3111

Table 1 Crystal data and structure refinement for 3111.
Identification code 3111
Empirical formula C49H58Br2Fe4N2O4Si2Zn
Formula weight 1243.74
Temperature/K 150
Crystal system monoclinic
Space group P21/n
a/Å 22.0084(17)
b/Å 11.8011(5)
c/Å 23.1333(18)
α/° 90
β/° 115.664(9)
γ/° 90
Volume/Å3 5415.5(7)
Z 4
ρcalcg/cm3 1.525
μ/mm‑1 3.044
F(000) 2520.0
Crystal size/mm3 0.2 × 0.1 × 0.1
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.84 to 51.998
Index ranges -28 ≤ h ≤ 17, -15 ≤ k ≤ 16, -28 ≤ l ≤ 31
Reflections collected 50421
Independent reflections 10638 [Rint = 0.0716, Rsigma = 0.0880]
Data/restraints/parameters 10638/42/591
Goodness-of-fit on F2 1.066
Final R indexes [I>=2σ (I)] R1 = 0.0563, wR2 = 0.1282
Final R indexes [all data] R1 = 0.0859, wR2 = 0.1390
Largest diff. peak/hole / e Å-3 1.48/-0.67

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for 3111. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Br18972.7(3)40.5(4)7303.3(3)38.11(17)
Br28902.1(4)2424.9(5)8405.7(3)44.08(18)
Zn19083.7(3)2062.6(5)7469.5(3)25.41(16)
Fe111679.6(4)3171.4(6)6920.8(4)22.10(18)
Fe210436.7(5)5670.7(7)8347.7(5)42.5(2)
Fe37762.2(4)6390.8(6)5637.6(4)28.1(2)
Fe48530.2(4)1837.3(6)5092.0(4)28.0(2)
Si110178.7(7)3438.3(11)7193.0(7)19.5(3)
Si28704.8(7)3832.4(11)6324.2(7)21.2(3)
O18489.1(18)3040(3)6769.9(17)27.3(8)
O29975.2(17)2409(3)7532.1(16)23.4(8)
O39524.6(17)3991(3)6597.9(16)22.1(8)
N110795(2)662(4)7756(2)28.1(10)
N27500(3)4032(4)6983(2)36.3(12)
C0AA8381(3)3327(4)5487(3)23.9(12)
C110729(3)2799(4)6846(2)19.2(11)
C1AA9162(3)825(4)5813(3)35.3(14)
C211197(2)1875(4)7130(2)19.6(11)
C2AA8531(3)291(5)5486(3)41.6(16)
C311450(3)1509(4)6689(3)28.5(13)
C3AA8666(3)3530(4)5046(3)28.3(12)
C411159(3)2190(4)6138(2)25.3(12)
C4AA8961(3)627(4)4757(3)35.0(14)
C510718(3)2973(4)6232(2)24.4(12)
C5AA8227(3)3105(5)4427(3)39.1(15)
C612262(3)4132(6)7702(3)47.3(18)
C6AA9430(3)1030(5)5367(3)38.9(15)
C712665(3)3324(6)7562(4)61(2)
C7AA8411(3)169(4)4835(3)39.1(15)
C812577(3)3555(6)6927(4)53(2)
C8AA7668(3)2620(5)4482(3)46.0(18)
C912153(3)4474(5)6705(3)46.0(17)
C9AA7764(3)2748(4)5128(3)38.2(15)
C1011962(3)4818(5)7168(3)41.7(16)
C1110657(3)4519(5)7790(3)37.2(15)
C1211036(4)4249(7)8468(4)72(3)
C1311422(5)5073(8)8835(5)86(3)
C1411362(3)5940(6)8416(4)57(2)
C1510852(5)5648(6)7724(5)81(3)
C169427(3)5762(7)8039(3)57(2)
C179733(4)5333(6)8661(4)53.7(19)
C1810195(4)6148(6)9053(4)54.3(19)
C1910153(4)7072(5)8676(4)56(2)
C209683(4)6839(6)8047(4)60(2)
C218369(3)5279(4)6341(2)19.5(11)
C227753(3)5580(4)6395(3)26.0(12)
C237751(3)6770(5)6492(3)31.6(13)
C248331(3)7229(4)6471(3)31.1(13)
C258698(3)6328(4)6382(2)27.8(12)
C267415(3)5649(5)4763(3)40.4(15)
C277820(5)6517(9)4786(3)82(3)
C287591(8)7443(8)4905(5)129(5)
C296999(7)7278(10)4963(4)130(5)
C306882(4)6064(8)4865(3)68(2)
