mo_B0425_0m

Table 1 Crystal data and structure refinement for mo_B0425_0m.
Identification code mo_B0425_0m
Empirical formula C36H60Fe2N2OSi4
Formula weight 760.92
Temperature/K 99.99
Crystal system triclinic
Space group P-1
a/Å 9.7419(18)
b/Å 13.252(3)
c/Å 17.228(3)
α/° 98.993(5)
β/° 98.779(5)
γ/° 110.464(5)
Volume/Å3 2005.8(6)
Z 2
ρcalcg/cm3 1.260
μ/mm‑1 0.872
F(000) 812.0
Crystal size/mm3 0.294 × 0.26 × 0.07
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.528 to 59.356
Index ranges -13 ≤ h ≤ 13, -18 ≤ k ≤ 18, -23 ≤ l ≤ 23
Reflections collected 101034
Independent reflections 11305 [Rint = 0.0374, Rsigma = 0.0219]
Data/restraints/parameters 11305/0/421
Goodness-of-fit on F2 1.132
Final R indexes [I>=2σ (I)] R1 = 0.0418, wR2 = 0.1106
Final R indexes [all data] R1 = 0.0512, wR2 = 0.1206
Largest diff. peak/hole / e Å-3 2.20/-0.53

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for mo_B0425_0m. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Fe15097.8(3)1505.0(2)3171.4(2)13.24(8)
Fe27834.3(3)4151.3(2)6548.5(2)15.08(8)
Si14253.6(7)1766.8(5)1182.1(3)19.19(12)
Si22468.2(6)1524.1(4)4342.1(3)13.52(11)
Si33923.1(6)2710.4(4)6124.9(3)15.18(11)
Si49841.9(7)3996.6(5)8391.8(4)22.20(13)
O13758.3(16)2222.6(12)5166.6(8)19.3(3)
N1740(2)678.0(16)1572.1(12)26.4(4)
N26362(2)3661.8(14)8791.7(10)17.9(3)
C13388(2)1933.7(15)3505.2(11)14.0(3)
C22999(2)1414.0(15)2659.2(11)14.3(3)
C34102(2)2028.0(16)2256.4(11)15.0(3)
C45183(2)2955.2(16)2873.9(12)16.9(4)
C54757(2)2894.4(16)3626.2(12)16.3(4)
C65593(2)571.2(19)3933.3(13)21.7(4)
C75053(3)-62.5(18)3122.6(13)22.6(4)
C86045(3)482.8(19)2654.0(13)22.8(4)
C97180(2)1457(2)3173.6(14)23.4(4)
C106903(2)1511(2)3964.7(13)23.3(4)
C113248(3)2501(2)619.7(14)28.7(5)
C126305(3)2373(2)1164.9(15)30.6(5)
C133489(3)264(2)673.7(14)29.4(5)
C141608(2)415.2(17)2230.9(12)18.8(4)
C15209(3)1520(2)1858.5(17)36.5(6)
C16-540(3)-320(2)1119.9(19)44.6(7)
C171849(2)13.9(17)4315.4(14)23.2(4)
C18813(2)1919.9(19)4336.6(13)22.2(4)
C192541(2)1672(2)6533.1(14)24.4(4)
C203520(3)3995.8(19)6244.8(14)26.3(5)
C215874(2)2923.3(15)6612.5(11)13.7(3)
C226771(2)3518.7(15)7407.6(11)13.2(3)
C238223(2)3438.2(16)7499.9(11)16.0(4)
C248208(2)2777.6(17)6747.9(12)18.5(4)
C256791(2)2465.1(16)6212.1(11)16.3(4)
C267254(3)5060.9(18)5790.3(13)25.3(4)
C277848(3)5713.6(17)6590.9(13)22.9(4)
C289338(3)5759.6(18)6832.2(14)25.1(4)
C299658(3)5137(2)6184.1(16)30.1(5)
C308363(3)4702(2)5537.6(14)29.4(5)
