mo_B0083_0m

Table 1 Crystal data and structure refinement for mo_B0083_0m.
Identification code mo_B0083_0m
Empirical formula C36H58Fe2Li2N2OSi2
Formula weight 716.60
Temperature/K 100.0
Crystal system monoclinic
Space group P21
a/Å 12.2143(5)
b/Å 12.0951(6)
c/Å 14.2648(7)
α/° 90
β/° 113.848(2)
γ/° 90
Volume/Å3 1927.46(16)
Z 2
ρcalcg/cm3 1.235
μ/mm‑1 0.843
F(000) 764.0
Crystal size/mm3 0.553 × 0.236 × 0.176
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.592 to 55.998
Index ranges -15 ≤ h ≤ 16, -15 ≤ k ≤ 15, -18 ≤ l ≤ 18
Reflections collected 56891
Independent reflections 9291 [Rint = 0.0213, Rsigma = 0.0152]
Data/restraints/parameters 9291/3/438
Goodness-of-fit on F2 1.129
Final R indexes [I>=2σ (I)] R1 = 0.0180, wR2 = 0.0476
Final R indexes [all data] R1 = 0.0189, wR2 = 0.0527
Largest diff. peak/hole / e Å-3 0.38/-0.23
Flack parameter-0.004(2)

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for mo_B0083_0m. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Fe26852.7(2)4896.8(2)4585.0(2)13.58(6)
Fe17365.9(2)2799.7(2)8472.6(2)14.08(6)
Si29302.8(5)5312.7(4)3986.3(4)17.7(1)
Si15535.3(5)3143.6(4)9793.2(4)16.4(1)
O18439.2(15)7162.6(13)8411.0(12)28.5(3)
N29923.6(14)5269.5(14)7477.1(12)18.9(3)
N14951.7(14)5087.3(14)6632.7(12)19.1(3)
C178360.7(17)5721.8(15)4681.6(14)16.6(3)
C188440.6(16)5420.1(15)5688.4(14)14.8(3)
C197488.1(16)5901.3(15)5916.5(14)15.3(3)
C206813.9(17)6520.9(16)5001.2(14)17.0(4)
C217320.0(18)6420.4(15)4258.5(14)18.1(4)
C226653.0(19)3598.4(17)3604.2(16)22.2(4)
C236826.4(17)3200.5(17)4594.2(15)20.2(4)
C245872.9(17)3625.8(16)4827.2(15)18.0(4)
C255129.1(17)4295.3(17)3983.3(15)21.1(4)
C265614.0(19)4268.0(17)3230.4(15)23.1(4)
C309391.3(17)4709.0(15)6467.5(14)18.1(4)
C3110552(2)6278.4(19)7395.1(17)28.3(5)
C3210768.2(19)4518(2)8228.1(16)26.9(4)
C299920(2)3877.0(18)4309.6(19)32.3(5)
C2810595.8(19)6282.7(18)4323.9(18)26.4(4)
C278406(2)5422(2)2571.2(17)34.4(5)
C16573.7(17)3698.7(15)9251.3(14)16.5(3)
C26300.9(16)4176.7(15)8251.4(14)17.0(4)
C37366.1(17)4504.5(16)8111.1(15)18.0(4)
C48313.6(17)4204.0(16)9081.4(15)18.3(4)
C57858.7(17)3728.4(15)9768.6(14)17.5(4)
C66849.5(19)1179.8(17)8449.5(17)23.0(4)
C76425.5(19)1609.7(17)7434.9(16)24.2(4)
C87437(2)1952.6(18)7251.1(16)24.3(4)
C98487.2(18)1741.9(17)8157.5(17)22.6(4)
C108118.9(19)1260.8(17)8894.8(16)22.6(4)
C145026.5(17)4303.5(17)7447.6(15)20.6(4)
C155125(2)6228.8(18)7031.6(17)27.2(5)
C163763.5(18)5001(2)5775.9(15)27.6(4)
C136400(2)2221.8(19)10902.7(16)26.0(4)
C124246.2(18)2371.0(18)8815.2(15)22.3(4)
C114897(2)4311.3(19)10279.4(18)30.0(5)
