3113

Table 1 Crystal data and structure refinement for 3113.
Identification code 3113
Empirical formula C55H74Br4Fe4N4O5Si2Zn2
Formula weight 1601.14
Temperature/K 173
Crystal system monoclinic
Space group C2/c
a/Å 47.515(3)
b/Å 10.31587(19)
c/Å 33.897(2)
α/° 90
β/° 132.838(10)
γ/° 90
Volume/Å3 12183.5(18)
Z 8
ρcalcg/cm3 1.746
μ/mm‑1 4.414
F(000) 6432.0
Crystal size/mm3 0.2 × 0.2 × 0.1
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.676 to 56
Index ranges -62 ≤ h ≤ 62, -13 ≤ k ≤ 13, -44 ≤ l ≤ 43
Reflections collected 155041
Independent reflections 14607 [Rint = 0.0441, Rsigma = 0.0233]
Data/restraints/parameters 14607/4/709
Goodness-of-fit on F2 1.046
Final R indexes [I>=2σ (I)] R1 = 0.0432, wR2 = 0.1153
Final R indexes [all data] R1 = 0.0562, wR2 = 0.1243
Largest diff. peak/hole / e Å-3 1.70/-0.58

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for 3113. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Br1726.1(2)2207.3(4)6714.0(2)46.54(11)
Br2748.5(2)1111.8(4)7878.1(2)44.62(11)
Zn1849.0(2)2798.3(4)7511.3(2)31.67(10)
Fe11415.0(2)7495.7(5)7714.6(2)27.95(11)
Fe2-198.2(2)7784.4(5)6205.4(2)36.28(13)
Si1588.9(3)5662.3(9)7140.3(4)28.02(18)
O1537.8(7)4300(2)7323.6(10)30.8(5)
O2580.7(8)5411(3)6653.3(11)38.9(6)
N11430.5(8)3326(3)8076.4(12)33.1(6)
N2-207.0(9)3787(3)6651.5(14)44.5(8)
C11058.2(9)6395(3)7720.8(13)28.1(6)
C21426.9(9)5778(3)8014.7(13)27.7(6)
C31720.7(10)6620(4)8441.4(14)32.5(7)
C41542.3(11)7755(4)8415.5(15)34.0(7)
C51139.6(10)7619(3)7981.8(14)31.1(7)
C61137.8(12)7827(5)6931.3(16)48(1)
C71474.1(12)7092(4)7187.9(16)41.1(9)
C81792.8(11)7840(3)7628.4(15)33.9(7)
C91645.3(11)9025(4)7632.6(16)37.8(8)
C101244.1(13)9017(4)7207.7(18)47.6(10)
C111510.3(10)4495(3)7899.0(15)33.2(7)
C121566.0(14)3530(4)8614.0(16)49.8(10)
C131641.2(12)2212(4)8108.8(19)49.5(10)
C14166.9(10)6660(3)6883.8(14)33.0(7)
C15-218(1)6142(4)6507.7(14)34.7(7)
C16-476.1(11)7071(4)6426.0(16)40.1(8)
C17-260.3(11)8173(4)6736.5(17)47.9(10)
C18132.4(11)7933(4)7016.5(16)41.9(9)
C194.8(15)7727(6)5833(2)65.3(15)
C20-376.9(15)7326(5)5477.8(19)55.2(11)
C21-599.7(13)8335(5)5416.9(17)53.8(11)
C22-360.8(18)9378(5)5731(2)70.8(16)
C2322.1(17)8986(7)5997(2)79(2)
C24-326.6(11)4837(4)6251.2(15)39.0(8)
C25-257.9(15)2486(4)6436(2)71.7(17)
C26-409.1(14)3940(6)6844(2)71.1(17)
Br3-2337.8(2)10819.0(4)3953.8(2)48.71(11)
Br4-1228.7(2)12088.2(4)4944.8(2)44.11(10)
Zn2-1657.7(2)10369.5(4)4667.0(2)32.27(10)
Fe3-1985.3(2)5661.0(5)4916.0(2)30.01(11)
