3021

Table 1 Crystal data and structure refinement for 3021.
Identification code 3021
Empirical formula C52H69Fe4N4O9Si4
Formula weight 1229.87
Temperature/K 173
Crystal system monoclinic
Space group P21/n
a/Å 13.2912(7)
b/Å 13.5363(7)
c/Å 30.9964(18)
α/° 90
β/° 96.859(5)
γ/° 90
Volume/Å3 5536.8(5)
Z 4
ρcalcg/cm3 1.475
μ/mm‑1 1.171
F(000) 2564.0
Crystal size/mm3 0.14 × 0.11 × 0.06
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.31 to 53.998
Index ranges -16 ≤ h ≤ 16, -17 ≤ k ≤ 17, -38 ≤ l ≤ 39
Reflections collected 42828
Independent reflections 11995 [Rint = 0.0745, Rsigma = 0.0936]
Data/restraints/parameters 11995/5/686
Goodness-of-fit on F2 1.017
Final R indexes [I>=2σ (I)] R1 = 0.0634, wR2 = 0.1325
Final R indexes [all data] R1 = 0.1265, wR2 = 0.1626
Largest diff. peak/hole / e Å-3 0.81/-0.64

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for 3021. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Fe1823.1(5)3237.9(5)5927.8(2)40.0(2)
Fe2-366.1(6)8541.0(6)6074.4(3)44.0(2)
Fe35218.9(5)9798.9(5)6352.8(2)36.37(19)
Fe46294.2(6)4351.4(5)6639.7(2)42.5(2)
Si12410.2(10)5076.4(10)6345.6(4)30.8(3)
Si21632.8(10)7052.6(10)5960.4(4)30.6(3)
Si33570.7(10)7898.5(10)6451.9(4)28.1(3)
Si44471.5(9)5925.9(10)6201.8(4)26.7(3)
O11943(3)5121(3)6799.8(11)47.7(10)
O21895(2)5887(2)6001.8(10)34.0(8)
O31762(3)7416(3)5473.4(10)44.6(9)
O42371(2)7649(2)6324.9(9)32.6(8)
O53804(3)7859(3)6971.5(10)40.0(8)
O64226(2)7102(2)6212.5(9)30.1(7)
O74513(2)5597(2)5705.9(10)36.0(8)
O83614(2)5327(2)6428.6(9)32.4(7)
N13161(3)4495(4)5180.3(13)49.3(12)
N2869(3)6537(3)7126.4(13)45.4(11)
N33281(4)8602(4)5212.7(14)63.9(15)
N45050(3)6621(3)7457.4(13)48.0(12)
C12223(3)3836(4)6108.4(16)35.7(12)
C22107(4)3552(4)5653.1(17)42.6(13)
C31910(4)2529(4)5629(2)54.8(15)
C41897(4)2164(4)6053(2)61.8(18)
C52092(4)2948(4)6347.5(19)48.9(14)
C6-348(4)3929(6)5573(2)66.2(19)
C7-555(4)2922(6)5590(2)68.8(19)
C8-543(4)2667(5)6029(2)62.4(18)
C9-348(4)3533(5)6279.5(19)50.9(15)
C10-221(4)4312(4)5994(2)54.2(16)
C112130(4)4234(4)5276.1(16)44.2(14)
C123712(4)3619(5)5069(2)75(2)
C133060(5)5225(5)4821.0(16)72(2)
C14314(4)7206(3)6070.6(16)35.5(12)
C15-85(4)7402(4)6482.8(15)38.1(12)
C16-1121(4)7528(4)6396.4(18)46.9(14)
C17-1419(4)7450(4)5944.3(19)50.3(14)
C18-543(4)7235(4)5748.1(18)46.8(14)
C19714(5)9555(4)5979(2)64.0(18)
C20394(5)9703(4)6377(3)67.5(19)
C21-668(5)9888(4)6332(2)60.4(17)
C22-975(5)9875(4)5882(2)64.1(18)
C23-128(6)9659(5)5663(2)77(2)
C24550(4)7479(4)6919.5(16)43.2(13)
C256(5)5970(5)7238(2)69.0(19)
C261573(5)6723(5)7523.3(17)61.8(17)
C273821(3)9147(4)6267.5(15)33.2(11)
C284117(4)9489(4)5854.4(16)37.2(12)
C294279(4)10527(4)5890(2)50.6(15)
C304089(4)10843(4)6301(2)54.6(16)
C313801(4)10016(4)6533.7(19)44.6(14)
C326254(4)8732(4)6550(2)49.0(15)
C336554(4)9250(5)6193(2)55.6(16)
C346667(4)10256(4)6313(2)51.4(15)
C356447(4)10351(4)6743.4(19)51.8(15)
C366171(4)9411(4)6889.9(19)54.1(15)
C374247(4)8848(4)5472.2(16)47.3(14)
C383473(6)7969(6)4848.8(19)106(3)
C392728(5)9488(6)5067(2)104(3)
C405714(3)5734(3)6516.2(14)28.5(10)
C415980(4)5569(4)6977.7(15)35.7(11)
C427018(4)5363(4)7051.1(19)51.9(15)
C437425(4)5377(4)6650(2)54.7(16)
