3239

Table 1 Crystal data and structure refinement for 3239.
Identification code 3239
Empirical formula C96H156Cl6Fe6N6Si6
Formula weight 2110.60
Temperature/K 173.15
Crystal system monoclinic
Space group P21
a/Å 13.7887(10)
b/Å 26.7489(19)
c/Å 15.0402(18)
α/° 90.0
β/° 101.546(9)
γ/° 90.0
Volume/Å3 5435.1(8)
Z 2
ρcalcg/cm3 1.290
μ/mm‑1 1.037
F(000) 2232.0
Crystal size/mm3 0.1 × 0.02 × 0.01
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.732 to 52
Index ranges -16 ≤ h ≤ 17, -32 ≤ k ≤ 32, -18 ≤ l ≤ 16
Reflections collected 44583
Independent reflections 21323 [Rint = 0.0984, Rsigma = 0.1960]
Data/restraints/parameters 21323/13/1121
Goodness-of-fit on F2 1.009
Final R indexes [I>=2σ (I)] R1 = 0.0765, wR2 = 0.1133
Final R indexes [all data] R1 = 0.1572, wR2 = 0.1450
Largest diff. peak/hole / e Å-3 1.37/-0.49
Flack parameter0.011(14)

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for 3239. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Fe18200.9(12)8303.5(6)7813.4(14)29.8(5)
Si110284(2)7609.8(13)8747(3)33.7(10)
N18785(8)7228(3)5790(8)39(3)
C18969(8)7639(4)8127(9)27(3)
C28526(8)7684(4)7163(9)24(3)
C37495(9)7726(4)7080(10)34(4)
C47269(9)7724(4)7961(10)35(4)
C58144(9)7676(4)8579(10)34(3)
C69054(14)8882(5)8375(15)71(6)
C79011(12)8891(5)7462(14)50(5)
C88044(12)8936(5)7027(11)50(4)
C97437(11)8964(5)7638(15)59(6)
C108058(19)8933(6)8529(14)81(7)
C1110320(10)7816(5)9940(9)51(4)
C1211129(9)8000(5)8220(11)55(5)
C1310745(10)6951(5)8772(11)62(5)
C149052(9)7682(4)6391(9)33(3)
C159162(11)6752(5)6282(11)62(5)
C169156(9)7284(5)4947(9)41(4)
Fe25876.3(12)5852.3(6)7907.8(13)25.4(4)
Si24020(3)6597.0(14)8495(4)48.2(13)
N24608(7)6867(3)5678(8)32(3)
C175186(9)6515(4)8052(10)30(3)
C185359(8)6444(4)7143(10)27(3)
C196393(9)6393(4)7181(10)30(3)
C206867(9)6438(4)8109(9)26(3)
C216129(10)6508(4)8623(10)32(3)
C224912(9)5278(4)7969(12)39(4)
C235345(11)5224(4)7220(10)42(4)
C246369(10)5182(4)7542(11)39(4)
C256567(10)5212(5)8483(11)43(4)
C265646(11)5281(4)8742(10)42(4)
C274301(12)6350(6)9694(12)86(7)
C282911(10)6281(6)7786(14)90(8)
C293711(10)7267(5)8506(12)61(5)
C304598(9)6410(4)6280(10)35(3)
C314387(9)7338(4)6128(10)36(4)
C323940(10)6787(5)4793(11)52(4)
Fe35557.8(12)4174.5(6)2195.9(13)26.4(5)
Si37447(3)4950.7(14)1693(3)36.1(10)
N36228(7)5370(3)4232(7)27(3)
C336218(8)4845(4)2002(9)29(3)
