3148

Table 1 Crystal data and structure refinement for 3148.
Identification code 3148
Empirical formula C44H60Fe2N2O3Si4
Formula weight 889.00
Temperature/K 173.15
Crystal system triclinic
Space group P-1
a/Å 11.2756(3)
b/Å 12.7949(4)
c/Å 16.9084(4)
α/° 75.308(2)
β/° 87.164(2)
γ/° 74.135(2)
Volume/Å3 2269.22(11)
Z 2
ρcalcg/cm3 1.301
μ/mm‑1 0.784
F(000) 940.0
Crystal size/mm3 0.15 × 0.05 × 0.05
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.342 to 53.998
Index ranges -14 ≤ h ≤ 14, -16 ≤ k ≤ 16, -21 ≤ l ≤ 21
Reflections collected 47916
Independent reflections 9895 [Rint = 0.0301, Rsigma = 0.0224]
Data/restraints/parameters 9895/0/506
Goodness-of-fit on F2 1.016
Final R indexes [I>=2σ (I)] R1 = 0.0285, wR2 = 0.0689
Final R indexes [all data] R1 = 0.0348, wR2 = 0.0722
Largest diff. peak/hole / e Å-3 0.39/-0.21

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for 3148. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Fe18852.4(2)3388.1(2)1193.2(2)21.31(6)
Fe27355.1(2)-1353.3(2)4537.9(2)25.05(6)
Si16871.7(4)2123.7(3)2549.9(2)18.82(9)
Si28430.5(4)-329.1(3)2582.7(2)19.60(9)
Si34240.5(4)2282.2(4)1932.5(3)24.84(10)
Si47646.7(5)-927.0(4)1029.1(3)32.84(11)
O17920.8(9)929.6(8)2713.6(6)22.1(2)
O25537(1)1910.5(9)2467.2(7)25.1(2)
O38067.2(11)-302.9(9)1660.2(6)27.1(2)
N15352.8(12)5285.0(11)2044.9(9)29.4(3)
N29796.2(16)-3567.2(12)3171.2(10)40.5(4)
C17217.8(13)3041.0(12)1584.3(9)21.2(3)
C27073.4(14)4237.5(13)1352.1(10)24.3(3)
C37396.3(14)4534.4(14)517.4(10)30.1(4)
C47747.6(15)3555.7(15)221.6(10)31.4(4)
C57643.2(14)2638.9(14)873.1(9)26.2(3)
C69990.5(15)3402.5(14)2093.6(10)28.7(3)
C710154.6(15)4158.2(15)1351.4(11)31.7(4)
C810534.3(15)3541.4(16)757.9(11)35.0(4)
C910597.7(15)2403.5(16)1131.8(12)35.8(4)
C1010260.6(15)2318.6(14)1958.3(11)30.4(4)
C116677.0(14)5032.1(13)1890.2(10)27.4(3)
C124632.6(17)5899.6(16)1297.3(12)41.2(4)
C135061.1(19)5927.5(16)2657.9(12)42.2(5)
C146851.6(14)2691.6(12)3465.5(9)22.5(3)
C155741.7(16)3113.3(14)3826(1)30.9(4)
C165719.0(19)3546.3(15)4505.0(11)39.4(4)
C176799(2)3566.4(15)4834.6(11)41.0(5)
C187916.7(19)3153.7(15)4489.2(11)38.2(4)
C197934.3(16)2715.9(14)3815.9(10)29.2(3)
C207675.8(14)-1267.7(13)3322.0(9)22.9(3)
C218157.3(15)-2395.9(13)3818.5(9)25.2(3)
C227154.7(17)-2749.5(15)4247.9(10)33.3(4)
C236062.7(17)-1864.8(16)4037.8(11)34.4(4)
C246373.3(15)-955.5(14)3473.8(9)27.7(3)
C258694.4(17)-1226.9(16)5251.4(10)34.5(4)
C267895(2)-1783.5(18)5738.6(11)43.4(5)
C276689.1(19)-1048(2)5621.9(11)47.9(5)
C286752.3(18)-44.4(17)5065.5(12)42.6(5)
C297991.1(17)-150.6(15)4833.7(10)33.8(4)
C309464.6(16)-3098.8(13)3878.2(10)28.7(3)
C319069(3)-4332(2)3125.6(17)72.3(8)
C3211108(2)-4115(2)3196.9(16)66.1(7)
C3310140.1(14)-741.7(12)2686.7(9)22.1(3)
C3410737.6(15)-677.3(14)3370.2(10)28.0(3)
C3512008.6(16)-1021.4(14)3460.0(11)32.7(4)
C3612718.7(16)-1426.8(14)2857.6(11)33.9(4)
C3712160.5(17)-1481.8(16)2170.1(12)37.8(4)
C3810885.4(16)-1144.9(15)2085.7(10)32.1(4)
C393227.5(16)3552.8(15)2191.2(13)40.1(4)