Fe4-1845.6(2)5376.6(5)3373.6(2)34.94(12)
Si2-1757.0(3)7492.2(9)4266.0(4)28.25(19)
O3-1546.9(7)8892(2)4449.3(10)31.1(5)
O4-2223.2(7)7701(2)3759.4(10)35.0(5)
N3-1585.2(8)9761(3)5319.2(12)31.9(6)
N4-1435.9(9)9434(3)3801.2(13)36.1(7)
C27-1648.7(9)6701(3)4849.7(13)28.8(6)
C28-1662.2(10)7308(3)5223.9(14)30.0(7)
C29-1515.8(10)6406(4)5647.0(14)33.6(7)
C30-1418(1)5238(4)5539.2(14)33.2(7)
C31-1496.6(10)5423(3)5058.6(14)32.3(7)
C32-2531.3(11)5657(4)4174.0(16)42.7(9)
C33-2526.3(10)6178(4)4565.6(15)38.0(8)
C34-2378.6(11)5223(4)4966.2(17)41.6(9)
C35-2294.9(12)4109(4)4821.6(19)48.1(10)
C36-2386.4(12)4377(4)4333.7(19)50.8(11)
C37-1826.2(10)8599(3)5180.1(15)33.6(7)
C38-1175.4(11)9522(4)5797.5(15)38.4(8)
C39-1723.6(12)10841(4)5437.9(18)42.8(9)
C40-1560.6(10)6560(3)4026.7(14)31.4(7)
C41-1558.3(11)7088(3)3631.9(14)33.8(7)
C42-1373.8(11)6181(4)3553.1(15)38.4(8)
C43-1262.2(11)5098(4)3885.2(15)38.1(8)
C44-1372.0(11)5325(4)4178.8(15)36.0(8)
C45-2378.9(14)5125(6)3109(3)70.9(17)
C46-2404.6(14)5689(5)2716(3)82(2)
C47-2233.2(14)4828(5)2589.3(19)60.5(13)
C48-2110.4(12)3742(4)2921.9(18)44.9(9)
C49-2201.1(14)3946(5)3236(2)57.1(12)
C50-1698.6(11)8396(4)3387.1(15)38.2(8)
C51-1035.6(12)9307(4)4040.1(19)48(1)
C52-1592.0(13)10749(4)3572.0(17)44.3(9)
O5-641(2)2371(7)4414(3)145(2)
C53-197(4)3596(11)5297(4)215(8)
C54-334(2)2410(9)4916(4)101(2)
C55-49(3)1551(14)5145(4)171(5)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for 3113. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Br160.8(3)40.5(2)39.8(2)-1.08(16)34.8(2)6.27(18)
Br261.3(3)29.25(18)55.9(2)5.37(16)44.8(2)1.84(16)
Zn133.4(2)27.0(2)34.7(2)1.88(15)23.18(19)2.04(15)
Fe127.7(2)27.9(2)28.9(2)1.44(18)19.5(2)0.46(18)
Fe228.2(3)31.3(3)36.2(3)5.3(2)16.7(2)1.83(19)
Si127.5(4)26.9(4)28.9(4)0.6(3)18.8(4)0.3(3)
O130.1(12)27.1(11)34.9(12)2.3(9)21.9(11)1.1(9)
O252.2(16)33.3(14)38.3(14)-0.4(11)33.6(13)0.8(12)
N133.9(15)26.5(14)33.5(15)3.0(11)20.8(13)3.9(12)
N229.9(16)37.6(17)48.4(19)9.4(14)19.6(15)-2.3(13)
C131.0(17)27.2(16)30.7(16)0.8(12)22.8(15)-0.2(12)
C229.1(16)27.8(16)27.0(15)3.0(12)19.4(14)0.5(12)
C328.6(17)35.4(18)29.1(16)2.8(14)17.8(15)-0.4(14)
C435.8(18)36.1(18)32.9(17)-3.2(14)24.5(16)-4.7(14)
C530.6(17)33.6(17)32.1(17)-1.2(13)22.5(15)0.0(13)
C637(2)67(3)29.0(18)9.4(18)18.4(17)-9.8(19)
C757(2)41(2)43(2)-9.0(16)41(2)-11.1(17)
C835.1(18)36.1(18)38.5(18)1.0(14)28.1(17)-1.2(14)
C947(2)29.9(17)45(2)1.9(15)34.3(19)-2.5(15)
C1046(2)48(2)52(2)19.9(19)35(2)11.9(18)
C1127.6(16)31.9(17)35.5(18)3.5(14)19.6(15)4.6(13)
