3094

Table 1 Crystal data and structure refinement for 3094.
Identification code 3094
Empirical formula C40H52Cl2Fe2N2O4Si2
Formula weight 863.61
Temperature/K 150
Crystal system triclinic
Space group P-1
a/Å 12.3951(4)
b/Å 12.5719(4)
c/Å 13.6964(5)
α/° 78.754(3)
β/° 85.109(3)
γ/° 77.113(3)
Volume/Å3 2038.65(12)
Z 2
ρcalcg/cm3 1.407
μ/mm‑1 0.944
F(000) 904.0
Crystal size/mm3 0.3 × 0.2 × 0.1
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.242 to 51.998
Index ranges -15 ≤ h ≤ 15, -15 ≤ k ≤ 15, -16 ≤ l ≤ 16
Reflections collected 48054
Independent reflections 8022 [Rint = 0.0435, Rsigma = 0.0316]
Data/restraints/parameters 8022/10/492
Goodness-of-fit on F2 1.045
Final R indexes [I>=2σ (I)] R1 = 0.0517, wR2 = 0.1262
Final R indexes [all data] R1 = 0.0632, wR2 = 0.1337
Largest diff. peak/hole / e Å-3 1.30/-0.68

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for 3094. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Fe110567.6(4)-530.9(4)2508.3(3)27.48(12)
Fe23482.3(4)3954.1(4)2989.3(3)26.26(12)
Si17761.2(7)490.9(7)2882.4(6)23.76(18)
Si26298.5(7)2721.1(7)3152.8(6)25.36(19)
O17003.4(18)1449.3(18)3439.8(16)28.4(5)
O27360.0(18)749.5(18)1739.5(17)28.9(5)
O36804.9(19)3194.2(19)2057.9(18)33.0(5)
N18981(2)2892(2)1139(2)32.4(6)
N25269(2)1792(2)941(2)36.0(7)
C19218(2)579(2)2921(2)24.4(6)
C29927(3)1118(3)2186(2)25.8(6)
C311001(3)918(3)2582(3)32.1(7)
C410974(3)269(3)3542(3)34.5(8)
C59898(3)59(3)3757(2)30.0(7)
C610069(3)-1551(3)1723(3)53.6(11)
C710913(4)-1053(4)1183(3)54.2(11)
C811864(3)-1379(3)1759(3)44.0(9)
C911605(3)-2064(3)2651(3)42.4(9)
C1010503(3)-2167(3)2630(3)45.3(9)
C119635(3)1718(3)1160(2)29.2(7)
C129537(4)3563(3)1632(3)46.6(10)
C138751(4)3444(3)87(3)45.1(9)
C147542(3)-876(3)3584(3)35.3(8)
C156425(3)-1108(3)3461(2)33.0(7)
C165468(3)-488(3)3840(3)44.6(9)
C174444(4)-686(5)3763(4)78.0(18)
C184344(6)-1514(7)3311(5)108(3)
C195250(7)-2138(5)2884(4)101(2)
C206332(5)-1949(4)2969(3)60.5(13)
C214822(3)2667(2)3127(2)26.4(7)
C224176(3)2686(3)2288(3)29.7(7)
C233086(3)2592(3)2659(3)38.2(8)
C243036(3)2521(3)3704(3)37.7(8)
C254086(3)2567(3)4001(3)31.8(7)
C264024(3)5413(3)2553(3)42.8(9)
C273218(3)5350(3)1912(3)44.3(9)
C282227(3)5269(3)2482(3)43.9(9)
C292420(3)5266(3)3488(3)40.0(8)
C303529(3)5356(3)3534(3)40.5(9)
C314549(3)2823(3)1220(2)34.8(8)
C324745(3)813(3)1198(3)49.1(10)
C335597(4)1988(4)-137(3)68.0(15)
C346487(3)3509(3)4119(3)33.1(7)
C357642(3)3702(3)4138(2)30.6(7)
C367902(4)4717(3)3741(3)43.5(9)
C378987(4)4868(4)3766(3)57.4(12)
C389803(4)4015(4)4171(3)55.3(11)
C399561(3)3014(4)4549(3)50.5(10)
C408503(3)2849(3)4535(3)38.3(8)
Cl17545.9(8)-813.0(9)324.4(7)48.4(2)