C3111366(3)1374(4)7775(3)28.1(12)
C3210629(3)-287(4)7292(3)37.1(15)
C3310933(3)241(5)8398(3)46.3(17)
C347233(3)4751(5)6381(3)37.4(15)
C357674(3)4708(5)7569(3)42.9(16)
C366993(3)3129(5)6936(3)48.3(17)
O410777(3)7406(4)6473(3)70.4(16)
C3710264(4)7197(5)6024(3)38.9(15)
C3810131(4)6042(5)5718(4)54.5(19)
C399710(4)8048(5)5750(3)51.2(18)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for 3111. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Br133.3(4)23.8(3)62.9(4)1.7(3)26.1(3)-5.4(3)
Br242.9(4)50.4(4)51.8(4)0.9(3)32.7(3)-3.0(3)
Zn117.2(3)23.6(3)37.8(4)5.7(3)14.2(3)0.9(3)
Fe113.0(4)20.3(4)32.8(4)-1.5(3)9.8(3)-2.0(3)
Fe234.3(5)41.3(5)60.3(6)-30.6(4)28.4(5)-13.8(4)
Fe330.4(5)18.7(4)30.4(4)2.4(3)8.7(4)4.6(3)
Fe423.1(4)19.8(4)34.4(5)-4.7(3)6.1(4)0.6(3)
Si112.3(7)18.1(7)28.1(8)-3.1(6)8.8(6)-2.0(6)
Si215.2(8)18.3(7)30.7(8)1.8(6)10.6(6)2.4(6)
O119(2)26.3(19)41(2)9.6(16)17.0(18)5.4(16)
O213.4(19)24.7(18)29(2)5.5(15)6.6(16)3.4(15)
O319(2)19.2(17)32(2)1.9(14)14.6(17)4.4(15)
N118(2)27(2)36(3)16(2)9(2)10(2)
N227(3)41(3)50(3)12(2)26(3)8(2)
C0AA26(3)10(2)35(3)2(2)14(3)7(2)
C116(3)15(2)23(3)0.8(19)5(2)-1(2)
C1AA30(4)25(3)37(3)-1(2)2(3)11(3)
C210(3)18(2)25(3)1(2)2(2)-1(2)
C2AA40(4)22(3)67(5)0(3)27(4)1(3)
C316(3)22(3)45(4)-11(2)11(3)-4(2)
C3AA31(3)19(2)35(3)0(2)14(3)5(2)
C422(3)28(3)23(3)-8(2)8(2)-2(2)
C4AA37(4)25(3)45(4)-13(3)20(3)0(3)
C515(3)26(3)28(3)-4(2)6(2)-4(2)
C5AA48(4)29(3)34(4)-3(3)12(3)7(3)
C639(4)60(4)40(4)-14(3)15(3)-32(4)
C6AA23(3)25(3)66(4)-5(3)18(3)3(3)
C721(4)35(4)94(6)18(4)-8(4)-14(3)
C7AA26(3)22(3)59(4)-16(3)9(3)-4(3)
C827(4)55(4)90(6)-29(4)39(4)-18(3)
C8AA30(4)36(3)41(4)-9(3)-13(3)12(3)
C939(4)43(4)57(4)-1(3)22(3)-24(3)
C9AA24(3)23(3)60(4)-1(3)11(3)1(3)
C1023(3)27(3)74(5)-18(3)20(3)-16(3)
C1123(3)44(3)52(4)-28(3)22(3)-10(3)
C1236(4)94(6)64(5)-47(5)0(4)24(4)
C1360(6)93(7)106(8)-44(6)38(6)-12(5)
C1436(4)56(4)93(6)-56(4)39(4)-37(4)
C15108(7)57(5)139(8)-59(5)110(7)-49(5)
C1619(3)104(6)42(4)-29(4)10(3)3(4)
C1761(5)47(4)77(6)-19(4)53(5)-11(4)
C1855(5)64(5)52(4)-12(4)30(4)10(4)
C1973(6)33(4)74(5)-26(4)43(5)1(4)
C2069(6)46(4)60(5)-5(4)22(4)14(4)
C2116(3)19(2)24(3)2(2)9(2)0(2)
C2218(3)25(3)37(3)7(2)14(3)7(2)
C2328(3)32(3)29(3)-2(2)6(3)13(3)
C2434(4)22(3)33(3)-5(2)10(3)4(3)
C2524(3)26(3)34(3)1(2)13(3)-1(2)
C2650(4)35(3)20(3)-5(2)0(3)11(3)
C2781(6)131(7)35(4)-1(5)26(4)-56(6)
C28232(13)43(4)39(5)25(4)-10(8)-36(6)
C29160(10)119(7)35(5)-20(5)-29(6)128(7)
C3029(4)126(7)35(4)-4(4)-1(3)2(4)
C3119(3)27(3)33(3)2(2)5(2)0(2)
C3226(3)18(3)63(4)2(3)16(3)2(2)
C3335(4)48(4)51(4)22(3)14(3)3(3)
C3426(3)36(3)58(4)13(3)26(3)12(3)
C3540(4)52(4)46(4)8(3)28(3)8(3)
C3643(4)41(4)71(5)10(3)34(4)-1(3)
O440(3)59(3)77(4)-10(3)-7(3)3(3)
C3745(4)30(3)35(4)1(3)12(3)-2(3)
C3861(5)35(3)79(5)-16(3)42(4)-12(4)
C3950(5)29(3)64(5)6(3)15(4)6(3)

