mo_B0105_0m

Table 1 Crystal data and structure refinement for mo_B0105_0m.
Identification code mo_B0105_0m
Empirical formula C50H58Fe2N2O4Si2
Formula weight 918.86
Temperature/K 100.0
Crystal system orthorhombic
Space group P212121
a/Å 12.987(3)
b/Å 16.187(3)
c/Å 21.860(4)
α/° 90
β/° 90
γ/° 90
Volume/Å3 4595.6(16)
Z 4
ρcalcg/cm3 1.328
μ/mm‑1 0.729
F(000) 1936.0
Crystal size/mm3 0.254 × 0.168 × 0.12
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.496 to 52.79
Index ranges -16 ≤ h ≤ 13, -20 ≤ k ≤ 18, -27 ≤ l ≤ 22
Reflections collected 30298
Independent reflections 9340 [Rint = 0.0425, Rsigma = 0.0465]
Data/restraints/parameters 9340/0/555
Goodness-of-fit on F2 1.069
Final R indexes [I>=2σ (I)] R1 = 0.0345, wR2 = 0.0784
Final R indexes [all data] R1 = 0.0398, wR2 = 0.0806
Largest diff. peak/hole / e Å-3 0.53/-0.30
Flack parameter-0.002(7)

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for mo_B0105_0m. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Fe15770.7(4)2435.0(3)1857.1(2)14.77(12)
Fe29323.1(4)7280.8(3)1676.5(2)14.14(12)
Si16420.6(7)4407.7(6)2231.0(4)12.0(2)
Si28483.5(7)5422.2(6)2281.2(4)11.45(19)
O17388.9(18)4975.2(15)2449.1(11)15.5(5)
O26034.1(19)4698.8(18)1560.3(12)17.8(6)
O39040.6(19)4969.0(17)1711.2(12)19.4(6)
N18757(2)3476.2(19)1201.1(14)15.6(6)
N26331(2)6209.1(18)1040.9(13)14.7(6)
C16766(3)3297(2)2215.7(16)13.7(7)
C27265(2)2816(2)1741.4(16)13.6(7)
C37238(3)1964(2)1917.2(18)16.3(8)
C46740(3)1904(2)2489.2(16)16.6(8)
C56448(3)2710(2)2674.7(16)14.8(7)
C64609(3)3056(2)1422.2(18)22.1(9)
C75041(3)2460(3)1026.9(17)23.8(8)
C84913(3)1672(3)1307(2)27.4(9)
C94412(3)1791(2)1872(2)26.6(9)
C104219(3)2643(3)1944.7(18)25.4(8)
C117697(3)3140(2)1152.8(16)15.0(7)
C129490(3)2860(2)1424.0(18)23.8(9)
C139081(3)3773(3)591.4(16)24.1(9)
C145373(3)4541(2)2811.4(16)12.8(7)
C155511(3)4427(2)3458.8(15)14.4(7)
C166492(3)4250(2)3720.1(17)18.6(8)
C176601(3)4157(3)4339.0(18)22.5(9)
C185754(3)4224(2)4733.5(17)26.2(9)
C194792(3)4394(2)4499.3(17)21.5(8)
C204654(3)4499(2)3861.1(16)16.8(8)
C213668(3)4701(2)3614.1(18)19.2(8)
C223545(3)4819(2)3003.8(18)19.4(8)
C234394(3)4733(2)2600.4(16)16.2(7)
C248260(3)6521(2)2095.6(15)12.2(7)
C257835(3)6898(2)1546.5(16)13.5(7)
C267875(3)7774(2)1613.8(17)17.7(8)
C278300(3)7959(2)2195.1(17)16.2(8)
C288539(3)7198(2)2485.8(16)15.1(7)
C2910377(3)6556(3)1233.8(18)21.0(8)
C3010119(3)7252(2)864.0(17)20.6(8)
C3110381(3)7975(3)1196(2)26.5(9)
C3210801(3)7734(3)1764.2(18)28.7(9)
C3310801(3)6862(3)1789.8(18)26.7(9)
C347429(3)6465(2)989.1(16)15.3(7)
C355664(3)6889(2)1235.4(18)23.5(8)
C365989(3)5899(3)443.1(16)20.6(8)
C379301(3)5348(2)2984.2(15)13.7(7)
C389005(3)5677(2)3570.5(15)12.8(7)
C398033(3)6063(2)3663.0(16)17.9(8)
C407797(3)6434(3)4208.3(17)23.3(9)
C418503(3)6413(3)4697.1(17)25.3(9)
C429426(3)6015(2)4635.7(16)22.8(8)
C439699(3)5635(2)4076.0(16)16.4(8)
C4410650(3)5214(2)4004.7(17)19.9(8)
C4510911(3)4877(2)3453.7(17)19.4(8)
C4610248(3)4960(2)2945.7(17)17.0(8)
O42391(2)4835.9(18)5289.6(14)33.0(7)
C472624(4)5559(3)5625(2)42.8(12)