C319601(4)2933(2)9010.4(16)38.5(7)
C3210055(3)5352.4(18)9013.2(13)23.3(4)
C3311598(3)4197(3)7998.6(18)42.6(7)
C346274(2)4108.6(16)8066.2(11)16.2(4)
C355345(3)2506.3(19)8634.7(14)30.7(5)
C366025(3)4321.5(19)9442.0(12)23.4(4)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for mo_B0425_0m. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Fe111.21(13)14.71(14)13.87(13)3.75(10)2.06(9)5.15(10)
Fe216.34(14)14.70(14)13.20(13)3.71(10)5.12(10)3.75(11)
Si122.8(3)20.9(3)14.1(2)5.5(2)4.4(2)7.8(2)
Si210.8(2)15.8(2)14.2(2)4.50(18)2.60(18)5.03(19)
Si315.2(2)17.1(2)14.0(2)4.24(19)2.91(18)6.9(2)
Si421.1(3)25.2(3)18.0(3)-2.5(2)-2.4(2)12.0(2)
O115.4(7)24.9(7)14.7(6)3.0(5)1.1(5)5.9(6)
N124.2(9)24.6(9)25.5(9)1.8(7)-5.1(7)9.7(8)
N225.1(9)17.8(8)11.9(7)3.6(6)6.6(6)8.5(7)
C112.9(8)13.7(8)15.4(8)3.1(6)2.7(6)5.4(7)
C213.4(8)13.8(8)15.9(8)4.0(6)2.3(6)5.5(7)
C316.7(9)14.4(8)14.9(8)4.6(6)3.1(7)6.8(7)
C416.5(9)13.2(8)19.7(9)4.5(7)3.4(7)4.1(7)
C514.9(9)14.3(8)18.1(9)1.9(7)2.6(7)4.8(7)
C623(1)29.4(11)21.3(10)13.1(8)6.6(8)16.4(9)
C724.8(10)21(1)26.6(10)8.3(8)4.7(8)13.4(8)
C826.3(11)28.8(11)21.6(10)7.6(8)6.5(8)19.4(9)
C915.9(9)33.3(12)27(1)11.9(9)6.7(8)13.5(9)
C1016.3(9)32.4(11)21.7(10)6.1(8)0.3(7)11.8(9)
C1134.8(12)32.9(12)22.2(10)13.5(9)5.2(9)14.7(10)
C1227.7(12)40.9(14)25.7(11)12.7(10)12.9(9)11.1(10)
C1334.9(13)28.4(11)22.5(10)-0.8(9)0.9(9)14.5(10)
C1416.6(9)16.5(9)18.6(9)3.9(7)-0.5(7)2.5(7)
C1531.2(13)42.4(15)35.4(13)-2.0(11)-5.3(10)23.3(12)
C1638.0(15)33.4(14)44.0(16)0.0(12)-18.6(12)7.1(12)
C1721(1)18.5(9)29.7(11)9.0(8)7.1(8)4.9(8)
C1815.8(9)30.3(11)26.5(10)12.6(8)7.8(8)12.0(8)
C1917.2(10)30.3(11)24.9(10)10.3(9)6.8(8)5.8(9)
C2031.2(12)26.5(11)27.0(11)6.4(9)5.6(9)18.1(10)
C2116.2(8)11.2(8)13.3(8)3.6(6)3.8(6)4.0(7)
C2216.1(8)12.1(8)12.0(8)3.7(6)4.2(6)5.5(7)
C2318.2(9)16.0(8)13.7(8)1.6(7)3.1(7)7.2(7)
C2419.9(9)19.9(9)16.5(9)0.4(7)3.7(7)10.3(8)
C2517.9(9)14.8(8)14.3(8)0.4(6)3.3(7)5.5(7)
C2629.8(11)22.6(10)21.7(10)12.3(8)3.8(8)5.7(9)
C2728.4(11)16.0(9)25.9(10)8.9(8)8.6(8)7.6(8)
C2823.6(11)20.1(10)26.1(10)10.2(8)4.7(8)-0.2(8)
C2924.9(11)31.4(12)39.8(13)17.7(10)20.5(10)8.3(10)
C3040.7(13)26.7(11)21.2(10)10.4(9)15.8(9)7.8(10)
C3157.6(17)26.9(12)27.1(12)-0.8(9)-13.7(11)24.0(12)
C3223.5(10)20.9(10)18.7(9)0.3(8)1.4(8)3.7(8)
C3324.3(12)59.6(19)37.0(14)-10.5(13)-1.1(10)20.2(12)
C3419.2(9)17.5(9)13.8(8)3.4(7)5.1(7)8.9(7)
C3547.9(15)20.6(10)18.6(10)6.1(8)11.5(10)4.7(10)
C3629.2(11)28.4(11)14.3(9)2.5(8)8.1(8)12.6(9)

