mo_B0613_Cc

Table 1 Crystal data and structure refinement for mo_B0613_Cc.
Identification code mo_B0613_Cc
Empirical formula C38H44Fe2N2O3Si2
Formula weight 744.63
Temperature/K 100.01
Crystal system monoclinic
Space group Cc
a/Å 24.4022(13)
b/Å 14.0997(7)
c/Å 10.2884(6)
α/° 90
β/° 90.067(2)
γ/° 90
Volume/Å3 3539.9(3)
Z 4
ρcalcg/cm3 1.397
μ/mm‑1 0.927
F(000) 1560.0
Crystal size/mm3 0.52 × 0.498 × 0.318
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 5.176 to 62
Index ranges -35 ≤ h ≤ 35, -20 ≤ k ≤ 20, -14 ≤ l ≤ 14
Reflections collected 105245
Independent reflections 11142 [Rint = 0.0347, Rsigma = 0.0207]
Data/restraints/parameters 11142/2/432
Goodness-of-fit on F2 1.033
Final R indexes [I>=2σ (I)] R1 = 0.0201, wR2 = 0.0472
Final R indexes [all data] R1 = 0.0207, wR2 = 0.0474
Largest diff. peak/hole / e Å-3 0.30/-0.28
Flack parameter0.000(3)