 

Table 4 Bond Lengths for 3111.
AtomAtomLength/Å AtomAtomLength/Å
Br1Zn12.4126(8) N1C311.496(7)
Br2Zn12.4046(9) N1C321.484(7)
Zn1O11.956(3) N1C331.468(7)
Zn1O21.947(3) N2C341.515(7)
Fe1C12.070(5) N2C351.474(8)
Fe1C22.037(5) N2C361.512(8)
Fe1C32.039(5) C0AAC3AA1.431(7)
Fe1C42.034(5) C0AAC9AA1.423(8)
Fe1C52.038(5) C1C21.446(7)
Fe1C62.046(6) C1C51.425(7)
Fe1C72.037(6) C1AAC2AA1.409(8)
Fe1C82.020(6) C1AAC6AA1.415(8)
Fe1C92.038(6) C2C31.427(7)
Fe1C102.044(5) C2C311.494(7)
Fe2C112.070(5) C2AAC7AA1.419(9)
Fe2C122.077(7) C3C41.405(7)
Fe2C132.086(10) C3AAC5AA1.428(8)
Fe2C141.998(6) C4C51.423(7)
Fe2C152.014(7) C4AAC6AA1.421(8)
Fe2C162.022(6) C4AAC7AA1.406(8)
Fe2C172.014(7) C5AAC8AA1.413(9)
Fe2C182.002(6) C6C71.432(10)
Fe2C192.028(6) C6C101.383(9)
Fe2C202.035(7) C7C81.422(10)
Fe3C212.066(5) C8C91.376(9)
Fe3C222.003(5) C8AAC9AA1.422(9)
Fe3C232.038(5) C9C101.372(9)
Fe3C242.042(5) C11C121.457(10)
Fe3C252.034(6) C11C151.427(9)
Fe3C262.025(5) C12C131.329(11)
Fe3C272.035(7) C13C141.375(12)
Fe3C282.001(8) C14C151.544(11)
Fe3C292.021(8) C16C171.393(10)
Fe3C302.025(7) C16C201.387(10)
Fe4C0AA2.072(5) C17C181.409(10)
Fe4C1AA2.033(5) C18C191.374(9)
Fe4C2AA2.039(6) C19C201.399(10)
Fe4C3AA2.030(5) C21C221.459(7)
Fe4C4AA2.042(5) C21C251.415(7)
Fe4C5AA2.040(6) C22C231.422(7)
Fe4C6AA2.035(6) C22C341.495(7)
Fe4C7AA2.041(5) C23C241.408(8)
Fe4C8AA2.032(6) C24C251.403(7)
Fe4C9AA2.032(6) C26C271.344(10)
Si1O21.611(3) C26C301.383(9)
Si1O31.636(4) C27C281.283(15)
Si1C11.877(5) C28C291.381(17)
Si1C111.840(6) C29C301.456(14)
Si2O11.609(4) O4C371.183(8)
Si2O31.644(4) C37C381.506(8)
Si2C0AA1.849(5) C37C391.492(9)
Si2C211.868(5)    

 