 

Table 4 Bond Lengths for mo_B0425_0m.
AtomAtomLength/Å AtomAtomLength/Å
Fe1C12.0691(19) Si4C231.867(2)
Fe1C22.0539(19) Si4C311.868(3)
Fe1C32.0619(19) Si4C321.867(2)
Fe1C42.042(2) Si4C331.884(3)
Fe1C52.042(2) N1C141.470(3)
Fe1C62.054(2) N1C151.437(3)
Fe1C72.050(2) N1C161.462(3)
Fe1C82.056(2) N2C341.468(2)
Fe1C92.051(2) N2C351.459(3)
Fe1C102.053(2) N2C361.461(3)
Fe2C212.0624(19) C1C21.441(3)
Fe2C222.0530(18) C1C51.445(3)
Fe2C232.066(2) C2C31.446(3)
Fe2C242.046(2) C2C141.506(3)
Fe2C252.047(2) C3C41.448(3)
Fe2C262.055(2) C4C51.425(3)
Fe2C272.055(2) C6C71.426(3)
Fe2C282.049(2) C6C101.424(3)
Fe2C292.057(2) C7C81.429(3)
Fe2C302.059(2) C8C91.425(3)
Si1C31.867(2) C9C101.425(3)
Si1C111.875(2) C21C221.441(3)
Si1C121.882(3) C21C251.441(3)
Si1C131.873(2) C22C231.442(3)
Si2O11.6385(15) C22C341.513(3)
Si2C11.864(2) C23C241.441(3)
Si2C171.868(2) C24C251.422(3)
Si2C181.861(2) C26C271.421(3)
Si3O11.6376(15) C26C301.422(4)
Si3C191.870(2) C27C281.424(3)
Si3C201.865(2) C28C291.422(3)
Si3C211.861(2) C29C301.424(4)

 

