mo_B0129_0m

Table 1 Crystal data and structure refinement for mo_B0129_0m.
Identification code mo_B0129_0m
Empirical formula C40H48Fe2N2O3Si2
Formula weight 772.68
Temperature/K 100.0
Crystal system monoclinic
Space group P21/n
a/Å 11.0354(10)
b/Å 19.3902(15)
c/Å 17.5694(12)
α/° 90
β/° 101.549(3)
γ/° 90
Volume/Å3 3683.4(5)
Z 4
ρcalcg/cm3 1.393
μ/mm‑1 0.893
F(000) 1624.0
Crystal size/mm3 0.48 × 0.303 × 0.232
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.732 to 57.996
Index ranges -14 ≤ h ≤ 15, -22 ≤ k ≤ 26, -23 ≤ l ≤ 23
Reflections collected 42889
Independent reflections 9768 [Rint = 0.0289, Rsigma = 0.0275]
Data/restraints/parameters 9768/2/454
Goodness-of-fit on F2 1.022
Final R indexes [I>=2σ (I)] R1 = 0.0297, wR2 = 0.0687
Final R indexes [all data] R1 = 0.0378, wR2 = 0.0718
Largest diff. peak/hole / e Å-3 0.66/-0.67

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for mo_B0129_0m. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Fe11703.2(2)4297.2(2)4300.2(2)11.23(5)
Fe27463.0(2)3868.5(2)1211.0(2)13.45(5)
Si14412.6(4)3804.6(2)3710.0(2)12.08(8)
Si25919.2(4)4435.5(2)2589.8(2)13.43(8)
O23759.8(10)3222.2(5)3104.8(6)17.1(2)
O15548.8(10)4184.9(5)3403.6(6)15.8(2)
O34715.1(10)4511.2(6)1905.6(6)18.3(2)
N12339.1(12)4754.8(7)1932.8(7)17.1(2)
N24872.9(12)2485.1(6)2106.0(7)17.1(2)
C13250.1(13)4461.6(7)3837.8(8)13.0(3)
C22145.1(13)4677.5(7)3305.9(8)13.8(3)
C31543.0(14)5195.5(7)3675.2(9)16.0(3)
C42252.0(14)5307.2(7)4433.4(9)16.5(3)
C53293.2(14)4861.0(7)4536.1(8)14.4(3)
C61643.9(14)3262.7(7)4518.5(9)18.3(3)
C7548.8(14)3473.2(7)3996.3(9)17.5(3)
C8-44.3(14)3985.2(8)4374.1(9)17.8(3)
C9687.1(15)4091.2(8)5131.1(9)19.5(3)
C101730.0(15)3646.5(8)5220.5(9)19.5(3)
C111699.2(14)4418.2(7)2495.8(8)16.2(3)
C121941.0(16)4433.4(10)1169.8(9)26.5(4)
C132107.6(17)5496.9(8)1882.2(10)25.6(3)
C145113.6(14)3435.5(7)4683.6(8)14.8(3)
C155923.9(14)2819.5(7)4630.2(8)15.0(3)
C167138.3(15)2894.2(8)4526.0(9)22.0(3)
C177885.4(16)2323.9(9)4487.7(10)26.0(3)
C187426.0(16)1666.3(8)4537.1(9)24.1(3)
C196213.7(17)1583.7(8)4615(1)25.1(3)
C205472.2(15)2153.0(8)4665.5(9)21.3(3)
C216956.1(14)3796.7(7)2268.9(8)14.4(3)
C226635.9(14)3177.9(7)1813.5(8)15.5(3)
C237753.4(15)2890.1(7)1649.7(9)18.4(3)
C248754.6(14)3322.3(8)1979.3(9)18.4(3)
C258275.2(14)3874.2(7)2362.0(8)16.4(3)
C266202.9(17)4102.2(9)227.5(9)26.0(3)
C277267.2(17)3797.9(9)30.6(9)25.8(3)
C288302.9(16)4212.3(9)348.9(9)25.6(3)
C297878.5(17)4776.4(8)739.7(9)25.7(4)
C306574.8(17)4708.5(9)661.8(9)25.6(4)
C315374.4(14)2887.2(8)1520.2(9)17.7(3)
C325734.8(17)1949.8(9)2463.9(10)27.2(4)
C333706.4(16)2169.3(9)1716(1)26.8(4)
