mo_B0662_0m

Table 1 Crystal data and structure refinement for mo_B0662_0m.
Identification code mo_B0662_0m
Empirical formula C26H34Br2Fe2N2O2SiZn
Formula weight 771.53
Temperature/K 99.99
Crystal system monoclinic
Space group P21
a/Å 9.8916(13)
b/Å 14.438(2)
c/Å 20.415(3)
α/° 90
β/° 102.936(5)
γ/° 90
Volume/Å3 2841.6(7)
Z 4
ρcalcg/cm3 1.803
μ/mm‑1 4.726
F(000) 1544.0
Crystal size/mm3 0.218 × 0.175 × 0.109
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.224 to 59.342
Index ranges -13 ≤ h ≤ 13, -20 ≤ k ≤ 20, -28 ≤ l ≤ 28
Reflections collected 59808
Independent reflections 16000 [Rint = 0.0281, Rsigma = 0.0248]
Data/restraints/parameters 16000/1/667
Goodness-of-fit on F2 1.045
Final R indexes [I>=2σ (I)] R1 = 0.0294, wR2 = 0.0722
Final R indexes [all data] R1 = 0.0328, wR2 = 0.0741
Largest diff. peak/hole / e Å-3 0.94/-0.30
Flack parameter-0.004(2)

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for mo_B0662_0m. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Br1-870.9(4)20063.4(4)8276.4(3)43.12(11)
Br2-896.2(4)18133.7(3)9782.2(2)34.70(9)
Zn1203.0(4)18792.6(3)8970.5(2)27.91(10)
Fe14176.3(5)18220.2(4)7567.6(2)27.44(11)
Fe25751.6(5)21122.6(4)9589.9(3)25.65(10)
Si13231(1)19412.1(7)8923.3(5)24.81(18)
O12099(2)19130.0(19)9353.4(13)27.3(5)
O22578(3)20211(2)8361.4(13)31.3(5)
N1320(3)17709(2)8306.0(16)31.1(7)
N22557(3)19927(2)10530.8(16)29.1(6)
C13670(4)18356(3)8488.8(17)26.1(7)
C22668(4)17796(3)8030.2(18)28.0(7)
C33378(4)17009(3)7829.6(19)29.6(7)
C44791(4)17078(3)8142.5(18)30.1(7)
C54987(4)17891(3)8550.1(18)28.5(7)
C64163(6)19496(4)7155(3)54.4(13)
C73227(5)18906(4)6713(2)51.9(13)
C83986(4)18158(4)6545(2)45.4(10)
C95390(4)18275(3)6881(2)39.7(9)
C105525(5)19095(4)7259(2)45.0(11)
C111138(4)17957(3)7792.5(18)31.5(8)
C12884(4)16884(3)8700(2)36.2(9)
C13-1127(4)17516(4)7946(2)44.6(11)
C144752(3)19871(3)9546.6(18)25.6(7)
C154635(4)20408(3)10133.0(17)26.5(7)
C165995(4)20578(3)10533.0(18)27.9(7)
C176973(4)20174(3)10205.1(18)29.4(7)
C186223(4)19742(3)9605.7(19)28.1(7)
C195243(7)21681(4)8655(3)61.2(16)
C204577(6)22144(4)9073(4)69(2)
C215572(10)22517(4)9596(3)80(3)
C226882(6)22271(4)9492(3)69(2)
C236643(7)21755(4)8905(3)63.0(17)
C243318(4)20730(3)10296.8(19)28.8(7)
C251190(4)20235(3)10637(2)39.1(9)
C263378(4)19465(3)11141(2)33.8(8)
Br35942.7(4)15298.2(3)6567.8(2)39.12(10)
Br46067.6(4)13082.0(3)5291.7(2)35.16(9)
