3075

Table 1 Crystal data and structure refinement for 3075.
Identification code 3075
Empirical formula C41H50Br2Fe2N2O4Si2Zn
Formula weight 1027.90
Temperature/K 173
Crystal system triclinic
Space group P-1
a/Å 10.9344(4)
b/Å 14.4572(5)
c/Å 15.7160(6)
α/° 65.850(4)
β/° 75.359(3)
γ/° 87.591(3)
Volume/Å3 2188.05(15)
Z 2
ρcalcg/cm3 1.560
μ/mm‑1 3.120
F(000) 1044.0
Crystal size/mm3 0.08 × 0.06 × 0.05
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.628 to 53.994
Index ranges -13 ≤ h ≤ 13, -18 ≤ k ≤ 18, -20 ≤ l ≤ 19
Reflections collected 32328
Independent reflections 9491 [Rint = 0.0481, Rsigma = 0.0530]
Data/restraints/parameters 9491/2/501
Goodness-of-fit on F2 1.022
Final R indexes [I>=2σ (I)] R1 = 0.0359, wR2 = 0.0678
Final R indexes [all data] R1 = 0.0564, wR2 = 0.0754
Largest diff. peak/hole / e Å-3 0.53/-0.48

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for 3075. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Br19141.9(3)2479.8(2)4167.7(2)26.84(8)
Br212102.9(3)2641.1(2)5179.1(3)29.82(9)
Zn19870.8(3)2228.0(2)5562.8(2)17.37(8)
Fe17927.9(4)-2168.9(3)9120.6(3)18.83(10)
Fe26983.1(4)4245.2(3)8331.6(3)20.49(10)
Si19140.6(7)433.4(6)7607.5(6)15.40(17)
Si28167.3(7)2450.3(6)7354.2(6)15.77(17)
O19290.1(18)814.4(13)6465.9(14)17.5(4)
O28654.0(18)1337.8(13)7967.3(14)17.9(4)
O39129.4(17)3031.4(13)6302.1(14)17.4(4)
N17613(2)-223.9(18)6192.2(18)20.5(5)
N210721(2)4232.5(18)6507.3(18)21.6(6)
C17878(3)-627(2)8294(2)17.1(6)
C27296(3)-1248(2)7957(2)19.4(6)
C36254(3)-1866(2)8720(2)22.5(7)
C46200(3)-1659(2)9535(2)24.1(7)
C57175(3)-912(2)9279(2)19.9(6)
C69114(3)-3149(2)8732(2)30.0(8)
C78117(3)-3699(2)9561(2)28.1(8)
C88188(3)-3396(2)10298(2)29.1(8)
C99219(3)-2661(2)9931(3)32.6(8)
C109787(3)-2511(2)8971(3)30.2(8)
C117699(3)-1249(2)6971(2)22.0(7)
C128031(3)-256(2)5226(2)29.8(8)
C136331(3)153(2)6350(2)31.0(8)
C1410656(3)36.3(19)7936(2)17.0(6)
C1511672(3)-156(2)7301(2)26.0(7)
C1612732(3)-591(2)7597(3)32.3(8)
C1712802(3)-833(2)8526(3)32.2(8)
C1811817(3)-631(2)9167(2)30.4(8)
C1910769(3)-195(2)8860(2)23.6(7)
C208141(3)3168(2)8103(2)17.1(6)
C218861(3)4089(2)7876(2)20.3(6)
C228627(3)4276(2)8728(2)27.6(7)
C237759(3)3502(2)9473(2)28.4(7)
C247462(3)2820(2)9103(2)23.2(7)
C256152(4)4925(3)7220(3)45.7(10)
C266481(3)5636(3)7519(3)50.0(12)
C275829(4)5331(3)8511(3)47.1(11)
C285098(3)4423(3)8786(3)37.0(9)
C295309(3)4189(3)7994(3)38.7(9)
C309685(3)4775(2)6913(2)26.0(7)
C3111467(3)3659(3)7200(2)32.9(8)
C3211563(3)4975(2)5588(2)30.9(8)
C336540(3)2214(2)7282(2)20.0(6)
C346117(3)2716(2)6459(2)28.1(7)
C354885(3)2544(3)6440(3)37.5(9)
C364053(3)1849(3)7255(3)37.1(9)
C374448(3)1337(2)8081(3)32.8(8)
C385674(3)1510(2)8102(2)25.2(7)
O45400(4)2343(3)2672(5)157(3)
C395661(5)2795(5)3884(4)100(2)
C405978(5)2843(4)2912(5)68.3(16)