C482840(5)6248(3)5180(3)69.8(19)
C492147(3)4156(3)5669(2)33.9(11)
C502013(4)3398(3)5283(3)54.0(15)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for mo_B0105_0m. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Fe113.0(2)11.1(3)20.1(3)0.31(19)-3.9(2)-1.4(2)
Fe212.3(2)15.1(3)15.0(2)0.63(18)0.4(2)-2.9(2)
Si112.7(4)9.1(5)14.0(4)0.6(4)-1.0(4)-1.4(4)
Si212.4(4)9.2(5)12.8(4)-0.8(4)-0.9(4)-0.4(3)
O116.5(13)12.3(13)17.6(13)0.9(10)-0.9(10)-3.5(10)
O221.4(14)14.6(15)17.5(14)2.5(11)-2.8(10)-5.0(11)
O323.2(14)16.3(14)18.6(13)-5.1(11)5.0(11)-3.5(10)
N116.3(15)14.5(16)16.1(15)-1.0(12)1.1(12)-0.4(12)
N212.3(14)15.7(16)16.1(15)0.4(12)-3.0(12)-1.6(12)
C113.4(16)12.5(18)15.2(17)-0.5(14)-4.9(14)-1.4(13)
C211.1(15)13.1(18)16.6(18)-1.6(14)-5.4(14)-0.9(13)
C313.7(17)11.7(18)23.6(19)-3.1(15)-4.0(15)1.8(13)
C417.1(18)11.7(19)20.9(19)4.8(14)-7.3(15)-1.4(14)
C517.0(16)12.1(18)15.2(16)0.1(14)-2.1(14)-0.4(14)
C618.0(19)18(2)30(2)1.5(16)-13.0(16)-0.5(15)
C716.6(18)33(2)21(2)3.8(17)-9.2(15)-3.8(17)
C821(2)19(2)43(3)-8.9(18)-13.6(19)-0.6(16)
C915.4(18)26(2)39(2)11.2(18)-8.3(18)-9.2(16)
C1012.1(16)35(2)29(2)-0.5(17)-1.9(16)2.1(17)
C1116.2(17)13.6(19)15.2(17)-2.5(13)-2.6(14)2.5(14)
C1218.0(19)23(2)30(2)1.7(16)-0.7(16)5.0(16)
C1326(2)30(2)16.8(19)-2.2(16)1.5(16)-2.2(17)
C1417.2(17)4.5(16)16.7(17)1.3(13)-1.2(14)-1.4(12)
C1517.3(18)7.8(17)18.1(18)0.1(13)-0.7(14)-3.0(13)
C1618.2(18)17(2)20.8(19)2.3(15)-0.4(16)-2.7(15)
C1720(2)25(2)22(2)3.8(16)-6.7(16)-0.2(17)
C1832(2)30(2)16.6(18)4.3(15)-1.5(18)-5.9(19)
C1923(2)22(2)19.1(19)0.5(16)4.6(16)-6.7(16)
C2020.9(19)10.3(18)19.0(18)-0.9(14)1.2(15)-4.9(14)
C2117.2(18)13.3(19)27(2)-1.7(15)5.1(16)-2.0(15)
C2213.4(17)15.8(19)29(2)0.5(15)-2.5(16)0.9(14)
C2320.8(19)10.5(17)17.5(18)1.2(13)-1.8(15)-2.4(14)
C2411.1(16)10.9(18)14.5(17)0.6(13)2.4(13)-3.4(13)
C258.5(16)17.2(19)15.0(18)2.2(14)2.8(14)-1.1(13)
C2617.8(17)11.7(19)23.7(19)6.5(15)-0.1(15)0.2(14)
C2717.2(17)10.0(18)21.3(19)-3.2(14)2.6(15)-3.3(14)
C2816.0(17)14.2(19)15.3(16)-0.7(14)2.8(14)-3.9(14)
C2913.4(18)20(2)29(2)-1.5(16)7.0(16)0.2(14)
C3020.8(18)24(2)16.6(18)0.1(15)4.1(15)-0.2(16)
C3124(2)21(2)34(2)0.6(17)16.1(18)-5.7(16)
C3218.5(19)41(3)27(2)-6.2(18)2.9(18)-17.7(19)
C339.5(17)44(3)27(2)7.7(18)1.2(18)2.7(17)
C3414.6(17)17.0(19)14.3(17)1.9(14)0.7(14)0.2(14)
C3514.9(18)27(2)28(2)-5.3(16)-3.2(17)3.9(17)
C3619.8(19)28(2)13.7(18)0.4(15)-3.3(15)-2.7(16)
C3712.9(16)12.2(17)15.8(17)2.1(12)0.1(14)-1.1(14)
C3815.2(17)6.4(17)16.9(17)2.0(13)0.9(14)-3.3(13)
C3917.2(18)20(2)16.0(18)1.3(15)0.2(15)-1.5(15)
C4020(2)26(2)24(2)-1.5(16)6.3(17)1.4(17)
C4133(2)29(2)14.1(19)-3.1(16)7.4(17)-3.5(18)
C4230(2)24(2)14.6(18)2.1(15)-4.1(16)-4.6(17)
C4319.6(18)12.0(19)17.7(18)2.3(14)-2.2(15)-6.5(14)
C4419.5(18)17.3(19)22.9(19)3.5(14)-9.0(16)-2.4(16)
C4514.0(18)14.6(19)30(2)0.1(15)-4.6(16)2.8(14)
C4615.6(17)15.9(19)19.5(18)-1.3(14)2.4(14)1.1(14)
O434.7(16)27.1(17)37.4(17)0.7(13)-0.8(14)-2.6(13)
C4738(3)36(3)54(3)-11(2)0(2)0(2)
C4878(4)26(3)105(5)13(3)-22(4)-12(3)
C4921(2)38(3)44(3)8(2)0(2)-1.8(19)
C5042(3)31(3)89(4)-2(3)11(3)-6(2)