Zn24927.2(4)13885.9(3)6023.3(2)26.79(9)
Fe3893.1(5)13500.7(4)7403.7(3)27.66(11)
Fe4-700.1(5)16155.2(4)5304.4(3)25.2(1)
Si21897.1(9)14516.9(7)6029.2(5)23.70(18)
O32556(3)15338(2)6573.5(13)29.3(5)
O43045(3)14213.2(18)5615.3(13)26.4(5)
N34889(3)12950(2)6809.3(16)31.5(7)
N42484(3)14869(2)4393.9(15)27.5(6)
C271471(4)13496(3)6502.5(17)25.1(6)
C282486(3)13031(3)7024.3(18)27.8(7)
C291813(4)12265(3)7276.7(19)32.3(8)
C30415(4)12255(3)6926.3(19)31.1(7)
C31189(4)12996(3)6451.3(18)28.1(7)
C32611(4)14862(3)7601(2)40.4(9)
C331709(5)14482(4)8095(2)46.9(11)
C341172(5)13740(4)8415(2)50.1(13)
C35-270(5)13658(4)8107(2)41.7(10)
C36-610(4)14354(3)7614(2)37.4(9)
C373992(4)13269(3)7272.6(18)29.8(7)
C384477(5)12017(3)6536(2)42(1)
C396342(4)12920(4)7207(2)43.8(11)
C40353(4)14920(3)5392.7(17)25.2(6)
C41410(4)15400(3)4777.2(17)26.2(7)
C42-969(4)15525(3)4388.7(18)29.0(7)
C43-1903(4)15142(3)4755.2(19)30.6(7)
C44-1100(4)14773(3)5365.7(19)28.8(7)
C45276(4)16992(3)6073(2)34.1(8)
C46132(5)17460(3)5450(2)37.6(9)
C47-1298(5)17504(3)5144(2)39.6(9)
C48-2055(4)17067(3)5570(2)38.4(9)
C49-1072(4)16752(3)6151(2)35.6(8)
C501701(4)15701(3)4572.2(19)29.2(7)
C513843(4)15148(3)4262(2)36.2(9)
C521658(4)14335(3)3821(2)32.7(8)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for mo_B0662_0m. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Br132.13(18)42.8(3)51.3(3)8.4(2)2.65(17)5.49(17)
Br232.68(17)38.8(2)35.65(19)-0.37(17)14.17(14)2.01(17)
Zn124.89(18)30.0(2)28.8(2)-3.11(17)5.92(15)-0.52(16)
Fe127.1(2)32.1(3)23.5(2)2.5(2)6.54(18)-1.2(2)
Fe226.8(2)24.2(2)25.4(2)0.9(2)4.64(18)-1.21(19)
Si125.0(4)25.0(5)23.8(4)-0.5(4)4.1(3)-0.2(4)
O125.6(11)29.8(13)27.1(12)-2.3(10)7.1(9)-2.9(10)
O231.2(12)30.8(14)29.9(13)4.2(11)2.7(10)1.7(11)
N125.2(13)36.7(18)32.1(16)-6.0(14)7.8(12)-4.9(12)
N228.4(14)30.9(16)29.4(15)-5.1(13)9.1(12)-1.0(12)
C128.6(15)27.2(18)22.5(15)2.0(13)5.7(12)-1.3(13)
C231.7(16)29.7(18)23.9(16)-3.8(13)8.9(13)-4.9(14)
C334.8(18)28.9(18)26.8(17)-2.1(14)10.6(14)-3.5(15)
C435.3(18)31.3(19)25.5(17)0.3(14)10.3(14)0.4(15)
C528.8(16)29.5(18)26.6(16)2.6(14)4.9(13)-0.5(13)
C687(4)38(2)50(3)17(2)39(3)9(3)
C745(2)70(4)40(2)27(2)8.6(19)5(2)
C846(2)64(3)27.6(18)5(2)9.5(16)-10(2)
C937.8(19)52(3)33(2)5.9(19)14.7(16)-2.2(19)
C1048(2)52(3)37(2)8(2)13.4(18)-16(2)
C1127.1(15)41(2)26.3(17)-7.0(15)6.4(13)-5.5(15)