C338828(2)7058(2)9496.8(17)31.5(5)
C347824(3)6999(3)9847(2)42.6(6)
C357949(5)8270(4)8119(6)35.5(13)
C35B7826(14)8094(12)7713(10)49(3)
C368197(5)8681(3)7263(4)34.8(13)
C36B8793(15)8880(9)7892(13)63(4)
Li26544(3)4855(3)6501(2)20.6(6)
Li18299(3)5802(3)7602(3)21.3(7)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for mo_B0083_0m. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Fe215.42(12)14.22(12)11.94(11)-0.70(9)6.38(9)-1.83(9)
Fe114.75(12)14.76(12)13.00(11)2.43(9)5.90(9)1.52(9)
Si221.3(2)17.9(2)18.3(2)-1.49(19)12.6(2)-3.46(19)
Si118.9(2)18.5(2)14.2(2)0.80(18)9.18(19)0.62(19)
O139.0(9)22.7(8)27.4(8)3.1(6)17.2(7)4.9(7)
N217.0(7)22.0(8)14.8(7)0.0(6)3.6(6)-0.9(6)
N120.1(7)22.0(9)15.0(7)5.7(6)6.7(6)6.7(6)
C1719.1(8)16.2(8)16.2(8)-1.3(7)9.1(7)-4.4(7)
C1816.6(8)14.1(8)14.4(8)-1.9(7)7.0(7)-3.1(7)
C1917.5(8)14.3(8)14.7(8)-1.6(6)7.0(7)-1.1(7)
C2019.1(9)14.9(8)17.6(9)-0.4(7)8.0(7)-0.4(7)
C2124.3(9)15.4(8)16.4(8)1.3(7)10.0(7)-3.3(7)
C2226.6(10)22.6(9)21.1(9)-10.9(7)13.4(8)-9.8(8)
C2322.6(10)14.4(8)23.6(10)-3.8(7)9.4(8)-3.0(7)
C2420.3(9)17.3(9)17.8(9)-1.9(7)9.2(7)-5.1(7)
C2517.2(9)21.1(10)22.6(9)-0.9(7)5.6(7)-2.7(7)
C2626.6(10)24.1(10)15.1(9)-2.6(7)4.9(8)-8.4(8)
C3018.6(8)18.1(10)17.9(8)-1.4(7)7.6(7)0.7(7)
C3124.7(10)30.8(12)27.2(10)-4.1(9)8.2(9)-10.1(9)
C3221.3(10)36.2(11)20.2(9)4.0(8)5.3(8)4.7(8)
C2950.8(14)20.7(10)39.0(12)0.4(9)32.4(11)3.0(9)
C2824.7(10)24.9(10)36.2(11)-4.1(9)19.2(9)-5.6(8)
C2732.4(12)54.0(15)21(1)-2.8(10)15.3(9)-2.3(11)
C118.4(8)17.7(8)14.6(8)1.4(7)8.0(7)1.7(7)
C218.4(9)16.8(9)17.5(8)3.9(7)8.9(7)3.0(7)
C318.2(9)16.6(8)20.5(9)3.7(7)9.2(7)1.8(7)
C417.2(9)17.7(9)19.4(9)0.5(7)6.9(7)-1.2(7)
C520.2(9)16.8(9)14.5(8)0.3(7)6.2(7)-0.2(7)
C626.6(10)15.4(9)31.7(11)-1.3(8)16.4(9)-2.0(8)
C723.2(10)22.5(10)23(1)-7.0(8)5.3(8)0.7(8)
C833.9(11)23(1)19.5(9)-0.2(8)14.4(9)5.8(8)
C922.1(10)20.2(9)28.9(10)1.7(8)13.8(8)4.7(8)
C1026.8(10)17.0(9)23.7(10)5.1(7)9.7(8)4.4(7)
C1417.7(9)25.6(10)20.3(9)9.3(7)9.5(7)5.4(7)
C1534.6(12)22.3(10)24.9(10)5.1(8)12.2(9)11.8(9)
C1620.8(9)40.2(12)19.8(9)6.7(9)6.1(8)9.1(9)
C1327.9(11)32.4(11)18.4(9)7.2(8)10.1(8)0.8(9)
C1220.3(9)26.8(10)21.0(9)-0.1(8)9.6(8)-1.7(8)
C1133.6(12)28.6(11)36.0(12)-6.8(9)22.5(10)0.0(9)
C3331.3(11)36.4(12)24.5(11)-12.2(9)9.0(9)-5.4(9)
C3446.8(15)53.4(16)33.0(13)-4.3(12)21.7(12)1.9(12)
C3549(3)22(2)45(3)11(2)29(3)12.3(19)
C35B77(7)41(6)32(6)-6(5)26(6)8(5)
C3655(3)23.9(19)29(2)5.5(16)20(2)4.6(17)
C36B97(10)43(6)70(10)-8(5)56(10)1(5)
Li220.3(15)23.3(16)20.0(15)2.0(14)9.9(12)-1.5(14)
Li123.0(16)23.5(16)17.9(15)-0.1(13)8.7(13)0.6(13)