 

Table 4 Bond Lengths for mo_B0105_0m.
AtomAtomLength/Å AtomAtomLength/Å
Fe1C12.057(3) C6C101.416(6)
Fe1C22.052(3) C7C81.424(6)
Fe1C32.057(3) C8C91.409(6)
Fe1C42.058(3) C9C101.411(6)
Fe1C52.041(3) C14C151.438(5)
Fe1C62.047(4) C14C231.388(5)
Fe1C72.048(4) C15C161.426(5)
Fe1C82.053(4) C15C201.423(5)
Fe1C92.050(4) C16C171.368(5)
Fe1C102.052(4) C17C181.402(6)
Fe2C242.063(3) C18C191.377(6)
Fe2C252.049(3) C19C201.417(5)
Fe2C262.048(4) C20C211.427(5)
Fe2C272.063(4) C21C221.357(5)
Fe2C282.046(3) C22C231.419(5)
Fe2C292.046(4) C24C251.455(5)
Fe2C302.055(4) C24C281.435(5)
Fe2C312.062(4) C25C261.427(5)
Fe2C322.063(4) C25C341.501(5)
Fe2C332.051(4) C26C271.418(5)
Si1O11.629(2) C27C281.421(5)
Si1O21.620(3) C29C301.427(6)
Si1C11.853(4) C29C331.424(6)
Si1C141.873(4) C30C311.419(6)
Si2O11.637(2) C31C321.411(6)
Si2O31.617(3) C32C331.412(6)
Si2C241.848(4) C37C381.440(5)
Si2C371.871(3) C37C461.384(5)
N1C111.484(4) C38C391.423(5)
N1C121.462(5) C38C431.427(5)
N1C131.478(5) C39C401.370(5)
N2C341.490(4) C40C411.409(6)
N2C351.464(5) C41C421.367(6)
N2C361.468(4) C42C431.414(5)
C1C21.450(5) C43C441.420(5)
C1C51.442(5) C44C451.365(5)
C2C31.431(5) C45C461.412(5)
C2C111.499(5) O4C471.414(6)
C3C41.411(5) O4C491.414(5)
C4C51.419(5) C47C481.506(8)
C6C71.412(6) C49C501.500(7)