C1241(2)29.8(19)44(2)-7.4(17)20.8(17)-6.6(16)
C1329.7(18)63(3)41(2)-18(2)7.8(16)-13.7(19)
C1424.6(14)25.2(17)26.5(16)1.1(13)4.3(12)-0.3(13)
C1529.8(15)23.5(16)26.0(16)1.5(14)5.7(13)-2.1(13)
C1629.8(16)26.6(17)25.6(16)-0.2(13)2.4(13)-0.8(13)
C1726.6(15)30.0(19)29.4(17)1.0(14)1.8(13)0.1(14)
C1827.8(16)26.5(17)30.0(17)0.2(14)6.3(13)0.6(13)
C1992(4)42(3)37(3)13(2)-11(3)-17(3)
C2045(3)53(3)112(5)51(4)24(3)14(2)
C21180(8)23(2)57(3)5(2)67(5)0(3)
C2267(3)65(4)57(3)35(3)-22(3)-39(3)
C2384(4)49(3)73(4)30(3)52(3)24(3)
C2429.5(16)25.9(17)31.0(18)-1.8(14)7.1(13)0.7(14)
C2531.2(17)47(2)43(2)-4.5(19)16.0(16)3.7(17)
C2641(2)32.3(19)29.2(18)0.8(15)10.0(15)0.5(16)
Br330.11(17)35.2(2)49.6(2)-4.38(18)3.78(15)-4.54(15)
Br433.58(17)39.1(2)36.03(19)-1.70(17)14.73(14)0.52(17)
Zn224.89(17)28.5(2)27.3(2)2.06(17)6.45(15)0.77(16)
Fe325.6(2)34.7(3)23.1(2)-1.5(2)6.21(18)1.4(2)
Fe426.6(2)24.0(2)24.3(2)0.0(2)4.27(18)1.83(19)
Si224.5(4)22.8(4)23.4(4)-0.4(4)4.4(3)0.1(3)
O329.6(12)27.2(13)29.9(12)-4.8(11)4.2(10)-1.6(10)
O426.1(11)27.3(13)26.0(12)0.6(10)6.0(9)0.6(10)
N326.3(13)35.2(18)34.1(16)7.5(13)8.8(12)5.9(13)
N429.3(14)29.5(16)24.8(14)1.5(12)8.0(12)-1.0(12)
C2728.5(15)23.9(15)23.3(15)-0.7(13)6.8(12)1.8(13)
C2828.2(15)29.3(18)27.0(16)2.4(14)8.5(13)4.0(14)
C2935.9(18)32.4(19)30.4(18)6.1(15)11.4(15)4.5(16)
C3034.9(18)30.3(19)29.0(18)2.1(15)9.3(14)-1.0(15)
C3129.2(15)26.6(18)27.8(16)-0.8(14)5.2(13)-1.9(14)
C3241(2)43(2)39(2)-14.2(19)13.0(17)-1.0(18)
C3336(2)63(3)42(2)-25(2)8.9(18)-1(2)
C3448(2)74(4)26.8(19)-5(2)5.3(17)17(2)
C3542(2)54(3)33(2)-1.7(19)16.2(17)7(2)
C3631.7(17)44(2)37(2)-9.8(18)10.4(15)4.2(17)
C3727.3(15)35(2)27.5(17)4.0(15)6.2(13)4.0(14)
C3852(2)29(2)53(3)7.0(18)29(2)7.0(18)
C3928.2(17)60(3)44(2)19(2)8.9(16)7.0(18)
C4026.7(15)23.7(16)24.7(16)-0.7(13)4.7(12)0.4(13)
C4128.2(15)24.7(16)26.0(16)-2.2(14)6.4(13)1.0(13)
C4231.4(16)29.9(19)23.8(16)-1.1(14)2.0(13)2.2(14)
C4328.1(16)32.3(19)29.5(17)-0.8(15)2.2(13)-0.3(14)
C4428.9(16)26.2(17)31.1(18)0.9(14)5.9(14)-0.3(13)
C4537.5(19)28.7(19)34(2)-7.7(16)2.8(15)0.9(15)
C4650(2)24.9(18)43(2)-5.7(16)19.4(19)-3.9(16)
C4756(2)28.2(19)32(2)0.8(16)3.8(18)10.3(18)
C4834.7(19)35(2)44(2)-9.1(18)6.4(16)5.9(17)
C4945(2)32(2)31.4(19)-4.0(16)13.2(16)2.5(17)
C5032.3(17)25.4(17)30.0(18)1.5(14)7.1(14)-1.1(14)
C5134.7(18)38(2)39(2)0.7(17)15.9(16)-3.4(16)
C5240.5(19)29.0(19)29.5(18)-2.9(15)9.8(15)-1.1(15)