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for mo_B0613_Cc. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Fe16771.5(2)1668.0(2)3887.7(2)10.81(5)
Fe23243.9(2)3490.9(2)3961.5(2)9.78(5)
Si15623.8(2)2726.1(3)5171.7(5)9.57(9)
Si24378.4(2)2279.6(3)5010.0(5)9.90(9)
O14994.4(6)2462.6(11)5581.1(13)12.8(2)
O25647.0(6)3512.1(10)4040.5(17)18.7(3)
O34387.9(6)1725.6(11)3642.5(15)18.1(3)
N15155.8(7)935.7(12)2194.5(16)15.0(3)
N24889.2(6)4410.4(12)2640.9(15)13.3(3)
C15999.9(7)1636.9(12)4677.1(18)9.7(3)
C26021.5(7)1126.8(13)3458.8(18)12.1(3)
C36414.4(8)376.8(14)3586(2)16.1(4)
C46642.8(8)414.1(14)4856(2)16.0(4)
C56393.1(7)1188.1(13)5524.6(18)12.2(3)
C66940.7(8)3061.3(16)3499(2)19.8(4)
C76991.9(8)2508.4(19)2352(2)24.5(5)
C87399.1(9)1796.6(19)2579(2)24.3(4)
C97598.3(8)1922.1(15)3865(2)18.4(4)
C107315.4(8)2701.7(14)4438(2)16.1(4)
C115713.3(7)1349.6(14)2233.3(18)14.2(3)
C125165.2(9)-99.9(16)2322(3)25.3(4)
C134890.5(9)1196.1(19)962(2)25.8(5)
C145962.7(8)3157.9(14)6692(2)15.1(4)
C156334.3(8)3913.4(16)6672(2)22.4(4)
C166585.6(10)4227.9(18)7824(3)33.6(6)
C176467.9(10)3794.9(19)8991(3)35.6(6)
C186103.5(10)3041.0(18)9036(2)29.5(5)
C195855.5(9)2725.7(15)7890(2)20.0(4)
C204008.4(7)3425.1(12)4802.3(18)9.7(3)
C214000.1(7)4068.6(12)3707.6(17)10.7(3)
C223605.1(7)4797.9(12)3961(2)13.7(3)
C233361.4(7)4613.3(13)5198.4(19)13.4(3)
C243607.4(7)3775.4(13)5706.5(18)11.2(3)
C253106.1(8)2184.6(15)3151(2)19.5(4)
C263037.2(9)2912.2(18)2215(2)23.6(4)
C272614.7(8)3530.3(16)2650(2)21.5(4)
C282421.2(8)3180.9(14)3859(2)16.9(3)
C292726.6(8)2353.7(14)4180(2)17.2(4)
C304334.2(7)3996.5(13)2490.2(17)12.8(3)
C314861.3(9)5428.5(15)2937(2)20.2(4)
C325200.9(9)4278.0(18)1437(2)23.0(4)
C333990.0(8)1589.8(14)6257(2)15.8(4)
C343974.4(9)1852.8(16)7563(2)23.1(4)
C353632.0(11)1374(2)8439(3)35.6(6)
C363307.9(10)630(2)8004(3)41.1(7)
C373330.9(10)341(2)6728(3)38.1(7)
C383668.1(9)815.5(17)5857(2)25.0(5)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for mo_B0613_Cc. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Fe16.92(10)15.56(11)9.96(11)-0.94(10)0.58(9)1.45(9)
Fe26.42(10)12.06(10)10.85(11)0.08(10)-1.42(9)0.21(8)
Si16.87(19)10.7(2)11.1(2)-0.41(17)-1.01(16)1.56(16)
Si26.82(19)11.2(2)11.6(2)-0.42(17)0.00(16)1.49(16)
O16.6(5)18.6(6)13.2(5)0.0(5)-0.1(5)2.3(4)
O212.0(6)19.1(6)24.9(8)10.3(6)-0.3(6)2.8(5)
O312.1(7)22.9(7)19.3(7)-9.7(5)-1.8(5)4.3(5)
N110.4(7)19.8(8)14.9(7)-6.4(6)-1.7(6)-1.1(6)
N29.3(6)17.9(7)12.6(7)3.9(6)-0.3(5)-2.9(5)
C17.5(7)11.1(7)10.3(8)0.6(6)0.2(6)0.1(6)
C29.0(7)13.7(8)13.7(8)-2.2(6)0.4(6)-0.8(6)
C315.0(8)14.6(8)18.8(9)-5.9(7)-1.5(7)3.3(6)
C416.3(9)13.1(8)18.7(9)0.4(7)-1.8(7)5.1(7)
C511.6(7)12.7(8)12.4(8)1.1(6)0.4(6)1.0(6)
C612.2(8)21.7(10)25.5(10)10.5(8)1.0(7)-2.4(7)
C713.5(9)44.6(13)15.3(9)11.1(9)-0.1(7)-6.1(9)
C812.4(9)41.8(13)18.7(10)-6.8(9)7.0(8)-3.5(8)
C97.7(7)27.0(9)20.6(10)-1.8(9)0.1(7)0.5(7)
C1011.8(8)18.8(9)17.7(9)0.3(7)-0.6(7)-3.7(7)
C1110.7(8)19.9(8)11.9(8)-2.8(7)-1.1(6)-1.2(6)
C1221.8(10)20.2(10)34.1(12)-8.3(9)-1.8(9)-5.4(8)
C1318.3(9)39.7(13)19.4(10)-6.1(9)-8.2(8)-1.9(9)
C1411.7(8)14.4(8)19.1(9)-7.2(7)-4.4(7)6.0(6)
C1515.8(9)18.4(9)33.0(11)-9.0(8)-4.4(8)2.1(7)
C1621.7(10)25.2(11)53.8(16)-22.0(11)-13.7(10)3.2(9)
C1731.9(12)39.6(13)35.3(14)-23.9(12)-21.5(11)18.8(10)
C1831.8(11)37.2(12)19.5(10)-9.6(10)-9.7(9)20.4(10)
C1918.4(9)23.4(10)18.2(9)-5.1(8)-5.3(7)9.3(8)
C207.1(7)11.4(8)10.4(8)-0.2(6)-0.8(6)-0.7(6)
C218.2(7)11.9(7)11.9(8)1.5(6)-1.1(6)-1.2(6)
C2211.7(7)11.0(7)18.4(8)2.1(7)-0.4(7)1.0(6)
C2311.0(8)13.1(8)16.1(8)-1.7(7)-0.1(6)1.9(6)
C249.1(7)12.8(8)11.8(8)-2.3(6)-1.3(6)1.0(6)
C2512.9(8)20.0(9)25.5(10)-10.3(8)-4.8(7)-0.7(7)
C2615.1(9)41.0(13)14.7(9)-6.7(9)-4.4(7)-5.8(8)
C2712.7(9)29.6(11)22(1)5.5(8)-9.6(8)-2.5(7)
C287.4(7)18.8(8)24.4(10)-1.6(8)-2.2(7)-1.2(6)
C2913.1(8)14.5(8)23.9(10)-0.9(7)-2.9(7)-3.6(6)
C3010.6(7)16.4(8)11.5(8)1.8(6)-0.3(6)-2.1(6)
C3122.2(9)17.3(9)21.1(10)5.7(7)-3.6(8)-7.4(8)
C3217.6(9)33.6(11)18.0(9)4.2(8)5.7(7)-5.3(8)
C339.9(8)14.7(8)22.9(10)6.8(7)0.6(7)4.8(6)
C3423.8(10)22.4(10)23.0(11)7.1(8)6.1(8)9.9(8)
C3534.3(13)40.3(14)32.1(13)20.5(11)15.3(11)20.9(11)
C3621.5(11)43.8(15)58.1(18)35.6(14)11.4(11)7.4(10)
C3723.2(11)31.1(12)60.2(18)26.0(12)-3.1(12)-6.6(9)
C3818.3(9)21.8(10)34.8(12)11.0(9)-3.9(9)-2.9(8)

