0(11)
C2018.7(13)19.8(12)22.4(13)2.8(10)2.9(10)2.3(10)
C2118.9(13)19.4(12)29.8(14)2.4(10)5.3(11)0.6(10)
C2224.9(14)18.2(12)34.9(15)-4.6(11)4.4(12)-1.0(11)
C2325.0(14)27.8(13)22.8(13)-3.1(11)0.6(11)0.0(11)
C2422.2(13)21.1(12)20.8(13)1.5(10)-0.7(10)2.7(10)
C2523.3(14)27.6(14)39.5(17)-3.2(12)4.0(12)-3.3(12)
C2624.2(15)37.7(16)36.8(16)3.3(13)-0.5(12)1.2(12)
C2721.0(14)28.0(14)57(2)0.6(14)5.2(13)7.5(12)
C2829.3(16)39.6(16)37.1(17)-6.8(13)15.4(13)-2.6(13)
C2930.3(16)30.2(14)37.5(17)6.6(12)11.0(13)-2.0(12)
C3032.2(16)21.9(13)34.7(16)5.9(11)6.0(13)7.9(11)
C3138(2)48(2)86(3)29.8(19)13.0(19)-3.1(16)
C3289(3)40.6(18)47(2)24.6(16)28(2)23.8(19)
C3323.7(13)19.4(12)18.4(13)0.9(10)-0.9(10)3(1)
C3428.5(15)32.9(14)22.4(14)6.1(11)1.7(12)-1.0(12)
C3521.6(15)49.1(17)33.9(16)3.0(14)-2.5(12)0.2(13)
C3633.8(16)40.7(16)22.2(14)5.8(12)-5.9(12)9.3(13)
C3738.2(17)28.3(14)21.4(14)6.8(11)5.1(12)5.1(12)
C3823.2(14)28.1(13)23.1(13)3.3(11)2.9(11)0.7(11)
C3936.1(17)29.5(15)41.3(17)0.0(13)2.1(13)-8.4(13)
C4024.5(15)59.1(19)32.2(16)1.7(14)6.3(13)-0.3(14)
C4129.3(15)39.1(15)23.1(14)-2.0(12)-4.4(12)-11.2(13)
C4227.3(16)45.4(17)33.9(16)-1.2(13)-3.5(13)9.9(13)
C4335(4)44(4)59(4)-2(3)-1(3)9(3)
C4443(2)112(4)103(4)-49(3)10(2)-3(2)
C4640(2)100(3)85(3)-47(3)-11(2)8(2)

 

Table 4 Bond Lengths for 3202.
AtomAtomLength/Å AtomAtomLength/Å
Fe1C12.048(2) N2C311.458(4)
Fe1C22.050(2) N2C321.465(4)
Fe1C32.057(3) C1C21.453(3)
Fe1C42.050(3) C1C51.443(3)
Fe1C52.032(3) C2C31.425(3)
Fe1C62.045(3) C2C111.499(3)
Fe1C72.038(3) C3C41.414(3)
Fe1C82.051(3) C4C51.418(3)
Fe1C92.054(3) C6C71.421(4)
Fe1C102.049(3) C6C101.416(4)
Fe2C202.056(2) C7C81.416(4)
Fe2C212.050(2) C8C91.417(4)
Fe2C222.051(2) C9C101.421(4)
Fe2C232.046(3) C14C151.401(3)
Fe2C242.038(2) C14C191.394(3)
Fe2C252.052(3) C15C161.394(3)
Fe2C262.048(3) C16C171.381(4)
Fe2C272.040(3) C17C181.385(4)
Fe2C282.045(3) C18C191.390(3)
Fe2C292.059(3) C20C211.449(3)
Si1O11.6422(17) C20C241.440(3)
Si1O21.6318(17) C21C221.423(3)
Si1C11.849(2) C21C301.504(3)
Si1C141.869(2) C22C231.417(3)
Si2O11.6368(16) C23C241.425(3)
Si2O31.6292(17) C25C261.420(4)
Si2C201.858(2) C25C291.416(4)
Si2C331.866(3) C26C271.416(4)
Si3Si42.3748(10) C27C281.420(4)
Si3O31.6578(18) C28C291.427(4)
Si3C391.867(3) C33C341.399(3)
Si3C401.863(3) C33C381.398(3)
Si4O21.6593(17) C34C351.386(4)
Si4C411.863(3) C35C361.385(4)
Si4C421.869(3) C36C371.376(4)
N1C111.461(3) C37C381.386(4)
N1C121.462(3) C43C441.289(7)
N1C131.450(4) C44C461.521(5)
N2C301.470(3) C46C4611.494(8)