 

Table 4 Bond Lengths for mo_B0662_0m.
AtomAtomLength/Å AtomAtomLength/Å
Br1Zn12.4143(7) Br3Zn22.4295(7)
Br2Zn12.3747(6) Br4Zn22.3675(6)
Zn1O11.926(3) Zn2O41.921(3)
Zn1N12.091(3) Zn2N32.105(3)
Fe1C12.061(3) Fe3C272.045(3)
Fe1C22.030(4) Fe3C282.022(3)
Fe1C32.039(4) Fe3C292.045(4)
Fe1C42.037(4) Fe3C302.051(4)
Fe1C52.043(4) Fe3C312.047(4)
Fe1C62.023(5) Fe3C322.038(5)
Fe1C72.043(5) Fe3C332.034(5)
Fe1C82.056(4) Fe3C342.049(4)
Fe1C92.041(4) Fe3C352.044(4)
Fe1C102.036(4) Fe3C362.049(4)
Fe2C142.053(4) Fe4C402.053(4)
Fe2C152.016(4) Fe4C412.020(4)
Fe2C162.043(4) Fe4C422.042(4)
Fe2C172.057(4) Fe4C432.054(4)
Fe2C182.045(4) Fe4C442.044(4)
Fe2C192.028(5) Fe4C452.043(4)
Fe2C202.022(5) Fe4C462.050(4)
Fe2C212.022(5) Fe4C472.040(4)
Fe2C222.034(5) Fe4C482.037(4)
Fe2C232.030(5) Fe4C492.036(4)
Si1O11.622(3) Si2O31.655(3)
Si1O21.652(3) Si2O41.620(3)
Si1C11.864(4) Si2C271.862(4)
Si1C141.861(4) Si2C401.863(4)
N1C111.504(5) N3C371.506(5)
N1C121.475(6) N3C381.479(6)
N1C131.481(5) N3C391.485(5)
N2C241.517(5) N4C501.517(5)
N2C251.484(5) N4C511.485(5)
N2C261.484(5) N4C521.484(5)
C1C21.448(5) C27C281.455(5)
C1C51.446(5) C27C311.442(5)
C2C31.442(5) C28C291.444(5)
C2C111.501(5) C28C371.502(5)
C3C41.404(5) C29C301.408(5)
C4C51.426(5) C30C311.428(5)
C6C71.422(8) C32C331.416(7)
C6C101.438(7) C32C361.418(6)
C7C81.401(8) C33C341.419(8)
C8C91.415(6) C34C351.429(6)
C9C101.404(7) C35C361.409(7)
C14C151.453(5) C40C411.448(5)
C14C181.445(5) C40C441.442(5)
C15C161.430(5) C41C421.428(5)
C15C241.490(5) C41C501.495(5)
C16C171.419(5) C42C431.425(5)
C17C181.424(5) C43C441.423(5)
C19C201.364(9) C45C461.418(6)
C19C231.369(9) C45C491.421(6)
C20C211.389(10) C46C471.414(6)
C21C221.405(10) C47C481.417(7)
C22C231.385(9) C48C491.429(6)

 