C346768.5(14)5275.9(7)2816.4(9)18.2(3)
C355896.0(14)5880.0(7)2723.8(9)16.9(3)
C365658.5(18)6257.9(8)2032.9(10)25.9(4)
C374803.5(18)6789.4(8)1918(1)27.3(4)
C384168.7(16)6965.9(8)2494.6(10)23.1(3)
C394399.0(15)6602.1(8)3188.1(9)22.3(3)
C405245.6(15)6062.4(8)3297.7(9)19.3(3)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for mo_B0129_0m. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Fe112.68(10)9.96(9)12.09(9)-0.18(7)4.97(7)-0.75(7)
Fe215.29(11)13.2(1)12.78(10)0.14(7)5.00(8)0.04(7)
Si113.64(19)11.61(17)12.21(17)0.19(13)5.52(14)0.96(14)
Si214.9(2)12.46(17)14.03(18)-0.33(14)5.64(15)-0.87(14)
O218.3(5)15.9(5)17.8(5)-4.3(4)5.6(4)-0.5(4)
O115.4(5)18.2(5)15.6(5)1.0(4)7.3(4)-0.3(4)
O315.2(5)22.0(5)18.2(5)1.1(4)4.8(4)2.8(4)
N118.1(6)21.2(6)12.7(6)2.1(5)4.6(5)0.3(5)
N219.0(7)14.6(6)18.8(6)-2.4(5)6.7(5)-4.4(5)
C113.9(7)11.5(6)15.2(6)0.3(5)6.9(5)-1.6(5)
C215.3(7)12.2(6)15.4(6)2.3(5)7.1(5)-0.2(5)
C317.5(7)11.1(6)21.3(7)3.2(5)8.2(6)1.8(5)
C419.4(8)10.5(6)21.7(7)-2.3(5)9.2(6)-1.4(5)
C515.3(7)13.5(6)15.4(6)-1.9(5)5.5(5)-2.9(5)
C619.6(8)11.0(6)24.4(7)2.8(5)4.8(6)-1.9(5)
C719.5(8)14.5(6)18.2(7)-1.1(5)3.1(6)-5.0(6)
C815.0(7)18.4(7)21.3(7)1.8(6)6.5(6)-2.5(6)
C923.2(8)21.4(7)16.8(7)-0.1(6)10.8(6)-5.9(6)
C1021.9(8)20.1(7)16.0(7)5.8(6)2.2(6)-5.9(6)
C1115.9(7)18.1(7)15.3(7)1.7(5)4.7(5)-0.1(5)
C1224.2(9)39.9(10)14.8(7)-1.9(7)2.4(6)-3.0(7)
C1330.4(9)22.7(8)24.3(8)8.5(6)7.1(7)0.6(7)
C1417.6(7)13.7(6)14.2(6)0.3(5)5.8(5)1.3(5)
C1517.6(7)16.1(6)11.6(6)0.8(5)3.3(5)3.1(5)
C1620.1(8)19.0(7)28.7(8)-4.1(6)9.0(6)-1.8(6)
C1717.9(8)28.9(8)32.9(9)-3.3(7)9.4(7)3.0(7)
C1827.1(9)22.7(8)24.2(8)3.7(6)8.9(7)11.4(7)
C1932.4(10)15.3(7)30.7(9)7.1(6)14.0(7)3.5(6)
C2019.9(8)18.5(7)28.0(8)4.9(6)11.0(6)2.2(6)
C2116.2(7)14.0(6)13.5(6)2.4(5)4.3(5)0.8(5)
C2218.2(7)13.3(6)15.8(6)1.2(5)5.1(5)0.4(5)
C2321.9(8)13.3(6)20.9(7)0.5(5)6.4(6)3.6(6)
C2415.6(7)19.3(7)20.2(7)1.3(6)3.6(6)5.2(6)
C2515.4(7)17.2(7)16.1(7)0.5(5)1.7(5)1.4(5)
C2622.8(9)34.0(9)19.3(8)8.2(7)-0.5(6)0.5(7)
C2733.7(10)29.4(8)14.5(7)0.1(6)5.0(7)0.4(7)
C2823.7(9)35.3(9)20.7(8)6.3(7)11.6(7)-0.3(7)
C2935.9(10)21.0(8)20.9(8)5.9(6)7.4(7)-6.8(7)
C3032.2(10)24.2(8)22.5(8)10.6(6)10.6(7)9.8(7)
C3119.8(8)15.7(7)18.5(7)-1.3(5)6.0(6)-2.8(6)
C3234.6(10)20.1(8)27.8(8)4.8(6)8.8(7)0.4(7)
C3327.0(9)22.7(8)31.5(9)-7.5(7)8.0(7)-10.5(7)
C3418.2(8)14.5(6)23.3(7)-2.2(6)7.9(6)-2.0(6)
C3519.0(8)12.4(6)20.0(7)-2.3(5)5.9(6)-3.5(5)
C3642.2(11)16.6(7)23.9(8)1.7(6)18.8(7)1.0(7)
C3743.8(11)15.7(7)23.4(8)5.1(6)9.4(7)0.5(7)
C3823.4(9)16.2(7)27.9(8)-1.6(6)0.7(7)1.3(6)
C3920.1(8)27.1(8)20.0(7)-3.6(6)4.8(6)3.8(6)
C4019.3(8)23.3(7)15.3(7)0.3(6)3.5(6)1.6(6)