Cl26554.9(10)5520.7(10)1072.4(10)77.4(4)
O48346(5)6762(5)7(6)172(3)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for 3094. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Fe124.9(2)30.3(2)28.2(2)-10.34(18)-4.39(18)-2.12(18)
Fe223.9(2)24.0(2)30.5(2)-7.46(18)0.94(18)-3.02(18)
Si121.1(4)21.6(4)29.7(4)-6.5(3)0.3(3)-5.7(3)
Si224.6(4)24.5(4)28.4(4)-9.5(3)-1.0(3)-4.1(3)
O127.2(11)27.6(11)29.8(11)-5.6(9)2.3(9)-5.5(9)
O227.4(11)24.0(11)36.3(12)-7.7(9)-7.0(9)-3.4(9)
O335.1(13)26.1(12)36.5(13)-3.5(10)-0.3(10)-6.3(10)
N136.4(16)31.1(15)27.5(14)-5.7(11)0.2(12)-2.7(12)
N235.9(16)37.3(16)32.5(15)-11.9(12)-9.0(13)4.2(13)
C125.2(15)26.3(15)25.4(15)-11.3(12)-0.2(12)-7.4(12)
C223.6(15)27.4(16)28.8(16)-12.0(12)2.4(12)-5.5(12)
C325.3(16)34.2(17)41.5(19)-14.1(14)-0.1(14)-10.9(13)
C428.5(17)39.3(19)39.9(19)-14.8(15)-10.6(14)-6.1(14)
C534.6(17)34.8(17)22.7(15)-9.0(13)-3.0(13)-7.9(14)
C646(2)44(2)79(3)-42(2)-27(2)9.4(18)
C776(3)48(2)36(2)-24.7(18)-9(2)8(2)
C840(2)44(2)46(2)-19.1(17)6.5(17)2.4(17)
C936(2)32.8(19)56(2)-11.3(17)-10.0(17)4.8(15)
C1043(2)29.8(18)66(3)-19.8(18)-0.7(19)-5.2(16)
C1132.2(17)30.1(16)26.8(16)-11.4(13)3.5(13)-6.3(13)
C1257(2)32.8(19)53(2)-12.9(17)-4.9(19)-11.6(18)
C1356(2)41(2)29.7(18)-1.0(16)-1.3(17)2.8(18)
C1431.0(17)27.9(17)44(2)0.7(15)0.1(15)-6.0(14)
C1540.6(19)29.1(17)30.7(17)2.4(13)-1.4(15)-17.1(14)
C1634.6(19)43(2)50(2)8.8(17)1.6(17)-11.8(16)
C1738(2)93(4)89(4)38(3)-12(2)-29(2)
C18105(4)145(6)86(4)50(4)-50(4)-96(4)
C19198(7)88(4)49(3)13(3)-33(4)-113(4)
C20105(4)42(2)44(2)-2.2(18)-2(2)-39(2)
C2128.8(16)18.2(14)30.9(16)-4.0(12)1.1(13)-3.5(12)
C2228.4(16)21.6(15)40.3(18)-8.6(13)-4.1(14)-3.9(13)
C2331.4(18)24.5(17)61(2)-10.6(16)-5.4(17)-6.4(14)
C2429.2(17)28.1(17)53(2)-5.1(15)11.6(16)-7.8(14)
C2533.6(18)21.3(15)35.7(18)-0.9(13)3.6(14)-1.1(13)
C2643(2)21.8(17)62(2)-5.7(16)8.6(19)-10.0(15)
C2760(2)25.2(18)40(2)-1.8(15)-0.4(18)3.7(17)
C2840(2)27.0(18)59(2)-8.8(17)-12.4(18)8.8(15)
C2936.0(19)28.7(18)53(2)-14.9(16)6.0(17)1.3(15)
C3044(2)25.9(17)54(2)-16.9(16)-4.4(17)-0.9(15)
C3132.5(18)37.9(19)32.1(17)-10.7(14)-10.0(14)3.2(15)
C3243(2)44(2)68(3)-32(2)-7.8(19)-4.7(17)
C3377(3)79(3)26(2)-7(2)-1(2)28(3)
C3433.3(18)33.2(18)36.1(18)-17.2(14)-2.2(14)-4.3(14)
C3538.2(18)33.1(17)25.8(16)-12.1(13)-5.0(14)-11.5(14)
C3657(2)31.8(19)45(2)-9.7(16)-10.6(18)-11.6(17)
C3777(3)49(2)60(3)-17(2)9(2)-40(2)
C3843(2)71(3)63(3)-30(2)-6(2)-21(2)
C3941(2)61(3)54(2)-18(2)-14.6(19)-9.3(19)
C4044(2)37.5(19)34.3(18)-4.9(15)-9.7(16)-8.7(16)
Cl144.8(5)57.2(6)42.2(5)-20.3(4)-11.8(4)5.0(4)
Cl263.5(7)49.3(6)85.8(9)31.2(6)24.6(6)9.8(5)
O497(4)99(3)342(9)-115(5)119(5)-47(3)