C446632(4)5611(4)6322.4(17)42.3(13)
C455227(5)3356(4)6385(2)65.2(18)
C465408(6)3256(5)6831(2)74(2)
C476416(7)3018(5)6938(3)84(2)
C486891(5)2984(4)6556(3)75(2)
C496126(7)3219(4)6203(2)78(2)
C505268(4)5607(4)7319.8(15)46.1(14)
C514353(5)6580(5)7795.3(17)74(2)
C525993(5)7136(5)7620.2(18)62.3(17)
O92580(4)4181(4)7604.0(15)92.5(16)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for 3021. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Fe128.0(4)35.6(4)56.0(5)2.4(4)3.9(3)-7.2(3)
Fe232.3(4)38.6(4)59.1(5)1.7(4)-2.3(4)0.4(4)
Fe327.4(4)33.0(4)48.0(4)-3.6(3)1.2(3)-1.7(3)
Fe436.7(4)34.7(4)53.5(5)3.4(4)-5.2(4)2.5(4)
Si129.4(7)36.0(8)27.7(7)-0.4(6)5.8(5)-7.3(6)
Si226.8(7)35.2(7)29.3(7)-2.2(6)1.4(5)-0.8(6)
Si327.4(7)29.8(7)26.7(6)-2.0(6)1.7(5)-3.3(6)
Si424.6(7)30.1(7)24.9(6)-0.6(6)0.9(5)-3.6(6)
O155(2)54(2)37(2)8.6(19)16.0(18)0(2)
O229.7(18)36.9(19)34.2(18)-4.4(15)-0.9(14)-5.8(16)
O344(2)53(2)35.7(19)5.1(18)0.2(16)-9(2)
O429.1(17)35.2(19)34.1(17)-5.2(15)6.7(14)-3.8(15)
O546(2)42(2)30.4(18)-4.1(16)-1.7(16)1.9(18)
O628.0(17)29.9(17)32.3(17)0.5(14)2.7(14)-0.8(15)
O732.9(19)46(2)29.1(17)-7.3(16)3.1(15)-7.4(17)
O829.3(17)39.1(19)28.2(16)1.8(15)0.3(13)-6.1(16)
N140(3)72(3)37(2)-15(2)10(2)-22(3)
N240(3)58(3)39(2)2(2)8(2)-2(2)
N365(3)93(4)32(3)12(3)-2(2)-36(3)
N452(3)61(3)30(2)1(2)-1(2)5(3)
C123(2)33(3)50(3)2(2)3(2)-5(2)
C228(3)47(3)54(3)-11(3)10(2)-12(3)
C341(3)41(3)83(4)-17(3)9(3)-5(3)
C438(3)24(3)122(6)-4(4)5(4)-2(3)
C533(3)44(3)68(4)14(3)-2(3)-1(3)
C631(3)103(6)65(4)35(4)6(3)5(4)
C733(3)101(6)71(5)-14(4)0(3)-17(4)
C832(3)50(4)108(6)18(4)16(3)-10(3)
C934(3)66(4)54(3)12(3)10(3)1(3)
C1031(3)44(3)88(5)12(3)8(3)4(3)
C1136(3)61(4)37(3)-19(3)10(2)-19(3)
C1243(4)107(6)78(5)-49(4)18(3)-20(4)
C1366(4)123(6)27(3)0(3)6(3)-40(4)
C1429(3)34(3)43(3)-7(2)-1(2)-6(2)
C1543(3)37(3)35(3)-5(2)10(2)-11(3)
C1641(3)44(3)58(4)-4(3)16(3)3(3)
C1729(3)51(3)71(4)-6(3)2(3)-3(3)
C1840(3)48(3)50(3)-12(3)-2(3)-5(3)
C1942(4)46(4)105(6)10(4)12(4)-7(3)
C2050(4)36(3)112(6)-9(4)-10(4)-5(3)
C2158(4)39(3)82(5)-4(3)0(3)6(3)
C2254(4)52(4)84(5)20(4)-1(4)15(3)
C2389(6)69(5)75(5)22(4)14(4)0(4)
C2441(3)52(3)38(3)-7(3)11(2)4(3)
C2561(4)80(5)70(4)9(4)20(3)-11(4)
C2662(4)78(5)45(3)0(3)4(3)-3(4)
C2718(2)36(3)45(3)-6(2)1(2)-2(2)
C2827(3)41(3)42(3)3(2)-3(2)-6(2)
C2935(3)42(3)73(4)16(3)0(3)-2(3)
C3037(3)28(3)97(5)-4(3)1(3)3(3)
C3128(3)41(3)66(4)-12(3)10(3)2(2)
C3228(3)35(3)81(4)-2(3)-8(3)5(2)
C3331(3)70(4)65(4)-10(4)5(3)11(3)
C3432(3)53(4)68(4)6(3)6(3)-4(3)
C3539(3)47(3)65(4)-12(3)-11(3)-11(3)
C3644(3)60(4)55(4)-8(3)-11(3)-8(3)
C3745(3)62(4)35(3)10(3)4(2)-16(3)
C38107(6)173(9)43(4)-34(5)28(4)-87(6)
C3978(5)141(8)81(5)70(5)-42(4)-35(5)
C4028(2)24(2)32(2)-2(2)-3(2)-3(2)
C4135(3)34(3)37(3)-2(2)-3(2)-2(2)
C4241(3)57(4)52(3)-3(3)-17(3)1(3)
C4323(3)63(4)76(4)-5(3)-2(3)-4(3)
C4430(3)46(3)51(3)0(3)5(2)-6(3)
C4562(4)35(3)94(5)-10(4)-8(4)-12(3)
C46103(6)43(4)80(5)3(4)18(5)-15(4)
C47102(6)45(4)99(6)21(4)-11(5)8(4)
C4859(4)42(4)123(7)-3(4)9(5)14(3)
C49132(7)40(4)64(4)-9(3)20(5)-5(4)
C5051(3)52(3)32(3)11(3)-8(2)-5(3)
C5187(5)102(6)34(3)6(3)14(3)19(4)
C5270(4)67(4)45(3)-14(3)-12(3)-2(4)
O999(4)92(4)83(3)17(3)0(3)2(3)