Table 5 Bond Angles for mo_B0425_0m.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C2Fe1C140.92(7) C18Si2C17108.55(10)
C2Fe1C341.15(7) O1Si3C19109.91(9)
C2Fe1C6126.86(8) O1Si3C20109.22(9)
C2Fe1C8121.78(8) O1Si3C21104.67(8)
C3Fe1C169.96(8) C20Si3C19108.66(11)
C4Fe1C169.27(8) C21Si3C19110.02(9)
C4Fe1C268.55(8) C21Si3C20114.28(10)
C4Fe1C341.30(7) C23Si4C31107.98(11)
C4Fe1C6154.02(9) C23Si4C32113.60(10)
C4Fe1C7163.05(9) C23Si4C33107.24(11)
C4Fe1C8124.97(9) C31Si4C33108.69(15)
C4Fe1C9106.13(9) C32Si4C31110.97(11)
C4Fe1C10118.67(9) C32Si4C33108.21(12)
C5Fe1C141.16(7) Si3O1Si2140.66(10)
C5Fe1C268.51(8) C15N1C14112.37(19)
C5Fe1C369.53(8) C15N1C16109.4(2)
C5Fe1C440.85(8) C16N1C14109.85(19)
C5Fe1C6119.75(8) C35N2C34111.67(16)
C5Fe1C7155.47(9) C35N2C36109.97(18)
C5Fe1C8161.53(9) C36N2C34110.21(16)
C5Fe1C9123.90(9) Si2C1Fe1125.52(10)
C5Fe1C10106.14(9) C2C1Fe168.98(10)
C6Fe1C1107.55(8) C2C1Si2130.93(14)
C6Fe1C3163.85(9) C2C1C5106.02(16)
C6Fe1C868.25(9) C5C1Fe168.41(11)
C7Fe1C1120.91(8) C5C1Si2123.02(14)
C7Fe1C2109.31(8) C1C2Fe170.11(11)
C7Fe1C3125.98(8) C1C2C3110.21(16)
C7Fe1C640.66(9) C1C2C14125.94(17)
C7Fe1C840.71(9) C3C2Fe169.72(11)
C7Fe1C968.51(9) C3C2C14123.76(17)
C7Fe1C1068.46(9) C14C2Fe1129.53(14)
C8Fe1C1156.39(9) Si1C3Fe1125.91(10)
C8Fe1C3107.28(8) C2C3Fe169.13(11)
C9Fe1C1161.52(9) C2C3Si1130.87(14)
C9Fe1C2155.66(8) C2C3C4105.72(16)
C9Fe1C3119.12(8) C4C3Fe168.63(11)
C9Fe1C668.31(9) C4C3Si1123.41(14)
C9Fe1C840.58(9) C3C4Fe170.07(11)
C9Fe1C1040.64(9) C5C4Fe169.55(11)
C10Fe1C1124.62(8) C5C4C3109.07(17)
C10Fe1C2163.05(8) C1C5Fe170.43(11)
C10Fe1C3153.86(9) C4C5Fe169.60(11)
C10Fe1C640.58(9) C4C5C1108.98(17)
C10Fe1C868.28(9) C7C6Fe169.54(12)
C21Fe2C2369.60(8) C10C6Fe169.67(12)
C22Fe2C2141.00(7) C10C6C7108.18(19)
C22Fe2C2340.98(7) C6C7Fe169.80(12)
C22Fe2C26128.32(9) C6C7C8107.8(2)
C22Fe2C27108.64(8) C8C7Fe169.87(12)
C22Fe2C29152.79(9) C7C8Fe169.42(12)
C22Fe2C30165.71(10) C9C8Fe169.51(12)
C24Fe2C2169.04(8) C9C8C7108.03(19)
C24Fe2C2268.46(8) C8C9Fe169.90(12)
C24Fe2C2341.03(7) C8C9C10108.0(2)
C24Fe2C2540.67(8) C10C9Fe169.74(12)
C24Fe2C26151.56(9) C6C10Fe169.75(12)
C24Fe2C27166.51(9) C6C10C9108.0(2)
C24Fe2C28128.26(9) C9C10Fe169.62(12)
C24Fe2C29107.82(10) N1C14C2110.40(17)
C24Fe2C30117.87(9) Si3C21Fe2126.91(10)
C25Fe2C2141.07(7) C22C21Fe269.15(10)
C25Fe2C2268.50(7) C22C21Si3130.74(14)
C25Fe2C2369.06(8) C22C21C25106.35(16)
C25Fe2C26118.00(9) C25C21Fe268.88(11)
C25Fe2C27151.88(9) C25C21Si3122.92(14)
C25Fe2C28165.65(9) C21C22Fe269.85(10)
C25Fe2C29127.27(9) C21C22C23109.62(16)
C25Fe2C30107.26(9) C21C22C34126.14(17)
C26Fe2C21107.39(9) C23C22Fe269.99(11)
C26Fe2C23166.36(9) C23C22C34124.20(16)
C26Fe2C2740.45(9) C34C22Fe2128.27(13)
C26Fe2C2967.99(10) Si4C23Fe2128.36(11)
C26Fe2C3040.44(10) C22C23Fe269.04(10)
C27Fe2C21118.05(9) C22C23Si4129.90(14)
C27Fe2C23128.24(8) C24C23Fe268.75(11)
C27Fe2C2968.35(10) C24C23Si4123.85(15)
C27Fe2C3068.25(9) C24C23C22106.22(16)
C28Fe2C21152.52(9) C23C24Fe270.22(11)
C28Fe2C22119.35(8) C25C24Fe269.70(11)
C28Fe2C23108.24(9) C25C24C23109.01(17)
C28Fe2C2667.91(9) C21C25Fe270.05(11)
C28Fe2C2740.61(9) C24C25Fe269.64(11)
C28Fe2C2940.53(10) C24C25C21108.80(16)
C28Fe2C3068.06(10) C27C26Fe269.80(12)
C29Fe2C21165.08(9) C27C26C30108.6(2)
C29Fe2C23118.27(10) C30C26Fe269.94(13)
C29Fe2C3040.47(10) C26C27Fe269.76(12)
C30Fe2C21126.98(9) C26C27C28107.4(2)
C30Fe2C23151.79(10) C28C27Fe269.47(12)
C3Si1C11108.62(10) C27C28Fe269.92(12)
C3Si1C12107.70(10) C29C28Fe270.02(13)
C3Si1C13113.59(10) C29C28C27108.5(2)
C11Si1C12108.77(12) C28C29Fe269.45(12)
C13Si1C11109.93(11) C28C29C30107.8(2)
C13Si1C12108.12(12) C30C29Fe269.85(13)
O1Si2C1104.75(8) C26C30Fe269.62(12)
O1Si2C17109.28(9) C26C30C29107.8(2)
O1Si2C18109.68(9) C29C30Fe269.68(13)
C1Si2C17113.57(9) N2C34C22111.66(16)
C18Si2C1110.92(9)     