C345887(8)4837(4)2863(9)23(3)
C354849(8)4750(4)2682(9)27(3)
C364507(8)4710(4)1739(10)32(4)
C375342(9)4773(4)1331(10)32(3)
C386638(9)3639(5)2322(11)38(4)
C396136(10)3605(4)3055(10)36(3)
C405119(10)3510(4)2686(9)32(3)
C414984(10)3498(4)1726(10)36(4)
C425943(10)3576(4)1508(10)40(4)
C437621(9)4498(5)784(9)46(4)
C447383(11)5593(5)1159(11)63(5)
C458523(8)4876(5)2638(9)43(4)
C466480(8)4899(4)3779(9)27(3)
C476404(10)5820(5)3728(10)51(4)
C486746(9)5397(5)5207(10)48(4)
Fe41788.4(12)5886.7(6)1903.3(14)31.2(5)
Si4-237(3)6519.0(13)2458(3)36.5(10)
N41318(7)5524(4)4674(8)34(3)
C49480(8)5930(4)2362(9)28(3)
C501232(8)5667(4)2981(10)30(3)
C511535(9)5249(4)2555(10)35(4)
C52986(10)5244(5)1640(11)45(4)
C53362(9)5653(4)1526(9)32(3)
C542170(10)6572(5)1482(12)47(4)
C552800(10)6432(6)2319(12)51(4)
C563277(10)6005(6)2162(13)58(5)
C572946(10)5848(6)1255(12)53(4)
C582250(10)6208(5)838(12)49(4)
C59-782(10)6743(5)1275(10)49(4)
C60-1266(9)6353(4)3046(10)46(4)
C61514(9)7037(5)3080(11)58(5)
C621667(8)5820(5)3935(9)32(3)
C631493(9)4984(5)4606(10)48(4)
C641800(9)5715(6)5590(10)56(5)
Fe55980.1(11)3302.9(6)8514.3(13)24.0(4)
Si53812(2)2565.9(13)7987(3)31.7(9)
N54152(6)3613(3)5787(7)25(2)
C654490(8)3186(4)8121(9)24(3)
C664851(8)3470(4)7460(9)28(3)
C675301(8)3918(4)7889(9)26(3)
C685190(9)3907(4)8808(11)38(4)
C694705(8)3458(4)8952(9)30(3)
C706698(8)2641(5)8865(10)34(3)
C716907(9)2821(5)8049(10)38(4)
C727373(8)3302(5)8204(10)38(4)
C737417(9)3404(5)9134(11)43(4)
C746998(9)3001(5)9550(10)39(4)
C753609(10)2383(5)9146(10)52(4)
C762609(9)2654(5)7178(10)47(4)
C774498(9)2052(4)7567(10)47(4)
C784875(8)3343(4)6513(8)24(3)
C794279(8)4167(4)5837(9)29(3)
C804258(9)3422(4)4896(8)35(3)
Fe6-344.2(12)5026.0(6)8191.7(13)28.1(5)
Si61779(2)4262.6(14)8481(3)35.8(10)
N6-761(7)3937(4)5965(7)31(3)
C81421(9)4364(4)8248(10)29(3)
C82-350(8)4397(4)7429(9)21(3)
C83-1286(8)4461(4)7659(9)24(3)
C84-1155(9)4462(4)8614(10)33(4)
C85-111(9)4404(4)8975(10)34(3)
C86655(10)5592(4)8145(10)37(4)
C87-167(10)5629(4)7406(9)33(3)
C88-1023(10)5687(4)7775(11)38(4)
C89-750(9)5676(4)8744(11)42(4)
C90308(10)5612(4)8959(10)37(4)
C912390(8)4673(5)9453(9)39(4)
C922361(9)4414(6)7488(10)61(5)
C931973(10)3593(5)8841(12)66(5)
C94-200(8)4371(4)6472(9)28(3)
C95-395(9)3448(4)6402(10)39(4)
C96-702(9)3956(5)4966(9)44(4)
Cl16537(2)7043.9(12)4996(3)40.5(9)