 

Table 4 Bond Lengths for 3021.
AtomAtomLength/Å AtomAtomLength/Å
Fe1C12.044(5) N1C111.479(6)
Fe1C22.040(5) N1C121.457(7)
Fe1C32.045(6) N1C131.483(7)
Fe1C42.042(6) N2C241.467(6)
Fe1C52.042(5) N2C251.456(7)
Fe1C62.025(6) N2C261.476(7)
Fe1C72.043(6) N3C371.470(7)
Fe1C82.032(5) N3C381.463(8)
Fe1C92.043(5) N3C391.451(9)
Fe1C102.037(6) N4C501.476(7)
Fe2C142.021(5) N4C511.480(6)
Fe2C152.001(5) N4C521.470(7)
Fe2C162.030(5) C1C21.453(7)
Fe2C172.042(5) C1C51.433(7)
Fe2C182.036(5) C2C31.409(7)
Fe2C192.034(6) C2C111.493(7)
Fe2C202.036(6) C3C41.405(8)
Fe2C212.049(6) C4C51.404(8)
Fe2C222.038(6) C6C71.393(9)
Fe2C232.027(6) C6C101.397(8)
Fe3C272.045(5) C7C81.402(8)
Fe3C282.041(5) C8C91.413(8)
Fe3C292.040(5) C9C101.399(7)
Fe3C302.055(5) C14C151.465(6)
Fe3C312.051(5) C14C181.424(7)
Fe3C322.038(5) C15C161.381(7)
Fe3C332.039(5) C15C241.510(7)
Fe3C342.040(5) C16C171.414(7)
Fe3C352.054(5) C17C181.407(7)
Fe3C362.036(6) C19C201.366(8)
Fe4C402.043(4) C19C231.403(9)
Fe4C412.024(5) C20C211.423(8)
Fe4C422.033(5) C21C221.404(8)
Fe4C432.043(5) C22C231.414(9)
Fe4C442.045(5) C27C281.459(6)
Fe4C452.046(6) C27C311.439(7)
Fe4C462.026(6) C28C291.424(7)
Fe4C472.026(7) C28C371.495(7)
Fe4C482.042(6) C29C301.394(8)
Fe4C492.040(6) C30C311.410(7)
Si1O11.606(3) C32C331.409(8)
Si1O21.623(3) C32C361.412(7)
Si1O81.626(3) C33C341.415(8)
Si1C11.839(5) C34C351.405(7)
Si2O21.618(3) C35C361.414(8)
Si2O31.616(3) C40C411.449(6)
Si2O41.620(3) C40C441.433(6)
Si2C141.837(5) C41C421.400(7)
Si3O41.631(3) C41C501.503(7)
Si3O51.604(3) C42C431.413(7)
Si3O61.621(3) C43C441.410(7)
Si3C271.827(5) C45C461.382(9)
Si4O61.626(3) C45C491.392(9)
Si4O71.607(3) C46C471.379(10)
Si4O81.625(3) C47C481.407(10)
Si4C401.833(5) C48C491.438(10)

 