C417055(5)3581(4)2219(3)85.6(18)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for 3075. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Br139.1(2)22.25(16)20.50(17)-7.25(14)-12.48(14)1.76(13)
Br219.73(17)30.39(18)38.4(2)-17.17(16)-0.12(14)-2.64(13)
Zn120.22(18)15.62(17)14.31(18)-5.80(14)-1.58(13)0.01(13)
Fe120.7(2)13.7(2)18.5(2)-4.63(18)-2.29(18)-0.10(16)
Fe225.2(2)16.3(2)18.8(2)-7.85(19)-3.53(18)6.08(17)
Si118.8(4)12.5(4)14.3(4)-5.7(3)-3.0(3)1.3(3)
Si217.6(4)13.3(4)16.0(4)-6.7(3)-2.6(3)1.2(3)
O122.8(11)14.2(10)15(1)-5.7(9)-4.1(8)-0.5(8)
O222.5(11)14.7(10)16.7(11)-7.7(9)-3.5(8)3.3(8)
O318.6(11)15.4(10)16.3(11)-6.6(9)-1.4(8)0.6(8)
N125.8(14)19.3(13)18.8(14)-10.0(11)-6.0(11)-0.6(11)
N220.6(14)17.8(13)26.2(15)-9.6(12)-4.5(11)-0.6(10)
C120.6(15)12.4(13)16.4(15)-4.8(12)-4.2(12)5.9(11)
C222.1(16)16.8(14)20.1(16)-8.2(13)-6.2(12)3.3(12)
C317.0(16)19.1(15)29.1(18)-8.7(14)-4.2(13)0.2(12)
C421.2(16)22.4(16)21.4(17)-7.1(14)3.4(13)1.9(13)
C522.4(16)17.8(14)18.2(16)-8.9(13)-0.3(12)1.8(12)
C632.6(19)18.6(16)30.7(19)-7.1(15)-1.0(15)9.8(14)
C731.6(19)13.2(15)37(2)-7.4(15)-8.6(15)1.0(13)
C830.9(19)18.6(16)27.3(19)1.2(14)-7.3(14)-1.4(13)
C936(2)23.8(17)36(2)-4.4(16)-19.7(16)2.4(15)
C1020.6(17)19.2(16)41(2)-3.2(15)-6.4(15)2.5(13)
C1127.1(17)16.3(15)23.3(17)-9.1(13)-6.2(13)2.6(12)
C1245(2)24.9(17)22.2(18)-13.7(15)-5.8(15)-2.5(15)
C1331.1(19)31.7(18)33(2)-14.6(16)-11.9(15)7.3(15)
C1418.9(15)10.6(13)20.4(16)-6.1(12)-3.5(12)-1.4(11)
C1526.4(18)22.4(16)22.6(17)-6.7(14)1.0(13)-1.6(13)
C1619.9(17)27.6(18)38(2)-9.5(16)4.6(15)3.3(14)
C1723.4(18)20.7(16)46(2)-5.1(16)-13.7(16)2.3(13)
C1838(2)26.7(17)30.5(19)-8.8(16)-20.0(16)4.3(15)
C1927.3(18)23.5(16)24.1(17)-12.6(14)-9.1(14)5.9(13)
C2019.4(15)15.8(14)16.7(15)-8.1(13)-3.8(12)4.4(11)
C2121.3(16)17.0(14)24.8(17)-11.3(14)-5.4(13)3.3(12)
C2233.2(19)25.2(17)36(2)-20.5(16)-16.5(15)10.0(14)
C2339(2)28.9(17)20.0(17)-12.7(15)-9.4(14)14.0(15)
C2431.0(18)16.3(15)20.6(17)-6.9(13)-6.4(13)8.6(13)
C2543(2)63(3)30(2)-17(2)-13.9(18)25(2)
C2629(2)19.0(18)73(3)9(2)-11(2)5.5(15)
C2747(2)52(2)80(3)-55(2)-36(2)34(2)
C2825.6(19)40(2)35(2)-9.9(18)-1.2(15)11.1(16)
C2933(2)37(2)60(3)-28(2)-22.0(19)14.7(16)
C3022.1(17)18.1(15)37(2)-13.5(15)-2.7(14)0.9(12)
C3127.6(19)41(2)31(2)-14.3(17)-12.8(15)10.1(15)
C3233.3(19)21.0(16)32(2)-9.6(15)1.8(15)-8.3(14)
C3320.2(16)18.2(15)24.0(17)-13.1(14)-2.6(13)2.9(12)
C3428.8(18)23.7(17)30.8(19)-10.6(15)-7.0(15)1.1(14)
C3536(2)37(2)50(2)-21.1(19)-25.1(18)10.0(16)
C3620.6(18)42(2)60(3)-33(2)-11.0(17)4.5(15)
C3721.8(18)34.8(19)42(2)-22.9(18)5.6(15)-7.8(14)
C3824.1(17)27.8(17)25.3(18)-15.3(15)-1.3(13)-0.5(13)
O4119(4)134(4)366(8)-194(5)-167(5)90(3)
C3943(3)148(6)74(4)-10(4)-19(3)9(3)
C4056(3)60(3)132(5)-61(3)-65(3)36(2)
C4175(4)134(5)49(3)-36(3)-28(3)43(4)