 

Table 4 Bond Lengths for mo_B0083_0m.
AtomAtomLength/Å AtomAtomLength/Å
Fe2C172.0499(18) N2C321.464(3)
Fe2C182.0424(18) N2Li12.161(4)
Fe2C192.1199(18) N1C141.474(2)
Fe2C202.0581(19) N1C151.476(3)
Fe2C212.0381(18) N1C161.475(2)
Fe2C222.0512(19) N1Li22.047(4)
Fe2C232.052(2) C17C181.446(2)
Fe2C242.0613(19) C17C211.440(3)
Fe2C252.0584(19) C18C191.451(2)
Fe2C262.0585(19) C18C301.510(3)
Fe2Li22.907(3) C19C201.441(3)
Fe1C12.0547(18) C19Li22.099(4)
Fe1C22.0576(18) C19Li12.202(4)
Fe1C32.1255(19) C20C211.431(3)
Fe1C42.041(2) C22C231.424(3)
Fe1C52.0351(19) C22C261.415(3)
Fe1C62.054(2) C23C241.430(3)
Fe1C72.051(2) C24C251.430(3)
Fe1C82.053(2) C25C261.421(3)
Fe1C92.052(2) C1C21.448(2)
Fe1C102.055(2) C1C51.440(3)
Si2C171.8642(19) C2C31.449(3)
Si2C291.875(2) C2C141.522(3)
Si2C281.868(2) C3C41.446(3)
Si2C271.872(2) C3Li22.144(4)
Si1C11.8574(19) C3Li12.227(4)
Si1C131.874(2) C4C51.429(3)
Si1C121.877(2) C6C71.424(3)
Si1C111.877(2) C6C101.421(3)
O1C331.430(3) C7C81.424(3)
O1C351.458(5) C8C91.429(3)
O1C35B1.490(14) C9C101.425(3)
O1Li11.978(4) C33C341.501(3)
N2C301.483(2) C35C361.458(7)
N2C311.471(3) C35BC36B1.46(2)

 