Table 5 Bond Angles for 3021.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C1Fe1C369.0(2) O2Si1C1109.2(2)
C2Fe1C141.67(19) O8Si1C1109.76(19)
C2Fe1C340.4(2) O2Si2O4108.86(17)
C2Fe1C468.1(2) O2Si2C14107.3(2)
C2Fe1C568.7(2) O3Si2O2108.98(19)
C2Fe1C7125.0(2) O3Si2O4112.13(18)
C2Fe1C9155.5(2) O3Si2C14110.4(2)
C4Fe1C168.7(2) O4Si2C14109.01(19)
C4Fe1C340.2(2) O4Si3C27108.99(19)
C4Fe1C7120.8(3) O5Si3O4107.55(17)
C4Fe1C9126.7(3) O5Si3O6112.80(18)
C5Fe1C141.1(2) O5Si3C27108.9(2)
C5Fe1C367.9(2) O6Si3O4108.36(17)
C5Fe1C440.2(2) O6Si3C27110.11(19)
C5Fe1C7155.2(3) O6Si4C40107.33(18)
C5Fe1C9108.8(2) O7Si4O6108.67(17)
C6Fe1C1125.5(3) O7Si4O8112.44(17)
C6Fe1C2107.7(2) O7Si4C40109.72(19)
C6Fe1C3120.6(3) O8Si4O6109.07(17)
C6Fe1C4155.0(3) O8Si4C40109.48(18)
C6Fe1C5163.4(3) Si2O2Si1141.4(2)
C6Fe1C740.0(3) Si2O4Si3139.9(2)
C6Fe1C867.5(2) Si3O6Si4141.3(2)
C6Fe1C967.3(2) Si4O8Si1139.8(2)
C6Fe1C1040.2(2) C11N1C13107.9(4)
C7Fe1C1162.5(3) C12N1C11110.9(4)
C7Fe1C3108.0(3) C12N1C13111.6(5)
C8Fe1C1155.3(3) C24N2C26109.7(4)
C8Fe1C2162.0(3) C25N2C24111.5(4)
C8Fe1C3125.7(3) C25N2C26109.4(4)
C8Fe1C4108.5(2) C38N3C37109.5(5)
C8Fe1C5120.9(2) C39N3C37111.1(5)
C8Fe1C740.2(2) C39N3C38111.9(6)
C8Fe1C940.6(2) C50N4C51109.4(4)
C8Fe1C1067.9(2) C52N4C50110.6(4)
C9Fe1C1120.2(2) C52N4C51110.8(4)
C9Fe1C3163.2(2) Si1C1Fe1123.1(2)
C9Fe1C767.7(2) C2C1Fe169.0(3)
C10Fe1C1107.4(2) C2C1Si1128.6(4)
C10Fe1C2120.5(2) C5C1Fe169.4(3)
C10Fe1C3155.1(3) C5C1Si1125.3(4)
C10Fe1C4163.4(3) C5C1C2106.0(5)
C10Fe1C5126.4(3) C1C2Fe169.3(3)
C10Fe1C767.7(3) C1C2C11126.0(5)
C10Fe1C940.1(2) C3C2Fe170.0(3)
C14Fe2C1669.3(2) C3C2C1107.9(5)
C14Fe2C1769.4(2) C3C2C11126.0(5)
C14Fe2C1841.10(19) C11C2Fe1123.5(4)
C14Fe2C19106.2(2) C2C3Fe169.6(3)
C14Fe2C20119.7(2) C4C3Fe169.8(3)
C14Fe2C21155.0(2) C4C3C2108.7(5)
C14Fe2C22162.3(2) C3C4Fe170.0(3)
C14Fe2C23124.1(3) C5C4Fe169.9(3)
C15Fe2C1442.72(19) C5C4C3108.7(5)
C15Fe2C1640.1(2) C1C5Fe169.6(3)
C15Fe2C1768.9(2) C4C5Fe169.9(3)
C15Fe2C1869.4(2) C4C5C1108.8(5)
C15Fe2C19122.0(2) C7C6Fe170.7(4)
C15Fe2C20105.0(3) C7C6C10109.2(6)
C15Fe2C21118.0(2) C10C6Fe170.4(3)
C15Fe2C22154.8(2) C6C7Fe169.3(3)
C15Fe2C23160.2(3) C6C7C8107.5(6)
C16Fe2C1740.6(2) C8C7Fe169.5(3)
C16Fe2C1867.9(2) C7C8Fe170.3(3)
C16Fe2C19157.9(3) C7C8C9108.0(5)
C16Fe2C20122.8(3) C9C8Fe170.1(3)
C16Fe2C21106.2(2) C8C9Fe169.3(3)
C16Fe2C22122.6(2) C10C9Fe169.7(3)
C17Fe2C21124.0(2) C10C9C8107.9(5)
C18Fe2C1740.4(2) C6C10Fe169.4(3)
C18Fe2C20157.0(2) C6C10C9107.5(6)
C18Fe2C21161.7(2) C9C10Fe170.2(3)
C18Fe2C22127.3(3) N1C11C2114.3(4)
C19Fe2C17159.9(3) Si2C14Fe2122.7(2)
C19Fe2C18123.8(3) C15C14Fe267.9(3)
C19Fe2C2039.2(2) C15C14Si2129.5(4)
C19Fe2C2168.3(3) C18C14Fe270.0(3)
C19Fe2C2267.8(3) C18C14Si2125.0(4)
C20Fe2C17160.1(3) C18C14C15105.3(4)
C20Fe2C2140.8(2) C14C15Fe269.4(3)
C20Fe2C2266.9(3) C14C15C24124.9(4)
C22Fe2C17110.1(3) C16C15Fe271.1(3)
C22Fe2C2140.2(2) C16C15C14108.0(5)
C23Fe2C16159.5(3) C16C15C24127.1(4)
C23Fe2C17124.8(3) C24C15Fe2123.8(4)
C23Fe2C18110.7(3) C15C16Fe268.8(3)
C23Fe2C1940.4(3) C15C16C17109.7(5)
C23Fe2C2066.8(3) C17C16Fe270.1(3)
C23Fe2C2168.5(3) C16C17Fe269.2(3)
C23Fe2C2240.7(2) C18C17Fe269.6(3)
C27Fe3C3069.1(2) C18C17C16107.2(5)
C27Fe3C3141.12(18) C14C18Fe268.9(3)
C27Fe3C35151.5(2) C17C18Fe270.0(3)
