mo_B0110_0m

Table 1 Crystal data and structure refinement for mo_B0110_0m.
Identification code mo_B0110_0m
Empirical formula C46H52Fe4N2O3Si2
Formula weight 960.47
Temperature/K 100.0
Crystal system orthorhombic
Space group P212121
a/Å 12.9792(18)
b/Å 14.0736(18)
c/Å 23.484(3)
α/° 90
β/° 90
γ/° 90
Volume/Å3 4289.6(10)
Z 4
ρcalcg/cm3 1.487
μ/mm‑1 1.425
F(000) 1992.0
Crystal size/mm3 0.413 × 0.387 × 0.214
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 5.502 to 55.99
Index ranges -12 ≤ h ≤ 17, -13 ≤ k ≤ 18, -24 ≤ l ≤ 30
Reflections collected 30567
Independent reflections 10295 [Rint = 0.0442, Rsigma = 0.0536]
Data/restraints/parameters 10295/0/526
Goodness-of-fit on F2 1.027
Final R indexes [I>=2σ (I)] R1 = 0.0333, wR2 = 0.0661
Final R indexes [all data] R1 = 0.0421, wR2 = 0.0688
Largest diff. peak/hole / e Å-3 0.45/-0.44
Flack parameter-0.006(7)

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for mo_B0110_0m. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Fe16373.6(4)9211.1(3)6833.0(2)16.30(11)
Fe27628.0(4)5858.7(3)8396.3(2)14.04(11)
Fe39733.5(4)3766.6(3)5998.2(2)14.16(11)
Fe45133.3(4)4496.1(3)5933.3(2)15.33(11)
Si17339.6(8)6955.0(6)7073.9(4)12.21(18)
Si27604.1(7)5186.4(6)6279.3(4)12.71(19)
O17228.3(19)5913.8(14)6776.3(9)16.1(5)
O28484(2)7388.2(16)7016.3(10)16.7(5)
O37805(2)5712.1(18)5677.6(10)18.7(5)
N17397(2)7512.2(18)5357.5(11)18.7(6)
N210281(2)6633.9(17)6722.1(11)16.3(6)
C16416(3)7773(2)6715.8(13)13.7(7)
C26517(3)8280(2)6181.0(13)15.7(7)
C35608(3)8846(2)6104.7(14)20.4(8)
C44952(3)8710(2)6577.9(14)20.7(7)
C55437(3)8055(2)6949.9(14)16.3(7)
C67760(3)9555(2)7178.5(15)23.3(8)
C77523(3)10187(2)6728.0(16)26.4(9)
C86591(3)10655(2)6860.1(16)28.0(9)
C96253(3)10319(2)7397.8(15)24.2(8)
C106976(3)9639(2)7595.0(15)21.0(8)
C117429(3)8274(2)5788.2(13)18.7(7)
C128348(3)7551(3)5015.1(16)28.1(9)
C136509(3)7619(3)4981.8(15)25.8(9)
C146980(3)6814(2)7832.9(13)12.8(7)
C157431(3)7289(2)8318.7(13)14.7(7)
C166945(3)6952(2)8822.7(14)16.7(7)
C176202(3)6271(2)8669.0(13)17.8(7)
C186218(3)6183(2)8062.6(13)15.0(7)
C198753(3)5114(2)7975.7(15)21.6(8)
C209178(3)5569(2)8461.4(14)21.8(8)
C218633(3)5235(2)8949.7(14)24.3(8)
C227887(3)4570(2)8762.2(16)25.8(8)
C237956(3)4496(2)8158.6(16)23.5(8)
C249874(3)4954(2)6481.8(12)14.9(7)
C258828(3)4614(2)6503.2(12)12.5(7)
C268886(3)3659(2)6729.3(12)14.9(7)
C279931(3)3433(2)6844.5(13)16.6(7)
C2810541(3)4229(2)6690.5(13)15.3(7)
C2910144(3)4133(3)5189.5(14)28.8(9)
C309115(3)3823(3)5197.7(14)24.9(8)
C319102(3)2873(3)5407.0(15)26.8(9)
C3210136(4)2610(3)5522.9(15)30.8(10)
C3310781(3)3383(3)5391.4(15)30.1(9)
C3410247(3)5908(2)6269.8(13)16.4(7)
C3510622(3)7542(2)6477.0(16)24.2(8)
C3610983(3)6368(2)7184.8(15)21.4(8)
C376597(3)4264(2)6239.4(13)13.9(7)
C386361(3)3635(2)5773.5(13)16.8(7)
C395494(3)3077(2)5915.7(15)18.5(7)
C405163(3)3344(2)6475.1(13)17.4(7)
C415838(3)4067(2)6671.0(13)16.2(7)
C425048(3)5468(2)5290.4(14)26.0(9)
C434248(4)4803(3)5237.4(18)35.7(11)
C443639(3)4841(3)5740(2)38.6(11)