1-X,1-Y,2-Z

 

Table 5 Bond Angles for 3202.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C1Fe1C241.52(9) O2Si4Si3108.67(7)
C1Fe1C369.05(9) O2Si4C41108.08(10)
C1Fe1C469.34(10) O2Si4C42108.53(11)
C1Fe1C8156.51(10) C41Si4Si3108.64(9)
C1Fe1C9160.68(10) C41Si4C42109.30(13)
C1Fe1C10123.33(10) C42Si4Si3113.48(9)
C2Fe1C340.60(9) Si2O1Si1138.48(11)
C2Fe1C8121.76(10) Si1O2Si4142.89(11)
C2Fe1C9156.75(10) Si2O3Si3136.97(11)
C4Fe1C268.60(10) C11N1C12109.2(2)
C4Fe1C340.26(10) C13N1C11111.1(2)
C4Fe1C8125.40(11) C13N1C12109.5(2)
C4Fe1C9107.74(11) C31N2C30110.4(2)
C5Fe1C141.43(9) C31N2C32109.6(2)
C5Fe1C269.06(10) C32N2C30109.4(3)
C5Fe1C368.12(10) Si1C1Fe1128.89(13)
C5Fe1C440.66(10) C2C1Fe169.32(13)
C5Fe1C6120.13(10) C2C1Si1131.59(17)
C5Fe1C7155.93(10) C5C1Fe168.69(14)
C5Fe1C8161.38(10) C5C1Si1122.25(17)
C5Fe1C9124.07(10) C5C1C2106.07(19)
C5Fe1C10106.57(10) C1C2Fe169.15(13)
C6Fe1C1106.14(10) C1C2C11126.7(2)
C6Fe1C2124.86(10) C3C2Fe169.96(14)
C6Fe1C3162.51(10) C3C2C1107.9(2)
C6Fe1C4155.46(10) C3C2C11125.4(2)
C6Fe1C868.14(11) C11C2Fe1125.66(17)
C6Fe1C968.15(11) C2C3Fe169.44(14)
C6Fe1C1040.47(10) C4C3Fe169.61(15)
C7Fe1C1120.31(10) C4C3C2109.0(2)
C7Fe1C2107.90(10) C3C4Fe170.13(15)
C7Fe1C3126.03(10) C3C4C5107.9(2)
C7Fe1C4162.34(11) C5C4Fe168.98(15)
C7Fe1C640.72(10) C1C5Fe169.88(14)
C7Fe1C840.53(11) C4C5Fe170.37(15)
C7Fe1C968.23(11) C4C5C1109.1(2)
C7Fe1C1068.29(11) C7C6Fe169.34(15)
C8Fe1C3109.19(11) C10C6Fe169.90(16)
C8Fe1C940.39(10) C10C6C7107.9(2)
C9Fe1C3121.84(11) C6C7Fe169.93(15)
C10Fe1C2161.39(10) C8C7Fe170.26(16)
C10Fe1C3156.17(10) C8C7C6108.0(2)
C10Fe1C4120.61(11) C7C8Fe169.21(15)
C10Fe1C868.02(11) C7C8C9108.2(2)
C10Fe1C940.52(10) C9C8Fe169.91(15)
C20Fe2C29129.65(10) C8C9Fe169.70(15)
C21Fe2C2041.33(9) C8C9C10107.8(2)
C21Fe2C2240.62(10) C10C9Fe169.54(15)
C21Fe2C25131.14(10) C6C10Fe169.63(15)
C21Fe2C29169.27(10) C6C10C9108.1(2)
C22Fe2C2069.01(9) C9C10Fe169.94(15)
C22Fe2C25169.56(11) N1C11C2113.8(2)
C22Fe2C29148.86(11) C15C14Si1121.84(18)
C23Fe2C2069.40(10) C19C14Si1120.79(19)