 

Table 6 Torsion Angles for mo_B0425_0m.
ABCDAngle/˚ ABCDAngle/˚
Fe1C1C2C3-58.27(13) C10C6C7C80.6(2)
Fe1C1C2C14125.01(19) C11Si1C3Fe1-176.19(12)
Fe1C1C5C459.10(14) C11Si1C3C291.2(2)
Fe1C2C3Si1120.01(17) C11Si1C3C4-89.71(18)
Fe1C2C3C4-59.18(13) C12Si1C3Fe1-58.56(15)
Fe1C2C14N1-145.14(16) C12Si1C3C2-151.13(19)
Fe1C3C4C5-58.77(14) C12Si1C3C427.9(2)
Fe1C4C5C1-59.61(14) C13Si1C3Fe161.15(16)
Fe1C6C7C859.80(14) C13Si1C3C2-31.4(2)
Fe1C6C10C9-59.34(15) C13Si1C3C4147.64(17)
Fe1C7C8C958.98(15) C14C2C3Fe1-124.70(18)
Fe1C8C9C1059.54(15) C14C2C3Si1-4.7(3)
Fe1C9C10C659.42(15) C14C2C3C4176.13(18)
Fe2C21C22C23-58.81(13) C15N1C14C2-62.6(3)
Fe2C21C22C34123.30(18) C16N1C14C2175.4(2)
Fe2C21C25C2459.03(14) C17Si2O1Si3-82.54(17)
Fe2C22C23Si4123.08(17) C17Si2C1Fe1-49.38(15)
Fe2C22C23C24-58.95(14) C17Si2C1C242.7(2)
Fe2C22C34N2-147.67(14) C17Si2C1C5-135.07(16)
Fe2C23C24C25-59.08(14) C18Si2O1Si336.35(18)
Fe2C24C25C21-59.28(13) C18Si2C1Fe1-171.95(11)
Fe2C26C27C2859.54(14) C18Si2C1C2-79.9(2)
Fe2C26C30C29-59.45(16) C18Si2C1C5102.36(17)
Fe2C27C28C2959.62(15) C19Si3O1Si241.26(19)
Fe2C28C29C3059.57(16) C19Si3C21Fe2-168.59(12)
Fe2C29C30C2659.41(15) C19Si3C21C22-75.2(2)
Si1C3C4Fe1-119.76(14) C19Si3C21C25104.31(17)
Si1C3C4C5-178.53(14) C20Si3O1Si2-77.86(18)
Si2C1C2Fe1-119.38(17) C20Si3C21Fe2-46.05(15)
Si2C1C2C3-177.65(15) C20Si3C21C2247.4(2)
Si2C1C2C145.6(3) C20Si3C21C25-133.15(16)
Si2C1C5Fe1119.21(14) C21Si3O1Si2159.37(15)
Si2C1C5C4178.31(14) C21C22C23Fe258.73(13)
Si3C21C22Fe2-121.34(16) C21C22C23Si4-178.18(15)
Si3C21C22C23179.85(15) C21C22C23C24-0.2(2)
Si3C21C22C342.0(3) C21C22C34N2120.5(2)
Si3C21C25Fe2121.12(14) C22C21C25Fe2-59.28(12)
Si3C21C25C24-179.85(14) C22C21C25C24-0.2(2)
Si4C23C24Fe2-122.74(15) C22C23C24Fe259.14(13)
Si4C23C24C25178.18(15) C22C23C24C250.1(2)
O1Si2C1Fe169.79(13) C23C22C34N2-57.1(2)
O1Si2C1C2161.83(17) C23C24C25Fe259.40(14)
O1Si2C1C5-15.90(18) C23C24C25C210.1(2)
O1Si3C21Fe273.38(13) C25C21C22Fe259.10(13)
O1Si3C21C22166.78(17) C25C21C22C230.3(2)
O1Si3C21C25-13.72(18) C25C21C22C34-177.60(17)
C1Si2O1Si3155.45(15) C26C27C28Fe2-59.72(14)
C1C2C3Fe158.49(13) C26C27C28C29-0.1(2)
C1C2C3Si1178.51(15) C27C26C30Fe259.29(15)
C1C2C3C4-0.7(2) C27C26C30C29-0.2(2)
C1C2C14N1121.8(2) C27C28C29Fe2-59.56(15)
C2C1C5Fe1-59.00(13) C27C28C29C300.0(3)
C2C1C5C40.1(2) C28C29C30Fe2-59.32(16)
C2C3C4Fe159.50(13) C28C29C30C260.1(3)
C2C3C4C50.7(2) C30C26C27Fe2-59.38(15)
C3C2C14N1-54.5(3) C30C26C27C280.2(2)
C3C4C5Fe159.08(14) C31Si4C23Fe2-177.00(14)
C3C4C5C1-0.5(2) C31Si4C23C2289.2(2)
C5C1C2Fe158.64(13) C31Si4C23C24-88.5(2)
C5C1C2C30.4(2) C32Si4C23Fe259.48(16)
C5C1C2C14-176.35(18) C32Si4C23C22-34.4(2)
C6C7C8Fe1-59.76(14) C32Si4C23C24148.00(17)
C6C7C8C9-0.8(2) C33Si4C23Fe2-60.03(17)
C7C6C10Fe159.07(14) C33Si4C23C22-153.9(2)
C7C6C10C9-0.3(2) C33Si4C23C2428.5(2)
C7C8C9Fe1-58.92(15) C34C22C23Fe2-123.33(18)
C7C8C9C100.6(2) C34C22C23Si4-0.2(3)
C8C9C10Fe1-59.64(15) C34C22C23C24177.72(18)
C8C9C10C6-0.2(2) C35N2C34C22-63.3(2)
C10C6C7Fe1-59.15(15) C36N2C34C22174.18(17)