C454069(3)5546(3)6098.4(16)28.8(9)
C464939(3)5930(2)5824.4(14)20.9(8)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for mo_B0110_0m. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Fe118.3(3)13.08(19)17.5(2)-0.13(18)-4.2(2)1.9(2)
Fe215.2(3)13.54(19)13.3(2)2.22(17)-0.2(2)3.14(19)
Fe316.8(3)13.93(19)11.8(2)-0.87(17)0.1(2)1.04(19)
Fe414.1(3)16.2(2)15.6(2)-0.04(17)-2.3(2)-0.51(19)
Si112.9(5)11.4(3)12.3(4)0.6(3)-0.4(4)0.3(4)
Si213.6(5)11.6(3)12.8(4)-0.2(3)-0.9(4)-0.1(4)
O119.5(13)13.9(10)15(1)-0.3(8)0.4(10)-0.4(10)
O213.3(14)14.6(10)22.1(12)1.6(9)0.7(11)0.5(10)
O322.5(15)15.7(12)18.0(12)3.4(9)2.7(11)3.4(11)
N124.9(18)17.8(12)13.3(12)1.8(10)1.8(13)-1.4(13)
N214.7(15)13.7(11)20.5(14)-1.2(10)0.7(13)-1.3(11)
C114.4(18)12.7(13)14.1(15)-2.2(11)-4.6(14)0.3(13)
C215.5(19)15.9(14)15.8(15)-2.1(12)-2.7(15)-0.3(13)
C325(2)17.4(15)19.2(17)2.3(13)-8.9(15)1.9(15)
C416.4(19)18.9(15)26.9(17)-2.1(13)-4.2(16)1.9(14)
C515(2)16.2(14)17.4(16)-0.3(12)-2.6(14)-0.9(13)
C617(2)20.9(15)32.1(19)-8.3(14)-6.2(17)-1.9(15)
C732(2)21.4(15)25.4(18)-2.6(14)-1.6(18)-10.2(16)
C839(3)12.8(15)32.1(19)-0.7(14)-13.5(19)-0.5(15)
C924(2)20.4(16)28.3(18)-9.7(14)-7.6(18)4.8(16)
C1023(2)19.0(15)20.9(17)-2.6(13)-6.1(16)1.9(15)
C1122(2)18.0(14)15.7(15)2.9(12)-2.0(15)-2.6(14)
C1236(3)26.2(18)21.7(17)2.5(15)11.5(18)-5.7(17)
C1336(2)24.4(17)17.3(16)0.9(14)-7.2(18)-4.5(17)
C149.9(18)12.8(14)15.7(15)0.9(11)-1.1(14)2.4(12)
C1516.5(19)12.9(12)14.7(14)-0.4(11)1.3(14)1.3(13)
C1620(2)16.7(14)13.5(15)-0.4(12)1.3(15)3.8(14)
C1719(2)16.7(15)17.8(15)3.6(13)5.2(15)4.2(14)
C1812.9(18)13.9(13)18.2(15)0.6(12)-1.6(14)1.0(13)
C1920(2)22.2(16)22.4(17)-0.9(14)-0.7(17)10.3(15)
C2017(2)25.5(17)22.8(17)0.1(14)-2.4(16)8.9(15)
C2127(2)29.5(17)16.7(16)6.2(14)-3.6(17)11.1(17)
C2226(2)18.7(16)32.1(19)11.4(15)1.9(18)8.0(16)
C2325(2)14.2(14)30.9(19)-1.0(14)-3.3(17)5.8(15)
C2417.3(19)14.6(14)12.7(14)-2.5(11)0.7(15)-1.3(13)
C2513.5(18)14.7(14)9.2(14)-2.0(11)-1.7(13)0.1(12)
C2616.1(19)15.0(14)13.7(15)-0.1(11)0.4(14)-2.1(13)
C2720(2)17.8(14)12.5(14)1.5(12)0.5(15)0.8(14)
C2811.7(17)20.1(14)14.1(15)-2.5(12)-1.6(13)2.1(13)
C2944(3)27.5(17)14.5(15)-0.4(14)6.9(18)-3.9(19)
C3030(2)32.0(18)12.3(15)-5.3(14)-5.5(16)6.1(18)
C3132(2)28.6(19)19.6(17)-10.1(15)-1.0(18)-6.8(18)
C3251(3)23.9(17)17.4(16)-5.4(14)2.6(19)12(2)
C3323(2)48(2)18.6(18)-9.5(17)2.4(17)7.2(19)
C3414.9(18)15.9(14)18.4(15)0.7(12)1.1(15)-2.5(14)
C3525(2)15.4(15)32(2)-2.0(14)5.2(17)-4.4(15)
C3616(2)24.4(17)24.1(17)-6.2(14)-1.6(16)-1.7(15)
C3712.3(18)12.9(13)16.3(15)-0.1(12)-2.6(14)1.6(13)
C3815.3(19)18.1(14)17.0(15)-2.4(12)-0.8(15)1.5(14)
C3919(2)14.7(14)21.6(17)-2.3(13)-5.6(16)-1.8(13)
C4016.0(19)16.9(14)19.2(16)2.5(12)-3.1(15)-4.4(14)
C4119.1(19)16.0(14)13.6(15)0.2(12)-2.6(14)-0.3(13)
C4234(3)25.1(16)18.9(16)6.6(14)1.3(17)12.2(17)
C4348(3)25.7(18)33(2)-4.5(17)-24(2)9(2)
C4416(2)35(2)65(3)18(2)-13(2)-0.7(19)
C4526(2)34(2)26.2(19)7.1(16)6.1(17)13.1(18)
C4621(2)17.7(15)23.4(17)0.4(13)-6.3(16)3.4(15)