 

Table 4 Bond Lengths for 3075.
AtomAtomLength/Å AtomAtomLength/Å
Br1Zn12.4043(5) C1C21.448(4)
Br2Zn12.4001(4) C1C51.436(4)
Zn1O11.9683(18) C2C31.433(4)
Zn1O31.9763(18) C2C111.499(4)
Fe1C12.077(3) C3C41.416(4)
Fe1C22.040(3) C4C51.411(4)
Fe1C32.056(3) C6C71.422(4)
Fe1C42.047(3) C6C101.419(5)
Fe1C52.045(3) C7C81.415(5)
Fe1C62.053(3) C8C91.415(4)
Fe1C72.048(3) C9C101.407(5)
Fe1C82.046(3) C14C151.395(4)
Fe1C92.051(3) C14C191.387(4)
Fe1C102.050(3) C15C161.387(4)
Fe2C202.054(3) C16C171.378(5)
Fe2C212.032(3) C17C181.387(5)
Fe2C222.053(3) C18C191.384(4)
Fe2C232.052(3) C20C211.442(4)
Fe2C242.043(3) C20C241.439(4)
Fe2C252.041(4) C21C221.431(4)
Fe2C262.034(3) C21C301.498(4)
Fe2C272.038(3) C22C231.407(4)
Fe2C282.046(3) C23C241.417(4)
Fe2C292.044(4) C25C261.386(6)
Si1O11.612(2) C25C291.385(5)
Si1O21.6452(19) C26C271.426(6)
Si1C11.869(3) C27C281.414(5)
Si1C141.858(3) C28C291.382(5)
Si2O21.6485(19) C33C341.386(4)
Si2O31.614(2) C33C381.409(4)
Si2C201.855(3) C34C351.389(4)
Si2C331.865(3) C35C361.383(5)
N1C111.505(4) C36C371.375(5)
N1C121.490(4) C37C381.386(4)
N1C131.482(4) O4C401.203(5)
N2C301.508(4) C39C401.450(7)
N2C311.480(4) C40C411.489(7)
N2C321.493(4)    

 