Table 5 Bond Angles for mo_B0662_0m.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
Br2Zn1Br1120.26(2) Br4Zn2Br3119.57(2)
O1Zn1Br1107.85(8) O4Zn2Br3104.67(8)
O1Zn1Br2112.00(8) O4Zn2Br4113.55(8)
O1Zn1N1105.21(12) O4Zn2N3107.92(11)
N1Zn1Br1105.60(10) N3Zn2Br3105.45(10)
N1Zn1Br2104.66(10) N3Zn2Br4104.97(9)
C2Fe1C141.43(14) C27Fe3C2970.20(15)
C2Fe1C341.52(15) C27Fe3C3069.56(15)
C2Fe1C469.10(15) C27Fe3C3141.28(14)
C2Fe1C568.95(15) C27Fe3C34154.81(18)
C2Fe1C7107.36(17) C27Fe3C36123.52(16)
C2Fe1C8123.33(16) C28Fe3C2741.91(14)
C2Fe1C9159.62(17) C28Fe3C2941.57(15)
C2Fe1C10158.61(19) C28Fe3C3068.91(15)
C3Fe1C169.79(15) C28Fe3C3169.23(14)
C3Fe1C568.44(15) C28Fe3C32123.51(17)
C3Fe1C7120.6(2) C28Fe3C33106.08(17)
C3Fe1C8106.03(19) C28Fe3C34120.11(17)
C3Fe1C9122.36(18) C28Fe3C35156.34(17)
C4Fe1C169.70(15) C28Fe3C36161.09(17)
C4Fe1C340.30(15) C29Fe3C3040.21(15)
C4Fe1C540.93(15) C29Fe3C3168.63(15)
C4Fe1C7154.9(2) C29Fe3C34108.13(19)
C4Fe1C8119.8(2) C29Fe3C36156.26(17)
C4Fe1C9106.36(17) C31Fe3C3040.80(15)
C4Fe1C10123.28(19) C31Fe3C34163.1(2)
C5Fe1C141.26(14) C31Fe3C36107.72(16)
C5Fe1C7162.9(2) C32Fe3C27105.01(17)
C5Fe1C8156.00(18) C32Fe3C29161.93(17)
C6Fe1C1108.23(18) C32Fe3C30155.92(17)
C6Fe1C2122.05(19) C32Fe3C31119.90(17)
C6Fe1C3157.3(2) C32Fe3C3468.4(2)
C6Fe1C4161.8(2) C32Fe3C3568.31(19)
C6Fe1C5125.8(2) C32Fe3C3640.61(17)
C6Fe1C740.9(2) C33Fe3C27118.58(18)
C6Fe1C868.1(2) C33Fe3C29125.21(18)
C6Fe1C968.2(2) C33Fe3C30162.59(19)
C6Fe1C1041.5(2) C33Fe3C31154.7(2)
C7Fe1C1125.05(19) C33Fe3C3240.70(19)
C7Fe1C840.0(2) C33Fe3C3440.7(2)
C8Fe1C1160.93(16) C33Fe3C3568.54(19)
C9Fe1C1157.44(16) C33Fe3C3668.28(18)
C9Fe1C5121.43(16) C34Fe3C30126.2(2)
C9Fe1C767.86(19) C34Fe3C3668.17(18)
C9Fe1C840.39(16) C35Fe3C27161.26(16)
C10Fe1C1122.21(17) C35Fe3C29121.50(18)
C10Fe1C3158.76(19) C35Fe3C30108.97(18)
C10Fe1C5107.92(17) C35Fe3C31125.54(17)
C10Fe1C769.1(2) C35Fe3C3440.87(18)
C10Fe1C868.32(19) C35Fe3C3640.27(18)
C10Fe1C940.3(2) C36Fe3C30121.75(17)
C14Fe2C1769.59(14) C40Fe4C4369.49(15)
C15Fe2C1441.83(14) C41Fe4C4041.62(14)
C15Fe2C1641.25(14) C41Fe4C4241.14(14)
C15Fe2C1769.05(15) C41Fe4C4369.05(15)
C15Fe2C1869.12(15) C41Fe4C4469.00(15)
C15Fe2C19132.1(2) C41Fe4C45120.54(16)
C15Fe2C20109.82(19) C41Fe4C46108.93(16)
C15Fe2C21116.5(2) C41Fe4C47126.99(17)