 

Table 4 Bond Lengths for mo_B0110_0m.
AtomAtomLength/Å AtomAtomLength/Å
Fe1C12.044(3) N1C111.474(4)
Fe1C22.023(3) N1C121.473(5)
Fe1C32.043(3) N1C131.459(5)
Fe1C42.064(4) N2C341.474(4)
Fe1C52.050(3) N2C351.470(4)
Fe1C62.033(4) N2C361.467(5)
Fe1C72.043(4) C1C21.451(4)
Fe1C82.052(3) C1C51.440(5)
Fe1C92.053(3) C2C31.434(5)
Fe1C102.043(3) C2C111.501(5)
Fe2C142.065(3) C3C41.413(5)
Fe2C152.038(3) C4C51.417(4)
Fe2C162.039(3) C6C71.417(5)
Fe2C172.042(4) C6C101.417(5)
Fe2C182.042(3) C7C81.411(6)
Fe2C192.050(4) C8C91.417(5)
Fe2C202.058(4) C9C101.418(5)
Fe2C212.040(3) C14C151.447(4)
Fe2C222.035(3) C14C181.434(4)
Fe2C232.042(3) C15C161.423(5)
Fe3C242.028(3) C16C171.406(5)
Fe3C252.052(3) C17C181.429(4)
Fe3C262.045(3) C19C201.420(5)
Fe3C272.058(3) C19C231.417(5)
Fe3C282.041(3) C20C211.426(5)
Fe3C292.039(3) C21C221.417(5)
Fe3C302.046(3) C22C231.424(5)
Fe3C312.045(4) C24C251.441(5)
Fe3C322.042(3) C24C281.424(4)
Fe3C332.042(4) C24C341.512(4)
Fe4C372.057(3) C25C261.447(4)
Fe4C382.037(3) C26C271.420(5)
Fe4C392.052(3) C27C281.420(4)
Fe4C402.061(3) C29C301.405(6)
Fe4C412.050(3) C29C331.423(5)
Fe4C422.040(3) C30C311.424(5)
Fe4C432.044(4) C31C321.419(6)
Fe4C442.050(4) C32C331.407(6)
Fe4C452.060(4) C37C381.440(4)
Fe4C462.050(3) C37C411.440(5)
Si1O11.630(2) C38C391.413(5)
Si1O21.611(3) C39C401.432(5)
Si1C11.863(3) C40C411.419(4)
Si1C141.853(3) C42C431.404(6)
Si2O11.627(2) C42C461.420(5)
Si2O31.616(3) C43C441.422(6)
Si2C251.857(3) C44C451.416(6)
Si2C371.845(3) C45C461.407(5)

 