Table 5 Bond Angles for 3111.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
Br2Zn1Br1105.94(3) C8AAFe4C5AA40.6(3)
O1Zn1Br1117.76(11) C8AAFe4C6AA156.9(3)
O1Zn1Br2109.13(10) C8AAFe4C7AA105.8(2)
O2Zn1Br1104.41(10) C8AAFe4C9AA41.0(3)
O2Zn1Br2116.80(10) C9AAFe4C0AA40.5(2)
O2Zn1O1103.24(14) C9AAFe4C1AA124.2(3)
C2Fe1C141.24(18) C9AAFe4C2AA107.2(3)
C2Fe1C341.0(2) C9AAFe4C4AA156.2(2)
C2Fe1C568.1(2) C9AAFe4C5AA68.7(3)
C2Fe1C6113.5(2) C9AAFe4C6AA161.4(3)
C2Fe1C9179.4(3) C9AAFe4C7AA121.2(2)
C2Fe1C10140.7(2) O2Si1O3112.42(19)
C3Fe1C169.4(2) O2Si1C1105.79(19)
C3Fe1C6139.0(3) O2Si1C11110.3(2)
C3Fe1C10177.0(2) O3Si1C1107.2(2)
C4Fe1C169.2(2) O3Si1C11111.4(2)
C4Fe1C268.5(2) C11Si1C1109.5(2)
C4Fe1C340.3(2) O1Si2O3113.49(19)
C4Fe1C540.9(2) O1Si2C0AA113.4(2)
C4Fe1C6176.1(3) O1Si2C21106.8(2)
C4Fe1C7135.3(3) O3Si2C0AA107.5(2)
C4Fe1C9111.2(2) O3Si2C21105.5(2)
C4Fe1C10140.9(3) C0AASi2C21109.9(2)
C5Fe1C140.60(19) Si2O1Zn1126.6(2)
C5Fe1C368.2(2) Si1O2Zn1127.3(2)
C5Fe1C6142.7(3) Si1O3Si2134.3(2)
C5Fe1C10114.5(2) C32N1C31112.7(4)
C6Fe1C1114.6(2) C33N1C31110.9(4)
C7Fe1C1143.0(3) C33N1C32110.8(4)
C7Fe1C2113.2(2) C35N2C34112.7(5)
C7Fe1C3109.9(2) C35N2C36109.7(5)
C7Fe1C5175.7(3) C36N2C34110.4(5)
C7Fe1C641.1(3) Si2C0AAFe4132.3(3)
C7Fe1C967.4(3) C3AAC0AAFe468.0(3)
C7Fe1C1067.3(3) C3AAC0AASi2127.1(4)
C8Fe1C1176.0(3) C9AAC0AAFe468.2(3)
C8Fe1C2140.9(3) C9AAC0AASi2127.2(4)
C8Fe1C3110.3(2) C9AAC0AAC3AA105.4(5)
C8Fe1C4107.8(2) Si1C1Fe1134.0(3)
C8Fe1C5135.4(3) C2C1Fe168.2(3)
C8Fe1C668.5(3) C2C1Si1124.9(4)
C8Fe1C741.0(3) C5C1Fe168.5(3)
C8Fe1C939.7(3) C5C1Si1129.2(4)
C8Fe1C1066.9(3) C5C1C2105.3(4)
C9Fe1C1138.2(2) C2AAC1AAFe470.0(3)
C9Fe1C3139.1(2) C2AAC1AAC6AA108.0(5)
C9Fe1C5111.3(2) C6AAC1AAFe469.7(3)
C9Fe1C666.9(3) C1C2Fe170.6(3)
C9Fe1C1039.3(2) C1C2C31124.9(4)
C10Fe1C1113.5(2) C3C2Fe169.6(3)
C10Fe1C639.5(3) C3C2C1109.0(4)
C11Fe2C1241.1(3) C3C2C31126.1(5)
C11Fe2C1369.2(3) C31C2Fe1127.2(4)
C12Fe2C1337.2(3) C1AAC2AAFe469.5(3)
C14Fe2C1169.4(2) C1AAC2AAC7AA107.7(6)
C14Fe2C1263.4(3) C7AAC2AAFe469.7(3)
C14Fe2C1339.3(3) C2C3Fe169.4(3)
C14Fe2C1545.3(3) C4C3Fe169.6(3)
C14Fe2C16161.1(4) C4C3C2108.0(5)
C14Fe2C17156.8(3) C0AAC3AAFe471.2(3)
C14Fe2C18120.7(3) C5AAC3AAFe469.8(3)
C14Fe2C19108.0(3) C5AAC3AAC0AA109.9(5)
C14Fe2C20124.9(4) C3C4Fe170.1(3)
C15Fe2C1140.9(3) C3C4C5107.9(5)
C15Fe2C1268.1(4) C5C4Fe169.7(3)
C15Fe2C1372.2(4) C6AAC4AAFe469.3(3)
C15Fe2C16121.2(4) C7AAC4AAFe469.8(3)
C15Fe2C19126.0(3) C7AAC4AAC6AA107.4(5)
C15Fe2C20108.7(4) C1C5Fe170.9(3)
C16Fe2C11109.5(3) C4C5Fe169.4(3)
C16Fe2C12128.9(3) C4C5C1109.8(4)
C16Fe2C13159.3(4) C3AAC5AAFe469.1(3)
C16Fe2C1967.6(3) C8AAC5AAFe469.4(3)
C16Fe2C2040.0(3) C8AAC5AAC3AA106.8(5)
C17Fe2C11121.2(2) C7C6Fe169.1(4)
C17Fe2C12109.5(4) C10C6Fe170.2(3)
C17Fe2C13121.4(4) C10C6C7106.9(6)
C17Fe2C15155.9(3) C1AAC6AAFe469.6(3)
C17Fe2C1640.4(3) C1AAC6AAC4AA108.2(5)
C17Fe2C1967.5(3) C4AAC6AAFe469.9(3)
C17Fe2C2067.4(3) C6C7Fe169.8(4)
C18Fe2C11155.3(3) C8C7Fe168.9(4)
C18Fe2C12119.7(3) C8C7C6106.6(6)
C18Fe2C13103.6(3) C2AAC7AAFe469.6(3)
C18Fe2C15161.7(3) C4AAC7AAFe469.9(3)
C18Fe2C1668.5(3) C4AAC7AAC2AA108.7(5)
C18Fe2C1741.1(3) C7C8Fe170.1(4)
C18Fe2C1939.9(3) C9C8Fe170.8(4)