C15Fe2C22148.5(2) C41Fe4C48163.52(17)
C15Fe2C23170.2(2) C41Fe4C49154.59(16)
C16Fe2C1469.86(14) C42Fe4C4069.70(14)
C16Fe2C1740.49(14) C42Fe4C4340.71(15)
C16Fe2C1868.41(15) C42Fe4C4468.51(15)
C18Fe2C1441.28(14) C42Fe4C45155.30(17)
C18Fe2C1740.63(15) C42Fe4C46120.51(17)
C19Fe2C14107.08(19) C44Fe4C4041.21(14)
C19Fe2C16172.5(2) C44Fe4C4340.64(15)
C19Fe2C17145.8(2) C44Fe4C46164.81(17)
C19Fe2C18114.2(2) C45Fe4C40107.63(16)
C19Fe2C2267.0(2) C45Fe4C43163.15(17)
C19Fe2C2339.4(2) C45Fe4C44126.52(17)
C20Fe2C14113.9(2) C45Fe4C4640.54(17)
C20Fe2C16134.8(2) C46Fe4C40127.30(16)
C20Fe2C17173.8(3) C46Fe4C43153.96(17)
C20Fe2C18145.2(3) C47Fe4C40165.11(17)
C20Fe2C1939.4(3) C47Fe4C42107.71(16)
C20Fe2C2267.6(2) C47Fe4C43118.73(17)
C20Fe2C2366.4(2) C47Fe4C44152.72(17)
C21Fe2C14146.6(3) C47Fe4C4568.24(17)
C21Fe2C16111.65(19) C47Fe4C4640.44(18)
C21Fe2C17134.4(3) C48Fe4C40152.81(17)
C21Fe2C18172.1(3) C48Fe4C42124.93(16)
C21Fe2C1966.9(2) C48Fe4C43105.68(17)
C21Fe2C2040.2(3) C48Fe4C44117.84(17)
C21Fe2C2240.5(3) C48Fe4C4568.89(17)
C21Fe2C2367.0(2) C48Fe4C4668.55(18)
C22Fe2C14169.5(3) C48Fe4C4740.66(19)
C22Fe2C16117.06(19) C49Fe4C40118.53(16)
C22Fe2C17110.0(2) C49Fe4C42162.51(17)
C22Fe2C18131.8(3) C49Fe4C43124.87(17)
C23Fe2C14130.2(2) C49Fe4C44106.67(17)
C23Fe2C16147.6(2) C49Fe4C4540.79(17)
C23Fe2C17115.7(2) C49Fe4C4668.38(17)
C23Fe2C18108.46(19) C49Fe4C4768.39(17)
C23Fe2C2239.9(3) C49Fe4C4841.09(18)
O1Si1O2109.95(14) O3Si2C27108.61(15)
O1Si1C1108.35(16) O3Si2C40112.49(16)
O1Si1C14105.65(15) O4Si2O3109.12(14)
O2Si1C1109.70(16) O4Si2C27108.86(15)
O2Si1C14110.91(16) O4Si2C40106.35(15)
C14Si1C1112.17(16) C27Si2C40111.32(16)
Si1O1Zn1124.85(15) Si2O4Zn2124.39(15)
C11N1Zn1113.0(2) C37N3Zn2113.3(2)
C12N1Zn1108.6(2) C38N3Zn2110.3(3)
C12N1C11112.1(3) C38N3C37111.4(3)
C12N1C13109.0(3) C38N3C39109.3(4)
C13N1Zn1106.0(2) C39N3Zn2104.8(2)
C13N1C11108.0(3) C39N3C37107.4(3)
C25N2C24110.4(3) C51N4C50111.1(3)
C25N2C26111.0(3) C52N4C50112.3(3)
C26N2C24113.0(3) C52N4C51111.0(3)
Si1C1Fe1129.95(19) Si2C27Fe3127.29(19)
C2C1Fe168.2(2) C28C27Fe368.21(19)
C2C1Si1124.4(3) C28C27Si2123.1(3)
C5C1Fe168.7(2) C31C27Fe369.44(19)
C5C1Si1129.8(3) C31C27Si2131.0(3)
C5C1C2105.7(3) C31C27C28105.9(3)
C1C2Fe170.4(2) C27C28Fe369.88(19)
C1C2C11128.2(3) C27C28C37127.7(3)