Cl29220(2)5475.5(13)4954(3)38.5(9)
Cl34161(2)5353.6(11)4655(2)32.7(8)
Cl46967(2)3991.5(13)5688(3)43.6(10)
Cl51892(2)3634.7(12)5381(2)35.4(8)
Cl6A1754(3)7159(2)5715(5)61(2)
Cl6B7211(9)2806(4)5779(8)53(4)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for 3239. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Fe128.9(10)17.8(9)40.6(13)-4.8(10)2.1(9)1.2(8)
Si127(2)32(2)39(3)10(2)-0.8(18)0.3(17)
N143(7)21(6)49(9)-3(6)3(6)2(5)
C126(7)19(6)36(9)7(7)6(6)2(5)
C230(7)17(6)22(8)-8(6)-1(6)1(5)
C326(7)21(7)51(11)-3(7)0(7)0(5)
C424(7)24(7)55(12)3(7)1(7)2(6)
C541(8)24(7)33(9)0(7)-2(7)-10(6)
C677(13)23(9)89(18)3(11)-40(12)-9(9)
C756(11)17(7)83(15)0(9)28(11)-5(7)
C868(11)29(8)45(11)-5(8)-5(9)-2(8)
C939(9)17(7)130(20)-10(10)40(12)1(7)
C10170(20)28(9)61(16)-21(10)65(16)-20(12)
C1163(10)52(9)32(10)7(8)-1(8)-5(8)
C1231(8)66(11)65(13)31(10)0(8)-1(7)
C1344(9)41(9)92(16)-3(10)-7(9)16(7)
C1442(8)21(7)32(9)-5(7)1(7)-4(6)
C1587(12)31(8)59(13)-18(9)-3(10)8(8)
C1654(9)43(9)29(10)-4(7)20(8)5(7)
Fe227.6(10)18.9(9)29.3(12)0.5(9)4.8(9)0.5(8)
Si238(2)32(2)84(4)-19(2)34(3)-5.8(18)
N234(6)27(6)29(7)2(6)-9(5)-2(5)
C1726(7)18(7)46(10)-8(7)6(7)-3(6)
C1827(7)15(6)37(10)-1(6)2(7)7(5)
C1941(8)18(7)33(10)6(7)12(7)0(6)
C2023(7)14(6)41(10)-4(6)10(7)2(5)
C2158(9)15(6)27(9)-7(6)18(8)-4(6)
C2225(7)16(6)75(10)9(7)6(7)-7(5)
C2382(11)8(6)27(9)9(6)-12(8)-14(7)
C2441(9)23(7)57(12)4(8)19(8)11(6)
C2552(9)32(8)37(11)8(8)-14(8)15(7)
C2676(11)27(8)28(10)12(7)21(9)-1(8)
C27102(14)91(14)87(17)24(12)69(13)14(11)
C2835(9)77(12)170(20)-65(14)39(12)-11(8)
C2942(9)54(10)96(16)-23(10)30(10)11(8)
C3047(8)17(7)40(10)4(7)3(7)1(6)
C3143(8)8(6)51(11)1(6)-6(7)7(6)
C3255(9)33(8)63(13)12(9)-2(9)-2(7)
Fe333.1(10)19.2(9)27.5(12)-1.5(9)7.8(9)-0.8(8)
Si338(2)44(2)27(3)-4(2)9.6(19)-15.1(19)
N334(6)26(6)28(7)-8(5)20(5)-9(5)
C3327(7)22(7)36(10)2(7)2(7)-4(5)
C3430(7)16(6)22(8)1(6)6(6)4(5)
C3532(7)24(7)27(9)-3(7)6(6)-5(6)
C3624(7)22(7)50(11)-3(7)3(7)0(6)
C3741(8)25(7)29(9)3(7)3(7)-5(6)
C3830(8)31(8)52(11)0(8)9(8)8(6)
C3956(9)13(6)36(10)1(7)2(8)-1(6)
C4055(9)16(6)30(9)-4(6)21(7)-11(6)
C4145(8)16(7)45(11)-7(7)6(8)0(6)
C4264(10)26(8)37(10)-1(7)25(9)4(7)
C4341(8)71(11)32(10)-16(8)20(7)-17(7)
C4476(11)54(10)57(13)16(9)7(9)-36(8)
C4532(7)71(10)28(9)-3(8)8(7)-21(7)
C4631(7)22(7)28(9)-2(6)12(6)-5(6)
C4775(10)25(7)59(12)4(8)27(9)1(8)
C4826(7)66(11)54(12)-8(9)13(8)3(7)