 

Table 5 Bond Angles for mo_B0105_0m.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C1Fe1C469.10(14) Si1C1Fe1120.87(17)
C2Fe1C141.33(13) C2C1Fe169.13(19)
C2Fe1C340.77(14) C2C1Si1130.0(3)
C2Fe1C468.25(14) C5C1Fe168.80(19)
C2Fe1C8128.44(16) C5C1Si1123.9(3)
C2Fe1C10153.01(15) C5C1C2105.7(3)
C3Fe1C169.21(14) C1C2Fe169.53(18)
C3Fe1C440.11(15) C1C2C11126.4(3)
C5Fe1C141.21(14) C3C2Fe169.82(19)
C5Fe1C268.59(14) C3C2C1108.4(3)
C5Fe1C368.01(15) C3C2C11125.2(3)
C5Fe1C440.49(14) C11C2Fe1124.4(2)
C5Fe1C6128.13(15) C2C3Fe169.41(19)
C5Fe1C7166.23(15) C4C3Fe170.0(2)
C5Fe1C8151.43(16) C4C3C2108.4(3)
C5Fe1C9117.93(16) C3C4Fe169.9(2)
C5Fe1C10107.80(15) C3C4C5108.2(3)
C6Fe1C1107.89(15) C5C4Fe169.1(2)
C6Fe1C2119.52(15) C1C5Fe169.98(19)
C6Fe1C3153.46(16) C4C5Fe170.4(2)
C6Fe1C4165.49(16) C4C5C1109.3(3)
C6Fe1C740.33(16) C7C6Fe169.9(2)
C6Fe1C867.85(16) C7C6C10108.3(4)
C6Fe1C967.80(16) C10C6Fe170.0(2)
C6Fe1C1040.43(16) C6C7Fe169.8(2)
C7Fe1C1127.97(15) C6C7C8107.6(4)
C7Fe1C2108.82(14) C8C7Fe169.9(2)
C7Fe1C3119.51(16) C7C8Fe169.5(2)
C7Fe1C4152.42(16) C9C8Fe169.8(2)
C7Fe1C840.64(16) C9C8C7107.9(4)
C7Fe1C967.99(16) C8C9Fe170.0(2)
C7Fe1C1067.98(15) C8C9C10108.3(4)
C8Fe1C1166.51(16) C10C9Fe170.0(2)
C8Fe1C3108.50(15) C6C10Fe169.6(2)
C8Fe1C4118.30(16) C9C10Fe169.8(2)
C9Fe1C1151.64(16) C9C10C6107.8(4)
C9Fe1C2165.66(16) N1C11C2114.5(3)
C9Fe1C3127.46(15) C15C14Si1124.1(3)
C9Fe1C4107.69(15) C23C14Si1117.8(3)
C9Fe1C840.16(17) C23C14C15118.0(3)
C9Fe1C1040.24(16) C16C15C14122.1(3)
C10Fe1C1118.04(15) C20C15C14120.0(3)
C10Fe1C3164.75(16) C20C15C16117.9(3)
C10Fe1C4127.37(15) C17C16C15120.7(4)
C10Fe1C867.69(16) C16C17C18121.2(4)
C25Fe2C2441.43(13) C19C18C17119.9(3)
C25Fe2C2768.30(14) C18C19C20120.3(4)
C25Fe2C30110.32(15) C15C20C21119.1(3)
C25Fe2C31136.26(16) C19C20C15120.0(3)
C25Fe2C32175.94(16) C19C20C21120.9(3)
C25Fe2C33143.06(16) C22C21C20120.7(3)
C26Fe2C2469.35(14) C21C22C23120.3(4)
C26Fe2C2540.76(14) C14C23C22121.8(3)
C26Fe2C2740.35(14) Si2C24Fe2124.47(18)
C26Fe2C30114.37(15) C25C24Fe268.76(18)