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for mo_B0425_0m.
AtomxyzU(eq)
H460403514279120
H552883403412620
H65154397437626
H74187-728292927
H85963239209427
H979821980302028
H1074892074443128
H11A2181220163343
H11B335023925943
H11C3688329287343
H12A67063173138546
H12B6421222560846
H12C68552035149246
H13A3970-12499144
H13B369618113344
H13C2401-5263044
H14A1898-197201023
H14B979170261823
H15A-4891251220355
H15B-3111698139855
H15C10642185217055
H16A-1177-620148467
H16B-174-87288467
H16C-1125-13768967
H17A2701-213429535
H17B1042-404383635
H17C1480-133480135
H18A4251783481933
H18B271479385433
H18C11152707433433
H19A15181523624437
H19B26581963710937
H19C2723984646037
H20A42174539601739
H20B36484303681939
H20C24853821596239
H2490162582662922
H2564962026567820
H2662784892547630
H2773456056690727
H28100056142734030
H29105735030618336
H3082594253502835
H31A105193149942958
H31B94072216866358
H31C87512877926458
H32A101135882866935
H32B109775634943835
H32C91875253925935
H33A117264742766464
H33B115123491767464
H33C124704460845364
H34A69194906820619
H34B52264031786519
H35A43042448848346
H35B54762223912246
H35C55712071819446
H36A49994289927835
H36B67375091955835
H36C61124027992735

Experimental

Single crystals of C36H60Fe2N2OSi4 [mo_B0425_0m] were []. A suitable crystal was selected and [] on a Bruker D8 Venture diffractometer. The crystal was kept at 99.99 K during data collection. Using Olex2 [1], the structure was solved with the ShelXT [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_B0425_0m]

Crystal Data for C36H60Fe2N2OSi4 (=760.92 g/mol): triclinic, space group P-1 (no. 2), a = 9.7419(18) Å, b = 13.252(3) Å, c = 17.228(3) Å, α = 98.993(5)°, β = 98.779(5)°, γ = 110.464(5)°, = 2005.8(6) Å3, Z = 2, T = 99.99 K, μ(MoKα) = 0.872 mm-1, Dcalc = 1.260 g/cm3, 101034 reflections measured (4.528° ≤ 2Θ ≤ 59.356°), 11305 unique (Rint = 0.0374, Rsigma = 0.0219) which were used in all calculations. The final R1 was 0.0418 (I > 2σ(I)) and wR2 was 0.1206 (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:
C14(H14A,H14B), C34(H34A,H34B)
2.b Aromatic/amide H refined with riding coordinates:
C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C24(H24), C25(H25),
C26(H26), C27(H27), C28(H28), C29(H29), C30(H30)
2.c Idealised Me refined as rotating group:
C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,
H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,
H19B,H19C), C20(H20A,H20B,H20C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C),
C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C)

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