C1262(3)38(2)33.1(19)4.0(16)26(2)-5.6(19)
C1338(2)33(2)60(3)0.3(18)27(2)6.3(16)
C1432.4(17)32.4(17)29.3(16)4.0(13)19.0(15)3.7(14)
C1532.0(18)35.7(18)32.7(17)3.1(14)20.5(16)0.3(14)
C1630.5(18)44(2)40(2)4.3(16)21.6(17)5.0(15)
C1735(2)50(2)46(2)1.6(18)22.4(19)13.5(17)
C1832.8(19)41(2)36.5(19)-1.3(16)17.6(17)6.2(15)
C1949(3)85(4)66(3)44(3)41(3)25(3)
C2070(3)53(3)49(2)7(2)43(3)0(2)
C2136(2)76(3)37(2)18(2)20.0(18)11(2)
C2292(4)41(3)60(3)21(2)44(3)16(3)
C2360(3)91(4)52(3)17(3)24(3)-32(3)
C2432.4(18)36.6(19)36.9(19)4.3(15)19.2(16)-1.9(15)
C2549(3)36(2)68(3)2(2)15(2)-10(2)
C2641(2)99(4)72(3)41(3)38(3)7(3)
Br334.1(2)40.2(2)46.6(2)-2.43(17)17.43(18)8.44(16)
Br444.9(2)29.61(18)50.7(2)-0.16(15)29.7(2)-5.06(15)
Zn233.0(2)27.0(2)34.3(2)-0.76(15)21.96(18)1.62(15)
Fe328.9(2)28.5(2)33.5(2)-0.71(19)21.6(2)0.38(18)
Fe434.6(3)30.3(3)38.8(3)-4.1(2)24.5(2)0.8(2)
Si229.0(5)25.9(4)29.6(4)-0.1(3)19.8(4)1.8(3)
O334.1(12)25.6(11)34.4(12)-0.5(9)23.6(11)0.9(9)
O429.5(13)32.0(13)33.4(13)-1.6(10)17.4(11)2.7(10)
N332.0(15)29.4(14)35.3(15)-4.3(12)23.3(13)-1.6(11)
N443.5(17)32.2(15)35.9(16)0.9(12)28.4(15)-2.8(13)
C2727.1(16)30.2(16)30.1(16)-1.0(13)19.9(14)0.7(13)
C2827.4(16)30.1(16)30.8(16)-5.2(13)19.2(14)-2.7(13)
C2931.6(17)38.1(18)30.3(17)-2.2(14)20.7(15)-1.5(14)
C3027.4(16)36.2(18)33.5(17)4.3(14)19.7(15)3.2(14)
C3130.8(17)32.8(17)36.8(18)2.1(14)24.4(16)3.3(13)
C3231.0(19)52(2)37.3(19)-2.5(17)20.0(17)-7.6(16)
C3326.8(17)38.5(19)42(2)2.4(15)20.6(16)3.1(14)
C3435.0(19)47(2)49(2)6.0(17)30.8(19)0.8(16)
C3537(2)34(2)65(3)6.6(18)32(2)-0.3(16)
C3642(2)47(2)62(3)-22(2)35(2)-13.4(18)
C3733.6(18)33.0(18)40.0(19)-2.8(14)27.4(16)-0.2(14)
C3834.9(19)36.6(19)36.8(19)-4.0(15)21.6(17)-0.5(15)
C3951(2)32.7(19)54(2)-7.0(17)39(2)0.6(16)
C4030.9(17)29.8(16)32.7(17)-0.4(13)21.3(15)1.0(13)
C4136.1(18)33.5(18)30.5(17)-1.4(14)22.1(16)-1.9(14)
C4239(2)45(2)36.7(19)-2.2(16)27.8(17)-0.3(16)
C4335.9(19)41(2)40.9(19)0.4(16)27.6(17)6.0(15)
C4437.0(19)37.0(19)33.7(18)3.6(14)24.0(16)5.9(15)
C4545(3)64(3)98(4)-38(3)46(3)-16(2)
C4637(3)41(3)74(4)-14(2)1(3)4(2)
C4756(3)51(3)41(2)-10(2)20(2)-13(2)
C4850(2)34(2)57(2)-13.5(17)39(2)-10.5(17)
C4960(3)52(3)79(3)-23(2)55(3)-18(2)
C5042(2)36.5(19)32.2(18)-0.8(15)23.7(17)-4.6(16)
C5146(2)45(2)57(3)-1.4(19)36(2)-4.5(18)
C5259(3)35(2)44(2)4.6(16)37(2)1.6(17)
O5139(6)133(6)133(6)-3(4)81(5)1(4)
C53307(18)124(9)94(7)25(6)89(9)-39(11)
C5473(5)106(6)83(5)-6(4)37(4)-4(4)
C55149(10)227(14)97(7)40(8)67(7)-11(10)