C404559.4(18)2582.6(18)822.6(11)40.8(4)
C413554.0(16)1085.4(14)2212.6(11)31.1(4)
C427554(2)25.1(18)-4.7(11)53.3(6)
C436120(3)-1168(3)1314.8(17)71.2(8)
C448795(2)-2286.3(18)1067.1(14)58.6(6)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for 3148. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Fe116.17(11)22.95(11)23.63(11)-4.51(8)1.28(8)-4.68(8)
Fe225.11(12)28.97(13)18.28(11)-4.78(9)2.74(9)-4.17(9)
Si116.11(19)18.61(19)21.02(19)-5.18(15)0.51(15)-3.31(15)
Si222.2(2)18.63(19)17.05(18)-5.24(15)1.12(15)-3.38(16)
Si318.0(2)26.9(2)27.2(2)-2.02(17)-0.81(16)-6.22(17)
Si446.1(3)33.1(3)22.7(2)-12.28(19)-0.2(2)-11.1(2)
O120.8(5)20.0(5)24.5(5)-6.8(4)-1.5(4)-2.6(4)
O219.2(5)27.2(6)27.7(5)-2.4(4)-0.7(4)-8.1(4)
O336.2(6)26.8(6)18.3(5)-6.1(4)-0.8(4)-8.2(5)
N121.7(7)25.1(7)35.1(7)-3.3(6)3.8(6)-0.7(5)
N252.9(10)27.5(8)41.4(9)-16.3(7)14.4(7)-6.5(7)
C115.4(7)22.5(7)24.2(7)-4.0(6)-1.5(6)-4.2(6)
C215.8(7)23.1(8)30.5(8)-2.2(6)-1.5(6)-3.4(6)
C319.6(8)30.7(9)32.0(8)5.2(7)-2.7(6)-5.1(7)
C424.4(8)43.8(10)23.7(8)-2.8(7)-1.0(6)-10.5(7)
C522.0(8)32.8(9)26.3(8)-9.1(6)-0.1(6)-9.6(7)
C621.5(8)35.5(9)30.5(8)-11.0(7)-1.0(6)-7.2(7)
C724.8(8)30.5(9)41.7(10)-7.0(7)-1.9(7)-11.8(7)
C820.7(8)50.7(11)32.4(9)-6.9(8)5.0(7)-11.9(8)
C919.9(8)41.9(10)46.1(10)-22.1(8)-0.2(7)1.1(7)
C1020.3(8)27.9(8)38.0(9)-2.2(7)-6.1(7)-3.0(6)
C1122.2(8)18.2(7)38.6(9)-3.4(6)0.3(7)-3.4(6)
C1225.6(9)39.2(10)45.3(11)1.7(8)-0.7(8)2.3(8)
C1342.7(11)29.4(9)48.6(11)-9.6(8)11.9(9)-2.1(8)
C1427.1(8)16.9(7)21.8(7)-4.1(6)1.6(6)-3.8(6)
C1530.9(9)27.5(8)33.6(9)-9.4(7)7.1(7)-6.1(7)
C1649.3(12)31.5(9)34.3(9)-12.3(8)16.0(8)-4.4(8)
C1765.1(14)31.8(9)26.2(8)-12.8(7)3.2(8)-8.5(9)
C1848.7(11)34.8(10)31.9(9)-10.3(7)-8.2(8)-9.3(8)
C1931.0(9)28.3(8)27.4(8)-7.9(7)0.2(7)-5.6(7)
C2026.7(8)24.2(8)19.2(7)-7.3(6)0.4(6)-7.6(6)
C2131.1(9)23.6(8)22.2(7)-6.9(6)1.6(6)-8.4(6)
C2240.7(10)30.8(9)29.8(8)-3.6(7)5.0(7)-16.2(8)
C2329.4(9)42.6(10)33.6(9)-7.3(8)4.5(7)-16.2(8)
C2426.0(8)33.1(9)23.1(7)-6.0(6)-0.6(6)-7.4(7)
C2530.4(9)44.9(10)26.8(8)-14.6(7)-2.6(7)-2.0(8)
C2654.0(12)51.0(12)20.0(8)-3.4(8)-3.2(8)-10.2(10)
C2740.2(11)81.9(16)26.6(9)-23.4(10)11.9(8)-17.7(11)
C2837.8(11)50.9(12)36.4(10)-26.4(9)-5.2(8)7.7(9)
C2941.3(10)35.2(9)27.5(8)-15.1(7)-0.8(7)-7.7(8)
C3035.5(9)19.3(7)27.7(8)-3.3(6)2.3(7)-4.1(7)
C31112(2)54.6(15)75.3(17)-44.7(13)27.5(16)-41.0(15)
C3267.3(16)44.8(13)67.0(15)-14.6(11)24.4(13)13.0(11)
C3324.2(8)15.7(7)23.8(7)-3.0(6)3.0(6)-3.3(6)
C3428.2(8)28.8(8)28.9(8)-11.2(7)5.0(7)-7.8(7)
C3529.2(9)32.5(9)38.3(9)-11.3(7)-2.7(7)-8.8(7)
C3623.6(8)27.7(9)47.3(10)-7.6(7)4.1(7)-4.3(7)
C3730.6(9)39(1)39.3(10)-14.0(8)11.5(8)0.0(8)
C3831.8(9)35.4(9)26.2(8)-10.7(7)2.7(7)-1.6(7)
C3922.4(9)34.5(10)61.0(12)-12.3(9)-2.2(8)-3.1(7)
C4033.9(10)52.0(12)28.7(9)3.7(8)-3.7(7)-10.7(9)
C4124.8(8)34.8(9)35.0(9)-6.0(7)-3.0(7)-12.3(7)
C4280.9(17)51.0(13)23.6(9)-10.9(8)-7.6(10)-7.6(11)
C4375.3(18)94(2)76.6(17)-51.8(16)17.4(14)-51.2(16)
C4488.8(18)39.5(12)44.8(12)-22.5(10)-10.4(12)0.2(11)