C18Fe2C2067.9(3) C9C8C7107.7(6)
C19Fe2C11164.1(3) C5AAC8AAFe470.0(4)
C19Fe2C12152.8(3) C5AAC8AAC9AA108.2(5)
C19Fe2C13119.3(3) C9AAC8AAFe469.5(3)
C19Fe2C2040.3(3) C8C9Fe169.5(4)
C20Fe2C11127.5(3) C10C9Fe170.6(3)
C20Fe2C12165.9(3) C10C9C8109.2(6)
C20Fe2C13156.5(3) C0AAC9AAFe471.3(3)
C22Fe3C2141.98(19) C8AAC9AAFe469.5(3)
C22Fe3C2341.2(2) C8AAC9AAC0AA109.6(6)
C22Fe3C2468.9(2) C6C10Fe170.3(3)
C22Fe3C2568.5(2) C9C10Fe170.1(3)
C22Fe3C26121.6(2) C9C10C6109.6(6)
C22Fe3C27155.6(4) Si1C11Fe2135.3(3)
C22Fe3C29127.0(5) C12C11Fe269.7(3)
C22Fe3C30108.2(3) C12C11Si1122.0(5)
C23Fe3C2169.6(2) C15C11Fe267.5(3)
C23Fe3C2440.4(2) C15C11Si1131.9(6)
C24Fe3C2169.0(2) C15C11C12105.1(6)
C25Fe3C2140.38(19) C11C12Fe269.2(4)
C25Fe3C2367.7(2) C13C12Fe271.8(5)
C25Fe3C2440.3(2) C13C12C11115.9(9)
C25Fe3C27110.9(3) C12C13Fe271.0(5)
C26Fe3C21110.3(2) C12C13C14104.8(9)
C26Fe3C23155.0(3) C14C13Fe266.9(5)
C26Fe3C24164.5(3) C13C14Fe273.8(5)
C26Fe3C25129.4(2) C13C14C15111.6(6)
C26Fe3C2738.7(3) C15C14Fe267.9(3)
C26Fe3C3039.9(3) C11C15Fe271.7(4)
C27Fe3C21121.2(4) C11C15C14102.4(7)
C27Fe3C23162.9(3) C14C15Fe266.8(4)
C27Fe3C24127.5(3) C17C16Fe269.5(4)
C28Fe3C21151.8(5) C20C16Fe270.5(4)
C28Fe3C22165.3(5) C20C16C17108.0(6)
C28Fe3C23127.5(4) C16C17Fe270.1(4)
C28Fe3C24108.2(3) C16C17C18107.9(7)
C28Fe3C25119.3(5) C18C17Fe269.0(4)
C28Fe3C2664.6(3) C17C18Fe269.9(4)
C28Fe3C2737.1(4) C19C18Fe271.1(4)
C28Fe3C2940.2(5) C19C18C17107.6(7)
C28Fe3C3067.2(4) C18C19Fe269.1(4)
C29Fe3C21167.1(5) C18C19C20108.7(7)
C29Fe3C23106.2(3) C20C19Fe270.1(4)
C29Fe3C24116.3(3) C16C20Fe269.5(4)
C29Fe3C25150.5(4) C16C20C19107.9(7)
C29Fe3C2668.0(3) C19C20Fe269.6(4)
C29Fe3C2766.1(5) Si2C21Fe3133.7(3)
C29Fe3C3042.2(4) C22C21Fe366.7(3)
C30Fe3C21128.3(3) C22C21Si2128.0(4)
C30Fe3C23119.3(3) C25C21Fe368.6(3)
C30Fe3C24152.5(3) C25C21Si2127.2(4)
C30Fe3C25166.2(3) C25C21C22104.4(4)
C30Fe3C2766.2(3) C21C22Fe371.3(3)
C1AAFe4C0AA108.6(2) C21C22C34124.7(5)
C1AAFe4C2AA40.5(2) C23C22Fe370.7(3)
C1AAFe4C4AA68.6(2) C23C22C21108.7(5)
C1AAFe4C5AA159.0(3) C23C22C34126.5(5)
C1AAFe4C6AA40.7(2) C34C22Fe3126.2(4)
C1AAFe4C7AA68.2(2) C22C23Fe368.1(3)
C2AAFe4C0AA122.1(2) C24C23Fe370.0(3)
C2AAFe4C4AA68.4(2) C24C23C22108.0(5)
C2AAFe4C5AA158.4(3) C23C24Fe369.7(3)
C2AAFe4C7AA40.7(2) C25C24Fe369.5(3)
C3AAFe4C0AA40.8(2) C25C24C23107.6(5)
C3AAFe4C1AA123.9(2) C21C25Fe371.0(3)
C3AAFe4C2AA158.8(2) C24C25Fe370.2(3)
C3AAFe4C4AA124.5(2) C24C25C21111.2(5)
C3AAFe4C5AA41.1(2) C27C26Fe371.1(4)
C3AAFe4C6AA109.4(2) C27C26C30108.8(7)
C3AAFe4C7AA159.7(2) C30C26Fe370.0(4)
C3AAFe4C8AA68.3(2) C26C27Fe370.3(4)
C3AAFe4C9AA68.0(2) C28C27Fe370.0(6)
C4AAFe4C0AA161.6(2) C28C27C26109.9(10)
C5AAFe4C0AA69.4(2) C27C28Fe372.9(5)
C5AAFe4C4AA106.3(2) C27C28C29112.1(9)
C5AAFe4C7AA122.0(2) C29C28Fe370.7(6)
C6AAFe4C0AA125.3(2) C28C29Fe369.1(5)
C6AAFe4C2AA68.2(2) C28C29C30103.5(8)
C6AAFe4C4AA40.8(2) C30C29Fe369.1(4)
C6AAFe4C5AA122.4(3) C26C30Fe370.0(4)
C6AAFe4C7AA68.0(2) C26C30C29105.6(8)
C7AAFe4C0AA157.2(2) C29C30Fe368.7(5)
C7AAFe4C4AA40.3(2) C2C31N1110.4(4)
C8AAFe4C0AA69.0(2) C22C34N2111.0(5)
C8AAFe4C1AA159.7(3) O4C37C38121.3(6)
C8AAFe4C2AA122.5(3) O4C37C39121.8(6)
C8AAFe4C4AA120.1(3) C39C37C38116.9(6)