 

Table 4 Bond Lengths for 3113.
AtomAtomLength/Å AtomAtomLength/Å
Br1Zn12.4230(6) Zn2O31.917(2)
Br2Zn12.3680(5) Zn2N32.089(3)
Zn1O11.926(2) Fe3C272.061(3)
Zn1N12.098(3) Fe3C282.038(3)
Fe1C12.052(3) Fe3C292.047(4)
Fe1C22.024(3) Fe3C302.043(3)
Fe1C32.032(3) Fe3C312.040(3)
Fe1C42.032(4) Fe3C322.045(4)
Fe1C52.040(3) Fe3C332.038(4)
Fe1C62.036(4) Fe3C342.039(4)
Fe1C72.030(4) Fe3C352.047(4)
Fe1C82.036(3) Fe3C362.042(4)
Fe1C92.044(4) Fe4C402.037(3)
Fe1C102.044(4) Fe4C412.030(4)
Fe2C142.054(3) Fe4C422.057(4)
Fe2C152.015(4) Fe4C432.059(4)
Fe2C162.046(4) Fe4C442.041(4)
Fe2C172.052(5) Fe4C452.050(5)
Fe2C182.044(4) Fe4C462.018(5)
Fe2C192.045(5) Fe4C472.030(5)
Fe2C202.045(5) Fe4C482.038(4)
Fe2C212.043(4) Fe4C492.044(5)
Fe2C222.048(5) Si2O31.620(2)
Fe2C232.034(5) Si2O41.652(3)
Si1O11.620(2) Si2C271.860(3)
Si1O21.645(3) Si2C401.866(4)
Si1C11.857(4) N3C371.496(4)
Si1C141.862(4) N3C381.479(5)
N1C111.506(5) N3C391.482(5)
N1C121.478(5) N4C501.514(5)
N1C131.478(5) N4C511.482(5)
N2C241.513(5) N4C521.487(5)
N2C251.467(6) C27C281.455(5)
N2C261.491(6) C27C311.438(5)
C1C21.447(5) C28C291.432(5)
C1C51.436(5) C28C371.498(5)
C2C31.431(5) C29C301.426(5)
C2C111.508(5) C30C311.415(5)
C3C41.413(5) C32C331.417(6)
C4C51.420(5) C32C361.416(6)
C6C71.413(6) C33C341.418(5)
C6C101.413(7) C34C351.409(6)
C7C81.429(5) C35C361.422(7)
C8C91.414(5) C40C411.452(5)
C9C101.405(6) C40C441.437(5)
C14C151.444(5) C41C421.426(5)
C14C181.433(5) C41C501.484(5)
C15C161.428(5) C42C431.408(6)
C15C241.491(5) C43C441.423(5)
C16C171.408(6) C45C461.380(9)
C17C181.427(5) C45C491.372(8)
C19C201.393(7) C46C471.454(8)
C19C231.393(9) C47C481.405(7)
C20C211.396(7) C48C491.410(6)
C21C221.391(8) O5C541.286(10)
C22C231.434(9) C53C541.564(14)
Br3Zn22.4246(7) C54C551.339(14)
Br4Zn22.3611(6)    