Table 5 Bond Angles for 3075.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
Br2Zn1Br1112.892(17) O3Si2C20110.16(12)
O1Zn1Br1104.44(6) O3Si2C33112.33(12)
O1Zn1Br2115.43(6) C20Si2C33111.24(13)
O1Zn1O3104.07(8) Si1O1Zn1121.07(11)
O3Zn1Br1117.36(6) Si1O2Si2128.44(13)
O3Zn1Br2102.78(6) Si2O3Zn1118.34(10)
C2Fe1C141.18(11) C12N1C11110.2(2)
C2Fe1C340.96(11) C13N1C11112.4(2)
C2Fe1C468.49(12) C13N1C12111.4(3)
C2Fe1C568.27(12) C31N2C30112.7(3)
C2Fe1C6108.30(13) C31N2C32110.7(3)
C2Fe1C7126.06(13) C32N2C30109.9(2)
C2Fe1C8163.01(12) Si1C1Fe1132.69(15)
C2Fe1C9155.29(12) C2C1Fe168.05(15)
C2Fe1C10121.09(13) C2C1Si1129.6(2)
C3Fe1C169.10(11) C5C1Fe168.41(15)
C4Fe1C168.85(11) C5C1Si1124.8(2)
C4Fe1C340.37(12) C5C1C2105.3(2)
C4Fe1C6154.53(13) C1C2Fe170.77(16)
C4Fe1C7119.51(12) C1C2C11126.2(3)
C4Fe1C9125.63(14) C3C2Fe170.11(17)
C4Fe1C10163.01(14) C3C2C1108.9(3)
C5Fe1C140.77(11) C3C2C11124.9(3)
C5Fe1C367.90(12) C11C2Fe1125.5(2)
C5Fe1C440.35(11) C2C3Fe168.93(17)
C5Fe1C6164.00(12) C4C3Fe169.48(17)
C5Fe1C7154.06(12) C4C3C2107.7(3)
C5Fe1C8119.89(13) C3C4Fe170.15(16)
C5Fe1C9108.15(13) C5C4Fe169.74(16)
C5Fe1C10126.73(12) C5C4C3108.2(3)
C6Fe1C1126.42(12) C1C5Fe170.82(15)
C6Fe1C3120.52(13) C4C5Fe169.92(16)
C7Fe1C1163.81(12) C4C5C1110.0(3)
C7Fe1C3107.51(12) C7C6Fe169.52(17)
C7Fe1C640.57(12) C10C6Fe169.62(18)
C7Fe1C968.08(13) C10C6C7107.4(3)
C7Fe1C1067.96(12) C6C7Fe169.91(17)
C8Fe1C1154.33(13) C8C7Fe169.71(17)
C8Fe1C3125.32(12) C8C7C6107.8(3)
C8Fe1C4107.26(13) C7C8Fe169.84(18)
C8Fe1C668.02(13) C9C8Fe169.95(18)
C8Fe1C740.45(13) C9C8C7108.3(3)
C8Fe1C940.42(12) C8C9Fe169.63(19)
C8Fe1C1067.68(13) C10C9Fe169.89(19)
C9Fe1C1119.93(12) C10C9C8107.8(3)
C9Fe1C3162.41(13) C6C10Fe169.90(18)
C9Fe1C668.01(14) C9C10Fe169.97(18)
C10Fe1C1108.24(12) C9C10C6108.6(3)
C10Fe1C3155.76(14) C2C11N1111.9(2)
C10Fe1C640.47(13) C15C14Si1121.2(2)
C10Fe1C940.14(13) C19C14Si1121.1(2)
C21Fe2C2041.33(11) C19C14C15117.3(3)
C21Fe2C2241.01(12) C16C15C14121.0(3)