 

Table 6 Hydrogen Bonds for 3111.
DHAd(D-H)/Åd(H-A)/Åd(D-A)/ÅD-H-A/°
N1H1O20.99(2)1.70(3)2.639(5)156(6)
N2H2O11.00(2)1.75(4)2.698(6)158(8)

 

Table 7 Torsion Angles for 3111.
ABCDAngle/˚ ABCDAngle/˚
Fe1C1C2C3-59.2(3) C1C2C3Fe159.8(3)
Fe1C1C2C31122.3(5) C1C2C3C40.7(6)
Fe1C1C5C458.6(4) C1C2C31N173.9(6)
Fe1C2C3C4-59.1(4) C1AAC2AAC7AAFe4-59.4(4)
Fe1C2C31N1165.1(3) C1AAC2AAC7AAC4AA-0.2(6)
Fe1C3C4C5-59.7(4) C2C1C5Fe1-58.5(3)
Fe1C4C5C1-59.5(4) C2C1C5C40.1(5)
Fe1C6C7C859.3(4) C2C3C4Fe159.0(3)
Fe1C6C10C9-59.3(4) C2C3C4C5-0.7(6)
Fe1C7C8C961.2(4) C2AAC1AAC6AAFe459.7(4)
Fe1C8C9C1059.6(4) C2AAC1AAC6AAC4AA0.3(6)
Fe1C9C10C659.4(4) C3C2C31N1-104.3(6)
Fe2C11C12C13-56.2(6) C3C4C5Fe159.9(4)
Fe2C11C15C1460.1(4) C3C4C5C10.4(6)
Fe2C12C13C14-58.7(6) C3AAC0AAC9AAFe458.1(3)
Fe2C13C14C15-57.6(5) C3AAC0AAC9AAC8AA-1.0(6)
Fe2C14C15C11-63.6(4) C3AAC5AAC8AAFe4-59.2(4)
Fe2C16C17C1858.9(5) C3AAC5AAC8AAC9AA0.1(6)
Fe2C16C20C19-59.2(5) C5C1C2Fe158.8(3)
Fe2C17C18C1961.4(5) C5C1C2C3-0.5(5)
Fe2C18C19C2059.1(5) C5C1C2C31-178.9(5)
Fe2C19C20C1659.2(5) C5AAC8AAC9AAFe4-59.6(4)
Fe3C21C22C23-61.1(4) C5AAC8AAC9AAC0AA0.6(6)
Fe3C21C22C34121.7(5) C6C7C8Fe1-59.9(4)
Fe3C21C25C2458.8(4) C6C7C8C91.3(7)
Fe3C22C23C24-58.8(4) C6AAC1AAC2AAFe4-59.6(4)
Fe3C22C34N2161.1(4) C6AAC1AAC2AAC7AA-0.1(6)
Fe3C23C24C25-59.4(4) C6AAC4AAC7AAFe459.4(4)
Fe3C24C25C21-59.3(4) C6AAC4AAC7AAC2AA0.4(6)
Fe3C26C27C28-58.9(6) C7C6C10Fe159.6(4)
Fe3C26C30C2959.9(5) C7C6C10C90.3(7)
Fe3C27C28C29-60.1(8) C7C8C9Fe1-60.7(4)
Fe3C28C29C30-61.0(6) C7C8C9C10-1.1(7)
Fe3C29C30C26-60.7(5) C7AAC4AAC6AAFe4-59.7(4)
Fe4C0AAC3AAC5AA59.3(4) C7AAC4AAC6AAC1AA-0.5(6)
Fe4C0AAC9AAC8AA-59.1(4) C8C9C10Fe1-58.9(4)
Fe4C1AAC2AAC7AA59.5(4) C8C9C10C60.5(7)
Fe4C1AAC6AAC4AA-59.4(4) C9AAC0AAC3AAFe4-58.2(3)
Fe4C2AAC7AAC4AA59.2(4) C9AAC0AAC3AAC5AA1.1(6)
Fe4C3AAC5AAC8AA59.4(4) C10C6C7Fe1-60.3(4)
Fe4C4AAC6AAC1AA59.2(4) C10C6C7C8-1.0(7)
Fe4C4AAC7AAC2AA-58.9(4) C11Si1O2Zn1107.3(3)
Fe4C5AAC8AAC9AA59.3(4) C11Si1O3Si2-115.7(3)
Fe4C8AAC9AAC0AA60.2(4) C11Si1C1Fe1-7.9(4)
Si1C1C2Fe1-129.3(4) C11Si1C1C284.6(5)
Si1C1C2C3171.5(4) C11Si1C1C5-105.4(5)
Si1C1C2C31-6.9(7) C11C12C13Fe254.9(5)
Si1C1C5Fe1130.0(4) C11C12C13C14-3.8(9)
Si1C1C5C4-171.4(4) C12C11C15Fe2-59.9(4)