 

Table 4 Bond Lengths for 3094.
AtomAtomLength/Å AtomAtomLength/Å
Fe1C12.042(3) C1C51.440(4)
Fe1C22.023(3) C2C31.432(4)
Fe1C32.034(3) C2C111.492(4)
Fe1C42.043(3) C3C41.408(5)
Fe1C52.036(3) C4C51.412(5)
Fe1C62.047(4) C6C71.418(7)
Fe1C72.030(4) C6C101.409(6)
Fe1C82.038(4) C7C81.413(6)
Fe1C92.049(4) C8C91.408(6)
Fe1C102.050(4) C9C101.404(5)
Fe2C212.036(3) C14C151.507(5)
Fe2C222.013(3) C15C161.387(5)
Fe2C232.023(3) C15C201.389(5)
Fe2C242.043(3) C16C171.364(6)
Fe2C252.043(3) C17C181.343(10)
Fe2C262.056(3) C18C191.375(10)
Fe2C272.044(4) C19C201.431(8)
Fe2C282.056(3) C21C221.448(5)
Fe2C292.059(3) C21C251.445(5)
Fe2C302.057(4) C22C231.425(5)
Si1O11.627(2) C22C311.485(5)
Si1O21.633(2) C23C241.413(5)
Si1C11.840(3) C24C251.413(5)
Si1C141.862(3) C26C271.411(6)
Si2O11.632(2) C26C301.425(6)
Si2O31.629(2) C27C281.410(6)
Si2C211.850(3) C28C291.417(6)
Si2C341.858(3) C29C301.411(5)
N1C111.513(4) C34C351.507(5)
N1C121.484(5) C35C361.382(5)
N1C131.494(4) C35C401.395(5)
N2C311.497(4) C36C371.404(6)
N2C321.486(5) C37C381.364(7)
N2C331.484(5) C38C391.354(6)
C1C21.447(4) C39C401.374(5)

 