 

Table 4 Bond Lengths for 3148.
AtomAtomLength/Å AtomAtomLength/Å
Fe1C12.0517(15) N1C131.452(2)
Fe1C22.0444(15) N2C301.458(2)
Fe1C32.0424(16) N2C311.456(3)
Fe1C42.0432(16) N2C321.451(3)
Fe1C52.0301(16) C1C21.446(2)
Fe1C62.0458(16) C1C51.436(2)
Fe1C72.0401(17) C2C31.422(2)
Fe1C82.0418(17) C2C111.497(2)
Fe1C92.0400(17) C3C41.415(3)
Fe1C102.0457(16) C4C51.418(2)
Fe2C202.0502(15) C6C71.415(2)
Fe2C212.0327(15) C6C101.411(2)
Fe2C222.0393(18) C7C81.410(3)
Fe2C232.0471(18) C8C91.416(3)
Fe2C242.0363(16) C9C101.415(3)
Fe2C252.0434(18) C14C151.397(2)
Fe2C262.0417(18) C14C191.394(2)
Fe2C272.0354(18) C15C161.392(2)
Fe2C282.0342(18) C16C171.373(3)
Fe2C292.0401(18) C17C181.389(3)
Si1O11.6249(10) C18C191.388(2)
Si1O21.6197(11) C20C211.444(2)
Si1C11.8468(15) C20C241.441(2)
Si1C141.8664(15) C21C221.429(2)
Si2O11.6232(10) C21C301.495(2)
Si2O31.6221(11) C22C231.415(3)
Si2C201.8496(16) C23C241.419(2)
Si2C331.8589(16) C25C261.406(3)
Si3O21.6472(11) C25C291.410(3)
Si3C391.8534(18) C26C271.417(3)
Si3C401.8553(18) C27C281.403(3)
Si3C411.8472(17) C28C291.411(3)
Si4O31.6402(11) C33C341.397(2)
Si4C421.849(2) C33C381.396(2)
Si4C431.850(3) C34C351.383(2)
Si4C441.851(2) C35C361.381(2)
N1C111.464(2) C36C371.375(3)
N1C121.457(2) C37C381.387(2)

