2925

Table 1 Crystal data and structure refinement for 2925.
Identification code 2925
Empirical formula C28H38Fe2N2O2Si
Formula weight 574.39
Temperature/K 173.15
Crystal system monoclinic
Space group P21/n
a/Å 10.3208(4)
b/Å 10.0402(6)
c/Å 26.4327(13)
α/° 90
β/° 95.095(4)
γ/° 90
Volume/Å3 2728.2(2)
Z 4
ρcalcg/cm3 1.398
μ/mm‑1 1.135
F(000) 1208.0
Crystal size/mm3 0.34 × 0.14 × 0.07
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.342 to 53.998
Index ranges -12 ≤ h ≤ 13, -12 ≤ k ≤ 12, -33 ≤ l ≤ 33
Reflections collected 37528
Independent reflections 5949 [Rint = 0.0598, Rsigma = 0.0468]
Data/restraints/parameters 5949/0/322
Goodness-of-fit on F2 1.025
Final R indexes [I>=2σ (I)] R1 = 0.0398, wR2 = 0.0789
Final R indexes [all data] R1 = 0.0658, wR2 = 0.0903
Largest diff. peak/hole / e Å-3 0.52/-0.30

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for 2925. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Fe15969.4(3)9053.5(4)973.1(2)24.98(11)
Fe210586.4(3)9709.4(4)2504.9(2)25.57(11)
Si19010.4(6)7977.7(7)1473.5(3)21.82(16)
O18448.1(17)6770.5(19)1799.1(7)32.6(5)
O210427.0(16)7588.4(18)1277.9(7)28.1(4)
N17361(2)4999(2)660.7(11)43.3(7)
N210322(2)11581(2)982.3(9)32.8(6)
C17796(2)8277(3)929.4(9)24.0(6)
C26801(2)7410(3)687.2(10)26.9(6)
C36108(3)8149(3)290.6(10)33.2(7)
C46631(3)9447(3)281.9(11)33.4(7)
C57669(3)9532(3)669.5(10)28.0(6)
C65618(3)9081(3)1720.5(10)31.4(6)
C74596(3)8412(3)1433.5(10)33.6(7)
C84034(3)9314(3)1065.0(11)40.3(8)
C94709(3)10534(3)1125.7(12)42.3(8)
C105704(3)10396(3)1531.4(11)36.7(7)
C116480(3)6013(3)830.7(11)34.1(7)
C127396(4)5023(4)112.7(14)63.7(11)
C136942(4)3697(3)830.8(16)65.8(11)
C149132(3)5668(3)2003.0(14)49.2(9)
C1510593(3)6791(3)847.2(11)40.2(8)
C169267(2)9464(3)1882.6(10)23.9(6)
C1710064(2)10627(2)1829.4(10)23.1(6)
C189887(2)11503(3)2240.3(10)28.0(6)
C199002(2)10915(3)2552.6(11)31.6(7)
C208629(2)9664(3)2339.4(10)28.0(6)
C2111948(3)8256(4)2492.4(15)54.9(10)
C2212555(3)9493(3)2572.6(12)41.0(8)