Table 5 Bond Angles for 3094.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C1Fe1C469.48(13) C21Si2C34110.12(15)
C1Fe1C6109.40(14) Si1O1Si2138.76(15)
C1Fe1C9153.24(15) C12N1C11113.2(3)
C1Fe1C10120.24(14) C12N1C13110.5(3)
C2Fe1C141.71(12) C13N1C11109.7(3)
C2Fe1C341.34(12) C32N2C31113.1(3)
C2Fe1C468.93(13) C33N2C31110.3(3)
C2Fe1C569.08(13) C33N2C32110.4(3)
C2Fe1C6118.55(15) Si1C1Fe1126.02(15)
C2Fe1C7106.36(15) C2C1Fe168.44(17)
C2Fe1C8125.88(15) C2C1Si1130.7(2)
C2Fe1C9164.03(14) C5C1Fe169.08(18)
C2Fe1C10153.47(14) C5C1Si1123.6(2)
C3Fe1C169.88(12) C5C1C2105.7(3)
C3Fe1C440.41(14) C1C2Fe169.85(17)
C3Fe1C568.39(14) C1C2C11126.8(3)
C3Fe1C6151.08(17) C3C2Fe169.74(18)
C3Fe1C8105.07(15) C3C2C1108.3(3)
C3Fe1C9126.17(14) C3C2C11124.7(3)
C3Fe1C10165.03(15) C11C2Fe1123.1(2)
C4Fe1C6168.24(18) C2C3Fe168.92(18)
C4Fe1C9107.71(15) C4C3Fe170.16(19)
C4Fe1C10129.45(16) C4C3C2108.2(3)
C5Fe1C141.37(12) C3C4Fe169.43(19)
C5Fe1C440.51(13) C3C4C5108.4(3)
C5Fe1C6131.15(17) C5C4Fe169.45(18)
C5Fe1C8150.60(15) C1C5Fe169.55(17)
C5Fe1C9119.21(15) C4C5Fe170.04(19)
C5Fe1C10110.98(16) C4C5C1109.4(3)
C6Fe1C967.70(15) C7C6Fe169.0(2)
C6Fe1C1040.24(17) C10C6Fe170.0(2)
C7Fe1C1128.30(15) C10C6C7107.7(4)
C7Fe1C3115.74(17) C6C7Fe170.3(2)
C7Fe1C4149.10(18) C8C7Fe170.0(2)
C7Fe1C5168.42(16) C8C7C6107.8(4)
C7Fe1C640.72(19) C7C8Fe169.4(2)
C7Fe1C840.67(17) C9C8Fe170.3(2)
C7Fe1C968.04(17) C9C8C7107.9(4)
C7Fe1C1068.04(18) C8C9Fe169.4(2)
C8Fe1C1165.62(14) C10C9Fe170.0(2)
C8Fe1C4115.95(15) C10C9C8108.2(4)
C8Fe1C668.14(17) C6C10Fe169.7(2)
C8Fe1C940.31(16) C9C10Fe169.9(2)
C8Fe1C1067.74(17) C9C10C6108.4(4)
C9Fe1C1040.06(15) C2C11N1113.0(3)
C21Fe2C2469.33(13) C15C14Si1114.3(2)
C21Fe2C2541.51(13) C16C15C14120.6(3)
C21Fe2C26108.75(14) C16C15C20118.7(4)
C21Fe2C27128.25(14) C20C15C14120.8(4)
C21Fe2C28165.85(15) C17C16C15122.5(5)
C21Fe2C29152.55(15) C18C17C16119.5(6)