 

Table 4 Bond Lengths for mo_B0613_Cc.
AtomAtomLength/Å AtomAtomLength/Å
Fe1C12.0520(17) C1C21.446(3)
Fe1C22.0311(18) C1C51.442(2)
Fe1C32.042(2) C2C31.433(3)
Fe1C42.053(2) C2C111.501(3)
Fe1C52.0373(19) C3C41.421(3)
Fe1C62.047(2) C4C51.427(3)
Fe1C72.048(2) C6C71.421(3)
Fe1C82.049(2) C6C101.422(3)
Fe1C92.0493(19) C7C81.431(3)
Fe1C102.0503(19) C8C91.420(3)
Fe2C202.0574(18) C9C101.426(3)
Fe2C212.0342(17) C14C151.399(3)
Fe2C222.0427(18) C14C191.400(3)
Fe2C232.0507(19) C15C161.405(3)
Fe2C242.0413(18) C16C171.377(5)
Fe2C252.049(2) C17C181.387(4)
Fe2C262.036(2) C18C191.397(3)
Fe2C272.044(2) C20C211.446(2)
Fe2C282.0570(19) C20C241.438(2)
Fe2C292.0532(19) C21C221.433(2)
Si1O11.6358(15) C21C301.499(2)
Si1O21.6081(15) C22C231.430(3)
Si1C11.8602(18) C23C241.424(3)
Si1C141.870(2) C25C261.417(3)
Si2O11.6339(14) C25C291.427(3)
Si2O31.6095(15) C26C271.422(3)
Si2C201.8626(18) C27C281.420(3)
Si2C331.869(2) C28C291.423(3)
N1C111.481(2) C33C341.395(3)
N1C121.466(3) C33C381.406(3)
N1C131.470(3) C34C351.403(3)
N2C301.483(2) C35C361.389(5)
N2C311.469(3) C36C371.375(5)
N2C321.467(3) C37C381.389(3)

 