 

Table 4 Bond Lengths for mo_B0129_0m.
AtomAtomLength/Å AtomAtomLength/Å
Fe1C12.0570(13) C1C51.4437(19)
Fe1C22.0432(13) C2C31.4297(19)
Fe1C32.0477(14) C2C111.497(2)
Fe1C42.0494(14) C3C41.420(2)
Fe1C52.0382(14) C4C51.421(2)
Fe1C62.0457(14) C6C71.423(2)
Fe1C72.0466(15) C6C101.427(2)
Fe1C82.0498(15) C7C81.424(2)
Fe1C92.0502(14) C8C91.426(2)
Fe1C102.0464(14) C9C101.421(2)
Fe2C212.0502(14) C14C151.5060(19)
Fe2C222.0332(14) C15C161.396(2)
Fe2C232.0487(14) C15C201.391(2)
Fe2C242.0506(15) C16C171.389(2)
Fe2C252.0414(15) C17C181.381(2)
Fe2C262.0403(17) C18C191.381(2)
Fe2C272.0461(16) C19C201.387(2)
Fe2C282.0396(15) C21C221.446(2)
Fe2C292.0364(15) C21C251.440(2)
Fe2C302.0410(16) C22C231.434(2)
Si1O21.6179(11) C22C311.495(2)
Si1O11.6359(11) C23C241.415(2)
Si1C11.8533(14) C24C251.421(2)
Si1C141.8727(15) C26C271.418(2)
Si2O11.6376(10) C26C301.417(3)
Si2O31.6101(12) C27C281.417(3)
Si2C211.8492(15) C28C291.420(2)
Si2C341.8823(15) C29C301.424(3)
N1C111.4774(18) C34C351.504(2)
N1C121.464(2) C35C361.397(2)
N1C131.461(2) C35C401.395(2)
N2C311.4838(18) C36C371.385(2)
N2C321.462(2) C37C381.385(2)
N2C331.466(2) C38C391.387(2)
C1C21.442(2) C39C401.390(2)