 

Table 5 Bond Angles for 3113.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
Br2Zn1Br1114.77(2) O3Zn2Br4111.23(7)
O1Zn1Br1106.56(7) O3Zn2N3106.12(11)
O1Zn1Br2112.38(7) N3Zn2Br3105.18(8)
O1Zn1N1109.36(11) N3Zn2Br4109.09(8)
N1Zn1Br1104.63(9) C28Fe3C2741.57(13)
N1Zn1Br2108.77(8) C28Fe3C2941.03(14)
C2Fe1C141.56(13) C28Fe3C3069.15(14)
C2Fe1C341.32(14) C28Fe3C3168.86(14)
C2Fe1C469.10(14) C28Fe3C32121.02(16)
C2Fe1C568.83(14) C28Fe3C34123.78(16)
C2Fe1C6125.07(17) C28Fe3C35160.59(17)
C2Fe1C7106.80(15) C28Fe3C36156.79(18)
C2Fe1C8119.89(14) C29Fe3C2769.44(14)
C2Fe1C9155.39(15) C30Fe3C2769.40(14)
C2Fe1C10162.52(17) C30Fe3C2940.81(14)
C3Fe1C169.89(14) C30Fe3C32161.71(16)
C3Fe1C568.60(14) C30Fe3C35107.28(16)
C3Fe1C6161.99(18) C31Fe3C2741.04(13)
C3Fe1C8106.15(15) C31Fe3C2968.31(14)
C3Fe1C9120.04(15) C31Fe3C3040.56(14)
C3Fe1C10155.29(18) C31Fe3C32125.37(16)
C4Fe1C169.65(14) C31Fe3C35121.61(16)
C4Fe1C340.69(15) C31Fe3C36108.35(16)
C4Fe1C540.84(14) C32Fe3C27107.23(15)
C4Fe1C6156.49(18) C32Fe3C29156.41(16)
C4Fe1C8123.65(15) C32Fe3C3568.31(17)
C4Fe1C9107.22(15) C33Fe3C27124.40(15)
C4Fe1C10120.93(17) C33Fe3C28107.02(15)
C5Fe1C141.09(13) C33Fe3C29120.79(15)
C5Fe1C9125.21(15) C33Fe3C30155.95(15)
C5Fe1C10108.48(16) C33Fe3C31162.08(15)
C6Fe1C1107.44(15) C33Fe3C3240.62(16)
C6Fe1C5121.80(17) C33Fe3C3440.72(16)
C6Fe1C868.62(16) C33Fe3C3568.03(16)
C6Fe1C967.95(17) C33Fe3C3668.15(17)
C6Fe1C1040.52(19) C34Fe3C27161.36(15)
C7Fe1C1120.30(15) C34Fe3C29106.77(16)
C7Fe1C3124.24(16) C34Fe3C30120.39(15)
C7Fe1C4161.11(17) C34Fe3C31156.05(15)
C7Fe1C5156.55(16) C34Fe3C3268.54(17)
C7Fe1C640.66(18) C34Fe3C3540.33(17)
C7Fe1C841.16(15) C34Fe3C3668.33(18)
C7Fe1C968.39(16) C35Fe3C27156.72(16)
C7Fe1C1068.40(18) C35Fe3C29123.98(17)
C8Fe1C1155.88(14) C36Fe3C27121.05(17)
C8Fe1C5161.27(15) C36Fe3C29161.20(18)
C8Fe1C940.56(15) C36Fe3C30124.67(17)
C8Fe1C1068.33(16) C36Fe3C3240.54(18)
C9Fe1C1161.96(15) C36Fe3C3540.71(19)
C9Fe1C1040.22(17) C40Fe4C4269.60(14)
C10Fe1C1125.08(16) C40Fe4C4369.43(14)
C15Fe2C1441.56(14) C40Fe4C4441.26(14)
C15Fe2C1641.15(15) C40Fe4C45105.18(18)
C15Fe2C1768.53(17) C40Fe4C48158.02(16)
C15Fe2C1868.77(16) C40Fe4C49121.09(17)
C15Fe2C19119.6(2) C41Fe4C4041.84(14)
C15Fe2C20107.12(18) C41Fe4C4240.84(15)
C15Fe2C21125.06(18) C41Fe4C4368.42(15)
C15Fe2C22162.0(2) C41Fe4C4468.85(15)