 

Table 5 Bond Angles for 3148.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C2Fe1C141.33(6) C41Si3C40109.29(9)
C2Fe1C6110.83(6) O3Si4C42106.83(8)
C2Fe1C10134.80(7) O3Si4C43109.79(9)
C3Fe1C168.96(6) O3Si4C44109.99(9)
C3Fe1C240.72(6) C42Si4C43110.02(13)
C3Fe1C440.52(7) C42Si4C44110.65(10)
C3Fe1C6134.89(7) C43Si4C44109.53(13)
C3Fe1C10174.45(7) Si2O1Si1150.08(7)
C4Fe1C169.21(6) Si1O2Si3146.83(7)
C4Fe1C268.79(7) Si2O3Si4149.06(8)
C4Fe1C6173.12(7) C12N1C11111.29(13)
C4Fe1C10144.58(7) C13N1C11109.86(14)
C5Fe1C141.20(6) C13N1C12110.11(14)
C5Fe1C268.97(6) C31N2C30111.04(16)
C5Fe1C368.32(7) C32N2C30110.09(17)
C5Fe1C440.74(7) C32N2C31111.47(19)
C5Fe1C6146.02(7) Si1C1Fe1129.62(8)
C5Fe1C7171.95(7) C2C1Fe169.07(8)
C5Fe1C8132.39(7) C2C1Si1130.68(12)
C5Fe1C9108.48(7) C5C1Fe168.60(9)
C5Fe1C10114.40(7) C5C1Si1122.85(11)
C6Fe1C1115.35(6) C5C1C2106.37(13)
C7Fe1C1146.32(7) C1C2Fe169.61(8)
C7Fe1C2115.16(7) C1C2C11126.68(14)
C7Fe1C3109.86(7) C3C2Fe169.57(9)
C7Fe1C4132.92(7) C3C2C1107.86(14)
C7Fe1C640.54(7) C3C2C11125.45(15)
C7Fe1C840.41(7) C11C2Fe1125.54(11)
C7Fe1C1068.15(7) C2C3Fe169.72(9)
C8Fe1C1172.50(7) C4C3Fe169.77(9)
C8Fe1C2145.11(7) C4C3C2108.98(14)
C8Fe1C3113.91(7) C3C4Fe169.71(9)
C8Fe1C4108.12(7) C3C4C5107.64(15)
C8Fe1C668.02(7) C5C4Fe169.13(9)
C8Fe1C1068.22(7) C1C5Fe170.21(9)
C9Fe1C1133.22(7) C4C5Fe170.12(9)
C9Fe1C2173.92(7) C4C5C1109.14(14)
C9Fe1C3144.26(7) C7C6Fe169.52(9)
C9Fe1C4113.18(7) C10C6Fe169.82(9)
C9Fe1C667.95(7) C10C6C7108.17(15)
C9Fe1C768.10(7) C6C7Fe169.95(9)
C9Fe1C840.60(8) C8C7Fe169.86(10)
C9Fe1C1040.53(7) C8C7C6108.05(15)
C10Fe1C1109.60(6) C7C8Fe169.73(10)
C10Fe1C640.35(7) C7C8C9107.89(16)
C21Fe2C2041.42(6) C9C8Fe169.63(10)
C21Fe2C2241.08(7) C8C9Fe169.77(10)
C21Fe2C2369.01(7) C10C9Fe169.95(9)
C21Fe2C2469.12(6) C10C9C8108.12(15)
C21Fe2C25108.57(7) C6C10Fe169.83(9)
C21Fe2C26118.89(7) C6C10C9107.78(15)
C21Fe2C27152.59(8) C9C10Fe169.52(10)
C21Fe2C28165.86(8) N1C11C2112.79(13)
C21Fe2C29128.09(7) C15C14Si1120.93(13)
C22Fe2C2069.27(6) C19C14Si1121.73(12)