C26Fe2C31111.43(16) C25C24Si2130.1(3)
C26Fe2C32136.23(16) C28C24Fe268.90(19)
C26Fe2C33175.31(17) C28C24Si2124.4(3)
C27Fe2C2469.05(13) C28C24C25105.5(3)
C27Fe2C32111.02(15) C24C25Fe269.82(18)
C28Fe2C2440.88(13) C24C25C34127.4(3)
C28Fe2C2568.33(14) C26C25Fe269.6(2)
C28Fe2C2668.05(15) C26C25C24108.5(3)
C28Fe2C2740.46(14) C26C25C34124.1(3)
C28Fe2C29134.78(15) C34C25Fe2125.8(2)
C28Fe2C30174.94(16) C25C26Fe269.7(2)
C28Fe2C31143.87(16) C27C26Fe270.4(2)
C28Fe2C32113.95(15) C27C26C25108.5(3)
C28Fe2C33109.86(15) C26C27Fe269.3(2)
C29Fe2C24108.41(15) C26C27C28107.6(3)
C29Fe2C25113.05(15) C28C27Fe269.1(2)
C29Fe2C26143.72(15) C24C28Fe270.23(19)
C29Fe2C27174.82(16) C27C28Fe270.4(2)
C29Fe2C3040.72(16) C27C28C24109.9(3)
C29Fe2C3168.05(16) C30C29Fe270.0(2)
C29Fe2C3268.01(16) C33C29Fe269.8(2)
C29Fe2C3340.67(16) C33C29C30107.4(4)
C30Fe2C24134.96(15) C29C30Fe269.3(2)
C30Fe2C27144.15(15) C31C30Fe270.1(2)
C30Fe2C3140.31(16) C31C30C29107.8(3)
C30Fe2C3267.71(15) C30C31Fe269.6(2)
C31Fe2C24175.26(15) C32C31Fe270.0(2)
C31Fe2C27114.74(15) C32C31C30108.3(4)
C31Fe2C3240.01(16) C31C32Fe270.0(2)
C32Fe2C24142.46(15) C31C32C33108.2(4)
C33Fe2C24112.07(15) C33C32Fe269.4(2)
C33Fe2C27135.43(16) C29C33Fe269.5(2)
C33Fe2C3068.06(15) C32C33Fe270.4(2)
C33Fe2C3167.55(17) C32C33C29108.3(4)
C33Fe2C3240.15(17) N2C34C25113.8(3)
O1Si1C1111.46(14) C38C37Si2123.8(3)
O1Si1C14107.33(14) C46C37Si2118.9(3)
O2Si1O1109.88(14) C46C37C38117.3(3)
O2Si1C1109.93(16) C39C38C37121.7(3)
O2Si1C14110.77(15) C39C38C43118.1(3)
C1Si1C14107.43(16) C43C38C37120.2(3)
O1Si2C24109.77(14) C40C39C38121.0(3)
O1Si2C37106.25(14) C39C40C41120.2(4)
O3Si2O1111.15(14) C42C41C40120.5(4)
O3Si2C24109.75(15) C41C42C43120.6(4)
O3Si2C37110.48(15) C42C43C38119.4(3)
C24Si2C37109.37(15) C42C43C44121.5(3)
Si1O1Si2148.68(17) C44C43C38119.1(3)
C12N1C11112.2(3) C45C44C43120.3(3)
C12N1C13109.7(3) C44C45C46120.3(3)
C13N1C11108.6(3) C37C46C45122.5(3)
C35N2C34112.3(3) C47O4C49112.8(4)
C35N2C36109.7(3) O4C47C48108.5(4)
C36N2C34108.5(3) O4C49C50109.4(4)