C23Fe2C2168.70(10) C19C14C15117.3(2)
C23Fe2C2240.47(10) C16C15C14121.0(2)
C23Fe2C25149.31(10) C17C16C15120.1(3)
C23Fe2C26168.22(10) C16C17C18120.1(2)
C23Fe2C29116.07(11) C17C18C19119.3(2)
C24Fe2C2041.17(9) C18C19C14122.1(2)
C24Fe2C2168.76(10) Si2C20Fe2128.96(13)
C24Fe2C2268.21(10) C21C20Fe269.12(13)
C24Fe2C2340.83(9) C21C20Si2130.00(18)
C24Fe2C25117.29(10) C24C20Fe268.76(13)
C24Fe2C26150.31(10) C24C20Si2123.82(17)
C24Fe2C27167.75(11) C24C20C21106.1(2)
C24Fe2C28129.05(11) C20C21Fe269.55(13)
C24Fe2C29108.02(10) C20C21C30127.1(2)
C25Fe2C20108.72(10) C22C21Fe269.72(14)
C25Fe2C2940.29(11) C22C21C20108.2(2)
C26Fe2C20117.22(11) C22C21C30124.7(2)
C26Fe2C21109.19(11) C30C21Fe2126.52(18)
C26Fe2C22130.60(11) C21C22Fe269.66(14)
C26Fe2C2540.52(10) C23C22Fe269.57(14)
C26Fe2C2968.19(11) C23C22C21108.9(2)
C27Fe2C20150.02(11) C22C23Fe269.96(15)
C27Fe2C21117.01(11) C22C23C24107.6(2)
C27Fe2C22108.50(11) C24C23Fe269.31(14)
C27Fe2C23129.16(11) C20C24Fe270.07(14)
C27Fe2C2568.04(11) C23C24Fe269.86(14)
C27Fe2C2640.53(11) C23C24C20109.2(2)
C27Fe2C2840.70(11) C26C25Fe269.60(16)
C27Fe2C2968.29(11) C29C25Fe270.14(15)
C28Fe2C20168.14(11) C29C25C26108.6(2)
C28Fe2C21149.16(10) C25C26Fe269.88(16)
C28Fe2C22116.21(11) C27C26Fe269.42(16)
C28Fe2C23107.13(11) C27C26C25107.7(2)
C28Fe2C2568.12(11) C26C27Fe270.05(15)
C28Fe2C2668.38(12) C26C27C28108.4(2)
C28Fe2C2940.71(10) C28C27Fe269.83(15)
O1Si1C1108.49(10) C27C28Fe269.47(15)
O1Si1C14107.58(10) C27C28C29107.8(2)
O2Si1O1108.99(8) C29C28Fe270.20(14)
O2Si1C1108.43(10) C25C29Fe269.57(14)
O2Si1C14107.39(10) C25C29C28107.6(2)
C1Si1C14115.80(10) C28C29Fe269.10(15)
O1Si2C20108.36(9) N2C30C21113.0(2)
O1Si2C33109.58(10) C34C33Si2122.79(18)
O3Si2O1108.97(9) C38C33Si2119.99(19)
O3Si2C20109.24(10) C38C33C34117.0(2)
O3Si2C33106.58(10) C35C34C33121.5(2)
C20Si2C33114.01(11) C36C35C34119.9(3)
O3Si3Si4108.12(6) C37C36C35119.8(3)
O3Si3C39109.26(12) C36C37C38120.1(2)
O3Si3C40106.50(11) C37C38C33121.6(2)
C39Si3Si4109.46(10) C43C44C46110.5(4)
C40Si3Si4113.81(10) C461C46C44112.5(4)
C40Si3C39109.57(13)     