C21Fe2C2368.53(12) C17C16C15120.3(3)
C21Fe2C2468.60(12) C16C17C18120.0(3)
C21Fe2C25112.87(14) C19C18C17119.0(3)
C21Fe2C26111.60(13) C18C19C14122.4(3)
C21Fe2C27138.69(14) Si2C20Fe2131.84(16)
C21Fe2C28179.20(13) C21C20Fe268.54(15)
C21Fe2C29140.87(14) C21C20Si2129.4(2)
C22Fe2C2069.18(11) C24C20Fe269.05(15)
C23Fe2C2069.14(12) C24C20Si2124.5(2)
C23Fe2C2240.08(13) C24C20C21105.7(2)
C24Fe2C2041.11(11) C20C21Fe270.13(16)
C24Fe2C2267.86(12) C20C21C30127.0(3)
C24Fe2C2340.48(12) C22C21Fe270.27(17)
C24Fe2C28112.06(13) C22C21C20108.5(3)
C24Fe2C29111.08(14) C22C21C30124.4(3)
C25Fe2C20110.21(14) C30C21Fe2123.7(2)
C25Fe2C22142.48(15) C21C22Fe268.72(17)
C25Fe2C23177.24(15) C23C22Fe269.90(19)
C25Fe2C24137.36(15) C23C22C21108.3(3)
C25Fe2C2867.01(15) C22C23Fe270.02(18)
C25Fe2C2939.64(15) C22C23C24108.2(3)
C26Fe2C20137.20(15) C24C23Fe269.44(18)
C26Fe2C22114.31(14) C20C24Fe269.84(16)
C26Fe2C23142.41(16) C23C24Fe270.08(17)
C26Fe2C24177.10(17) C23C24C20109.3(3)
C26Fe2C2539.76(16) C26C25Fe269.9(2)
C26Fe2C2741.01(16) C29C25Fe270.3(2)
C26Fe2C2867.76(14) C29C25C26108.3(4)
C26Fe2C2966.82(15) C25C26Fe270.4(2)
C27Fe2C20178.00(15) C25C26C27108.0(3)
C27Fe2C22112.08(13) C27C26Fe269.6(2)
C27Fe2C23112.85(14) C26C27Fe269.34(19)
C27Fe2C24140.62(16) C28C27Fe270.05(18)
C27Fe2C2567.82(16) C28C27C26106.4(3)
C27Fe2C2840.50(15) C27C28Fe269.45(19)
C27Fe2C2967.32(14) C29C28Fe270.2(2)
C28Fe2C20139.47(13) C29C28C27108.0(3)
C28Fe2C22138.64(14) C25C29Fe270.1(2)
C28Fe2C23111.62(14) C28C29Fe270.3(2)
C29Fe2C20111.48(12) C28C29C25109.2(3)
C29Fe2C22177.70(15) C21C30N2112.7(2)
C29Fe2C23137.83(15) C34C33Si2123.2(2)
C29Fe2C2839.51(14) C34C33C38117.3(3)
O1Si1O2111.04(10) C38C33Si2119.4(2)
O1Si1C1109.55(12) C33C34C35121.7(3)
O1Si1C14112.15(12) C36C35C34119.9(3)
O2Si1C1105.51(11) C37C36C35119.7(3)
O2Si1C14107.63(11) C36C37C38120.5(3)
C14Si1C1110.75(12) C37C38C33120.9(3)
O2Si2C20104.00(12) O4C40C39122.9(6)
O2Si2C33107.08(11) O4C40C41122.0(6)
O3Si2O2111.70(10) C39C40C41115.1(4)