Table 5 Bond Angles for mo_B0083_0m.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C17Fe2C1970.57(7) C35BO1Li1109.8(6)
C17Fe2C2068.96(7) C30N2Li199.18(14)
C17Fe2C22105.92(8) C31N2C30109.87(15)
C17Fe2C23120.14(8) C31N2Li1106.58(16)
C17Fe2C24156.71(8) C32N2C30109.23(16)
C17Fe2C25160.01(8) C32N2C31109.70(16)
C17Fe2C26122.84(8) C32N2Li1121.56(15)
C17Fe2Li2113.57(8) C14N1C15110.13(16)
C18Fe2C1741.39(7) C14N1C16109.55(16)
C18Fe2C1940.74(7) C14N1Li2103.05(14)
C18Fe2C2066.88(7) C15N1Li299.81(16)
C18Fe2C22125.23(8) C16N1C15108.95(17)
C18Fe2C23108.50(8) C16N1Li2124.56(15)
C18Fe2C24122.47(7) Si2C17Fe2124.48(10)
C18Fe2C25157.43(8) C18C17Fe269.02(10)
C18Fe2C26161.16(8) C18C17Si2130.76(14)
C18Fe2Li274.01(8) C21C17Fe268.93(10)
C19Fe2Li246.14(8) C21C17Si2124.26(14)
C20Fe2C1940.31(7) C21C17C18104.95(15)
C20Fe2C24125.51(7) C17C18Fe269.58(10)
C20Fe2C25108.59(8) C17C18C19112.54(16)
C20Fe2C26121.97(8) C17C18C30126.71(16)
C20Fe2Li273.64(9) C19C18Fe272.50(10)
C21Fe2C1741.25(8) C19C18C30120.74(16)
C21Fe2C1868.25(7) C30C18Fe2126.78(13)
C21Fe2C1969.61(7) Fe2C19Li1141.90(13)
C21Fe2C2040.90(7) C18C19Fe266.76(10)
C21Fe2C22120.22(8) C18C19Li2117.83(16)
C21Fe2C23155.79(8) C18C19Li1100.10(15)
C21Fe2C24161.41(8) C20C19Fe267.54(10)
C21Fe2C25123.92(8) C20C19C18102.81(15)
C21Fe2C26106.68(8) C20C19Li2117.98(16)
C21Fe2Li2112.66(9) C20C19Li1149.09(16)
C22Fe2C19161.70(8) Li2C19Fe287.12(11)
C22Fe2C20156.52(8) Li2C19Li167.05(14)
C22Fe2C2340.63(8) C19C20Fe272.15(10)
C22Fe2C2468.06(8) C21C20Fe268.80(10)
C22Fe2C2568.00(8) C21C20C19111.53(16)
C22Fe2C2640.29(9) C17C21Fe269.82(11)
C22Fe2Li2127.11(9) C20C21Fe270.30(10)
C23Fe2C19124.63(7) C20C21C17108.17(16)
C23Fe2C20161.84(8) C23C22Fe269.72(11)
C23Fe2C2440.68(8) C26C22Fe270.13(11)
C23Fe2C2568.49(8) C26C22C23108.55(17)
C23Fe2C2668.23(8) C22C23Fe269.65(12)
C23Fe2Li288.19(9) C22C23C24107.48(18)
C24Fe2C19107.72(7) C24C23Fe270.01(11)
C24Fe2Li261.62(9) C23C24Fe269.31(11)
C25Fe2C19121.23(8) C23C24C25107.93(17)
C25Fe2C2440.63(8) C25C24Fe269.57(11)
C25Fe2C2640.39(8) C24C25Fe269.79(11)
C25Fe2Li283.48(9) C26C25Fe269.81(11)
C26Fe2C19156.45(8) C26C25C24107.81(17)
C26Fe2C2468.01(8) C22C26Fe269.58(11)
C26Fe2Li2123.42(9) C22C26C25108.23(18)