 

Table 5 Bond Angles for mo_B0129_0m.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C2Fe1C141.18(6) C21Si2C34109.39(7)
C2Fe1C340.91(5) Si1O1Si2139.71(7)
C2Fe1C468.72(6) C12N1C11109.20(12)
C2Fe1C6122.42(6) C13N1C11112.00(12)
C2Fe1C7107.54(6) C13N1C12110.30(13)
C2Fe1C8123.31(6) C32N2C31111.74(12)
C2Fe1C9159.60(6) C32N2C33109.84(13)
C2Fe1C10158.42(6) C33N2C31108.04(12)
C3Fe1C169.25(6) Si1C1Fe1126.20(7)
C3Fe1C440.56(6) C2C1Fe168.90(8)
C3Fe1C8107.68(6) C2C1Si1129.58(10)
C3Fe1C9123.15(6) C2C1C5105.95(12)
C4Fe1C169.35(5) C5C1Fe168.66(8)
C4Fe1C8122.35(6) C5C1Si1124.47(11)
C4Fe1C9107.23(6) C1C2Fe169.93(7)
C5Fe1C141.28(5) C1C2C11126.38(12)
C5Fe1C268.73(6) C3C2Fe169.71(8)
C5Fe1C368.36(6) C3C2C1108.62(12)
C5Fe1C440.67(6) C3C2C11124.99(13)
C5Fe1C6123.12(6) C11C2Fe1127.06(10)
C5Fe1C7159.61(6) C2C3Fe169.38(8)
C5Fe1C8158.11(6) C4C3Fe169.79(8)
C5Fe1C9122.07(6) C4C3C2108.31(13)
C5Fe1C10107.12(6) C3C4Fe169.66(8)
C6Fe1C1106.63(6) C3C4C5107.81(12)
C6Fe1C3158.75(6) C5C4Fe169.24(8)
C6Fe1C4159.29(6) C1C5Fe170.06(8)
C6Fe1C740.69(6) C4C5Fe170.09(8)
C6Fe1C868.46(6) C4C5C1109.31(13)
C6Fe1C968.46(6) C7C6Fe169.69(8)
C6Fe1C1040.83(6) C7C6C10107.98(13)
C7Fe1C1122.71(6) C10C6Fe169.62(8)
C7Fe1C3122.80(6) C6C7Fe169.62(8)
C7Fe1C4158.45(6) C6C7C8108.04(13)
C7Fe1C840.69(6) C8C7Fe169.78(8)
C7Fe1C968.47(6) C7C8Fe169.53(8)
C8Fe1C1159.45(6) C7C8C9107.94(14)
C8Fe1C940.70(6) C9C8Fe169.66(8)
C9Fe1C1157.96(6) C8C9Fe169.64(8)
C10Fe1C1121.72(6) C10C9Fe169.56(8)
C10Fe1C3159.09(6) C10C9C8108.07(13)
C10Fe1C4122.80(6) C6C10Fe169.56(8)
C10Fe1C768.56(6) C9C10Fe169.84(8)
C10Fe1C868.47(6) C9C10C6107.96(14)
C10Fe1C940.60(6) N1C11C2112.21(12)
C21Fe2C2469.39(6) C15C14Si1112.83(9)
C22Fe2C2141.48(5) C16C15C14121.56(13)
C22Fe2C2341.14(6) C20C15C14120.77(13)
C22Fe2C2469.05(6) C20C15C16117.65(13)
C22Fe2C2569.00(6) C17C16C15121.23(15)
C22Fe2C26106.64(7) C18C17C16120.20(15)