Fe430.4(10)22.8(10)42.8(14)5.9(10)12.6(10)1.1(8)
Si433(2)28(2)49(3)-2(2)10(2)2.6(17)
N425(6)45(7)32(8)1(6)6(5)2(5)
C4918(6)25(7)42(10)-8(7)10(6)-4(5)
C5023(7)26(7)41(10)-2(7)8(7)-6(6)
C5147(9)25(7)40(10)12(7)27(8)11(6)
C5247(9)37(9)60(13)-8(8)31(9)-3(7)
C5333(7)34(8)29(9)-4(7)3(7)-7(6)
C5440(9)37(9)62(13)14(9)9(9)-2(7)
C5544(10)54(10)54(13)4(9)7(9)-31(8)
C5622(8)65(12)88(16)41(11)13(9)2(8)
C5745(9)46(9)73(14)19(10)24(9)4(8)
C5841(9)54(10)55(12)6(9)17(8)-7(8)
C5954(9)37(8)58(12)6(8)17(9)8(7)
C6048(9)28(7)65(13)0(8)19(8)11(6)
C6141(8)38(8)96(15)-19(9)18(9)0(7)
C6232(7)24(7)38(9)8(7)3(6)-8(6)
C6350(8)38(8)64(12)18(9)27(8)7(7)
C6436(8)91(13)37(11)-2(10)1(8)12(8)
Fe523.1(9)18.1(9)29.0(12)-0.6(9)0.7(8)1.2(8)
Si531(2)26(2)35(3)4.4(19)0.7(18)-8.4(17)
N522(5)20(5)33(7)3(5)8(5)2(4)
C6521(6)21(7)29(9)-2(6)6(6)1(5)
C6629(7)22(7)33(9)-5(6)6(6)2(5)
C6721(7)21(7)33(9)-1(6)-1(6)1(5)
C6837(8)15(7)60(12)-6(7)5(8)5(6)
C6925(7)29(7)37(9)7(7)9(6)4(5)
C7028(7)30(8)43(10)4(8)2(7)7(6)
C7144(8)38(8)25(9)-2(7)-7(7)13(7)
C7215(6)43(8)58(11)15(9)13(7)8(6)
C7335(8)30(8)60(12)-4(8)0(8)6(6)
C7437(8)44(9)35(10)7(8)6(7)17(7)
C7560(10)55(10)43(11)4(8)14(8)-9(8)
C7649(9)44(9)41(11)-15(8)-5(7)-19(7)
C7758(9)26(7)51(11)-15(8)-2(8)-9(7)
C7825(6)14(6)31(8)8(6)3(6)1(5)
C7937(7)18(6)27(8)6(6)-3(6)-3(6)
C8040(8)39(8)25(9)4(7)7(7)5(6)
Fe630.8(10)21.6(9)33.8(13)1.8(9)10.9(9)-0.2(8)
Si629(2)42(2)34(3)-4(2)1.6(19)6.4(18)
N622(5)40(7)28(7)-5(6)-4(5)-3(5)
C8135(7)16(6)35(10)-1(6)5(7)12(6)
C8236(7)14(6)17(8)3(6)12(6)-5(5)
C8319(6)21(7)31(9)3(6)2(6)0(5)
C8436(8)22(7)46(11)6(7)19(7)9(6)
C8542(8)32(8)27(9)7(7)2(7)9(6)
C8638(8)21(7)52(12)5(7)9(8)-5(6)
C8758(9)20(7)21(9)5(6)6(7)-5(6)
C8835(8)27(8)50(11)3(8)4(8)9(6)
C8934(8)36(8)59(12)-4(8)19(8)2(6)
C9056(9)18(7)37(10)-6(7)9(8)-10(6)
C9139(7)38(8)37(10)7(7)-1(7)9(6)
C9223(7)114(14)46(12)-16(10)8(8)-8(8)
C9354(10)55(10)83(15)-14(10)-3(9)28(8)
C9422(6)19(6)40(10)7(6)-1(6)3(5)
C9534(7)31(8)52(11)-1(7)9(7)2(6)
C9636(8)65(10)24(9)-2(8)-9(7)4(7)
Cl144(2)40(2)37(2)-6.8(18)6.0(17)-5.4(16)
Cl226.7(16)53(2)37(2)6.4(18)8.2(15)1.4(15)
Cl326.1(16)32.6(18)41(2)-1.9(17)11.8(16)1.6(14)
Cl427.3(18)53(2)49(3)13(2)5.0(17)-0.8(16)
Cl527.1(17)37.6(18)41(2)-2.8(18)4.7(16)-0.1(14)
Cl6A10(3)82(5)88(6)-8(4)0(3)0(3)
Cl6B77(9)41(7)44(9)-21(6)19(7)-27(6)

 

Table 4 Bond Lengths for 3239.