C15Fe2C23154.4(2) C41Fe4C45124.59(19)
C16Fe2C1469.60(15) C41Fe4C47123.53(18)
C16Fe2C1740.20(17) C41Fe4C48159.12(16)
C16Fe2C22125.6(2) C41Fe4C49159.30(17)
C17Fe2C1469.14(15) C42Fe4C4340.02(16)
C18Fe2C1440.94(15) C44Fe4C4268.03(15)
C18Fe2C1668.41(17) C44Fe4C4340.61(14)
C18Fe2C1740.77(16) C44Fe4C45119.5(2)
C18Fe2C19125.4(2) C44Fe4C49106.0(2)
C18Fe2C20161.64(19) C45Fe4C42162.8(2)
C18Fe2C22122.0(2) C45Fe4C43155.1(2)
C19Fe2C14106.31(16) C46Fe4C40120.50(19)
C19Fe2C16155.2(2) C46Fe4C41109.37(19)
C19Fe2C17163.0(2) C46Fe4C42127.9(3)
C19Fe2C2267.9(2) C46Fe4C43163.7(3)
C20Fe2C14124.19(18) C46Fe4C44155.1(3)
C20Fe2C16121.06(19) C46Fe4C4539.7(3)
C20Fe2C17156.07(19) C46Fe4C4742.1(2)
C20Fe2C1939.8(2) C46Fe4C4868.03(19)
C20Fe2C2267.2(2) C46Fe4C4966.4(3)
C21Fe2C14161.55(19) C47Fe4C40158.62(18)
C21Fe2C16108.52(17) C47Fe4C42109.6(2)
C21Fe2C17122.02(18) C47Fe4C43124.5(2)
C21Fe2C18156.80(19) C47Fe4C44159.66(19)
C21Fe2C1967.25(19) C47Fe4C4569.0(2)
C21Fe2C2040.0(2) C47Fe4C4840.40(19)
C21Fe2C2239.8(2) C47Fe4C4968.1(2)
C22Fe2C14155.9(2) C48Fe4C42123.22(16)
C22Fe2C17109.2(2) C48Fe4C43107.89(17)
C23Fe2C14119.4(2) C48Fe4C44122.64(17)
C23Fe2C16163.4(3) C48Fe4C4567.58(19)
C23Fe2C17126.9(3) C48Fe4C4940.42(17)
C23Fe2C18108.3(2) C49Fe4C42157.56(18)
C23Fe2C1940.0(3) C49Fe4C43121.5(2)
C23Fe2C2067.2(2) C49Fe4C4539.2(2)
C23Fe2C2167.6(2) O3Si2O4108.88(13)
C23Fe2C2241.1(3) O3Si2C27109.29(14)
O1Si1O2109.91(14) O3Si2C40105.46(14)
O1Si1C1109.37(14) O4Si2C27111.61(15)
O1Si1C14105.30(15) O4Si2C40109.19(15)
O2Si1C1108.64(15) C27Si2C40112.19(15)
O2Si1C14109.60(15) Si2O3Zn2126.70(14)
C1Si1C14113.96(16) C37N3Zn2111.6(2)
Si1O1Zn1122.86(14) C38N3Zn2110.9(2)
C11N1Zn1112.1(2) C38N3C37111.5(3)
C12N1Zn1111.2(3) C38N3C39108.9(3)
C12N1C11111.2(3) C39N3Zn2106.1(2)
C12N1C13108.3(3) C39N3C37107.6(3)
C13N1Zn1105.7(2) C51N4C50112.7(3)
C13N1C11108.1(3) C51N4C52111.4(3)
C25N2C24111.9(4) C52N4C50110.9(3)
C25N2C26112.2(4) Si2C27Fe3132.10(18)
C26N2C24110.8(3) C28C27Fe368.37(19)
Si1C1Fe1128.27(17) C28C27Si2126.5(3)
C2C1Fe168.18(18) C31C27Fe368.67(19)
C2C1Si1124.8(2) C31C27Si2127.5(3)
C5C1Fe168.98(19) C31C27C28105.7(3)
C5C1Si1129.6(3) C27C28Fe370.07(19)
C5C1C2105.6(3) C27C28C37128.6(3)
C1C2Fe170.26(18) C29C28Fe369.8(2)
C1C2C11128.0(3) C29C28C27108.3(3)
C3C2Fe169.63(19) C29C28C37122.8(3)