C22Fe2C27121.09(6) C19C18C17119.22(15)
C22Fe2C28156.94(7) C18C19C20120.63(15)
C22Fe2C29160.42(7) C19C20C15121.01(15)
C22Fe2C30123.27(7) Si2C21Fe2121.92(7)
C23Fe2C2169.30(6) C22C21Fe268.63(8)
C23Fe2C2440.38(6) C22C21Si2128.81(11)
C25Fe2C2141.20(6) C25C21Fe269.07(8)
C25Fe2C2368.14(6) C25C21Si2124.66(11)
C25Fe2C2440.65(6) C25C21C22106.20(12)
C25Fe2C27160.17(7) C21C22Fe269.89(8)
C26Fe2C21121.30(7) C21C22C31127.67(13)
C26Fe2C23123.58(7) C23C22Fe270.01(8)
C26Fe2C24159.76(7) C23C22C21108.01(13)
C26Fe2C25158.03(7) C23C22C31124.26(13)
C26Fe2C2740.60(7) C31C22Fe2123.58(10)
C26Fe2C3040.63(7) C22C23Fe268.85(8)
C27Fe2C21157.18(7) C24C23Fe269.88(8)
C27Fe2C23107.23(6) C24C23C22108.65(13)
C27Fe2C24123.44(7) C23C24Fe269.73(9)
C28Fe2C21160.47(7) C23C24C25107.79(13)
C28Fe2C23121.47(7) C25C24Fe269.33(8)
C28Fe2C24107.36(7) C21C25Fe269.73(8)
C28Fe2C25124.00(7) C24C25Fe270.02(9)
C28Fe2C2668.43(7) C24C25C21109.35(13)
C28Fe2C2740.60(7) C27C26Fe269.92(10)
C28Fe2C3068.57(7) C30C26Fe269.72(9)
C29Fe2C21123.49(6) C30C26C27108.18(16)
C29Fe2C23157.30(7) C26C27Fe269.48(9)
C29Fe2C24122.05(7) C28C27Fe269.45(9)
C29Fe2C25107.95(6) C28C27C26108.04(15)
C29Fe2C2668.55(7) C27C28Fe269.95(9)
C29Fe2C2768.43(7) C27C28C29108.03(15)
C29Fe2C2840.77(7) C29C28Fe269.49(9)
C29Fe2C3040.87(7) C28C29Fe269.74(9)
C30Fe2C21106.88(6) C28C29C30107.89(15)
C30Fe2C23160.22(7) C30C29Fe269.74(9)
C30Fe2C24158.13(7) C26C30Fe269.66(9)
C30Fe2C25122.55(6) C26C30C29107.86(15)
C30Fe2C2768.35(7) C29C30Fe269.39(9)
O2Si1O1111.61(5) N2C31C22114.20(12)
O2Si1C1109.36(6) C35C34Si2111.74(10)
O2Si1C14112.44(6) C36C35C34120.47(13)
O1Si1C1108.94(6) C40C35C34122.01(14)
O1Si1C14105.61(6) C40C35C36117.43(14)
C1Si1C14108.75(6) C37C36C35121.40(15)
O1Si2C21110.20(6) C36C37C38120.46(15)
O1Si2C34105.84(6) C37C38C39119.10(15)
O3Si2O1111.47(6) C38C39C40120.30(14)
O3Si2C21107.58(6) C39C40C35121.29(14)
O3Si2C34112.37(7)     