Table 5 Bond Angles for mo_B0110_0m.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C1Fe1C469.29(13) C44Fe4C39116.22(16)
C1Fe1C541.20(13) C44Fe4C40109.89(16)
C1Fe1C8168.85(15) C44Fe4C41132.73(17)
C1Fe1C9147.30(14) C44Fe4C4540.30(17)
C2Fe1C141.79(12) C44Fe4C4667.86(16)
C2Fe1C341.29(13) C45Fe4C40117.44(14)
C2Fe1C468.98(14) C46Fe4C37108.26(14)
C2Fe1C569.02(13) C46Fe4C39169.71(14)
C2Fe1C6112.01(15) C46Fe4C40148.61(13)
C2Fe1C7106.09(15) C46Fe4C4540.05(15)
C2Fe1C8130.67(14) O1Si1C1107.75(13)
C2Fe1C9170.91(14) O1Si1C14107.07(13)
C2Fe1C10144.90(14) O2Si1O1112.70(13)
C3Fe1C169.60(13) O2Si1C1108.77(14)
C3Fe1C440.25(14) O2Si1C14110.70(14)
C3Fe1C567.94(13) C14Si1C1109.78(15)
C3Fe1C8109.97(14) O1Si2C25109.04(13)
C3Fe1C9133.99(15) O1Si2C37105.46(14)
C3Fe1C10173.20(15) O3Si2O1112.79(12)
C5Fe1C440.31(13) O3Si2C25107.98(14)
C5Fe1C8149.70(16) O3Si2C37113.07(14)
C5Fe1C9118.12(15) C37Si2C25108.36(14)
C6Fe1C1105.42(14) Si2O1Si1147.84(16)
C6Fe1C3145.51(15) C12N1C11108.9(3)
C6Fe1C4171.37(14) C13N1C11111.2(3)
C6Fe1C5131.36(14) C13N1C12109.1(3)
C6Fe1C740.69(15) C35N2C34109.2(2)
C6Fe1C868.29(15) C36N2C34112.1(3)
C6Fe1C968.21(15) C36N2C35108.9(3)
C6Fe1C1040.68(15) Si1C1Fe1124.63(16)
C7Fe1C1129.09(15) C2C1Fe168.36(16)
C7Fe1C3115.01(14) C2C1Si1129.6(3)
C7Fe1C4147.92(14) C5C1Fe169.62(17)
C7Fe1C5169.49(15) C5C1Si1124.5(2)
C7Fe1C840.30(16) C5C1C2105.9(3)
C7Fe1C967.82(16) C1C2Fe169.85(17)
C7Fe1C1068.18(15) C1C2C11126.9(3)
C8Fe1C4118.05(15) C3C2Fe170.09(18)
C8Fe1C940.40(15) C3C2C1107.9(3)
C9Fe1C4112.27(15) C3C2C11125.1(3)
C10Fe1C1113.55(13) C11C2Fe1122.8(2)
C10Fe1C4134.17(15) C2C3Fe168.61(18)
C10Fe1C5110.09(14) C4C3Fe170.67(19)
C10Fe1C868.19(14) C4C3C2108.8(3)
C10Fe1C940.51(14) C3C4Fe169.1(2)
C15Fe2C1441.30(12) C3C4C5107.8(3)
C15Fe2C1640.87(13) C5C4Fe169.30(19)
C15Fe2C1768.54(13) C1C5Fe169.18(18)
C15Fe2C1868.46(13) C4C5Fe170.39(19)
C15Fe2C19123.44(14) C4C5C1109.6(3)
C15Fe2C20108.95(15) C7C6Fe170.0(2)
C15Fe2C21124.19(15) C10C6Fe170.1(2)
C15Fe2C23158.36(14) C10C6C7107.8(3)
C16Fe2C1469.29(13) C6C7Fe169.3(2)
C16Fe2C1740.32(14) C8C7Fe170.2(2)
C16Fe2C1868.29(13) C8C7C6108.4(3)
C16Fe2C19158.75(15) C7C8Fe169.49(19)
C16Fe2C20122.56(15) C7C8C9107.8(3)
C16Fe2C21106.85(14) C9C8Fe169.84(19)
C16Fe2C23159.01(14) C8C9Fe169.76(19)
C17Fe2C1469.34(13) C8C9C10108.1(3)
C17Fe2C1840.97(12) C10C9Fe169.37(19)
C17Fe2C19160.25(14) C6C10Fe169.3(2)
C17Fe2C20156.71(13) C6C10C9107.8(3)
C17Fe2C23122.78(15) C9C10Fe170.12(19)
C18Fe2C1440.87(13) N1C11C2113.9(3)
C18Fe2C19124.56(14) Si1C14Fe2125.70(17)
C18Fe2C20161.54(13) C15C14Fe268.35(17)
C19Fe2C14108.30(13) C15C14Si1127.3(2)
C19Fe2C2040.43(14) C18C14Fe268.72(17)
C20Fe2C14125.08(14) C18C14Si1127.0(2)
C21Fe2C14161.56(15) C18C14C15105.6(3)
C21Fe2C17120.12(14) C14C15Fe270.36(16)
C21Fe2C18156.01(14) C16C15Fe269.61(17)
C21Fe2C1968.40(14) C16C15C14108.7(3)
C21Fe2C2040.74(14) C15C16Fe269.52(18)
C21Fe2C2368.71(15) C17C16Fe269.96(19)
C22Fe2C14156.64(15) C17C16C15108.6(3)
C22Fe2C15159.90(14) C16C17Fe269.7(2)
C22Fe2C16122.49(15) C16C17C18107.8(3)
C22Fe2C17105.70(15) C18C17Fe269.5(2)
C22Fe2C18120.62(15) C14C18Fe270.40(19)
C22Fe2C1968.29(15) C17C18Fe269.5(2)
C22Fe2C2068.30(16) C17C18C14109.3(3)
C22Fe2C2140.69(15) C20C19Fe270.1(2)