C3C2Fe169.5(2) C29C28Fe370.1(2)
C3C2C1108.5(3) C29C28C27108.5(3)
C3C2C11123.3(3) C29C28C37123.8(3)
C11C2Fe1126.6(3) C37C28Fe3126.4(3)
C2C3Fe168.9(2) C28C29Fe368.4(2)
C4C3Fe169.8(2) C30C29Fe370.1(2)
C4C3C2108.2(3) C30C29C28107.8(3)
C3C4Fe169.9(2) C29C30Fe369.7(2)
C3C4C5108.4(3) C29C30C31108.9(3)
C5C4Fe169.8(2) C31C30Fe369.5(2)
C1C5Fe170.0(2) C27C31Fe369.28(19)
C4C5Fe169.3(2) C30C31Fe369.7(2)
C4C5C1109.2(3) C30C31C27108.9(3)
C7C6Fe170.3(3) C33C32Fe369.5(3)
C7C6C10108.0(5) C33C32C36107.9(4)
C10C6Fe169.7(3) C36C32Fe370.1(3)
C6C7Fe168.8(3) C32C33Fe369.8(3)
C8C7Fe170.5(3) C32C33C34108.3(4)
C8C7C6108.0(4) C34C33Fe370.2(3)
C7C8Fe169.5(3) C33C34Fe369.1(3)
C7C8C9108.1(5) C33C34C35107.5(4)
C9C8Fe169.2(2) C35C34Fe369.4(2)
C8C9Fe170.4(2) C34C35Fe369.8(2)
C10C9Fe169.7(2) C36C35Fe370.1(2)
C10C9C8109.2(4) C36C35C34108.1(4)
C6C10Fe168.8(3) C32C36Fe369.3(2)
C9C10Fe170.1(2) C35C36Fe369.6(2)
C9C10C6106.7(4) C35C36C32108.3(4)
C2C11N1113.5(3) C28C37N3113.4(3)
Si1C14Fe2130.57(19) Si2C40Fe4130.78(19)
C15C14Fe267.7(2) C41C40Fe468.0(2)
C15C14Si1123.5(3) C41C40Si2124.8(3)
C18C14Fe269.1(2) C44C40Fe469.0(2)
C18C14Si1131.0(3) C44C40Si2129.5(3)
C18C14C15105.3(3) C44C40C41105.6(3)
C14C15Fe270.4(2) C40C41Fe470.4(2)
C14C15C24126.0(3) C40C41C50125.7(3)
C16C15Fe270.4(2) C42C41Fe470.2(2)
C16C15C14108.9(3) C42C41C40108.9(3)
C16C15C24125.1(3) C42C41C50125.3(3)
C24C15Fe2125.3(3) C50C41Fe4126.4(3)
C15C16Fe268.4(2) C41C42Fe468.6(2)
C17C16Fe270.3(2) C43C42Fe470.1(2)
C17C16C15108.3(3) C43C42C41108.1(3)
C16C17Fe269.2(2) C42C43Fe469.2(2)
C16C17C18107.9(3) C44C43Fe469.3(2)
C18C17Fe269.2(2) C44C43C42107.7(3)
C14C18Fe269.6(2) C40C44Fe469.7(2)
C17C18Fe270.1(2) C43C44Fe470.1(2)
C17C18C14109.6(3) C43C44C40109.6(3)
C20C19Fe270.1(3) C46C45Fe470.0(2)
C20C19C23108.6(5) C46C45C49107.9(4)
C23C19Fe270.4(3) C49C45Fe469.3(2)
C19C20Fe270.5(3) C45C46Fe469.5(2)
C19C20C21108.3(5) C47C46Fe469.4(2)
C21C20Fe269.9(3) C47C46C45107.9(4)
C20C21Fe269.9(3) C46C47Fe470.2(2)
C20C21C22107.7(5) C46C47C48108.8(4)
C22C21Fe270.2(3) C48C47Fe469.5(2)
C21C22Fe269.2(3) C47C48Fe469.8(2)
C23C22Fe269.9(3) C47C48C49107.2(4)
C23C22C21106.5(5) C49C48Fe469.4(2)
C19C23Fe270.2(3) C45C49Fe469.9(2)
C19C23C22109.1(5) C45C49C48108.1(4)
C22C23Fe270.2(3) C48C49Fe469.5(2)
C15C24N2110.6(3) C41C50N4110.6(3)