Table 5 Bond Angles for mo_B0613_Cc.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C1Fe1C469.44(7) O3Si2C33110.80(9)
C2Fe1C141.48(7) C20Si2C33106.49(8)
C2Fe1C341.20(7) Si2O1Si1143.81(9)
C2Fe1C469.12(8) C12N1C11112.07(16)
C2Fe1C569.24(7) C12N1C13109.43(18)
C2Fe1C6120.01(8) C13N1C11109.18(16)
C2Fe1C7106.69(8) C31N2C30111.34(16)
C2Fe1C8124.37(8) C32N2C30109.64(15)
C2Fe1C9161.83(8) C32N2C31108.87(17)
C2Fe1C10155.49(8) Si1C1Fe1122.94(9)
C3Fe1C169.48(7) C2C1Fe168.48(10)
C3Fe1C440.59(8) C2C1Si1131.77(13)
C3Fe1C6155.80(8) C5C1Fe168.81(10)
C3Fe1C7120.73(9) C5C1Si1121.66(14)
C3Fe1C8107.34(9) C5C1C2106.32(15)
C3Fe1C9125.03(8) C1C2Fe170.03(10)
C3Fe1C10162.12(8) C1C2C11127.26(16)
C5Fe1C141.29(7) C3C2Fe169.81(11)
C5Fe1C368.64(8) C3C2C1108.24(16)
C5Fe1C440.84(7) C3C2C11124.44(17)
C5Fe1C6124.88(8) C11C2Fe1123.67(13)
C5Fe1C7161.79(9) C2C3Fe168.99(11)
C5Fe1C8155.89(9) C4C3Fe170.13(11)
C5Fe1C9120.99(9) C4C3C2108.56(16)
C5Fe1C10107.57(8) C3C4Fe169.27(11)
C6Fe1C1106.45(8) C3C4C5107.73(16)
C6Fe1C4162.17(9) C5C4Fe168.97(11)
C6Fe1C740.60(10) C1C5Fe169.90(10)
C6Fe1C868.64(9) C4C5Fe170.19(11)
C6Fe1C968.36(8) C4C5C1109.15(16)
C6Fe1C1040.63(8) C7C6Fe169.73(13)
C7Fe1C1124.05(8) C7C6C10108.14(19)
C7Fe1C4155.91(10) C10C6Fe169.82(11)
C7Fe1C840.90(10) C6C7Fe169.67(12)
C7Fe1C968.31(9) C6C7C8108.12(19)
C7Fe1C1068.35(9) C8C7Fe169.59(13)
C8Fe1C1161.64(8) C7C8Fe169.51(12)
C8Fe1C4120.65(9) C9C8Fe169.75(12)
C8Fe1C940.55(9) C9C8C7107.5(2)
C8Fe1C1068.56(9) C8C9Fe169.70(11)
C9Fe1C1155.82(8) C8C9C10108.42(19)
C9Fe1C4107.89(8) C10C9Fe169.68(11)
C9Fe1C1040.71(8) C6C10Fe169.56(12)
C10Fe1C1120.00(8) C6C10C9107.78(19)
C10Fe1C4125.27(8) C9C10Fe169.60(11)
C21Fe2C2041.40(7) N1C11C2113.55(16)
C21Fe2C2241.17(7) C15C14Si1121.46(17)
C21Fe2C2369.17(7) C15C14C19117.76(19)
C21Fe2C2468.96(7) C19C14Si1120.78(16)
C21Fe2C25117.14(8) C14C15C16120.7(2)
C21Fe2C26105.72(8) C17C16C15120.3(2)
C21Fe2C27125.81(8) C16C17C18120.2(2)
C21Fe2C28164.55(8) C17C18C19119.5(3)
C21Fe2C29152.21(8) C18C19C14121.6(2)
C22Fe2C2069.50(7) Si2C20Fe2121.77(9)
C22Fe2C2340.89(8) C21C20Fe268.44(10)
C22Fe2C25151.79(9) C21C20Si2129.77(14)
C22Fe2C27107.40(8) C24C20Fe268.86(10)
C22Fe2C28127.79(7) C24C20Si2123.61(14)
C22Fe2C29165.90(8) C24C20C21106.22(15)
C23Fe2C2069.38(7) C20C21Fe270.16(10)
C23Fe2C28109.35(8) C20C21C30126.94(16)
C23Fe2C29128.33(8) C22C21Fe269.74(10)
C24Fe2C2041.09(7) C22C21C20108.49(15)
C24Fe2C2268.65(8) C22C21C30124.55(16)
C24Fe2C2340.74(7) C30C21Fe2125.07(12)
C24Fe2C25127.25(8) C21C22Fe269.10(10)
C24Fe2C27154.26(9) C23C22Fe269.86(11)
C24Fe2C28120.64(8) C23C22C21108.17(16)
C24Fe2C29108.88(8) C22C23Fe269.26(10)
C25Fe2C20106.18(7) C24C23Fe269.28(10)
C25Fe2C23165.64(9) C24C23C22107.59(16)
C25Fe2C2868.20(8) C20C24Fe270.06(10)
C25Fe2C2940.72(9) C23C24Fe269.98(10)
C26Fe2C20125.20(8) C23C24C20109.52(16)
C26Fe2C22117.88(9) C26C25Fe269.21(12)
C26Fe2C23153.01(9) C26C25C29107.86(18)
C26Fe2C24164.09(8) C29C25Fe269.79(11)
C26Fe2C2540.59(10) C25C26Fe270.20(12)
C26Fe2C2740.81(9) C25C26C27108.38(19)
C26Fe2C2868.23(9) C27C26Fe269.88(12)
C26Fe2C2968.41(9) C26C27Fe269.31(11)
C27Fe2C20163.52(8) C28C27Fe270.24(11)
C27Fe2C23119.55(9) C28C27C26107.75(19)
C27Fe2C2568.47(9) C27C28Fe269.25(11)
C27Fe2C2840.52(9) C27C28C29108.25(19)
C27Fe2C2968.42(9) C29C28Fe269.60(11)
C28Fe2C20153.66(8) C25C29Fe269.50(11)
C29Fe2C20118.42(7) C28C29Fe269.89(11)
C29Fe2C2840.50(8) C28C29C25107.76(19)
O1Si1C1110.28(8) N2C30C21112.56(15)
O1Si1C14105.84(8) C34C33Si2122.50(16)
O2Si1O1112.13(8) C34C33C38118.2(2)
O2Si1C1110.68(8) C38C33Si2119.17(17)
O2Si1C14111.41(9) C33C34C35120.6(3)
C1Si1C14106.25(8) C36C35C34119.7(3)
O1Si2C20110.49(8) C37C36C35120.5(2)
O1Si2C33107.61(8) C36C37C38119.9(3)
O3Si2O1112.14(8) C37C38C33121.1(3)
O3Si2C20109.15(8)     