C2312151(3)10028(3)3018.0(12)41.5(8)
C2411284(3)9128(5)3215.7(13)60.0(11)
C2511172(4)8027(4)2884.8(18)67.0(13)
C2610951(2)10848(3)1415.5(10)26.9(6)
C2711026(3)11362(4)534.3(12)55.7(10)
C2810278(4)12992(3)1095.7(15)58.5(10)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for 2925. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Fe122.9(2)30.6(2)21.4(2)1.07(16)1.74(15)5.35(16)
Fe220.78(19)29.8(2)25.7(2)-0.15(17)-0.65(15)-1.38(16)
Si119.7(3)23.8(4)22.0(4)-1.0(3)2.0(3)1.6(3)
O126.9(10)31.1(11)40.2(12)10.2(9)5.2(8)1.9(8)
O223.3(9)31.1(11)30.3(11)-6.2(8)4.9(8)3.2(8)
N143.0(15)32.5(15)53.9(18)-14.4(12)1.5(13)3.4(12)
N230.7(13)33.6(14)33.6(14)7.9(11)0.5(10)-0.8(11)
C124.4(13)28.2(15)19.9(13)-3.4(11)5.1(10)5.1(11)
C224.3(13)34.9(16)21.4(14)-5.3(11)2.3(11)5.8(12)
C329.2(15)50.0(19)20.1(14)-8.1(13)-0.2(11)4.6(13)
C432.8(15)43.3(18)24.7(15)8.8(13)6.6(12)8.4(13)
C528.7(14)32.3(16)24.1(15)2.6(12)7.9(11)2.0(12)
C630.6(15)41.6(17)22.7(15)-0.5(12)6.5(11)6.9(13)
C727.5(14)46.2(18)28.5(16)1.1(13)9.5(12)-0.2(13)
C824.7(15)64(2)32.2(17)-4.5(15)3.8(12)10.7(15)
C943.7(18)42.2(19)42.3(19)3.6(15)11.7(15)22.5(15)
C1038.9(17)36.2(17)35.9(17)-10.6(14)9.1(13)6.3(14)
C1130.0(15)34.7(17)36.4(17)-9.4(13)-3.0(13)-2.9(13)
C1272(3)61(3)58(3)-30(2)10(2)10(2)
C1366(2)33(2)98(3)-8(2)2(2)-2.7(18)
C1439.0(18)47(2)63(2)25.2(17)11.0(16)10.1(15)
C1536.7(17)46.5(19)38.5(18)-8.4(15)10.1(14)10.6(14)
C1619.6(13)30.4(15)21.6(14)-2.1(11)1(1)2.4(11)
C1719.6(12)24.2(14)25.4(14)0.3(11)2.3(10)4.2(10)
C1824.6(13)24.8(15)34.0(16)-5.6(12)-1.1(12)2.5(11)
C1923.5(14)41.2(17)29.9(16)-10.8(13)1.5(11)6.2(12)
C2017.3(12)41.1(17)25.5(15)-2.9(12)1.8(11)-1.2(12)
C2151(2)44(2)65(3)-10.8(18)-21.2(19)22.2(17)
C2223.7(14)56(2)42.7(19)13.5(16)-2.6(13)5.8(14)
C2336.0(16)43.8(19)41.1(19)-1.1(15)-16.6(14)-0.5(14)
C2440.3(19)105(3)35(2)32(2)0.5(15)8(2)
C2549(2)46(2)100(3)39(2)-32(2)-14.6(18)
C2624.6(13)24.4(14)32.1(16)3.6(12)4.1(11)1.5(11)
C2754(2)76(3)38(2)19.0(18)13.4(16)6.1(19)
C2867(2)35.1(19)70(3)12.7(18)-11(2)5.9(18)