C22Fe2C2340.50(7) C19C14C15117.34(15)
C22Fe2C25128.36(7) C16C15C14121.24(17)
C22Fe2C26108.22(8) C17C16C15120.20(17)
C22Fe2C29166.34(7) C16C17C18119.88(16)
C23Fe2C2069.32(7) C19C18C17119.66(18)
C24Fe2C2041.29(6) C18C19C14121.66(16)
C24Fe2C2268.36(7) Si2C20Fe2128.94(8)
C24Fe2C2340.66(7) C21C20Fe268.64(8)
C24Fe2C25153.32(7) C21C20Si2131.32(12)
C24Fe2C26164.62(8) C24C20Fe268.83(8)
C24Fe2C29118.87(7) C24C20Si2122.37(12)
C25Fe2C20119.12(7) C24C20C21106.27(14)
C25Fe2C23165.31(7) C20C21Fe269.94(8)
C26Fe2C20153.09(8) C20C21C30127.14(14)
C26Fe2C23127.16(8) C22C21Fe269.71(9)
C26Fe2C2540.27(8) C22C21C20108.02(14)
C27Fe2C20164.68(8) C22C21C30124.84(15)
C27Fe2C22118.27(8) C30C21Fe2126.54(11)
C27Fe2C23107.04(8) C21C22Fe269.21(9)
C27Fe2C24126.51(8) C23C22Fe270.04(10)
C27Fe2C2568.03(8) C23C22C21108.74(15)
C27Fe2C2640.67(8) C22C23Fe269.45(10)
C27Fe2C2968.06(8) C22C23C24107.84(15)
C28Fe2C20127.08(7) C24C23Fe269.26(10)
C28Fe2C22151.72(8) C20C24Fe269.87(9)
C28Fe2C23117.90(8) C23C24Fe270.08(10)
C28Fe2C24107.41(7) C23C24C20109.14(15)
C28Fe2C2568.00(7) C26C25Fe269.80(11)
C28Fe2C2668.04(8) C26C25C29108.17(17)
C28Fe2C2740.35(9) C29C25Fe269.67(10)
C28Fe2C2940.54(8) C25C26Fe269.93(10)
C29Fe2C20107.82(7) C25C26C27107.87(18)
C29Fe2C23152.24(7) C27C26Fe269.43(10)
C29Fe2C2540.41(7) C26C27Fe269.91(10)
C29Fe2C2667.95(8) C28C27Fe269.78(10)
O1Si1C1108.30(6) C28C27C26107.93(18)
O1Si1C14107.71(6) C27C28Fe269.87(11)
O2Si1O1108.97(6) C27C28C29108.23(17)
O2Si1C1109.55(6) C29C28Fe269.95(10)
O2Si1C14107.83(7) C25C29Fe269.92(10)
C1Si1C14114.36(7) C25C29C28107.81(17)
O1Si2C20108.57(6) C28C29Fe269.51(11)
O1Si2C33107.94(6) N2C30C21111.76(14)
O3Si2O1108.53(6) C34C33Si2121.82(11)
O3Si2C20109.24(6) C38C33Si2121.19(12)
O3Si2C33108.30(6) C38C33C34116.98(15)
C20Si2C33114.13(7) C35C34C33121.75(15)
O2Si3C39108.11(8) C36C35C34119.80(16)
O2Si3C40110.14(7) C37C36C35119.91(16)
O2Si3C41107.11(7) C36C37C38120.11(16)
C39Si3C40110.15(10) C37C38C33121.44(16)
C41Si3C39112.00(9)     

 