C22Fe2C2340.89(15) C23C19Fe269.4(2)
C23Fe2C14121.40(13) C23C19C20108.5(3)
C23Fe2C18106.97(14) C19C20Fe269.5(2)
C23Fe2C1940.52(14) C19C20C21107.8(3)
C23Fe2C2068.30(15) C21C20Fe268.9(2)
C24Fe3C2541.37(13) C20C21Fe270.3(2)
C24Fe3C2668.86(12) C22C21Fe269.48(19)
C24Fe3C2768.66(12) C22C21C20107.8(3)
C24Fe3C2840.97(13) C21C22Fe269.83(19)
C24Fe3C29106.83(14) C21C22C23108.3(3)
C24Fe3C30121.20(14) C23C22Fe269.82(19)
C24Fe3C31157.34(15) C19C23Fe270.06(19)
C24Fe3C32160.00(17) C19C23C22107.6(3)
C24Fe3C33123.26(16) C22C23Fe269.3(2)
C25Fe3C2769.26(12) C25C24Fe370.19(17)
C26Fe3C2541.35(12) C25C24C34127.4(3)
C26Fe3C2740.49(13) C28C24Fe370.01(17)
C26Fe3C30124.29(15) C28C24C25108.9(3)
C28Fe3C2569.43(13) C28C24C34123.7(3)
C28Fe3C2668.37(13) C34C24Fe3125.2(2)
C28Fe3C2740.52(12) Si2C25Fe3125.35(15)
C28Fe3C30157.08(14) C24C25Fe368.44(17)
C28Fe3C31160.56(14) C24C25Si2130.7(2)
C28Fe3C32123.94(15) C24C25C26105.8(3)
C28Fe3C33107.35(15) C26C25Fe369.08(17)
C29Fe3C25122.75(14) C26C25Si2123.5(3)
C29Fe3C26160.28(16) C25C26Fe369.57(17)
C29Fe3C27157.63(16) C27C26Fe370.26(19)
C29Fe3C28121.80(16) C27C26C25109.1(3)
C29Fe3C3040.23(16) C26C27Fe369.26(18)
C29Fe3C3168.15(16) C28C27Fe369.09(18)
C29Fe3C3268.02(15) C28C27C26107.9(3)
C29Fe3C3340.81(15) C24C28Fe369.02(17)
C30Fe3C25106.49(14) C27C28Fe370.38(19)
C30Fe3C27160.93(15) C27C28C24108.3(3)
C31Fe3C25121.32(15) C30C29Fe370.2(2)
C31Fe3C26107.98(15) C30C29C33108.5(3)
C31Fe3C27124.42(14) C33C29Fe369.7(2)
C31Fe3C3040.76(15) C29C30Fe369.6(2)
C32Fe3C25157.80(16) C29C30C31108.0(4)
C32Fe3C26122.53(14) C31C30Fe369.6(2)
C32Fe3C27108.30(14) C30C31Fe369.7(2)
C32Fe3C3068.22(15) C32C31Fe369.6(2)
C32Fe3C3140.64(17) C32C31C30107.4(4)
C32Fe3C3340.30(16) C31C32Fe369.8(2)
C33Fe3C25159.79(15) C33C32Fe369.9(2)
C33Fe3C26157.60(15) C33C32C31108.6(3)
C33Fe3C27122.04(15) C29C33Fe369.5(2)
C33Fe3C3068.29(16) C32C33Fe369.8(2)
C33Fe3C3168.32(17) C32C33C29107.5(4)
C37Fe4C4069.02(14) N2C34C24112.8(2)
C37Fe4C45131.86(15) Si2C37Fe4124.08(16)
C38Fe4C3741.18(12) C38C37Fe468.67(19)
C38Fe4C3940.43(13) C38C37Si2128.4(3)
C38Fe4C4068.36(14) C38C37C41105.7(3)
C38Fe4C4168.36(13) C41C37Fe469.22(19)
C38Fe4C42107.75(14) C41C37Si2125.8(2)
C38Fe4C43114.72(15) C37C38Fe470.15(19)
C38Fe4C44147.19(16) C39C38Fe470.33(19)
C38Fe4C45170.46(15) C39C38C37109.3(3)
C38Fe4C46131.21(14) C38C39Fe469.24(18)
C39Fe4C3769.01(13) C38C39C40108.0(3)
C39Fe4C4040.76(13) C40C39Fe469.97(18)
C39Fe4C45148.80(16) C39C40Fe469.26(18)
C41Fe4C3741.05(13) C41C40Fe469.40(17)
C41Fe4C3968.19(13) C41C40C39107.5(3)
C41Fe4C4040.38(12) C37C41Fe469.73(18)
C41Fe4C45110.58(14) C40C41Fe470.22(18)
C41Fe4C46116.76(13) C40C41C37109.4(3)
C42Fe4C37114.52(15) C43C42Fe470.0(2)
C42Fe4C39130.55(14) C43C42C46108.1(4)
C42Fe4C40170.11(13) C46C42Fe470.06(19)
C42Fe4C41147.88(15) C42C43Fe469.8(2)
C42Fe4C4340.22(16) C42C43C44108.2(4)
C42Fe4C4468.08(17) C44C43Fe469.9(2)
C42Fe4C4567.78(14) C43C44Fe469.4(2)
C42Fe4C4640.62(13) C45C44Fe470.2(2)
C43Fe4C37146.32(17) C45C44C43107.5(4)
C43Fe4C39108.52(15) C44C45Fe469.5(2)
C43Fe4C40132.08(16) C46C45Fe469.6(2)
C43Fe4C41171.40(17) C46C45C44108.3(3)
C43Fe4C4440.67(18) C42C46Fe469.32(18)
C43Fe4C4567.80(16) C45C46Fe470.3(2)
C43Fe4C4667.88(15) C45C46C42107.9(3)
C44Fe4C37171.28(17)     