C21Fe2C30119.27(14) C17C18C19121.3(5)
C22Fe2C2141.91(13) C18C19C20119.8(5)
C22Fe2C2341.34(14) C15C20C19118.2(5)
C22Fe2C2469.22(14) Si2C21Fe2128.12(16)
C22Fe2C2569.68(14) C22C21Fe268.18(17)
C22Fe2C26117.58(15) C22C21Si2129.5(2)
C22Fe2C27106.38(15) C25C21Fe269.49(18)
C22Fe2C28126.38(15) C25C21Si2124.1(2)
C22Fe2C29164.79(14) C25C21C22106.4(3)
C22Fe2C30152.49(14) C21C22Fe269.91(18)
C23Fe2C2169.82(13) C21C22C31127.0(3)
C23Fe2C2440.67(15) C23C22Fe269.72(19)
C23Fe2C2568.73(15) C23C22C21107.9(3)
C23Fe2C26150.52(17) C23C22C31125.0(3)
C23Fe2C27116.25(16) C31C22Fe2124.1(2)
C23Fe2C28106.24(15) C22C23Fe268.94(18)
C23Fe2C29127.17(15) C24C23Fe270.4(2)
C23Fe2C30165.92(15) C24C23C22108.5(3)
C24Fe2C2540.46(14) C23C24Fe268.93(19)
C24Fe2C26168.31(16) C25C24Fe269.77(18)
C24Fe2C27149.88(17) C25C24C23108.6(3)
C24Fe2C28117.11(16) C21C25Fe269.01(17)
C24Fe2C29108.26(15) C24C25Fe269.77(19)
C24Fe2C30129.51(16) C24C25C21108.5(3)
C25Fe2C26130.69(15) C27C26Fe269.4(2)
C25Fe2C27168.09(15) C27C26C30107.7(3)
C25Fe2C28151.02(15) C30C26Fe269.8(2)
C25Fe2C29118.79(15) C26C27Fe270.3(2)
C25Fe2C30110.13(15) C28C27Fe270.3(2)
C26Fe2C2967.79(15) C28C27C26108.3(4)
C26Fe2C3040.54(16) C27C28Fe269.4(2)
C27Fe2C2640.25(16) C27C28C29108.1(4)
C27Fe2C2840.24(16) C29C28Fe270.0(2)
C27Fe2C2967.83(16) C28C29Fe269.7(2)
C27Fe2C3067.86(16) C30C29Fe269.9(2)
C28Fe2C2667.59(16) C30C29C28107.9(3)
C28Fe2C2940.31(16) C26C30Fe269.7(2)
C28Fe2C3067.56(16) C29C30Fe270.0(2)
C30Fe2C2940.10(15) C29C30C26108.0(4)
O1Si1O2106.72(12) C22C31N2113.3(3)
O1Si1C1107.86(13) C35C34Si2114.7(2)
O1Si1C14107.64(14) C36C35C34121.8(3)
O2Si1C1111.50(13) C36C35C40117.1(3)
O2Si1C14112.76(15) C40C35C34121.1(3)
C1Si1C14110.10(15) C35C36C37120.4(4)
O1Si2C21107.80(13) C38C37C36120.7(4)
O1Si2C34108.84(14) C39C38C37119.4(4)
O3Si2O1104.75(12) C38C39C40120.8(4)
O3Si2C21112.21(14) C39C40C35121.6(4)
O3Si2C34112.82(15)     