C28Fe3C2741.83(18) C17C18C14109.7(5)
C28Fe3C3068.3(2) C20C19Fe270.5(4)
C28Fe3C3168.7(2) C20C19C23107.8(6)
C28Fe3C35165.7(2) C23C19Fe269.5(4)
C29Fe3C2769.3(2) C19C20Fe270.3(4)
C29Fe3C2840.8(2) C19C20C21110.5(7)
C29Fe3C3039.8(2) C21C20Fe270.1(3)
C29Fe3C3167.5(2) C20C21Fe269.1(3)
C29Fe3C35128.0(2) C22C21Fe269.5(3)
C31Fe3C3040.2(2) C22C21C20105.3(6)
C31Fe3C35118.6(2) C21C22Fe270.3(3)
C32Fe3C27107.7(2) C21C22C23108.9(6)
C32Fe3C28118.7(2) C23C22Fe269.2(4)
C32Fe3C29152.7(2) C19C23Fe270.0(4)
C32Fe3C30166.4(3) C19C23C22107.5(6)
C32Fe3C31129.0(2) C22C23Fe270.1(4)
C32Fe3C3340.5(2) N2C24C15115.7(4)
C32Fe3C3468.0(2) Si3C27Fe3123.7(2)
C32Fe3C3567.7(2) C28C27Fe368.9(3)
C33Fe3C27127.9(2) C28C27Si3130.3(4)
C33Fe3C28107.9(2) C31C27Fe369.6(3)
C33Fe3C29118.9(2) C31C27Si3124.0(4)
C33Fe3C30151.7(3) C31C27C28105.6(4)
C33Fe3C31166.8(2) C27C28Fe369.2(3)
C33Fe3C3440.6(2) C27C28C37125.5(4)
C33Fe3C3567.8(2) C29C28Fe369.5(3)
C34Fe3C27166.5(2) C29C28C27107.4(5)
C34Fe3C28127.9(2) C29C28C37127.1(5)
C34Fe3C29108.3(2) C37C28Fe3125.3(4)
C34Fe3C30118.2(2) C28C29Fe369.6(3)
C34Fe3C31151.4(2) C30C29Fe370.7(3)
C34Fe3C3540.1(2) C30C29C28109.4(5)
C35Fe3C30108.5(2) C29C30Fe369.5(3)
C36Fe3C27117.4(2) C29C30C31108.3(5)
C36Fe3C28152.3(2) C31C30Fe369.7(3)
C36Fe3C29165.5(2) C27C31Fe369.2(3)
C36Fe3C30128.2(3) C30C31Fe370.1(3)
C36Fe3C31108.4(2) C30C31C27109.3(5)
C36Fe3C3240.5(2) C33C32Fe369.8(3)
C36Fe3C3368.4(2) C33C32C36108.5(5)
C36Fe3C3468.2(2) C36C32Fe369.7(3)
C36Fe3C3540.5(2) C32C33Fe369.7(3)
C40Fe4C4369.0(2) C32C33C34107.6(5)
C40Fe4C4441.04(18) C34C33Fe369.7(3)
C40Fe4C45107.6(2) C33C34Fe369.7(3)
C41Fe4C4041.75(18) C35C34Fe370.5(3)
C41Fe4C4240.36(19) C35C34C33108.1(5)
C41Fe4C4368.6(2) C34C35Fe369.4(3)
C41Fe4C4468.9(2) C34C35C36108.3(5)
C41Fe4C45124.1(2) C36C35Fe369.1(3)
C41Fe4C46106.4(2) C32C36Fe369.8(3)
C41Fe4C47120.0(3) C32C36C35107.5(5)
C41Fe4C48155.7(3) C35C36Fe370.4(3)
C41Fe4C49160.5(3) N3C37C28112.9(5)
C42Fe4C4068.9(2) Si4C40Fe4121.7(2)
C42Fe4C4340.6(2) C41C40Fe468.4(3)
C42Fe4C4468.0(2) C41C40Si4130.1(3)
C42Fe4C45160.1(3) C44C40Fe469.5(3)
C42Fe4C48121.9(3) C44C40Si4123.5(3)
C42Fe4C49158.2(3) C44C40C41106.1(4)
C43Fe4C4440.4(2) C40C41Fe469.8(3)
C43Fe4C45158.2(3) C40C41C50126.3(4)
C44Fe4C45123.1(3) C42C41Fe470.2(3)
C46Fe4C40120.4(3) C42C41C40108.1(4)
C46Fe4C42123.9(3) C42C41C50125.7(5)
C46Fe4C43160.9(3) C50C41Fe4125.4(3)
C46Fe4C44156.9(3) C41C42Fe469.4(3)
C46Fe4C4539.7(3) C41C42C43109.2(5)
C46Fe4C4739.8(3) C43C42Fe470.1(3)
C46Fe4C4867.8(3) C42C43Fe469.3(3)
C46Fe4C4967.8(3) C44C43Fe469.9(3)
C47Fe4C40155.5(3) C44C43C42107.8(5)
C47Fe4C42107.9(3) C40C44Fe469.4(3)
C47Fe4C43125.4(3) C43C44Fe469.8(3)
C47Fe4C44162.2(3) C43C44C40108.9(5)
C47Fe4C4566.6(3) C46C45Fe469.4(4)
C47Fe4C4840.5(3) C46C45C49109.7(7)
C47Fe4C4968.3(3) C49C45Fe469.8(4)
C48Fe4C40161.9(3) C45C46Fe470.9(4)
C48Fe4C43108.8(3) C47C46Fe470.1(4)
C48Fe4C44125.7(3) C47C46C45108.2(7)
C48Fe4C4567.4(3) C46C47Fe470.1(4)
C49Fe4C40123.7(3) C46C47C48108.9(7)
C49Fe4C43122.9(3) C48C47Fe470.4(4)
C49Fe4C44108.7(2) C47C48Fe469.2(4)
C49Fe4C4539.9(3) C47C48C49106.7(6)
C49Fe4C4841.3(3) C49C48Fe469.3(4)
O1Si1O2111.9(2) C45C49Fe470.3(4)
O1Si1O8109.26(19) C45C49C48106.5(6)
O1Si1C1109.7(2) C48C49Fe469.4(4)
O2Si1O8107.00(17) N4C50C41113.4(4)