 

Table 6 Hydrogen Bonds for mo_B0110_0m.
DHAd(D-H)/Åd(H-A)/Åd(D-A)/ÅD-H-A/°
O2H2N20.84(4)1.84(5)2.654(4)163(4)
O3H3N10.65(5)2.06(5)2.695(4)166(6)

 

Table 7 Torsion Angles for mo_B0110_0m.
ABCDAngle/˚ ABCDAngle/˚
Fe1C1C2C3-60.0(2) C5C1C2Fe159.8(2)
Fe1C1C2C11116.5(3) C5C1C2C3-0.2(3)
Fe1C1C5C458.9(2) C5C1C2C11176.3(3)
Fe1C2C3C4-59.4(2) C6C7C8Fe1-58.9(2)
Fe1C2C11N1177.6(2) C6C7C8C90.6(4)
Fe1C3C4C5-58.7(2) C7C6C10Fe160.1(2)
Fe1C4C5C1-58.2(2) C7C6C10C90.4(4)
Fe1C6C7C859.5(2) C7C8C9Fe1-59.3(2)
Fe1C6C10C9-59.8(2) C7C8C9C10-0.4(4)
Fe1C7C8C959.6(2) C8C9C10Fe1-59.2(2)
Fe1C8C9C1058.9(2) C8C9C10C60.0(4)
Fe1C9C10C659.2(2) C10C6C7Fe1-60.1(2)
Fe2C14C15C16-59.2(2) C10C6C7C8-0.6(4)
Fe2C14C18C1758.7(2) C11C2C3Fe1-116.7(3)
Fe2C15C16C17-59.3(2) C11C2C3C4-176.1(3)
Fe2C16C17C18-59.4(2) C12N1C11C2-177.5(3)
Fe2C17C18C14-59.3(2) C13N1C11C262.1(3)
Fe2C19C20C2158.5(2) C14Si1O1Si2-152.0(3)
Fe2C19C23C22-59.4(2) C14Si1C1Fe173.3(2)
Fe2C20C21C2259.6(2) C14Si1C1C2162.7(3)
Fe2C21C22C2359.4(2) C14Si1C1C5-14.4(3)
Fe2C22C23C1959.8(2) C14C15C16Fe259.7(2)
Fe3C24C25Si2-118.7(2) C14C15C16C170.4(4)
Fe3C24C25C2659.28(19) C15C14C18Fe2-58.7(2)
Fe3C24C28C27-59.6(2) C15C14C18C170.1(4)
Fe3C24C34N2-179.2(2) C15C16C17Fe259.0(2)
Fe3C25C26C2759.3(2) C15C16C17C18-0.4(4)
Fe3C26C27C2858.4(2) C16C17C18Fe259.5(2)
Fe3C27C28C2458.8(2) C16C17C18C140.2(4)
Fe3C29C30C31-59.2(2) C18C14C15Fe258.9(2)
Fe3C29C33C3259.7(2) C18C14C15C16-0.3(3)
Fe3C30C31C32-59.6(2) C19C20C21Fe2-58.8(2)
Fe3C31C32C33-59.3(2) C19C20C21C220.7(4)
Fe3C32C33C29-59.5(2) C20C19C23Fe259.4(2)
Fe4C37C38C39-59.6(2) C20C19C23C220.0(4)
Fe4C37C41C4059.2(2) C20C21C22Fe2-60.1(2)
Fe4C38C39C40-59.4(2) C20C21C22C23-0.7(4)
Fe4C39C40C41-59.1(2) C21C22C23Fe2-59.4(2)
Fe4C40C41C37-58.9(2) C21C22C23C190.4(4)
Fe4C42C43C4459.5(3) C23C19C20Fe2-59.0(2)
Fe4C42C46C45-60.0(2) C23C19C20C21-0.5(4)
Fe4C43C44C4560.2(3) C24C25C26Fe3-58.87(19)
Fe4C44C45C4658.9(3) C24C25C26C270.4(3)
Fe4C45C46C4259.4(2) C25Si2O1Si180.5(3)
Si1C1C2Fe1-117.7(3) C25Si2C37Fe4-173.53(17)
Si1C1C2C3-177.7(2) C25Si2C37C38-84.9(3)
Si1C1C2C11-1.2(5) C25Si2C37C4198.8(3)