 

Table 4 Bond Lengths for 2925.
AtomAtomLength/Å AtomAtomLength/Å
Fe1C12.052(2) N1C121.452(4)
Fe1C22.036(3) N1C131.460(4)
Fe1C32.036(3) N2C261.463(3)
Fe1C42.045(3) N2C271.459(4)
Fe1C52.050(3) N2C281.449(4)
Fe1C62.040(3) C1C21.451(4)
Fe1C72.052(3) C1C51.435(4)
Fe1C82.050(3) C2C31.424(4)
Fe1C92.040(3) C2C111.497(4)
Fe1C102.035(3) C3C41.411(4)
Fe2C162.055(2) C4C51.418(4)
Fe2C172.039(3) C6C71.413(4)
Fe2C182.041(3) C6C101.417(4)
Fe2C192.047(3) C7C81.415(4)
Fe2C202.029(2) C8C91.411(4)
Fe2C212.028(3) C9C101.424(4)
Fe2C222.035(3) C16C171.442(4)
Fe2C232.040(3) C16C201.440(3)
Fe2C242.037(3) C17C181.422(4)
Fe2C252.030(3) C17C261.504(3)
Si1O11.6234(19) C18C191.413(4)
Si1O21.6406(18) C19C201.416(4)
Si1C11.847(3) C21C221.399(5)
Si1C161.848(3) C21C251.385(5)
O1C141.395(3) C22C231.391(4)
O2C151.415(3) C23C241.405(5)
N1C111.462(4) C24C251.408(6)

 