 

Table 6 Hydrogen Bonds for 3021.
DHAd(D-H)/Åd(H-A)/Åd(D-A)/ÅD-H-A/°
O1H1AN21.00(2)1.69(3)2.661(6)163(6)
O1H1BO91.01(2)1.87(4)2.836(6)159(8)
O3H3N30.98(2)1.82(3)2.775(6)163(6)
O5H5N40.971(19)1.75(2)2.688(6)162(4)
O7H7N10.96(2)1.79(3)2.722(5)162(5)

 

Table 7 Torsion Angles for 3021.
ABCDAngle/˚ ABCDAngle/˚
Fe1C1C2C3-59.6(4) O8Si4C40C41-31.1(5)
Fe1C1C2C11117.1(5) O8Si4C40C44141.6(4)
Fe1C1C5C459.1(4) C1Si1O2Si2173.0(3)
Fe1C2C3C4-59.0(4) C1Si1O8Si498.8(4)
Fe1C2C11N1169.5(3) C1C2C3Fe159.1(3)
Fe1C3C4C5-59.4(4) C1C2C3C40.1(6)
Fe1C4C5C1-58.9(4) C1C2C11N182.0(6)
Fe1C6C7C859.2(4) C2C1C5Fe1-59.6(3)
Fe1C6C10C9-60.1(4) C2C1C5C4-0.6(6)
Fe1C7C8C960.3(4) C2C3C4Fe158.9(4)
Fe1C8C9C1059.3(4) C2C3C4C5-0.5(6)
Fe1C9C10C659.6(4) C3C2C11N1-102.0(6)
Fe2C14C15C1660.9(4) C3C4C5Fe159.5(4)
Fe2C14C15C24-117.5(5) C3C4C5C10.6(6)
Fe2C14C18C17-58.2(4) C5C1C2Fe159.8(3)
Fe2C15C16C1758.2(4) C5C1C2C30.3(6)
Fe2C15C24N2-166.2(3) C5C1C2C11176.9(5)
Fe2C16C17C1859.5(4) C6C7C8Fe1-59.1(4)
Fe2C17C18C1457.5(4) C6C7C8C91.2(7)
Fe2C19C20C21-58.7(4) C7C6C10Fe160.3(4)
Fe2C19C23C2260.3(5) C7C6C10C90.2(7)
Fe2C20C21C22-60.5(4) C7C8C9Fe1-60.4(4)
Fe2C21C22C23-58.6(5) C7C8C9C10-1.1(6)
Fe2C22C23C19-60.3(4) C8C9C10Fe1-59.0(4)
Fe3C27C28C29-59.3(3) C8C9C10C60.6(6)
Fe3C27C28C37119.3(5) C10C6C7Fe1-60.1(4)
Fe3C27C31C3058.7(4) C10C6C7C8-0.9(7)
Fe3C28C29C30-59.7(4) C11C2C3Fe1-117.5(5)
Fe3C28C37N3168.6(4) C11C2C3C4-176.5(5)
Fe3C29C30C31-59.2(4) C12N1C11C261.4(6)
Fe3C30C31C27-58.2(4) C13N1C11C2-176.1(4)
Fe3C32C33C3459.7(4) C14Si2O2Si1-95.7(4)
Fe3C32C36C35-60.7(4) C14Si2O4Si3-178.4(3)
Fe3C33C34C3560.2(4) C14C15C16Fe2-59.8(3)
Fe3C34C35C3658.3(4) C14C15C16C17-1.5(6)
Fe3C35C36C3260.3(4) C14C15C24N2-79.1(6)
Fe4C40C41C4260.0(4) C15C14C18Fe259.0(3)
Fe4C40C41C50-119.7(5) C15C14C18C170.8(6)
Fe4C40C44C43-58.7(4) C15C16C17Fe2-57.5(4)
Fe4C41C42C4359.0(4) C15C16C17C182.0(6)
Fe4C41C50N4-170.0(3) C16C15C24N2102.8(6)
Fe4C42C43C4459.5(4) C16C17C18Fe2-59.3(4)
Fe4C43C44C4058.5(3) C16C17C18C14-1.7(6)
Fe4C45C46C47-60.5(5) C18C14C15Fe2-60.4(3)
Fe4C45C49C4860.3(4) C18C14C15C160.4(6)
Fe4C46C47C48-59.9(5) C18C14C15C24-177.9(5)
Fe4C47C48C49-59.4(4) C19C20C21Fe258.8(4)
Fe4C48C49C45-60.9(4) C19C20C21C22-1.6(7)
Si1C1C2Fe1-116.3(4) C20C19C23Fe2-60.4(4)
Si1C1C2C3-175.9(4) C20C19C23C220.0(7)
Si1C1C2C110.8(7) C20C21C22Fe260.2(4)
Si1C1C5Fe1116.7(4) C20C21C22C231.6(7)
Si1C1C5C4175.7(4) C21C22C23Fe259.3(4)
Si2C14C15Fe2114.9(4) C21C22C23C19-1.0(7)
Si2C14C15C16175.7(4) C23C19C20Fe259.8(4)
Si2C14C15C24-2.6(8) C23C19C20C211.0(7)