 

Table 6 Hydrogen Bonds for 3094.
DHAd(D-H)/Åd(H-A)/Åd(D-A)/ÅD-H-A/°
O2H2Cl10.962(19)2.02(2)2.979(2)171(4)
O3H3Cl20.961(19)2.18(3)2.933(2)134(3)
N1H1O30.985(18)1.89(2)2.856(4)167(3)
N2H2AO20.991(18)1.87(2)2.836(4)163(3)
C11H11AO20.992.653.292(4)123.0
O4H4ACl20.872.293.099(5)153.8

 

Table 7 Torsion Angles for 3094.
ABCDAngle/˚ ABCDAngle/˚
Fe1C1C2C3-59.3(2) C5C1C2C30.0(3)
Fe1C1C2C11116.8(3) C5C1C2C11176.2(3)
Fe1C1C5C458.8(2) C6C7C8Fe1-60.4(3)
Fe1C2C3C4-59.3(2) C6C7C8C9-0.5(4)
Fe1C2C11N1169.5(2) C7C6C10Fe158.9(3)
Fe1C3C4C5-58.7(2) C7C6C10C9-0.5(4)
Fe1C4C5C1-58.5(2) C7C8C9Fe1-59.3(3)
Fe1C6C7C860.2(3) C7C8C9C100.2(4)
Fe1C6C10C9-59.5(3) C8C9C10Fe1-59.1(3)
Fe1C7C8C959.9(3) C8C9C10C60.2(4)
Fe1C8C9C1059.5(3) C10C6C7Fe1-59.6(3)
Fe1C9C10C659.4(3) C10C6C7C80.6(4)
Fe2C21C22C23-59.6(2) C11C2C3Fe1-116.9(3)
Fe2C21C22C31118.1(3) C11C2C3C4-176.2(3)
Fe2C21C25C2458.7(2) C12N1C11C254.5(4)
Fe2C22C23C24-59.5(2) C13N1C11C2178.4(3)
Fe2C22C31N2166.5(2) C14Si1O1Si2-146.2(2)
Fe2C23C24C25-58.6(2) C14Si1C1Fe154.2(2)
Fe2C24C25C21-58.3(2) C14Si1C1C2145.7(3)
Fe2C26C27C2860.3(2) C14Si1C1C5-33.1(3)
Fe2C26C30C29-59.8(2) C14C15C16C17-178.6(4)
Fe2C27C28C2959.5(2) C14C15C20C19179.4(4)
Fe2C28C29C3059.7(2) C15C16C17C180.4(7)
Fe2C29C30C2659.6(2) C16C15C20C19-0.3(5)
Si1C1C2Fe1-119.6(3) C16C17C18C19-2.9(8)
Si1C1C2C3-178.9(2) C17C18C19C203.6(9)
Si1C1C2C11-2.8(5) C18C19C20C15-2.0(7)
Si1C1C5Fe1120.1(2) C20C15C16C171.1(6)
Si1C1C5C4179.0(2) C21Si2O1Si199.3(2)
Si1C14C15C16-67.1(4) C21Si2C34C35-174.3(2)
Si1C14C15C20113.2(3) C21C22C23Fe259.7(2)
Si2C21C22Fe2-122.1(3) C21C22C23C240.3(4)
Si2C21C22C23178.3(2) C21C22C31N277.0(4)
Si2C21C22C31-4.0(5) C22C21C25Fe2-58.4(2)
Si2C21C25Fe2122.9(2) C22C21C25C240.3(3)
Si2C21C25C24-178.4(2) C22C23C24Fe258.5(2)
Si2C34C35C36102.9(3) C22C23C24C25-0.1(4)
Si2C34C35C40-75.3(4) C23C22C31N2-105.7(4)
O1Si1C1Fe1171.40(17) C23C24C25Fe258.1(2)
O1Si1C1C2-97.1(3) C23C24C25C21-0.2(4)
O1Si1C1C584.1(3) C25C21C22Fe259.2(2)
O1Si1C14C1572.1(3) C25C21C22C23-0.3(3)
O1Si2C21Fe2171.75(18) C25C21C22C31177.4(3)
O1Si2C21C22-96.3(3) C26C27C28Fe2-60.3(2)
O1Si2C21C2582.1(3) C26C27C28C29-0.8(4)
O1Si2C34C3567.8(3) C27C26C30Fe259.3(2)
O2Si1O1Si2-24.9(2) C27C26C30C29-0.4(4)
O2Si1C1Fe1-71.7(2) C27C28C29Fe2-59.2(2)
O2Si1C1C219.8(3) C27C28C29C300.5(4)
O2Si1C1C5-159.1(2) C28C29C30Fe2-59.6(2)
O2Si1C14C15-45.4(3) C28C29C30C260.0(4)
O3Si2O1Si1-20.4(3) C30C26C27Fe2-59.5(2)
O3Si2C21Fe2-73.4(2) C30C26C27C280.8(4)
O3Si2C21C2218.5(3) C31C22C23Fe2-118.0(3)
O3Si2C21C25-163.1(2) C31C22C23C24-177.5(3)
O3Si2C34C35-48.0(3) C32N2C31C2255.2(4)
C1Si1O1Si295.0(2) C33N2C31C22179.3(3)
C1Si1C14C15-170.6(2) C34Si2O1Si1-141.3(2)
C1C2C3Fe159.4(2) C34Si2C21Fe253.2(2)
C1C2C3C40.1(4) C34Si2C21C22145.1(3)
C1C2C11N181.0(4) C34Si2C21C25-36.5(3)
C2C1C5Fe1-58.9(2) C34C35C36C37-179.7(3)
C2C1C5C4-0.1(4) C34C35C40C39179.5(3)
C2C3C4Fe158.6(2) C35C36C37C380.7(6)
C2C3C4C5-0.1(4) C36C35C40C391.2(5)
C3C2C11N1-103.5(4) C36C37C38C390.3(7)
C3C4C5Fe158.7(2) C37C38C39C40-0.5(7)
C3C4C5C10.2(4) C38C39C40C35-0.2(6)
C5C1C2Fe159.4(2) C40C35C36C37-1.4(5)