 

Table 6 Hydrogen Bonds for mo_B0662_0m.
DHAd(D-H)/Åd(H-A)/Åd(D-A)/ÅD-H-A/°
N2H2AO10.83(5)1.80(5)2.611(4)165(5)
N4H4AO40.88(6)1.74(6)2.608(4)167(6)

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for mo_B0662_0m.
AtomxyzU(eq)
H2171820248832747
H2A2450(50)19590(40)10200(30)34(13)
H3296116527753636
H4549616655809136
H5584718094881934
H6392920055734865
H7225819002655862
H8362117659625554
H9612617863685448
H10635619338753154
H11A79217585738238
H11B97718618767138
H12A183117013895254
H12B89516361839654
H12C30116732901554
H13A-171017443827267
H13B-115216945768367
H13C-147418033764367
H166207209061094733
H177953201891035835
H18662919419929334
H19480821360825873
H20360122202901583
H21539822874996096
H22775822427976982
H23734021496870776
H24A272021017989435
H24B3527212061065535
H25A664196971073359
H25B674205461023159
H25C1331206671101759
H26A4268192601105751
H26B2864189291125151
H26C3544199021151851
H3A336015468653344
H4A2690(60)14560(40)4780(30)50(15)
H29223811844761839
H30-26711824699537
H31-66713137615034
H3268015368731348
H33264514689819456
H34167813366876960
H35-89113212821650
H36-150414465733845
H37A433412982772036
H37B408413948732836
H38A351712035627463
H38B455211576690763
H38C509111823624563
H39A696512773691066
H39B642712443755666
H39C659213524741966
H42-122015814396035
H43-288615134461737
H44-146514476570435
H45112516862638341
H4686617701527045
H47-168717782472248
H48-303416997548546
H49-128416436652443
H50A230116047494535
H50B145616119417935
H51A437114594419854
H51B436515503464554
H51C369215531385654
H52A77314151392349
H52B217413780374649
H52C148114720341549

Experimental

Single crystals of C26H34Br2Fe2N2O2SiZn [mo_B0662_0m] were []. A suitable crystal was selected and [] on a Bruker D8 Venture diffractometer. The crystal was kept at 99.99 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 [mo_B0662_0m]

Crystal Data for C26H34Br2Fe2N2O2SiZn (=771.53 g/mol): monoclinic, space group P21 (no. 4), a = 9.8916(13) Å, b = 14.438(2) Å, c = 20.415(3) Å, β = 102.936(5)°, = 2841.6(7) Å3, Z = 4, T = 99.99 K, μ(MoKα) = 4.726 mm-1, Dcalc = 1.803 g/cm3, 59808 reflections measured (4.224° ≤ 2Θ ≤ 59.342°), 16000 unique (Rint = 0.0281, Rsigma = 0.0248) which were used in all calculations. The final R1 was 0.0294 (I > 2σ(I)) and wR2 was 0.0741 (all data).

Refinement model description

Number of restraints - 1, 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) groups
2.a Secondary CH2 refined with riding coordinates:
C11(H11A,H11B), C24(H24A,H24B), C37(H37A,H37B), C50(H50A,H50B)
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), C16(H16),
C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C29(H29),
C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36),
C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49)
2.c Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C25(H25A,H25B,H25C), C26(H26A,H26B,
H26C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C51(H51A,H51B,H51C), C52(H52A,
H52B,H52C)
2.d Idealised tetrahedral OH refined as rotating group:
O2(H2), O3(H3A)

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.