C3C2C1108.8(3) C37C28Fe3122.0(2)
C3C2C11123.2(3) C28C29Fe369.1(2)
C11C2Fe1124.1(2) C30C29Fe369.5(2)
C2C3Fe169.05(19) C30C29C28108.3(3)
C4C3Fe169.6(2) C29C30Fe369.7(2)
C4C3C2108.0(3) C31C30Fe369.6(2)
C3C4Fe169.7(2) C31C30C29107.7(3)
C3C4C5108.2(3) C27C31Fe370.28(19)
C5C4Fe169.9(2) C30C31Fe369.9(2)
C1C5Fe169.92(18) C30C31C27110.0(3)
C4C5Fe169.3(2) C33C32Fe369.4(2)
C4C5C1109.5(3) C36C32Fe369.6(2)
C7C6Fe169.5(2) C36C32C33107.5(4)
C7C6C10108.3(4) C32C33Fe370.0(2)
C10C6Fe170.0(2) C32C33C34108.4(4)
C6C7Fe169.9(2) C34C33Fe369.7(2)
C6C7C8107.7(4) C33C34Fe369.6(2)
C8C7Fe169.7(2) C35C34Fe370.1(2)
C7C8Fe169.2(2) C35C34C33107.8(4)
C9C8Fe170.0(2) C34C35Fe369.6(2)
C9C8C7107.3(3) C34C35C36108.1(4)
C8C9Fe169.4(2) C36C35Fe369.5(2)
C10C9Fe169.9(2) C32C36Fe369.9(2)
C10C9C8108.7(4) C32C36C35108.1(4)
C6C10Fe169.4(2) C35C36Fe369.8(2)
C9C10Fe169.9(2) N3C37C28116.5(3)
C9C10C6108.0(4) Si2C40Fe4128.46(18)
N1C11C2114.6(3) C41C40Fe468.8(2)
Si1C14Fe2131.05(19) C41C40Si2121.8(3)
C15C14Fe267.8(2) C44C40Fe469.5(2)
C15C14Si1121.5(3) C44C40Si2132.5(3)
C18C14Fe269.2(2) C44C40C41105.6(3)
C18C14Si1132.6(3) C40C41Fe469.3(2)
C18C14C15105.7(3) C40C41C50125.1(3)
C14C15Fe270.7(2) C42C41Fe470.6(2)
C14C15C24125.3(3) C42C41C40108.5(3)
C16C15Fe270.6(2) C42C41C50126.3(3)
C16C15C14109.1(3) C50C41Fe4129.4(3)
C16C15C24125.6(3) C41C42Fe468.6(2)
C24C15Fe2125.4(3) C43C42Fe470.1(2)
C15C16Fe268.3(2) C43C42C41108.4(3)
C17C16Fe270.1(3) C42C43Fe469.9(2)
C17C16C15107.7(3) C42C43C44108.1(3)
C16C17Fe269.7(2) C44C43Fe469.0(2)
C16C17C18108.4(4) C40C44Fe469.2(2)
C18C17Fe269.3(2) C43C44Fe470.4(2)
C14C18Fe269.9(2) C43C44C40109.3(3)
C17C18Fe269.9(2) C46C45Fe468.9(3)
C17C18C14109.1(4) C49C45Fe470.2(3)
C20C19Fe270.1(3) C49C45C46107.9(5)
C20C19C23108.1(5) C45C46Fe471.4(3)
C23C19Fe269.6(3) C45C46C47109.2(5)
C19C20Fe270.1(3) C47C46Fe469.4(3)
C19C20C21108.5(5) C46C47Fe468.5(3)
C21C20Fe269.9(3) C48C47Fe470.1(3)
C20C21Fe270.1(3) C48C47C46105.1(5)
C22C21Fe270.3(3) C47C48Fe469.5(2)
C22C21C20108.7(5) C47C48C49108.3(4)
C21C22Fe269.9(3) C49C48Fe470.0(2)
C21C22C23106.8(5) C45C49Fe470.7(3)
C23C22Fe268.9(3) C45C49C48109.6(5)
C19C23Fe270.5(3) C48C49Fe469.6(2)
C19C23C22107.8(5) C41C50N4110.6(3)
C22C23Fe270.0(3) O5C54C53125.3(9)
C15C24N2110.7(3) O5C54C55122.5(10)
Br4Zn2Br3117.25(2) C55C54C53110.5(10)
O3Zn2Br3107.27(7)     