 

Table 6 Hydrogen Bonds for mo_B0613_Cc.
DHAd(D-H)/Åd(H-A)/Åd(D-A)/ÅD-H-A/°
O2H2N20.841.952.663(2)142.3
O3H3N10.841.922.642(2)143.3

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for mo_B0613_Cc.
AtomxyzU(eq)
H253323734391628
H347091548348027
H3A6507-70293119
H46913-1519819
H564731378639015
H666983581361924
H767912596156929
H875151326197829
H978731550427422
H1073682939529319
H11A56842047214217
H11B59251109148217
H12A5378-373160738
H12B4790-345229038
H12C5334-274315338
H13A4881188888039
H13B451694794839
H13C509892623639
H1564184217587227
H1668374741779840
H1766374013976743
H1860232741984035
H1956082206792524
H2235205314340316
H2330854983560816
H2435203492651813
H2533601675310323
H2632392976143128
H2724854079220926
H2821373453436720
H2926851981494321
H30A43693321224315
H30B41404329177715
H31A46925765220530
H31B52325674308030
H31C46415526372130
H32A5036465874235
H32B51953607119035
H32C55814481157335
H3441982360786128
H3536221559932743
H363068317859249
H373117-181644346
H383682613497730

Experimental

Single crystals of C38H44Fe2N2O3Si2 [mo_B0613_Cc] were [The material was recrystallised from acetone by slow evaporation]. A suitable crystal was selected and [The crystal was mounted on a MITIGEN holder oil] on a Bruker D8 VENTURE area detector diffractometer. The crystal was kept at 100.01 K during data collection. Using Olex2 [1], the structure was solved with the ShelXT [2] structure solution program using Intrinsic Phasing 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_B0613_Cc]

Crystal Data for C38H44Fe2N2O3Si2 (=744.63 g/mol): monoclinic, space group Cc (no. 9), a = 24.4022(13) Å, b = 14.0997(7) Å, c = 10.2884(6) Å, β = 90.067(2)°, = 3539.9(3) Å3, Z = 4, T = 100.01 K, μ(MoKα) = 0.927 mm-1, Dcalc = 1.397 g/cm3, 105245 reflections measured (5.176° ≤ 2Θ ≤ 62°), 11142 unique (Rint = 0.0347, Rsigma = 0.0207) which were used in all calculations. The final R1 was 0.0201 (I > 2σ(I)) and wR2 was 0.0474 (all data).

Refinement model description

Number of restraints - 2, number of constraints - unknown.

Details:

1. Twinned data refinement
Scales: 0.8520(7) 0.1480(7)
2. 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, All O(H) groups
3.a Secondary CH2 refined with riding coordinates:
C11(H11A,H11B), C30(H30A,H30B)
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), C15(H15),
C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C24(H24), C25(H25),
C26(H26), C27(H27), C28(H28), C29(H29), C34(H34), C35(H35), C36(H36),
C37(H37), C38(H38)
3.c Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C31(H31A,H31B,H31C), C32(H32A,H32B,
H32C)
3.d Idealised tetrahedral OH refined as rotating group:
O2(H2), O3(H3)

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