Si2C14C18Fe2-116.5(4) C24C15C16Fe2118.6(5)
Si2C14C18C17-174.8(4) C24C15C16C17176.8(5)
Si3C27C28Fe3-117.0(4) C25N2C24C15-65.0(6)
Si3C27C28C29-176.2(4) C26N2C24C15173.7(4)
Si3C27C28C372.3(7) C27Si3O4Si2100.5(3)
Si3C27C31Fe3117.6(4) C27Si3O6Si4177.0(3)
Si3C27C31C30176.4(4) C27C28C29Fe359.1(3)
Si4C40C41Fe4113.9(4) C27C28C29C30-0.6(6)
Si4C40C41C42174.0(4) C27C28C37N380.3(6)
Si4C40C41C50-5.8(7) C28C27C31Fe3-59.9(3)
Si4C40C44Fe4-115.2(3) C28C27C31C30-1.1(6)
Si4C40C44C43-173.9(4) C28C29C30Fe359.1(4)
O1Si1O2Si251.4(4) C28C29C30C31-0.1(6)
O1Si1O8Si4-140.9(3) C29C28C37N3-101.5(6)
O1Si1C1Fe162.5(3) C29C30C31Fe359.0(4)
O1Si1C1C2151.0(4) C29C30C31C270.8(6)
O1Si1C1C5-24.4(5) C31C27C28Fe360.3(3)
O2Si1O8Si4-19.6(4) C31C27C28C291.1(5)
O2Si1C1Fe1-60.4(3) C31C27C28C37179.6(5)
O2Si1C1C228.1(5) C32C33C34Fe3-59.7(4)
O2Si1C1C5-147.4(4) C32C33C34C350.5(6)
O2Si2O4Si364.8(4) C33C32C36Fe359.2(4)
O2Si2C14Fe2178.3(2) C33C32C36C35-1.5(6)
O2Si2C14C1591.2(5) C33C34C35Fe3-59.7(4)
O2Si2C14C18-94.3(5) C33C34C35C36-1.4(6)
O3Si2O2Si1144.7(3) C34C35C36Fe3-58.5(4)
O3Si2O4Si3-55.8(4) C34C35C36C321.8(6)
O3Si2C14Fe2-63.0(3) C36C32C33Fe3-59.1(4)
O3Si2C14C15-150.1(4) C36C32C33C340.6(6)
O3Si2C14C1824.3(5) C37C28C29Fe3-119.4(5)
O4Si2O2Si122.1(4) C37C28C29C30-179.1(5)
O4Si2C14Fe260.6(3) C38N3C37C28-179.5(5)
O4Si2C14C15-26.5(5) C39N3C37C2856.4(6)
O4Si2C14C18147.9(4) C40Si4O6Si3-101.4(3)
O4Si3O6Si4-63.9(4) C40Si4O8Si1-175.7(3)
O4Si3C27Fe3179.9(2) C40C41C42Fe4-59.8(3)
O4Si3C27C28-90.1(4) C40C41C42C43-0.8(6)
O4Si3C27C3193.0(4) C40C41C50N4-80.2(6)
O5Si3O4Si2-141.5(3) C41C40C44Fe458.9(3)
O5Si3O6Si455.1(4) C41C40C44C430.2(6)
O5Si3C27Fe362.8(3) C41C42C43Fe4-58.6(4)
O5Si3C27C28152.8(4) C41C42C43C440.9(7)
O5Si3C27C31-24.1(5) C42C41C50N4100.1(6)
O6Si3O4Si2-19.3(4) C42C43C44Fe4-59.2(4)
O6Si3C27Fe3-61.4(3) C42C43C44C40-0.7(6)
O6Si3C27C2828.6(5) C44C40C41Fe4-59.7(3)
O6Si3C27C31-148.3(4) C44C40C41C420.4(5)
O6Si4O8Si167.1(3) C44C40C41C50-179.4(5)
O6Si4C40Fe4174.6(2) C45C46C47Fe461.0(4)
O6Si4C40C4187.2(4) C45C46C47C481.2(8)
O6Si4C40C44-100.2(4) C46C45C49Fe4-58.0(4)
O7Si4O6Si3140.0(3) C46C45C49C482.3(7)
O7Si4O8Si1-53.5(4) C46C47C48Fe459.7(5)
O7Si4C40Fe4-67.5(3) C46C47C48C490.2(8)
O7Si4C40C41-154.9(4) C47C48C49Fe459.3(5)
O7Si4C40C4417.7(4) C47C48C49C45-1.5(7)
O8Si1O2Si2-68.3(4) C49C45C46Fe458.3(4)
O8Si1C1Fe1-177.4(2) C49C45C46C47-2.2(7)
O8Si1C1C2-88.9(5) C50C41C42Fe4119.9(5)
O8Si1C1C595.6(4) C50C41C42C43178.9(5)
O8Si4O6Si317.1(4) C51N4C50C41-179.6(4)
O8Si4C40Fe456.4(3) C52N4C50C41-57.4(5)