1-X,1-Y,2-Z

 

Table 6 Torsion Angles for 3202.
ABCDAngle/˚ ABCDAngle/˚
Fe1C1C2C3-59.46(17) C3C4C5C10.2(3)
Fe1C1C2C11119.6(2) C5C1C2Fe159.14(17)
Fe1C1C5C459.62(19) C5C1C2C3-0.3(3)
Fe1C2C3C4-58.50(19) C5C1C2C11178.8(2)
Fe1C2C11N1167.81(16) C6C7C8Fe1-60.02(18)
Fe1C3C4C5-58.81(19) C6C7C8C9-0.8(3)
Fe1C4C5C1-59.32(18) C7C6C10Fe159.13(18)
Fe1C6C7C860.23(19) C7C6C10C9-0.4(3)
Fe1C6C10C9-59.6(2) C7C8C9Fe1-58.81(19)
Fe1C7C8C959.3(2) C7C8C9C100.5(3)
Fe1C8C9C1059.31(19) C8C9C10Fe1-59.41(19)
Fe1C9C10C659.38(19) C8C9C10C60.0(3)
Fe2C20C21C22-59.22(17) C10C6C7Fe1-59.48(19)
Fe2C20C21C30120.9(3) C10C6C7C80.7(3)
Fe2C20C24C2359.06(17) C11C2C3Fe1-120.1(2)
Fe2C21C22C23-58.64(18) C11C2C3C4-178.6(2)
Fe2C21C30N2172.88(18) C12N1C11C2-171.9(2)
Fe2C22C23C24-59.32(17) C13N1C11C267.2(3)
Fe2C23C24C20-59.19(17) C14Si1O1Si2-120.58(16)
Fe2C25C26C2759.37(19) C14Si1O2Si4-178.54(16)
Fe2C25C29C28-58.84(19) C14Si1C1Fe1-80.42(17)
Fe2C26C27C2859.53(19) C14Si1C1C215.9(3)
Fe2C27C28C2960.00(19) C14Si1C1C5-167.9(2)
Fe2C28C29C2559.14(18) C14C15C16C17-0.4(4)
Si1C1C2Fe1-124.2(2) C15C14C19C180.5(3)
Si1C1C2C3176.3(2) C15C16C17C180.9(4)
Si1C1C2C11-4.6(4) C16C17C18C19-0.6(4)
Si1C1C5Fe1123.41(18) C17C18C19C14-0.1(4)
Si1C1C5C4-176.97(18) C19C14C15C16-0.3(3)
Si1C14C15C16177.62(18) C20Si2O1Si169.87(18)
Si1C14C19C18-177.39(19) C20Si2O3Si3-39.46(18)
Si2C20C21Fe2-123.9(2) C20Si2C33C3477.1(2)
Si2C20C21C22176.84(19) C20Si2C33C38-97.9(2)
Si2C20C21C30-3.0(4) C20C21C22Fe259.11(17)
Si2C20C24Fe2123.48(18) C20C21C22C230.5(3)
Si2C20C24C23-177.46(18) C20C21C30N282.0(3)
Si2C33C34C35-173.7(2) C21C20C24Fe2-59.31(16)
Si2C33C38C37174.14(19) C21C20C24C23-0.3(3)
Si3Si4O2Si1-50.91(18) C21C22C23Fe258.69(18)
Si4Si3O3Si2-48.59(16) C21C22C23C24-0.6(3)
O1Si1O2Si465.19(19) C22C21C30N2-97.8(3)
O1Si1C1Fe140.61(17) C22C23C24Fe259.74(18)
O1Si1C1C2136.9(2) C22C23C24C200.5(3)
O1Si1C1C5-46.9(2) C24C20C21Fe259.08(16)
O1Si1C14C15-52.9(2) C24C20C21C22-0.1(3)
O1Si1C14C19124.93(19) C24C20C21C30-180.0(2)
O1Si2O3Si378.76(17) C25C26C27Fe2-59.66(19)
O1Si2C20Fe256.74(17) C25C26C27C28-0.1(3)
O1Si2C20C21151.3(2) C26C25C29Fe259.17(19)
O1Si2C20C24-32.2(2) C26C25C29C280.3(3)
O1Si2C33C34-44.5(2) C26C27C28Fe2-59.67(19)
O1Si2C33C38140.45(18) C26C27C28C290.3(3)
O2Si1O1Si2-4.43(18) C27C28C29Fe2-59.54(19)
O2Si1C1Fe1158.84(13) C27C28C29C25-0.4(3)
O2Si1C1C2-104.9(2) C29C25C26Fe2-59.50(19)
O2Si1C1C571.3(2) C29C25C26C27-0.1(3)
O2Si1C14C15-170.10(18) C30C21C22Fe2-121.0(2)
O2Si1C14C197.7(2) C30C21C22C23-179.7(2)
O3Si2O1Si1-48.90(18) C31N2C30C2166.0(3)
O3Si2C20Fe2175.34(13) C32N2C30C21-173.2(2)
O3Si2C20C21-90.1(2) C33Si2O1Si1-165.17(15)
O3Si2C20C2486.4(2) C33Si2O3Si3-163.07(15)
O3Si2C33C34-162.3(2) C33Si2C20Fe2-65.56(18)
O3Si2C33C3822.7(2) C33Si2C20C2129.0(3)
C1Si1O1Si2113.44(16) C33Si2C20C24-154.5(2)
C1Si1O2Si4-52.7(2) C33C34C35C36-0.7(4)
C1Si1C14C1568.6(2) C34C33C38C37-1.2(4)
C1Si1C14C19-113.6(2) C34C35C36C37-0.6(4)
C1C2C3Fe158.95(16) C35C36C37C380.9(4)
C1C2C3C40.5(3) C36C37C38C330.0(4)
C1C2C11N178.4(3) C38C33C34C351.5(4)
C2C1C5Fe1-59.55(16) C39Si3O3Si270.46(18)
C2C1C5C40.1(3) C40Si3O3Si2-171.27(16)
C2C3C4Fe158.40(18) C41Si4O2Si1-168.64(17)
C2C3C4C5-0.4(3) C42Si4O2Si172.9(2)
C3C2C11N1-102.6(3) C43C44C46C461175.8(5)
C3C4C5Fe159.52(19)      