C1Fe1C241.22(7) C25C26Fe269.80(11)
C1Fe1C370.37(7) N2C30C18111.05(15)
C1Fe1C10125.00(8) Si1C1Fe1125.72(10)
C2Fe1C340.50(7) C2C1Fe169.50(10)
C4Fe1C168.88(8) C2C1Si1129.10(14)
C4Fe1C266.81(8) C5C1Fe168.66(10)
C4Fe1C340.56(7) C5C1Si1125.60(14)
C4Fe1C6156.64(8) C5C1C2105.30(16)
C4Fe1C7161.22(8) C1C2Fe169.28(10)
C4Fe1C8124.41(9) C1C2C3112.55(16)
C4Fe1C9107.34(8) C1C2C14122.69(16)
C4Fe1C10121.28(8) C3C2Fe172.27(11)
C5Fe1C141.22(7) C3C2C14124.76(16)
C5Fe1C268.22(7) C14C2Fe1125.98(14)
C5Fe1C369.87(8) Fe1C3Li2113.95(14)
C5Fe1C441.03(8) Fe1C3Li1144.39(13)
C5Fe1C6121.14(8) C2C3Fe167.23(10)
C5Fe1C7156.42(8) C2C3Li298.28(15)
C5Fe1C8161.42(8) C2C3Li1147.59(17)
C5Fe1C9124.37(8) C4C3Fe166.59(11)
C5Fe1C10107.50(8) C4C3C2102.41(16)
C6Fe1C1107.74(8) C4C3Li2157.19(17)
C6Fe1C2126.77(8) C4C3Li199.91(15)
C6Fe1C3162.07(8) Li2C3Li165.86(14)
C6Fe1C1040.47(9) C3C4Fe172.86(11)
C7Fe1C1120.85(8) C5C4Fe169.26(11)
C7Fe1C2108.81(8) C5C4C3112.03(17)
C7Fe1C3124.10(8) C1C5Fe170.12(10)
C7Fe1C640.58(9) C4C5Fe169.71(11)
C7Fe1C840.61(9) C4C5C1107.71(16)
C7Fe1C968.47(8) C7C6Fe169.59(12)
C7Fe1C1068.27(8) C10C6Fe169.81(12)
C8Fe1C1156.00(8) C10C6C7108.17(18)
C8Fe1C2120.98(8) C6C7Fe169.83(12)
C8Fe1C3105.90(8) C6C7C8107.91(18)
C8Fe1C668.19(9) C8C7Fe169.77(12)
C8Fe1C1068.25(8) C7C8Fe169.62(11)
C9Fe1C1161.83(8) C7C8C9108.04(18)
C9Fe1C2155.15(8) C9C8Fe169.60(11)
C9Fe1C3119.08(8) C8C9Fe169.66(11)
C9Fe1C668.27(8) C10C9Fe169.82(11)
C9Fe1C840.73(9) C10C9C8107.75(18)
C9Fe1C1040.59(8) C6C10Fe169.73(11)
C10Fe1C2163.37(8) C6C10C9108.13(18)
C10Fe1C3154.91(8) C9C10Fe169.59(11)
C17Si2C29112.86(9) N1C14C2112.16(15)
C17Si2C28109.61(9) O1C33C34114.0(2)
C17Si2C27109.70(10) C36C35O1110.6(4)
C28Si2C29107.71(11) C36BC35BO1102.9(12)
C28Si2C27107.36(11) N1Li2Fe2124.96(14)
C27Si2C29109.43(12) N1Li2C19130.46(19)
C1Si1C13108.67(9) N1Li2C388.86(14)
C1Si1C12112.30(9) C19Li2Fe246.74(8)
C1Si1C11109.73(10) C19Li2C3116.76(16)
C13Si1C12110.40(10) C3Li2Fe2145.87(15)
C13Si1C11108.19(11) O1Li1N2115.50(17)
C11Si1C12107.47(10) O1Li1C19119.09(18)
C33O1C35108.0(3) O1Li1C3109.33(17)
C33O1C35B130.4(6) N2Li1C1987.08(14)
C33O1Li1118.10(17) N2Li1C3115.16(17)
C35O1Li1132.0(3) C19Li1C3109.32(16)