Table 6 Torsion Angles for 3148.
ABCDAngle/˚ ABCDAngle/˚
Fe1C1C2C359.26(11) C5C1C2Fe1-58.69(10)
Fe1C1C2C11-119.76(15) C5C1C2C30.57(17)
Fe1C1C5C4-59.51(11) C5C1C2C11-178.45(14)
Fe1C2C3C458.87(11) C6C7C8Fe159.76(11)
Fe1C2C11N1-165.19(11) C6C7C8C90.36(19)
Fe1C3C4C558.93(11) C7C6C10Fe1-59.14(11)
Fe1C4C5C159.56(11) C7C6C10C90.25(19)
Fe1C6C7C8-59.71(12) C7C8C9Fe159.46(12)
Fe1C6C10C959.39(11) C7C8C9C10-0.21(19)
Fe1C7C8C9-59.40(12) C8C9C10Fe159.55(12)
Fe1C8C9C10-59.67(12) C8C9C10C6-0.03(19)
Fe1C9C10C6-59.58(11) C10C6C7Fe159.32(11)
Fe2C20C21C2259.54(11) C10C6C7C8-0.38(19)
Fe2C20C21C30-121.23(16) C11C2C3Fe1119.75(15)
Fe2C20C24C23-59.25(12) C11C2C3C4178.62(14)
Fe2C21C22C2359.05(12) C12N1C11C2-65.76(18)
Fe2C21C30N2-168.50(11) C13N1C11C2172.02(14)
Fe2C22C23C2458.81(12) C14Si1O1Si2148.81(14)
Fe2C23C24C2059.13(11) C14Si1O2Si3112.67(14)
Fe2C25C26C27-59.28(13) C14Si1C1Fe172.18(12)
Fe2C25C29C2859.41(12) C14Si1C1C2-23.56(16)
Fe2C26C27C28-59.66(13) C14Si1C1C5160.50(12)
Fe2C27C28C29-59.66(12) C14C15C16C170.0(3)
Fe2C28C29C25-59.67(12) C15C14C19C18-0.8(2)
Si1C1C2Fe1124.86(13) C15C16C17C180.0(3)
Si1C1C2C3-175.88(12) C16C17C18C19-0.5(3)
Si1C1C2C115.1(2) C17C18C19C140.9(3)
Si1C1C5Fe1-124.21(11) C19C14C15C160.4(2)
Si1C1C5C4176.28(11) C20Si2O1Si1-82.09(15)
Si1C14C15C16-179.48(13) C20Si2O3Si4-26.75(18)
Si1C14C19C18179.02(13) C20Si2C33C34-67.83(14)
Si2C20C21Fe2123.69(13) C20Si2C33C38111.35(13)
Si2C20C21C22-176.77(12) C20C21C22Fe2-59.68(10)
Si2C20C21C302.5(2) C20C21C22C23-0.63(19)
Si2C20C24Fe2-123.54(11) C20C21C30N2-77.0(2)
Si2C20C24C23177.21(12) C21C20C24Fe258.68(10)
Si2C33C34C35177.70(13) C21C20C24C23-0.58(17)
Si2C33C38C37-178.27(14) C21C22C23Fe2-58.54(12)
O1Si1O2Si3-130.68(13) C21C22C23C240.3(2)
O1Si1C1Fe1-47.92(11) C22C21C30N2102.08(18)
O1Si1C1C2-143.66(13) C22C23C24Fe2-58.93(12)
O1Si1C1C540.40(14) C22C23C24C200.20(19)
O1Si1C14C15-132.96(13) C24C20C21Fe2-58.80(10)
O1Si1C14C1947.19(14) C24C20C21C220.73(17)
O1Si2O3Si4-144.96(15) C24C20C21C30179.97(15)
O1Si2C20Fe2-43.44(12) C25C26C27Fe259.60(13)
O1Si2C20C21-138.42(14) C25C26C27C28-0.1(2)
O1Si2C20C2444.42(14) C26C25C29Fe2-59.39(13)
O1Si2C33C3452.96(14) C26C25C29C280.02(19)
O1Si2C33C38-127.86(13) C26C27C28Fe259.74(13)
O2Si1O1Si232.09(16) C26C27C28C290.1(2)
O2Si1C1Fe1-166.65(9) C27C28C29Fe259.61(13)
O2Si1C1C297.61(15) C27C28C29C25-0.1(2)
O2Si1C1C5-78.34(13) C29C25C26Fe259.31(12)
O2Si1C14C15-15.49(15) C29C25C26C270.0(2)
O2Si1C14C19164.66(12) C30C21C22Fe2121.06(15)
O3Si2O1Si136.54(16) C30C21C22C23-179.89(15)
O3Si2C20Fe2-161.62(9) C31N2C30C21-63.7(2)
O3Si2C20C21103.40(15) C32N2C30C21172.36(16)
O3Si2C20C24-73.77(13) C33Si2O1Si1153.70(14)
O3Si2C33C34170.27(12) C33Si2O3Si498.11(16)
O3Si2C33C38-10.55(15) C33Si2C20Fe276.99(11)
C1Si1O1Si2-87.02(15) C33Si2C20C21-17.99(17)
C1Si1O2Si3-12.36(16) C33Si2C20C24164.85(12)
C1Si1C14C15106.62(13) C33C34C35C360.9(3)
C1Si1C14C19-73.23(14) C34C33C38C370.9(2)
C1C2C3Fe1-59.28(10) C34C35C36C370.3(3)
C1C2C3C4-0.41(18) C35C36C37C38-0.9(3)
C1C2C11N1-75.30(19) C36C37C38C330.2(3)
C2C1C5Fe158.99(10) C38C33C34C35-1.5(2)
C2C1C5C4-0.52(17) C39Si3O2Si1-80.31(16)
C2C3C4Fe1-58.84(11) C40Si3O2Si140.08(17)
C2C3C4C50.09(18) C41Si3O2Si1158.83(14)
C3C2C11N1105.85(18) C42Si4O3Si2-177.87(16)
C3C4C5Fe1-59.29(11) C43Si4O3Si262.86(19)
C3C4C5C10.27(18) C44Si4O3Si2-57.73(19)