Table 5 Bond Angles for 2925.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C1Fe1C7126.91(11) C25Fe2C2440.51(16)
C2Fe1C141.58(10) O1Si1O2111.08(10)
C2Fe1C468.90(11) O1Si1C1106.53(11)
C2Fe1C568.96(11) O1Si1C16109.40(11)
C2Fe1C6119.15(11) O2Si1C1110.85(10)
C2Fe1C7107.57(12) O2Si1C16106.94(10)
C2Fe1C8126.47(12) C1Si1C16112.09(12)
C2Fe1C9164.05(12) C14O1Si1127.22(18)
C3Fe1C169.12(10) C15O2Si1124.28(17)
C3Fe1C240.94(11) C12N1C11111.5(3)
C3Fe1C440.46(12) C12N1C13110.8(3)
C3Fe1C568.12(11) C13N1C11108.6(3)
C3Fe1C6153.71(12) C27N2C26110.0(2)
C3Fe1C7119.49(12) C28N2C26110.5(2)
C3Fe1C8107.93(12) C28N2C27110.0(3)
C3Fe1C9126.63(12) Si1C1Fe1125.55(13)
C4Fe1C169.02(11) C2C1Fe168.61(14)
C4Fe1C540.51(11) C2C1Si1130.6(2)
C4Fe1C7153.31(11) C5C1Fe169.43(14)
C4Fe1C8119.17(12) C5C1Si1122.9(2)
C5Fe1C140.95(10) C5C1C2106.5(2)
C5Fe1C7165.00(11) C1C2Fe169.81(14)
C5Fe1C8153.28(12) C1C2C11127.9(2)
C6Fe1C1107.61(11) C3C2Fe169.52(15)
C6Fe1C4164.73(12) C3C2C1107.5(2)
C6Fe1C5127.43(11) C3C2C11124.6(2)
C6Fe1C740.40(11) C11C2Fe1123.74(19)
C6Fe1C867.97(11) C2C3Fe169.54(15)
C8Fe1C1164.66(12) C4C3Fe170.12(16)
C8Fe1C740.36(11) C4C3C2109.0(2)
C9Fe1C1153.28(12) C3C4Fe169.42(16)
C9Fe1C4107.78(12) C3C4C5108.0(3)
C9Fe1C5119.34(12) C5C4Fe169.92(15)
C9Fe1C668.13(12) C1C5Fe169.62(14)
C9Fe1C767.97(13) C4C5Fe169.57(15)
C9Fe1C840.37(13) C4C5C1108.9(2)
C10Fe1C1118.42(11) C7C6Fe170.27(16)
C10Fe1C2153.42(11) C7C6C10108.6(3)
C10Fe1C3164.26(12) C10C6Fe169.46(16)
C10Fe1C4126.66(12) C6C7Fe169.33(15)
C10Fe1C5107.70(12) C6C7C8107.8(3)
C10Fe1C640.71(12) C8C7Fe169.73(16)
C10Fe1C768.47(12) C7C8Fe169.90(15)
C10Fe1C868.53(12) C9C8Fe169.41(16)
C10Fe1C940.91(12) C9C8C7108.0(3)
C17Fe2C1641.24(10) C8C9Fe170.21(17)
C17Fe2C1840.81(10) C8C9C10108.4(3)
C17Fe2C1968.67(11) C10C9Fe169.37(16)
C17Fe2C23130.06(12) C6C10Fe169.83(16)
C18Fe2C1669.03(10) C6C10C9107.1(3)
C18Fe2C1940.46(11) C9C10Fe169.72(17)
C19Fe2C1669.15(10) N1C11C2114.7(2)
C20Fe2C1641.28(10) Si1C16Fe2127.97(13)
C20Fe2C1768.92(10) C17C16Fe268.78(14)
C20Fe2C1868.33(11) C17C16Si1130.53(19)
C20Fe2C1940.64(11) C20C16Fe268.41(14)
C20Fe2C22169.57(13) C20C16Si1123.4(2)
C20Fe2C23149.45(12) C20C16C17106.0(2)
C20Fe2C24117.14(13) C16C17Fe269.99(14)
C20Fe2C25109.58(13) C16C17C26125.4(2)
C21Fe2C16108.15(12) C18C17Fe269.66(15)
C21Fe2C17116.13(14) C18C17C16108.3(2)
C21Fe2C18148.65(15) C18C17C26126.3(2)
C21Fe2C19169.97(15) C26C17Fe2124.96(17)
C21Fe2C20131.16(13) C17C18Fe269.53(15)
C21Fe2C2240.28(13) C19C18Fe270.03(16)
C21Fe2C2367.37(13) C19C18C17108.7(2)
C21Fe2C2467.67(16) C18C19Fe269.52(15)
C21Fe2C2539.90(16) C18C19C20107.8(2)
C22Fe2C16130.01(12) C20C19Fe269.00(15)
C22Fe2C17108.04(11) C16C20Fe270.32(14)
C22Fe2C18116.38(12) C19C20Fe270.36(15)
C22Fe2C19148.67(13) C19C20C16109.2(2)
C22Fe2C2339.92(13) C22C21Fe270.13(18)
C22Fe2C2467.66(13) C25C21Fe270.1(2)
C23Fe2C16168.58(12) C25C21C22108.4(3)
C23Fe2C18108.93(12) C21C22Fe269.59(18)
C23Fe2C19117.11(12) C23C22Fe270.23(17)
C24Fe2C16149.19(14) C23C22C21107.9(3)
C24Fe2C17169.03(15) C22C23Fe269.85(17)
C24Fe2C18130.89(15) C22C23C24108.3(3)
C24Fe2C19109.37(14) C24C23Fe269.72(18)
C24Fe2C2340.33(14) C23C24Fe269.96(18)
C25Fe2C16116.31(14) C23C24C25107.1(3)
C25Fe2C17148.56(16) C25C24Fe269.5(2)
C25Fe2C18170.03(17) C21C25Fe270.0(2)
C25Fe2C19131.77(16) C21C25C24108.3(3)
C25Fe2C2267.45(14) C24C25Fe270.0(2)
C25Fe2C2367.57(14) N2C26C17112.8(2)