 

Table 6 Torsion Angles for mo_B0083_0m.
ABCDAngle/˚ ABCDAngle/˚
Fe2C17C18C19-59.88(13) C32N2C30C18175.46(15)
Fe2C17C18C30121.30(18) C29Si2C17Fe2-58.84(15)
Fe2C17C21C2060.09(13) C29Si2C17C1832.2(2)
Fe2C18C19C20-58.40(12) C29Si2C17C21-145.41(17)
Fe2C18C19Li273.22(14) C28Si2C17Fe2-178.89(11)
Fe2C18C19Li1142.50(13) C28Si2C17C18-87.81(19)
Fe2C18C30N2-141.12(14) C28Si2C17C2194.54(18)
Fe2C19C20C21-57.62(13) C27Si2C17Fe263.46(15)
Fe2C20C21C17-59.79(13) C27Si2C17C18154.54(18)
Fe2C22C23C2460.06(13) C27Si2C17C21-23.1(2)
Fe2C22C26C25-59.30(14) C1C2C3Fe157.66(14)
Fe2C23C24C2559.05(13) C1C2C3C4-0.1(2)
Fe2C24C25C2659.70(14) C1C2C3Li2170.23(17)
Fe2C25C26C2259.16(13) C1C2C3Li1-132.6(3)
Fe1C1C2C3-59.36(14) C1C2C14N1163.28(17)
Fe1C1C2C14120.24(18) C2C1C5Fe1-60.22(12)
Fe1C1C5C459.83(13) C2C1C5C4-0.4(2)
Fe1C2C3C4-57.75(13) C2C3C4Fe158.19(13)
Fe1C2C3Li2112.57(13) C2C3C4C5-0.2(2)
Fe1C2C3Li1169.8(3) C3C2C14N1-17.2(3)
Fe1C2C14N1-109.79(17) C3C4C5Fe160.44(14)
Fe1C3C4C5-58.36(14) C3C4C5C10.4(2)
Fe1C4C5C1-60.09(13) C5C1C2Fe159.66(12)
Fe1C6C7C859.62(14) C5C1C2C30.3(2)
Fe1C6C10C9-59.20(14) C5C1C2C14179.90(17)
Fe1C7C8C959.20(14) C6C7C8Fe1-59.66(14)
Fe1C8C9C1059.68(14) C6C7C8C9-0.5(2)
Fe1C9C10C659.28(14) C7C6C10Fe159.21(14)
Si2C17C18Fe2-118.04(16) C7C6C10C90.0(2)
Si2C17C18C19-177.92(14) C7C8C9Fe1-59.21(14)
Si2C17C18C303.3(3) C7C8C9C100.5(2)
Si2C17C21Fe2118.15(14) C8C9C10Fe1-59.57(14)
Si2C17C21C20178.24(13) C8C9C10C6-0.3(2)
Si1C1C2Fe1-119.95(16) C10C6C7Fe1-59.35(14)
Si1C1C2C3-179.31(15) C10C6C7C80.3(2)
Si1C1C2C140.3(3) C14C2C3Fe1-121.93(19)
Si1C1C5Fe1119.41(15) C14C2C3C4-179.68(18)
Si1C1C5C4179.24(14) C14C2C3Li2-9.4(2)
C17C18C19Fe258.21(13) C14C2C3Li147.8(4)
C17C18C19C20-0.2(2) C15N1C14C2-72.0(2)
C17C18C19Li2131.43(17) C16N1C14C2168.22(16)
C17C18C19Li1-159.29(16) C13Si1C1Fe169.22(14)
C17C18C30N2128.07(19) C13Si1C1C2160.85(18)
C18C17C21Fe2-60.01(12) C13Si1C1C5-18.69(19)
C18C17C21C200.1(2) C12Si1C1Fe1-53.21(14)
C18C19C20Fe257.86(11) C12Si1C1C238.4(2)
C18C19C20C210.2(2) C12Si1C1C5-141.12(16)
C19C18C30N2-50.7(2) C11Si1C1Fe1-172.67(12)
C19C20C21Fe259.57(13) C11Si1C1C2-81.04(19)
C19C20C21C17-0.2(2) C11Si1C1C599.42(18)
C21C17C18Fe259.95(12) C33O1C35C36145.9(5)
C21C17C18C190.1(2) C33O1C35BC36B77.0(12)
C21C17C18C30-178.76(17) C35O1C33C3471.0(3)
C22C23C24Fe2-59.84(13) C35BO1C33C3467.8(8)
C22C23C24C25-0.8(2) Li2N1C14C233.8(2)
C23C22C26Fe259.34(13) Li2C19C20Fe2-73.66(15)
C23C22C26C250.0(2) Li2C19C20C21-131.29(18)
C23C24C25Fe2-58.89(13) Li2C3C4Fe1-96.4(5)
C23C24C25C260.8(2) Li2C3C4C5-154.8(4)
C24C25C26Fe2-59.69(13) Li1O1C33C34-95.2(3)
C24C25C26C22-0.5(2) Li1O1C35C36-50.5(7)
C26C22C23Fe2-59.60(13) Li1O1C35BC36B-118.8(9)
C26C22C23C240.5(2) Li1N2C30C1847.29(18)
C30C18C19Fe2-122.89(17) Li1C19C20Fe2-165.3(3)
C30C18C19C20178.72(16) Li1C19C20C21137.1(3)
C30C18C19Li2-49.7(2) Li1C3C4Fe1-145.46(13)
C30C18C19Li119.6(2) Li1C3C4C5156.18(16)
C31N2C30C18-64.2(2)      