 

Table 6 Hydrogen Bonds for 3075.
DHAd(D-H)/Åd(H-A)/Åd(D-A)/ÅD-H-A/°
N1H1O10.998(18)1.657(19)2.638(3)166(3)
N2H2O30.984(18)1.71(2)2.673(3)165(3)

 

Table 7 Torsion Angles for 3075.
ABCDAngle/˚ ABCDAngle/˚
Fe1C1C2C360.0(2) C3C2C11N1118.9(3)
Fe1C1C2C11-120.4(3) C3C4C5Fe1-59.8(2)
Fe1C1C5C4-59.1(2) C3C4C5C1-0.2(3)
Fe1C2C3C458.9(2) C5C1C2Fe1-58.59(18)
Fe1C2C11N1-151.8(2) C5C1C2C31.4(3)
Fe1C3C4C559.6(2) C5C1C2C11-179.0(3)
Fe1C4C5C159.7(2) C6C7C8Fe159.8(2)
Fe1C6C7C8-59.6(2) C6C7C8C90.1(3)
Fe1C6C10C959.5(2) C7C6C10Fe1-59.5(2)
Fe1C7C8C9-59.6(2) C7C6C10C90.0(3)
Fe1C8C9C10-59.7(2) C7C8C9Fe159.5(2)
Fe1C9C10C6-59.4(2) C7C8C9C10-0.1(4)
Fe2C20C21C2260.1(2) C8C9C10Fe159.5(2)
Fe2C20C21C30-117.8(3) C8C9C10C60.1(4)
Fe2C20C24C23-59.1(2) C10C6C7Fe159.5(2)
Fe2C21C22C2358.9(2) C10C6C7C8-0.1(3)
Fe2C21C30N2-147.2(2) C11C2C3Fe1120.0(3)
Fe2C22C23C2459.2(2) C11C2C3C4178.9(3)
Fe2C23C24C2059.0(2) C12N1C11C2179.6(2)
Fe2C25C26C27-59.7(2) C13N1C11C2-55.5(3)
Fe2C25C29C2859.6(2) C14Si1O1Zn1-85.28(14)
Fe2C26C27C28-60.6(2) C14Si1O2Si2131.26(16)
Fe2C27C28C29-59.8(2) C14Si1C1Fe1-12.8(2)
Fe2C28C29C25-59.5(3) C14Si1C1C2-108.7(3)
Si1C1C2Fe1128.0(2) C14Si1C1C579.0(3)
Si1C1C2C3-172.0(2) C14C15C16C17-0.5(5)
Si1C1C2C117.5(4) C15C14C19C18-2.1(4)
Si1C1C5Fe1-127.8(2) C15C16C17C18-0.8(5)
Si1C1C5C4173.1(2) C16C17C18C190.6(5)
Si1C14C15C16-170.7(2) C17C18C19C140.9(5)
Si1C14C19C18170.5(2) C19C14C15C161.9(4)
Si2C20C21Fe2127.2(2) C20Si2O2Si1-167.09(15)
Si2C20C21C22-172.7(2) C20Si2O3Zn1155.77(12)
Si2C20C21C309.5(5) C20Si2C33C34107.2(3)
Si2C20C24Fe2-127.1(2) C20Si2C33C38-71.4(2)
Si2C20C24C23173.8(2) C20C21C22Fe2-60.0(2)
Si2C33C34C35-178.0(2) C20C21C22C23-1.1(3)
Si2C33C38C37178.3(2) C20C21C30N2-57.7(4)
O1Si1O2Si28.16(19) C21C20C24Fe259.00(19)
O1Si1C1Fe1111.4(2) C21C20C24C23-0.1(3)
O1Si1C1C215.5(3) C21C22C23Fe2-58.2(2)
O1Si1C1C5-156.8(2) C21C22C23C241.0(3)
O1Si1C14C15-15.9(3) C22C21C30N2124.8(3)
O1Si1C14C19171.8(2) C22C23C24Fe2-59.5(2)
O2Si1O1Zn135.18(15) C22C23C24C20-0.6(3)
O2Si1C1Fe1-128.99(19) C24C20C21Fe2-59.33(19)
O2Si1C1C2135.1(2) C24C20C21C220.7(3)
O2Si1C1C5-37.2(3) C24C20C21C30-177.1(3)
O2Si1C14C15-138.3(2) C25C26C27Fe260.2(2)
O2Si1C14C1949.4(3) C25C26C27C28-0.4(4)
O2Si2O3Zn140.72(15) C26C25C29Fe2-59.8(3)
O2Si2C20Fe2-146.78(18) C26C25C29C28-0.1(4)
O2Si2C20C21117.4(3) C26C27C28Fe260.1(2)
O2Si2C20C24-54.9(3) C26C27C28C290.3(4)
O2Si2C33C34-139.7(2) C27C28C29Fe259.3(2)
O2Si2C33C3841.7(2) C27C28C29C25-0.1(4)
O3Si2O2Si1-48.31(18) C29C25C26Fe260.0(3)
O3Si2C20Fe293.4(2) C29C25C26C270.3(4)
O3Si2C20C21-2.4(3) C30C21C22Fe2117.9(3)
O3Si2C20C24-174.7(2) C30C21C22C23176.8(3)
O3Si2C33C34-16.8(3) C31N2C30C21-51.5(3)
O3Si2C33C38164.6(2) C32N2C30C21-175.6(3)
C1Si1O1Zn1151.33(12) C33Si2O2Si175.06(18)
C1Si1O2Si2-110.45(16) C33Si2O3Zn1-79.62(14)
C1Si1C14C15106.9(2) C33Si2C20Fe2-31.8(2)
C1Si1C14C19-65.4(3) C33Si2C20C21-127.6(3)
C1C2C3Fe1-60.41(19) C33Si2C20C2460.0(3)
C1C2C3C4-1.5(3) C33C34C35C36-0.6(5)
C1C2C11N1-60.6(4) C34C33C38C37-0.4(4)
C2C1C5Fe158.35(18) C34C35C36C370.4(5)
C2C1C5C4-0.8(3) C35C36C37C38-0.2(5)
C2C3C4Fe1-58.5(2) C36C37C38C330.2(5)
C2C3C4C51.0(3) C38C33C34C350.6(4)