 

Table 6 Torsion Angles for 2925.
ABCDAngle/˚ ABCDAngle/˚
Fe1C1C2C359.54(18) C2C1C5Fe158.82(17)
Fe1C1C2C11-117.6(3) C2C1C5C40.2(3)
Fe1C1C5C4-58.60(19) C2C3C4Fe1-58.81(18)
Fe1C2C3C459.16(19) C2C3C4C50.7(3)
Fe1C2C11N1-168.58(19) C3C2C11N1104.3(3)
Fe1C3C4C559.50(19) C3C4C5Fe1-59.19(19)
Fe1C4C5C158.62(18) C3C4C5C1-0.6(3)
Fe1C6C7C8-59.31(19) C5C1C2Fe1-59.34(17)
Fe1C6C10C960.07(19) C5C1C2C30.2(3)
Fe1C7C8C9-59.1(2) C5C1C2C11-177.0(2)
Fe1C8C9C10-59.0(2) C6C7C8Fe159.05(19)
Fe1C9C10C6-60.14(19) C6C7C8C9-0.1(3)
Fe2C16C17C18-59.36(18) C7C6C10Fe1-59.54(19)
Fe2C16C17C26119.3(2) C7C6C10C90.5(3)
Fe2C16C20C1959.82(18) C7C8C9Fe159.5(2)
Fe2C17C18C19-59.23(19) C7C8C9C100.4(3)
Fe2C17C26N2-177.68(18) C8C9C10Fe159.6(2)
Fe2C18C19C20-58.58(18) C8C9C10C6-0.6(3)
Fe2C19C20C16-59.80(18) C10C6C7Fe159.04(19)
Fe2C21C22C2360.0(2) C10C6C7C8-0.3(3)
Fe2C21C25C24-59.8(2) C11C2C3Fe1117.6(3)
Fe2C22C23C2459.3(2) C11C2C3C4176.7(2)
Fe2C23C24C2559.8(2) C12N1C11C2-58.1(3)
Fe2C24C25C2159.8(2) C13N1C11C2179.4(3)
Si1C1C2Fe1119.1(2) C16Si1O1C14-103.3(3)
Si1C1C2C3178.67(19) C16Si1O2C15-159.9(2)
Si1C1C2C111.5(4) C16Si1C1Fe1-51.1(2)
Si1C1C5Fe1-119.80(18) C16Si1C1C2-142.3(2)
Si1C1C5C4-178.39(18) C16Si1C1C535.9(2)
Si1C16C17Fe2-122.4(2) C16C17C18Fe259.56(17)
Si1C16C17C18178.21(19) C16C17C18C190.3(3)
Si1C16C17C26-3.1(4) C16C17C26N293.2(3)
Si1C16C20Fe2122.11(19) C17C16C20Fe2-58.74(17)
Si1C16C20C19-178.07(18) C17C16C20C191.1(3)
O1Si1O2C1580.8(2) C17C18C19Fe258.93(18)
O1Si1C1Fe168.56(18) C17C18C19C200.3(3)
O1Si1C1C2-22.7(3) C18C17C26N2-88.4(3)
O1Si1C1C5155.5(2) C18C19C20Fe258.90(18)
O1Si1C16Fe266.48(18) C18C19C20C16-0.9(3)
O1Si1C16C17160.1(2) C20C16C17Fe258.50(17)
O1Si1C16C20-21.0(2) C20C16C17C18-0.9(3)
O2Si1O1C1414.5(3) C20C16C17C26177.8(2)
O2Si1C1Fe1-170.47(14) C21C22C23Fe2-59.6(2)
O2Si1C1C298.3(2) C21C22C23C24-0.3(3)
O2Si1C1C5-83.5(2) C22C21C25Fe259.9(2)
O2Si1C16Fe2-53.91(18) C22C21C25C240.2(4)
O2Si1C16C1739.7(3) C22C23C24Fe2-59.4(2)
O2Si1C16C20-141.4(2) C22C23C24C250.4(4)
C1Si1O1C14135.3(3) C23C24C25Fe2-60.1(2)
C1Si1O2C15-37.5(2) C23C24C25C21-0.4(4)
C1Si1C16Fe2-175.58(15) C25C21C22Fe2-59.9(2)
C1Si1C16C17-82.0(3) C25C21C22C230.1(4)
C1Si1C16C2097.0(2) C26C17C18Fe2-119.1(3)
C1C2C3Fe1-59.72(17) C26C17C18C19-178.3(2)
C1C2C3C4-0.6(3) C27N2C26C17-160.0(3)
C1C2C11N1-79.0(3) C28N2C26C1778.4(3)

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for 2925.
AtomxyzU(eq)
H3540778226840
H46339101425640
H581951029574534
H661598710199438
H743327517148040
H83327913082048
H945291131692951
H10631011060165244
H11A64915962120541
H11B5585580568641
H12A65224854-5196
H12B799243321196
H12C76985897896
H13A6050352368799
H13B69743687120299
H13C7522300771799
H14A100055656188474
H14B86694851189374
H14C92025722237574
H15A9772634173960
H15B11270612593460
H15C10851735557160
H181029612345229634
H19871011292285238
H2080499054247634
H21120507672221666
H22131399896236049
H231241710860316450
H24108559240351672
H25106537258292480
H26A1172711349155632
H26B112499974129732
H27A119081172359583
H27B105701181224183
H27C110711040546683
H28A977713132138988
H28B98611346980188
H28C1116413328117388

Experimental

Single crystals of C28H38Fe2N2O2Si [2925] were []. A suitable crystal was selected and [] on a Xcalibur, Sapphire3 diffractometer. The crystal was kept at 173.15 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 [2925]

Crystal Data for C28H38Fe2N2O2Si (=574.39 g/mol): monoclinic, space group P21/n (no. 14), a = 10.3208(4) Å, b = 10.0402(6) Å, c = 26.4327(13) Å, β = 95.095(4)°, = 2728.2(2) Å3, Z = 4, T = 173.15 K, μ(MoKα) = 1.135 mm-1, Dcalc = 1.398 g/cm3, 37528 reflections measured (4.342° ≤ 2Θ ≤ 53.998°), 5949 unique (Rint = 0.0598, Rsigma = 0.0468) which were used in all calculations. The final R1 was 0.0398 (I > 2σ(I)) and wR2 was 0.0903 (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), C26(H26A,H26B)
2.b Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C18(H18),
C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25)
2.c Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,
H15C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C)

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