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for mo_B0083_0m.
AtomxyzU(eq)
H2061206943490320
H2170216756360022
H2271513441325427
H2374602737502124
H2457543488543522
H2544354688393525
H2652964636258728
H30A90343998654222
H30B100274548622422
H31A112196079721342
H31B108616668805442
H31C99956761686442
H32A113894298799540
H32B103413860830040
H32C111404893889240
H29A105993881498048
H29B101883618378648
H29C92973382433248
H28A103007027408140
H28B111226034399840
H28C110456295506940
H27A77304908236552
H27B89145238220952
H27C81066179239952
H491414310924322
H5832134771044521
H66368889877328
H756121659696429
H874162266663429
H992881895825227
H1086321034956727
H14A47253573713825
H14B45064566778425
H15A44856418725241
H15B51036740649241
H15C59016287761641
H16A36484249549741
H16B37125529523841
H16C31415169602341
H13A678216311067339
H13B585518971117739
H13C701526551143939
H12A36642899836233
H12B38621914916433
H12C45401896841033
H11A555047521077145
H11B440440121061845
H11C44014780970345
H33A93437698983238
H33B93226382972638
H34A72906386949864
H34B73747694968264
H34C815468781058964
H35A70738254792043
H35B83088776871143
H35C74697850698959
H35D71918418789359
H36A78158196666952
H36B90648690745852
H36C78799432708952
H36D85249457736495
H36E94848494786395
H36F90229219856995

 

Table 8 Atomic Occupancy for mo_B0083_0m.
AtomOccupancy AtomOccupancy AtomOccupancy
C350.672(12) H35A0.672(12) H35B0.672(12)
C35B0.328(12) H35C0.328(12) H35D0.328(12)
C360.672(12) H36A0.672(12) H36B0.672(12)
H36C0.672(12) C36B0.328(12) H36D0.328(12)
H36E0.328(12) H36F0.328(12)   

Experimental

Single crystals of C36H58Fe2Li2N2OSi2 [mo_B0083_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 XT [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_B0083_0m]

Crystal Data for C36H58Fe2Li2N2OSi2 (=716.60 g/mol): monoclinic, space group P21 (no. 4), a = 12.2143(5) Å, b = 12.0951(6) Å, c = 14.2648(7) Å, β = 113.848(2)°, = 1927.46(16) Å3, Z = 2, T = 100.0 K, μ(MoKα) = 0.843 mm-1, Dcalc = 1.235 g/cm3, 56891 reflections measured (4.592° ≤ 2Θ ≤ 55.998°), 9291 unique (Rint = 0.0213, Rsigma = 0.0152) which were used in all calculations. The final R1 was 0.0180 (I > 2σ(I)) and wR2 was 0.0527 (all data).

Refinement model description

Number of restraints - 3, 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. Rigid bond restraints
C35B, C36B
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
C35, C36
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Others
Sof(C35B)=Sof(H35C)=Sof(H35D)=Sof(C36B)=Sof(H36D)=Sof(H36E)=Sof(H36F)=1-FVAR(1)
Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
C30(H30A,H30B), C14(H14A,H14B), C33(H33A,H33B), C35(H35A,H35B), C35B(H35C,H35D)
4.b Aromatic/amide H refined with riding coordinates:
C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C4(H4),
C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10)
4.c Idealised Me refined as rotating group:
C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C29(H29A,H29B,H29C), C28(H28A,H28B,
H28C), C27(H27A,H27B,H27C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C13(H13A,
H13B,H13C), C12(H12A,H12B,H12C), C11(H11A,H11B,H11C), C34(H34A,H34B,H34C),
C36(H36A,H36B,H36C), C36B(H36D,H36E,H36F)

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