Si1C1C5Fe1118.7(2) C25C24C28Fe359.6(2)
Si1C1C5C4177.6(2) C25C24C28C270.0(3)
Si1C14C15Fe2-119.1(3) C25C24C34N289.8(4)
Si1C14C15C16-178.3(2) C25C26C27Fe3-58.9(2)
Si1C14C18Fe2119.4(3) C25C26C27C28-0.4(3)
Si1C14C18C17178.1(2) C26C27C28Fe3-58.5(2)
Si2C25C26Fe3119.3(2) C26C27C28C240.3(3)
Si2C25C26C27178.6(2) C28C24C25Fe3-59.5(2)
Si2C37C38Fe4-117.3(3) C28C24C25Si2-178.3(2)
Si2C37C38C39-176.9(2) C28C24C25C26-0.2(3)
Si2C37C41Fe4117.7(2) C28C24C34N2-91.1(4)
Si2C37C41C40176.9(2) C29C30C31Fe359.3(2)
O1Si1C1Fe1-170.41(18) C29C30C31C32-0.3(4)
O1Si1C1C2-81.0(3) C30C29C33Fe3-59.7(2)
O1Si1C1C5101.8(3) C30C29C33C320.1(4)
O1Si1C14Fe255.0(2) C30C31C32Fe359.6(2)
O1Si1C14C15143.6(3) C30C31C32C330.3(4)
O1Si1C14C18-34.0(3) C31C32C33Fe359.2(2)
O1Si2C25Fe3-171.76(16) C31C32C33C29-0.2(4)
O1Si2C25C24-80.8(3) C33C29C30Fe359.4(2)
O1Si2C25C26101.4(3) C33C29C30C310.2(4)
O1Si2C37Fe469.8(2) C34C24C25Fe3119.7(3)
O1Si2C37C38158.4(3) C34C24C25Si21.0(5)
O1Si2C37C41-17.8(3) C34C24C25C26179.0(3)
O2Si1O1Si2-30.0(3) C34C24C28Fe3-119.6(3)
O2Si1C1Fe1-48.0(2) C34C24C28C27-179.3(3)
O2Si1C1C241.4(3) C35N2C34C24-178.4(3)
O2Si1C1C5-135.7(3) C36N2C34C2460.8(4)
O2Si1C14Fe2-68.2(2) C37Si2O1Si1-163.3(3)
O2Si1C14C1520.4(3) C37Si2C25Fe373.9(2)
O2Si1C14C18-157.2(3) C37Si2C25C24164.8(3)
O3Si2O1Si1-39.5(3) C37Si2C25C26-12.9(3)
O3Si2C25Fe3-48.9(2) C37C38C39Fe459.5(2)
O3Si2C25C2442.0(3) C37C38C39C400.1(4)
O3Si2C25C26-135.7(2) C38C37C41Fe4-59.3(2)
O3Si2C37Fe4-53.9(2) C38C37C41C40-0.1(4)
O3Si2C37C3834.7(3) C38C39C40Fe459.0(2)
O3Si2C37C41-141.5(3) C38C39C40C41-0.1(4)
C1Si1O1Si290.0(3) C39C40C41Fe459.0(2)
C1Si1C14Fe2171.67(18) C39C40C41C370.1(4)
C1Si1C14C15-99.7(3) C41C37C38Fe459.6(2)
C1Si1C14C1882.7(3) C41C37C38C390.0(4)
C1C2C3Fe159.9(2) C42C43C44Fe4-59.5(3)
C1C2C3C40.4(4) C42C43C44C450.7(4)
C1C2C11N189.3(4) C43C42C46Fe460.0(2)
C2C1C5Fe1-59.0(2) C43C42C46C450.0(4)
C2C1C5C4-0.1(3) C43C44C45Fe4-59.7(3)
C2C3C4Fe158.2(2) C43C44C45C46-0.8(4)
C2C3C4C5-0.5(4) C44C45C46Fe4-58.8(3)
C3C2C11N1-94.8(4) C44C45C46C420.5(4)
C3C4C5Fe158.5(2) C46C42C43Fe4-60.0(2)
C3C4C5C10.4(4) C46C42C43C44-0.4(4)