 

Table 8 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for 3021.
AtomxyzU(eq)
H1A1470(40)5660(30)6867(19)80(20)
H1B2160(70)4640(50)7040(20)190(40)
H32360(30)7830(40)5440(20)90(20)
H54240(30)7330(30)7093(14)43(15)
H73980(30)5180(30)5574(16)69(19)
H3A18042150537066
H417751497612774
H5A21322898665559
H6-3004297531579
H7A-6822488534983
H8-6482025613975
H9-3093578658761
H10-754980607365
H11A17593922501553
H11B17664849533553
H12A333432904818113
H12B378931655317113
H12C438238124997113
H13A275558334918108
H13B262749524571108
H13C373153734736108
H16-15667649660956
H17-20867527580060
H18-5267127544656
H1913889409592677
H208199684664681
H21-10809998655772
H22-16459991574777
H23-1289595535892
H24A11647869688352
H24B1597850711952
H25A-46058416974104
H25B-34763467444104
H25C24353417370104
H26A12297113772893
H26B21657087744893
H26C17936091765893
H29448410940566961
H30414411503640666
H31362210029682154
H3261298042656159
H3366608974592067
H34685910777613462
H35647910945690862
H3659669264716665
H37A46899192528557
H37B45928229557657
H38A381473634961159
H38B390583204664159
H38C282877994678159
H39A313298784884156
H39B259498815319156
H39C208493044898156
H4273905235732662
H4381105251660966
H4466965676602251
H4545873497622678
H4649233337703089
H47673828977224101
H4875822836653690
H4962153270590494
H50A46245283720655
H50B55685228757755
H51A467062058046111
H51B372062567677111
H51C420772537887111
H52A64297183738793
H52B63466766786593
H52C58337801771793

Experimental

Single crystals of C52H69Fe4N4O9Si4 [3021] were [The material was recrystallised from a mixture of acetone and water by slow evaporation]. A suitable crystal was selected and [The crystal was mounted on a MITIGEN holder oil] on a Xcalibur, Sapphire3 diffractometer. The crystal was kept at 173 K during data collection. Using Olex2 [1], the structure was solved with the XS [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 [3021]

Crystal Data for C52H69Fe4N4O9Si4 (=1229.87 g/mol): monoclinic, space group P21/n (no. 14), a = 13.2912(7) Å, b = 13.5363(7) Å, c = 30.9964(18) Å, β = 96.859(5)°, = 5536.8(5) Å3, Z = 4, T = 173 K, μ(MoKα) = 1.171 mm-1, Dcalc = 1.475 g/cm3, 42828 reflections measured (4.31° ≤ 2Θ ≤ 53.998°), 11995 unique (Rint = 0.0745, Rsigma = 0.0936) which were used in all calculations. The final R1 was 0.0634 (I > 2σ(I)) and wR2 was 0.1626 (all data).

Refinement model description

Number of restraints - 5, 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
O7-H7 = O5-H5 = O3-H3 = O1-H1A
1 with sigma of 0.02
O1-H1B
1 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
C11(H11A,H11B), C24(H24A,H24B), C37(H37A,H37B), C50(H50A,H50B)
3.b Aromatic/amide H refined with riding coordinates:
C3(H3A), C4(H4), C5(H5A), C6(H6), C7(H7A), C8(H8), C9(H9), C10(H10), C16(H16),
C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23),
C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36),
C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49)
3.c Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C25(H25A,H25B,H25C), C26(H26A,H26B,
H26C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C51(H51A,H51B,H51C), C52(H52A,
H52B,H52C)

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.