 

Table 6 Hydrogen Bonds for mo_B0129_0m.
DHAd(D-H)/Åd(H-A)/Åd(D-A)/ÅD-H-A/°
O2H2N20.902(16)1.847(16)2.7376(16)169(2)
O3H3N10.958(16)1.773(18)2.6740(17)156(2)

 

Table 7 Torsion Angles for mo_B0129_0m.
ABCDAngle/˚ ABCDAngle/˚
Fe1C1C2C359.16(9) C5C1C2C30.22(15)
Fe1C1C2C11-121.85(14) C5C1C2C11179.21(13)
Fe1C1C5C4-59.27(10) C6C7C8Fe159.32(10)
Fe1C2C3C459.11(10) C6C7C8C90.03(16)
Fe1C2C11N1-172.18(10) C7C6C10Fe1-59.34(10)
Fe1C3C4C558.92(10) C7C6C10C90.16(16)
Fe1C4C5C159.25(9) C7C8C9Fe159.20(10)
Fe1C6C7C8-59.41(10) C7C8C9C100.07(16)
Fe1C6C10C959.50(10) C8C9C10Fe159.18(10)
Fe1C7C8C9-59.29(10) C8C9C10C6-0.14(16)
Fe1C8C9C10-59.13(10) C10C6C7Fe159.30(10)
Fe1C9C10C6-59.33(10) C10C6C7C8-0.12(16)
Fe2C21C22C2359.88(10) C11C2C3Fe1121.70(14)
Fe2C21C22C31-117.48(15) C11C2C3C4-179.19(13)
Fe2C21C25C24-58.96(10) C12N1C11C2174.88(13)
Fe2C22C23C2458.68(10) C13N1C11C2-62.65(16)
Fe2C22C31N2-170.37(9) C14Si1O1Si2157.65(10)
Fe2C23C24C2559.09(10) C14Si1C1Fe1-59.65(10)
Fe2C24C25C2158.78(10) C14Si1C1C2-151.14(12)
Fe2C26C27C28-58.93(11) C14Si1C1C527.80(13)
Fe2C26C30C2959.08(11) C14C15C16C17179.13(15)
Fe2C27C28C29-59.27(11) C14C15C20C19179.86(14)
Fe2C28C29C30-59.54(11) C15C16C17C181.3(3)
Fe2C29C30C26-59.24(11) C16C15C20C191.3(2)
Si1C1C2Fe1120.15(11) C16C17C18C190.8(3)
Si1C1C2C3179.31(10) C17C18C19C20-1.8(3)
Si1C1C2C11-1.7(2) C18C19C20C150.7(3)
Si1C1C5Fe1-120.06(10) C20C15C16C17-2.3(2)
Si1C1C5C4-179.33(10) C21Si2O1Si1-99.17(11)
Si1C14C15C1680.42(16) C21Si2C34C35153.98(10)
Si1C14C15C20-98.06(14) C21C22C23Fe2-59.80(10)
Si2C21C22Fe2114.45(12) C21C22C23C24-1.12(16)
Si2C21C22C23174.32(11) C21C22C31N2-80.87(18)
Si2C21C22C31-3.0(2) C22C21C25Fe258.84(9)
Si2C21C25Fe2-115.07(11) C22C21C25C24-0.11(16)
Si2C21C25C24-174.03(10) C22C23C24Fe2-58.05(10)
Si2C34C35C36-96.00(15) C22C23C24C251.04(17)
Si2C34C35C4080.47(16) C23C22C31N2102.17(16)
O2Si1O1Si235.17(12) C23C24C25Fe2-59.35(10)
O2Si1C1Fe163.48(10) C23C24C25C21-0.57(17)
O2Si1C1C2-28.01(14) C25C21C22Fe2-59.13(9)
O2Si1C1C5150.93(11) C25C21C22C230.75(15)
O2Si1C14C1549.72(12) C25C21C22C31-176.60(14)
O1Si1C1Fe1-174.29(8) C26C27C28Fe258.95(11)
O1Si1C1C294.22(13) C26C27C28C29-0.33(18)
O1Si1C1C5-86.84(12) C27C26C30Fe2-59.57(11)
O1Si1C14C15-72.22(11) C27C26C30C29-0.49(18)
O1Si2C21Fe2172.77(7) C27C28C29Fe259.56(11)
O1Si2C21C2285.64(13) C27C28C29C300.02(18)
O1Si2C21C25-101.87(12) C28C29C30Fe259.53(11)
O1Si2C34C35-87.31(11) C28C29C30C260.29(18)
O3Si2O1Si120.20(12) C30C26C27Fe259.44(11)
O3Si2C21Fe251.06(10) C30C26C27C280.51(18)
O3Si2C21C22-36.07(14) C31C22C23Fe2117.66(14)
O3Si2C21C25136.42(12) C31C22C23C24176.35(13)
O3Si2C34C3534.57(12) C32N2C31C22-52.71(16)
C1Si1O1Si2-85.69(11) C33N2C31C22-173.66(13)
C1Si1C14C15170.99(10) C34Si2O1Si1142.65(10)
C1C2C3Fe1-59.29(9) C34Si2C21Fe2-71.26(10)
C1C2C3C4-0.18(16) C34Si2C21C22-158.39(12)
C1C2C11N1-80.91(17) C34Si2C21C2514.10(14)
C2C1C5Fe159.09(9) C34C35C36C37176.09(16)
C2C1C5C4-0.18(15) C34C35C40C39-176.94(15)
C2C3C4Fe1-58.85(9) C35C36C37C380.8(3)
C2C3C4C50.07(16) C36C35C40C39-0.4(2)
C3C2C11N197.93(16) C36C37C38C39-0.1(3)
C3C4C5Fe1-59.18(10) C37C38C39C40-0.7(2)
C3C4C5C10.07(16) C38C39C40C351.0(2)
C5C1C2Fe1-58.94(9) C40C35C36C37-0.5(2)