 

Table 6 Hydrogen Bonds for mo_B0105_0m.
DHAd(D-H)/Åd(H-A)/Åd(D-A)/ÅD-H-A/°
O2H2N20.76(5)2.00(5)2.723(4)161(5)
O3H3N10.81(6)1.89(6)2.687(4)168(6)

 

Table 7 Torsion Angles for mo_B0105_0m.
ABCDAngle/˚ ABCDAngle/˚
Fe1C1C2C3-59.2(2) C8C9C10Fe1-59.7(3)
Fe1C1C2C11118.3(3) C8C9C10C6-0.3(4)
Fe1C1C5C459.6(2) C10C6C7Fe1-59.6(3)
Fe1C2C3C4-59.3(2) C10C6C7C80.3(4)
Fe1C2C11N1172.5(2) C11C2C3Fe1-118.5(3)
Fe1C3C4C5-58.7(2) C11C2C3C4-177.8(3)
Fe1C4C5C1-59.3(2) C12N1C11C258.7(4)
Fe1C6C7C859.9(3) C13N1C11C2-179.9(3)
Fe1C6C10C9-59.6(3) C14Si1O1Si2-164.3(3)
Fe1C7C8C959.4(3) C14Si1C1Fe170.5(2)
Fe1C8C9C1059.7(3) C14Si1C1C2158.1(3)
Fe1C9C10C659.4(3) C14Si1C1C5-13.5(3)
Fe2C24C25C26-59.0(2) C14C15C16C17179.0(3)
Fe2C24C25C34120.2(3) C14C15C20C19-179.5(3)
Fe2C24C28C2759.4(2) C14C15C20C21-1.2(5)
Fe2C25C26C27-59.9(2) C15C14C23C220.1(5)
Fe2C25C34N2176.0(2) C15C16C17C180.8(6)
Fe2C26C27C28-58.7(2) C15C20C21C220.2(6)
Fe2C27C28C24-59.3(2) C16C15C20C19-0.1(5)
Fe2C29C30C3159.8(2) C16C15C20C21178.2(3)
Fe2C29C33C32-59.9(3) C16C17C18C19-0.7(6)
Fe2C30C31C3259.5(3) C17C18C19C200.3(6)
Fe2C31C32C3359.1(3) C18C19C20C150.2(6)
Fe2C32C33C2959.4(3) C18C19C20C21-178.1(4)
Si1C1C2Fe1-113.4(3) C19C20C21C22178.5(4)
Si1C1C2C3-172.6(3) C20C15C16C17-0.4(5)
Si1C1C2C114.9(5) C20C21C22C230.9(6)
Si1C1C5Fe1113.7(2) C21C22C23C14-1.1(6)
Si1C1C5C4173.3(2) C23C14C15C16-178.3(3)
Si1C14C15C164.0(5) C23C14C15C201.0(5)
Si1C14C15C20-176.7(3) C24Si2O1Si198.0(3)
Si1C14C23C22177.9(3) C24Si2C37C3860.4(3)
Si2C24C25Fe2-117.8(3) C24Si2C37C46-119.2(3)
Si2C24C25C26-176.8(3) C24C25C26Fe259.1(2)
Si2C24C25C342.4(5) C24C25C26C27-0.8(4)
Si2C24C28Fe2118.1(3) C24C25C34N285.1(4)
Si2C24C28C27177.5(3) C25C24C28Fe2-59.4(2)
Si2C37C38C392.5(5) C25C24C28C270.0(4)
Si2C37C38C43-176.4(3) C25C26C27Fe259.5(2)
Si2C37C46C45-180.0(3) C25C26C27C280.8(4)
O1Si1C1Fe1-172.24(17) C26C25C34N2-95.8(4)
O1Si1C1C2-84.5(3) C26C27C28Fe258.8(2)
O1Si1C1C5103.8(3) C26C27C28C24-0.5(4)
O1Si1C14C15-52.7(3) C28C24C25Fe259.5(2)
O1Si1C14C23129.7(3) C28C24C25C260.5(4)
O1Si2C24Fe2-165.98(18) C28C24C25C34179.7(3)
O1Si2C24C25-75.8(3) C29C30C31Fe2-59.3(2)
O1Si2C24C28107.4(3) C29C30C31C320.3(4)
O1Si2C37C38-58.0(3) C30C29C33Fe260.2(2)
O1Si2C37C46122.4(3) C30C29C33C320.2(4)
O2Si1O1Si2-43.8(3) C30C31C32Fe2-59.2(3)
O2Si1C1Fe1-50.1(2) C30C31C32C33-0.1(4)
O2Si1C1C237.5(3) C31C32C33Fe2-59.4(3)
O2Si1C1C5-134.1(3) C31C32C33C29-0.1(4)
O2Si1C14C15-172.6(3) C33C29C30Fe2-60.1(3)
O2Si1C14C239.7(3) C33C29C30C31-0.3(4)
O3Si2O1Si1-23.6(4) C34C25C26Fe2-120.1(3)
O3Si2C24Fe2-43.5(2) C34C25C26C27180.0(3)
O3Si2C24C2546.7(3) C35N2C34C2551.0(4)
O3Si2C24C28-130.1(3) C36N2C34C25172.4(3)
O3Si2C37C38-178.7(3) C37Si2O1Si1-143.8(3)
O3Si2C37C461.7(3) C37Si2C24Fe277.8(2)
C1Si1O1Si278.3(3) C37Si2C24C25168.0(3)
C1Si1C14C1567.3(3) C37Si2C24C28-8.8(3)
C1Si1C14C23-110.4(3) C37C38C39C40-174.4(3)
C1C2C3Fe159.0(2) C37C38C43C42175.4(3)
C1C2C3C4-0.3(4) C37C38C43C44-4.4(5)
C1C2C11N183.8(4) C38C37C46C450.4(5)
C2C1C5Fe1-59.6(2) C38C39C40C41-2.4(6)
C2C1C5C40.0(4) C38C43C44C452.1(5)
C2C3C4Fe159.0(2) C39C38C43C42-3.6(5)
C2C3C4C50.3(4) C39C38C43C44176.6(3)
C3C2C11N1-99.1(4) C39C40C41C42-0.7(6)
C3C4C5Fe159.2(2) C40C41C42C431.6(6)
C3C4C5C1-0.2(4) C41C42C43C380.6(6)
C5C1C2Fe159.4(2) C41C42C43C44-179.6(3)
C5C1C2C30.2(4) C42C43C44C45-177.7(4)
C5C1C2C11177.7(3) C43C38C39C404.5(5)
C6C7C8Fe1-59.9(2) C43C44C45C461.4(6)
C6C7C8C9-0.5(4) C44C45C46C37-2.7(6)
C7C6C10Fe159.6(2) C46C37C38C39-177.9(3)
C7C6C10C90.0(4) C46C37C38C433.2(5)
C7C8C9Fe1-59.2(3) C47O4C49C50-174.4(4)
C7C8C9C100.5(4) C49O4C47C48-178.3(4)