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for 3148.
AtomxyzU(eq)
H37379527120836
H480073519-31638
H57826188084431
H697423592259634
H7100314944126838
H810715383720542
H910827180287343
H10102231651235236
H11A71374702241933
H11B68925740162933
H12A37526043141762
H12B4826545489162
H12C48366615108162
H13A55425503316063
H13B41796069277463
H13C52656644245363
H1549883104360437
H1649543829474147
H1767813862529849
H1886663171471346
H1987042425358835
H227212-3461461440
H235264-1877423941
H245812-253323433
H259558-1524521141
H268124-2522608552
H275965-1206587557
H286078596487751
H298297404446341
H30A10020-2634392034
H30B9581-3718438134
H31A9249-49693609108
H31B9278-46062631108
H31C8189-39373106108
H32A11571-3582323499
H32B11333-4376269999
H32C11307-4757367699
H3410258-389378434
H3512392-979393439
H3613592-1667291841
H3712649-1751175245
H3810511-1189160939
H39A29543355275660
H39B25083858181960
H39C36854117213660
H40A4853325966261
H40B3802270151361
H40C5192194670661
H41A4159408213447
H41B28231245186547
H41C3315968278747
H42A6960747-980
H42B7285-310-40180
H42C8367143-15380
H43A6156-16061884107
H43B5895-1580956107
H43C5501-4441256107
H44A9535-215277888
H44B8443-273880588
H44C9013-2688163888

Experimental

Single crystals of C44H60Fe2N2O3Si4 [3148] 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 ShelXS [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. (2008). Acta Cryst. A64, 112-122.
  3. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Crystal structure determination of [3148]

Crystal Data for C44H60Fe2N2O3Si4 (=889.00 g/mol): triclinic, space group P-1 (no. 2), a = 11.2756(3) Å, b = 12.7949(4) Å, c = 16.9084(4) Å, α = 75.308(2)°, β = 87.164(2)°, γ = 74.135(2)°, = 2269.22(11) Å3, Z = 2, T = 173.15 K, μ(MoKα) = 0.784 mm-1, Dcalc = 1.301 g/cm3, 47916 reflections measured (4.342° ≤ 2Θ ≤ 53.998°), 9895 unique (Rint = 0.0301, Rsigma = 0.0224) which were used in all calculations. The final R1 was 0.0285 (I > 2σ(I)) and wR2 was 0.0722 (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), C30(H30A,H30B)
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), 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)
2.c Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C31(H31A,H31B,H31C), C32(H32A,H32B,
H32C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,
H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C)

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