1-X,1-Y,2-Z

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for 3202.
AtomxyzU(eq)
H341666519825030
H432525804915534
H537674831866229
H674434869856733
H778325894823435
H868556498926238
H9581758501021438
H1061834842978337
H11A57316498711326
H11B63275904690226
H12A59876688574460
H12B52616316511360
H12C64026053557960
H13A32706329663981
H13B33996462573481
H13C40726854636581
H1578064948716028
H1692635088620934
H1787474965490237
H1867514724453436
H1952944590548330
H2261911825638931
H2356292622547430
H2452523495628426
H2583983764728036
H2690222795776339
H2791662152659542
H2886252720538942
H2981643725581639
H30A68281738786935
H30B68092296839135
H31A43091639744086
H31B38651311819586
H31C51161137779886
H32A61281259903688
H32B48741451941588
H32C60461852947588
H3480113678865034
H3591723388972242
H36825828901072639
H37617926961065935
H3850192977958330
H39A16612676728653
H39B26192441792053
H39C30812654709553
H40A16973933891958
H40B15543268904258
H40C7113588841458
H41A26293423586346
H41B20964005553346
H41C12563601603946
H42A7744592713553
H42B16224980661253
H42C19004923752453
H43A12415965905569
H43B-925928866469
H43C10675713819869
H44A135450418991103
H44B-3350328679103
H46A76054741015490
H46B-6205515984090

 

Table 8 Atomic Occupancy for 3202.
AtomOccupancy AtomOccupancy AtomOccupancy
C430.5 H43A0.5 H43B0.5
H43C0.5     

Experimental

Single crystals of C89H119Fe4N4O6Si8 [3202] 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 [3202]

Crystal Data for C89H119Fe4N4O6Si8 (=1788.99 g/mol): monoclinic, space group P21/n (no. 14), a = 10.9706(5) Å, b = 23.7261(9) Å, c = 17.2222(7) Å, β = 91.143(4)°, = 4481.8(3) Å3, Z = 2, T = 173 K, μ(MoKα) = 0.795 mm-1, Dcalc = 1.326 g/cm3, 36392 reflections measured (4.362° ≤ 2Θ ≤ 51.994°), 8814 unique (Rint = 0.0490, Rsigma = 0.0475) which were used in all calculations. The final R1 was 0.0387 (I > 2σ(I)) and wR2 was 0.0855 (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. Others
Fixed Sof: C43(0.5) H43A(0.5) H43B(0.5) H43C(0.5)
3.a Secondary CH2 refined with riding coordinates:
C11(H11A,H11B), C30(H30A,H30B), C44(H44A,H44B), C46(H46A,H46B)
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), C15(H15),
C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C24(H24), C25(H25),
C26(H26), C27(H27), C28(H28), C29(H29), C34(H34), C35(H35), C36(H36),
C37(H37), C38(H38)
3.c Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C31(H31A,H31B,H31C), C32(H32A,H32B,
H32C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,
H42B,H42C), C43(H43A,H43B,H43C)

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