 

Table 6 Hydrogen Bonds for 3113.
DHAd(D-H)/Åd(H-A)/Åd(D-A)/ÅD-H-A/°
N2H2AO10.984(19)1.69(2)2.652(4)163(4)
N4H4BO30.968(19)1.70(2)2.644(4)165(5)

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for 3113.
AtomxyzU(eq)
H319836449869239
H416678468864341
H59578229788237
H68897572663258
H714866269708849
H820497593786841
H917909698787645
H1010789679712357
H11A13574431751540
H11B17784479807740
H12A14274235859875
H12B18353731886875
H12C15242756872575
H13A15791442819574
H13B19122371838374
H13C15692100776974
H16-7396967620748
H17-3578929675657
H183348510724850
H192127240594278
H20-4686522530966
H21-8648314520265
H22-43510175576385
H232439484623795
H24A-2034692611647
H24B-6024801594947
H25A-52623346132107
H25B-16318516709107
H25C-11924236325107
H26A-34747687015107
H26B-33032647096107
H26C-68138866543107
H29-14896557594240
H30-13204488574740
H31-14564808490139
H32-26156079386851
H33-26067006456146
H34-23435316527050
H35-21973334501258
H36-23563809415161
H37A-20718699481440
H37B-18778590541340
H38A-10798860571658
H38B-11499243609258
H38C-103210306589558
H39A-158811620550164
H39B-168010635575264
H39C-199310968513864
H42-13346286332246
H43-11384363390846
H44-13284762443043
H45-24665481326185
H46-25146492255898
H47-22104967234173
H48-19903013293354
H49-21493370349068
H50A-19568521324446
H50B-17098468309246
H51A-9348481421672
H51B-8829987429872
H51C-10329368376172
H52A-161810869326867
H52B-142011391384067
H52C-183910836346067
H53A4033865653322
H53B-15943305164322
H53C-38838005310322
H55A15317485520257
H55B-1446935105257
H55C4915954973257
H2A68(6)3960(50)6952(14)56(14)
H4B-1438(14)9320(50)4083(15)59(14)
H4A-2316(14)8470(30)3730(20)64(15)
H2614(15)4590(20)6620(20)63(15)

Experimental

Single crystals of C55H74Br4Fe4N4O5Si2Zn2 [3113] 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 [3113]

Crystal Data for C55H74Br4Fe4N4O5Si2Zn2 (=1601.14 g/mol): monoclinic, space group C2/c (no. 15), a = 47.515(3) Å, b = 10.31587(19) Å, c = 33.897(2) Å, β = 132.838(10)°, = 12183.5(18) Å3, Z = 8, T = 173 K, μ(MoKα) = 4.414 mm-1, Dcalc = 1.746 g/cm3, 155041 reflections measured (4.676° ≤ 2Θ ≤ 56°), 14607 unique (Rint = 0.0441, Rsigma = 0.0233) which were used in all calculations. The final R1 was 0.0432 (I > 2σ(I)) and wR2 was 0.1243 (all data).

Refinement model description

Number of restraints - 4, 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
O2-H2 = O4-H4A
0.9 with sigma of 0.02
N4-H4B = N2-H2A
1 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
C11(H11A,H11B), C24(H24A,H24B), C37(H37A,H37B), C50(H50A,H50B)
3.b Me refined with riding coordinates:
C53(H53A,H53B,H53C), C55(H55A,H55B,H55C)
3.c 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)
3.d 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)

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