 

Table 8 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for mo_B0110_0m.
AtomxyzU(eq)
H29030(30)7070(30)6980(17)29(12)
H37640(40)6140(30)5630(20)43(16)
H3A54719247578825
H443029005663625
H551587836730020
H683439147719828
H7792210281639432
H8625111112663034
H9564810516759229
H1069409300794425
H11A74688894559122
H11B80648201601822
H12A83938168482442
H12B83367043473042
H12C89467466526442
H13A58747574520639
H13B65187114469439
H13C65408239479339
H1579657751830418
H1670967153920020
H1757695930892321
H1857905771784618
H1989665208759326
H2097276015846126
H2187505426933229
H2274214231899931
H2375434104792128
H2683153249679118
H27101782851699820
H28112704272672118
H29103754742506935
H3085314183508430
H3185092487546032
H32103562012566537
H33115093401543036
H34A109455833610620
H34B97846129596220
H35A113357483634536
H35B105808041676736
H35C101777709615536
H36A107325788736932
H36B110136884746532
H36C116736256702932
H3867323601542520
H3951842607568122
H4045953085667821
H4157964373703119
H4255715588501731
H4341334397492043
H4430514462582246
H4538145730646135
H4653766413597125

Experimental

Single crystals of C46H52Fe4N2O3Si2 [mo_B0110_0m] were [The material was recrystallised from a mixture of water and acetone by slow evaporation]. A suitable crystal was selected and [The crystal was mounted on a MITIGEN holder oil] on a Bruker D8 Venture diffractometer. The crystal was kept at 100.0 K during data collection. Using Olex2 [1], the structure was solved with the XT [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. (2015). Acta Cryst. A71, 3-8.
  3. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Crystal structure determination of [mo_B0110_0m]

Crystal Data for C46H52Fe4N2O3Si2 (=960.47 g/mol): orthorhombic, space group P212121 (no. 19), a = 12.9792(18) Å, b = 14.0736(18) Å, c = 23.484(3) Å, = 4289.6(10) Å3, Z = 4, T = 100.0 K, μ(MoKα) = 1.425 mm-1, Dcalc = 1.487 g/cm3, 30567 reflections measured (5.502° ≤ 2Θ ≤ 55.99°), 10295 unique (Rint = 0.0442, Rsigma = 0.0536) which were used in all calculations. The final R1 was 0.0333 (I > 2σ(I)) and wR2 was 0.0688 (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.