 

Table 8 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for 3075.
AtomxyzU(eq)
H18210(30)260(20)6220(20)38(10)
H210250(30)3730(20)6420(30)54(11)
H35700-2331868627
H45608-19701014729
H57342-638969824
H69295-3200813036
H77512-4183961034
H87638-36431093035
H99481-23281027339
H1010502-2058855236
H11A7154-1760694426
H11B8583-1447685426
H12A8891-487513545
H12B8025425472345
H12C7452-727518645
H13A5718-314633847
H13B6329830583847
H13C6098193697847
H151163713665731
H1613411-722715639
H1713524-1138872839
H1811862-790980736
H1910101-49929728
H2289944828878133
H23742934461011434
H2469032226946028
H2564534939659255
H2670436224713160
H2758765671890757
H2845574040940844
H2949353614798246
H30A100735342697731
H30B91535070645431
H31A118754129736649
H31B121173313690549
H31C109043154778549
H32A110525347514146
H32B121854610529746
H32C120055455572346
H3466833191589334
H3546162902586845
H3632121725724444
H373876860864139
H3859351149867830
H39A546734713862150
H39B638025644166150
H39C492023174279150
H41A729834781621128
H41B777834752504128
H41C679842752076128

Experimental

Single crystals of C41H50Br2Fe2N2O4Si2Zn [3075] were []. A suitable crystal was selected and [] on a Xcalibur, Sapphire3 diffractometer. The crystal was kept at 173 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 [3075]

Crystal Data for C41H50Br2Fe2N2O4Si2Zn (=1027.90 g/mol): triclinic, space group P-1 (no. 2), a = 10.9344(4) Å, b = 14.4572(5) Å, c = 15.7160(6) Å, α = 65.850(4)°, β = 75.359(3)°, γ = 87.591(3)°, = 2188.05(15) Å3, Z = 2, T = 173 K, μ(MoKα) = 3.120 mm-1, Dcalc = 1.560 g/cm3, 32328 reflections measured (4.628° ≤ 2Θ ≤ 53.994°), 9491 unique (Rint = 0.0481, Rsigma = 0.0530) which were used in all calculations. The final R1 was 0.0359 (I > 2σ(I)) and wR2 was 0.0754 (all data).

Refinement model description

Number of restraints - 2, 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. Restrained distances
N1-H1 = N2-H2
1 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
C11(H11A,H11B), C30(H30A,H30B)
3.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)
3.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), C41(H41A,H41B,H41C)

This report has been created with Olex2, compiled on 2017.01.04 svn.r3372 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.