 

Table 8 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for mo_B0105_0m.
AtomxyzU(eq)
H26180(40)5140(30)1490(20)32(14)
H38900(40)4510(40)1600(30)59(18)
H3A75101516168820
H466221408271220
H560982842304318
H645833634135026
H75360256564429
H851271157114233
H942341369215532
H1038872895228431
H11A7697268884818
H11B7237358099818
H12A94982386114536
H12B92852677183336
H12C101803105144336
H13A9100330730536
H13B9768402062136
H13C8590418744436
H1670764195346222
H1772634046450427
H1858434152516231
H1942194441476726
H2130924752388023
H2228864961284623
H2342894810217419
H2676538167131921
H2784078496236019
H2888397145288018
H29102835991112825
H309824723546625
H31102898527106032
H32110428095207534
H33110436536212132
H34A7504683663218
H34B7855596891118
H35A58687073164535
H35B49476701124435
H35C5730735094735
H36A6020634714231
H36B5279569847531
H36C6439544631331
H3975406062334221
H4071546708425728
H4183376678507230
H4298885993497227
H44111075166434224
H45115424585341223
H46104604741256320
H47A32345463588751
H47B20365709589151
H48A342760984922105
H48B299967555406105
H48C223263404922105
H49A15034271589741
H49B27064067597041
H50A14693494498181
H50B18232930554481
H50C26613274507281

Experimental

Single crystals of C50H58Fe2N2O4Si2 [mo_B0105_0m] were []. A suitable crystal was selected and [] on a 'Bruker APEX-II CCD' diffractometer. The crystal was kept at 100.0 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_B0105_0m]

Crystal Data for C50H58Fe2N2O4Si2 (=918.86 g/mol): orthorhombic, space group P212121 (no. 19), a = 12.987(3) Å, b = 16.187(3) Å, c = 21.860(4) Å, = 4595.6(16) Å3, Z = 4, T = 100.0 K, μ(MoKα) = 0.729 mm-1, Dcalc = 1.328 g/cm3, 30298 reflections measured (4.496° ≤ 2Θ ≤ 52.79°), 9340 unique (Rint = 0.0425, Rsigma = 0.0465) which were used in all calculations. The final R1 was 0.0345 (I > 2σ(I)) and wR2 was 0.0806 (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), C47(H47A,H47B), C49(H49A,H49B)
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), C16(H16),
C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C26(H26), C27(H27),
C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C39(H39),
C40(H40), C41(H41), C42(H42), 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), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C)

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