 

Table 8 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for 3094.
AtomxyzU(eq)
H27480(40)190(30)1330(30)57(13)
H37150(30)3820(30)1840(30)63(13)
H18267(19)2880(30)1510(20)31(9)
H2A5970(20)1540(30)1300(30)45(11)
H3A116241179225438
H41157716397241
H59660-359435936
H69342-1481151164
H710850-58554765
H812555-1173157753
H912092-2399317751
H1010115-2582314054
H11A9195130286735
H11B10324173974235
H12A96393215233370
H12B90794313159370
H12C102613605129770
H13A94453560-27368
H13B823841628168
H13C84182973-23768
H14A8124-1469336242
H14B7633-907430142
H16552996416653
H173805-242402794
H183634-16723285129
H195158-26912534121
H206970-2387269773
H2324922580227046
H2424032454413445
H2542762538466538
H2647655481236451
H2733235359121553
H2815485224223553
H2918975214403448
H3038835374411749
H31A49643427106842
H31B3891304880742
H32A4554680191474
H32B5263160102374
H32C407195582574
H33A49392129-530102
H33B61231332-297102
H33C59462632-294102
H34A59634237400740
H34B62913100478040
H3673445315344952
H3791545572349869
H38105354124418966
H39101292417482661
H4083542138480246
H4A77796447104258
H4B85666817578258

Experimental

Single crystals of C40H52Cl2Fe2N2O4Si2 [3094] were []. A suitable crystal was selected and [] on a Xcalibur, Sapphire3 diffractometer. The crystal was kept at 150 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 [3094]

Crystal Data for C40H52Cl2Fe2N2O4Si2 (=863.61 g/mol): triclinic, space group P-1 (no. 2), a = 12.3951(4) Å, b = 12.5719(4) Å, c = 13.6964(5) Å, α = 78.754(3)°, β = 85.109(3)°, γ = 77.113(3)°, = 2038.65(12) Å3, Z = 2, T = 150 K, μ(MoKα) = 0.944 mm-1, Dcalc = 1.407 g/cm3, 48054 reflections measured (4.242° ≤ 2Θ ≤ 51.998°), 8022 unique (Rint = 0.0435, Rsigma = 0.0316) which were used in all calculations. The final R1 was 0.0517 (I > 2σ(I)) and wR2 was 0.1337 (all data).

Refinement model description

Number of restraints - 10, 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, All O(H,H) groups
2. Restrained distances
N2-H2A = N1-H1
1 with sigma of 0.02
O2-H2 = O3-H3
1 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O4) ≈ Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4.a Free rotating group:
O4(H4A,H4B)
4.b Secondary CH2 refined with riding coordinates:
C11(H11A,H11B), C14(H14A,H14B), C31(H31A,H31B), C34(H34A,H34B)
4.c 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), C20(H20), C23(H23), C24(H24), C25(H25), C26(H26),
C27(H27), C28(H28), C29(H29), C30(H30), C36(H36), C37(H37), C38(H38),
C39(H39), C40(H40)
4.d Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C32(H32A,H32B,H32C), C33(H33A,H33B,
H33C)

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