Si1C11C12Fe2-131.5(4) C12C11C15C140.2(6)
Si1C11C12C13172.3(6) C12C13C14Fe261.4(6)
Si1C11C15Fe2131.4(5) C12C13C14C153.8(9)
Si1C11C15C14-168.4(5) C13C14C15Fe261.1(6)
Si2C0AAC3AAFe4127.2(4) C13C14C15C11-2.5(8)
Si2C0AAC3AAC5AA-173.5(4) C15C11C12Fe258.4(4)
Si2C0AAC9AAFe4-127.3(4) C15C11C12C132.2(9)
Si2C0AAC9AAC8AA173.6(4) C16C17C18Fe2-59.5(5)
Si2C21C22Fe3-128.2(4) C16C17C18C191.9(8)
Si2C21C22C23170.7(4) C17C16C20Fe259.7(5)
Si2C21C22C34-6.5(8) C17C16C20C190.5(8)
Si2C21C25Fe3129.3(4) C17C18C19Fe2-60.7(5)
Si2C21C25C24-171.9(4) C17C18C19C20-1.6(8)
O1Si2O3Si16.1(4) C18C19C20Fe2-58.5(5)
O1Si2C0AAFe4-60.9(4) C18C19C20C160.7(8)
O1Si2C0AAC3AA-153.9(4) C20C16C17Fe2-60.3(5)
O1Si2C0AAC9AA32.5(5) C20C16C17C18-1.5(8)
O1Si2C21Fe3-125.8(3) C21Si2O1Zn1-128.5(3)
O1Si2C21C22-32.8(5) C21Si2O3Si1122.7(3)
O1Si2C21C25139.0(4) C21Si2C0AAFe4179.7(3)
O2Si1O3Si28.6(4) C21Si2C0AAC3AA86.6(5)
O2Si1C1Fe1-126.8(3) C21Si2C0AAC9AA-86.9(5)
O2Si1C1C2-34.3(5) C21C22C23Fe361.5(4)
O2Si1C1C5135.7(4) C21C22C23C242.8(6)
O2Si1C11Fe2-68.3(5) C21C22C34N269.7(7)
O2Si1C11C1224.6(6) C22C21C25Fe3-57.4(3)
O2Si1C11C15-168.3(6) C22C21C25C241.4(6)
O3Si1O2Zn1-17.6(3) C22C23C24Fe357.6(4)
O3Si1C1Fe1113.0(3) C22C23C24C25-1.8(6)
O3Si1C1C2-154.4(4) C23C22C34N2-107.0(6)
O3Si1C1C515.5(5) C23C24C25Fe359.5(4)
O3Si1C11Fe257.3(5) C23C24C25C210.2(6)
O3Si1C11C12150.1(5) C25C21C22Fe358.6(3)
O3Si1C11C15-42.8(7) C25C21C22C23-2.5(6)
O3Si2O1Zn1-12.7(3) C25C21C22C34-179.7(5)
O3Si2C0AAFe465.4(4) C26C27C28Fe359.1(6)
O3Si2C0AAC3AA-27.7(5) C26C27C28C29-1.0(12)
O3Si2C0AAC9AA158.8(4) C27C26C30Fe3-60.8(5)
O3Si2C21Fe3113.2(3) C27C26C30C29-0.9(8)
O3Si2C21C22-153.8(4) C27C28C29Fe361.4(7)
O3Si2C21C2517.9(5) C27C28C29C300.4(12)
C0AASi2O1Zn1110.4(3) C28C29C30Fe361.0(6)
C0AASi2O3Si1-120.1(3) C28C29C30C260.3(9)
C0AASi2C21Fe3-2.4(4) C30C26C27Fe360.1(5)
C0AASi2C21C2290.6(5) C30C26C27C281.2(9)
C0AASi2C21C25-97.7(5) C31C2C3Fe1-121.8(5)
C0AAC3AAC5AAFe4-60.1(4) C31C2C3C4179.1(5)
C0AAC3AAC5AAC8AA-0.8(6) C32N1C31C259.7(6)
C1Si1O2Zn1-134.3(3) C33N1C31C2-175.4(4)
C1Si1O3Si2124.5(3) C34C22C23Fe3-121.4(6)
C1Si1C11Fe2175.7(4) C34C22C23C24179.9(5)
C1Si1C11C12-91.4(5) C35N2C34C2262.1(6)
C1Si1C11C1575.7(7) C36N2C34C22-174.9(5)