 

Table 8 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for mo_B0129_0m.
AtomxyzU(eq)
H24220(20)3001(11)2811(12)47(7)
H33963(18)4653(13)2053(14)53(7)
H3A7965426345219
H420645624480620
H539194830499317
H622172926441822
H72633302348521
H8-7954215416021
H95094404551023
H1023713611566923
H11A18353914248519
H11B7994503234019
H12A21003936121240
H12B2402463580240
H12C1054451498440
H13A12195580171338
H13B25515701150738
H13C23985707239338
H14A56123796500118
H14B44433298495218
H1674603343448026
H1787152386442731
H1879381275451829
H1958841133463430
H2046432087472526
H2378122478136722
H2495973255195022
H2587514237263620
H26538239309231
H2772833388-26331
H289135412830831
H2983765135100631
H306048501586531
H31A48003271133521
H31B54042586107021
H32A53641687283641
H32B65052165273541
H32C59131639206041
H33A31242531149140
H33B33551903209340
H33C38611863130240
H34A72485264335622
H34B73595335246522
H3660936148163431
H3746517035144033
H3835837331241628
H3939766722359027
H4053845813377323

Experimental

Single crystals of C40H48Fe2N2O3Si2 [mo_B0129_0m] were [The material was recrystallised from Diethylether by slow evaporation]. A suitable crystal was selected and [The crystal was mounted on a MITIGEN holder in perfluoroether 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_B0129_0m]

Crystal Data for C40H48Fe2N2O3Si2 (=772.68 g/mol): monoclinic, space group P21/n (no. 14), a = 11.0354(10) Å, b = 19.3902(15) Å, c = 17.5694(12) Å, β = 101.549(3)°, = 3683.4(5) Å3, Z = 4, T = 100.0 K, μ(MoKα) = 0.893 mm-1, Dcalc = 1.393 g/cm3, 42889 reflections measured (4.732° ≤ 2Θ ≤ 57.996°), 9768 unique (Rint = 0.0289, Rsigma = 0.0275) which were used in all calculations. The final R1 was 0.0297 (I > 2σ(I)) and wR2 was 0.0718 (all data).

Refinement model description

Number of restraints - 2, 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
O2-H2 = O3-H3
0.98 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
C11(H11A,H11B), C14(H14A,H14B), C31(H31A,H31B), C34(H34A,H34B)
3.b Aromatic/amide H refined with riding coordinates:
C3(H3A), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C16(H16),
C17(H17), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C25(H25), C26(H26),
C27(H27), C28(H28), C29(H29), C30(H30), C36(H36), C37(H37), C38(H38),
C39(H39), C40(H40)
3.c Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C32(H32A,H32B,H32C), C33(H33A,H33B,
H33C)

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.