 

Table 8 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for 3111.
AtomxyzU(eq)
H110400(20)1160(40)7620(30)60(20)
H27940(20)3720(70)7020(40)110(30)
H1AA93701014625642
H2AA824056566850
H311762909675534
H3AA90853895515034
H4112412138576930
H4AA9009660436942
H5104553529593029
H5AA82973142405047
H6122114186808857
H6AA98511378545847
H7129382746783874
H7AA8023-167450647
H8127753148669763
H8AA72922268414655
H9120164816629555
H9AA74622488529346
H10116675433712850
H12110083527863786
H131168350669287103
H14116046634853869
H15107066103735097
H1691015384767468
H1796454617879664
H18104856072949765
H19104027755881867
H2095607332768972
H2374167182656038
H2484528007651037
H2591136410635233
H2674844878469048
H2782186454472399
H28780481594948155
H29673178265048155
H3065155644486982
H31A114601989809434
H31B11777903791034
H32A1045116685556
H32B10289-775733256
H32C11037-730738256
H33A11307-301853969
H33B10530-134838569
H33C11054878869969
H34A71024254600145
H34B68265165634345
H35A72785139753264
H35B80405232762464
H35C78194201794164
H36A65833489691573
H36B71862637731473
H36C68832676654873
H38A105615661581982
H38B98796121525282
H38C98675593588482
H39A97758639606977
H39B92767672563577
H39C97158389536677

 

Table 9 Solvent masks information for 3111.
NumberXYZVolumeElectron countContent
10.0000.0180.000412.427.7?
20.500-0.2510.500412.427.7?

Experimental

Single crystals of C49H58Br2Fe4N2O4Si2Zn [3111] 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 ShelXL [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 [3111]

Crystal Data for C49H58Br2Fe4N2O4Si2Zn (=1243.74 g/mol): monoclinic, space group P21/n (no. 14), a = 22.0084(17) Å, b = 11.8011(5) Å, c = 23.1333(18) Å, β = 115.664(9)°, = 5415.5(7) Å3, Z = 4, T = 150 K, μ(MoKα) = 3.044 mm-1, Dcalc = 1.525 g/cm3, 50421 reflections measured (4.84° ≤ 2Θ ≤ 51.998°), 10638 unique (Rint = 0.0716, Rsigma = 0.0880) which were used in all calculations. The final R1 was 0.0563 (I > 2σ(I)) and wR2 was 0.1390 (all data).

Refinement model description

Number of restraints - 42, 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. Rigid bond restraints
C26, C27, C28, C29, C30
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C29) ≈ Ueq, Uanis(C28) ≈ Ueq, Uanis(C27) ≈ Ueq, Uanis(C26)
≈ Ueq, Uanis(C30) ≈ Ueq: with sigma of 0.1 and sigma for terminal atoms
of 0.2
5.a Secondary CH2 refined with riding coordinates:
C31(H31A,H31B), C34(H34A,H34B)
5.b Aromatic/amide H refined with riding coordinates:
C1AA(H1AA), C2AA(H2AA), C3(H3), C3AA(H3AA), C4(H4), C4AA(H4AA), C5(H5),
C5AA(H5AA), C6(H6), C6AA(H6AA), C7(H7), C7AA(H7AA), C8(H8), C8AA(H8AA), C9(H9),
C9AA(H9AA), C10(H10), C12(H12), C13(H13), C14(H14), C15(H15), 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)
5.c Idealised Me refined as rotating group:
C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,
H36C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C)

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