AtomAtomLength/Å AtomAtomLength/Å
Fe1C12.075(11) Fe4C492.060(11)
Fe1C22.020(11) Fe4C502.015(13)
Fe1C32.030(12) Fe4C512.032(12)
Fe1C42.055(12) Fe4C522.040(13)
Fe1C52.045(12) Fe4C532.033(12)
Fe1C62.024(15) Fe4C542.042(13)
Fe1C72.056(13) Fe4C552.029(13)
Fe1C82.050(14) Fe4C562.036(13)
Fe1C92.048(13) Fe4C572.032(14)
Fe1C102.028(15) Fe4C582.030(14)
Si1C11.868(12) Si4C491.881(12)
Si1C111.868(14) Si4C591.885(15)
Si1C121.856(13) Si4C601.870(12)
Si1C131.870(12) Si4C611.865(13)
N1C141.514(14) N4C621.519(14)
N1C151.511(15) N4C631.472(15)
N1C161.466(15) N4C641.494(16)
C1C21.462(17) C49C501.432(16)
C1C51.440(16) C49C531.440(16)
C2C31.406(15) C50C511.394(16)
C2C141.487(16) C50C621.496(17)
C3C41.421(18) C51C521.432(19)
C4C51.373(17) C52C531.383(16)
C6C71.36(2) C54C551.43(2)
C6C101.44(2) C54C581.392(19)
C7C81.368(19) C55C561.363(19)
C8C91.36(2) C56C571.41(2)
C9C101.44(2) C57C581.416(18)
Fe2C172.044(12) Fe5C652.045(11)
Fe2C182.003(12) Fe5C662.037(13)
Fe2C192.027(12) Fe5C672.029(12)
Fe2C202.061(11) Fe5C682.047(12)
Fe2C212.051(12) Fe5C692.039(11)
Fe2C222.046(12) Fe5C702.046(12)
Fe2C232.033(12) Fe5C712.036(12)
Fe2C242.031(12) Fe5C722.066(11)
Fe2C252.064(12) Fe5C732.031(13)
Fe2C262.041(12) Fe5C742.043(13)
Si2C171.872(13) Si5C651.894(12)
Si2C271.885(18) Si5C751.884(14)
Si2C281.882(16) Si5C761.865(13)
Si2C291.842(13) Si5C771.850(12)
N2C301.523(14) N5C781.507(14)
N2C311.491(14) N5C791.491(13)
N2C321.475(17) N5C801.470(14)
C17C181.447(18) C65C661.419(16)
C17C211.408(18) C65C691.425(16)
C18C191.422(15) C66C671.440(15)
C18C301.499(17) C66C781.472(16)
C19C201.423(17) C67C681.422(17)
C20C211.408(15) C68C691.414(15)
C22C231.384(18) C70C711.402(17)
C22C261.380(19) C70C741.410(17)
C23C241.403(17) C71C721.436(17)
C24C251.390(18) C72C731.414(18)
C25C261.413(17) C73C741.425(17)
Fe3C332.058(11) Fe6C812.055(11)
Fe3C342.041(12) Fe6C822.035(11)
Fe3C352.036(11) Fe6C832.048(11)
Fe3C362.056(12) Fe6C842.053(12)
Fe3C372.047(12) Fe6C852.026(12)
Fe3C382.048(12) Fe6C862.057(12)
Fe3C392.053(12) Fe6C872.043(12)
Fe3C402.061(11) Fe6C882.040(12)
Fe3C412.044(12) Fe6C892.051(13)
Fe3C422.032(12) Fe6C902.045(12)
Si3C331.866(12) Si6C811.855(12)
Si3C431.877(13) Si6C911.887(13)
Si3C441.891(13) Si6C921.875(14)
Si3C451.848(13) Si6C931.876(14)
N3C461.507(13) N6C941.514(14)
N3C471.468(14) N6C951.505(14)
N3C481.499(16) N6C961.521(15)
C33C341.456(16) C81C821.459(17)
C33C371.423(16) C81C851.437(17)
C34C351.422(15) C82C831.412(15)
C34C461.464(16) C82C941.496(16)
C35C361.407(17) C83C841.411(17)
C36C371.419(15) C84C851.441(17)
C38C391.417(17) C86C871.423(17)
C38C421.405(19) C86C901.401(17)
C39C401.424(16) C87C881.411(16)
C40C411.419(17) C88C891.430(18)
C41C421.439(17) C89C901.439(17)

 

Table 5 Bond Angles for 3239.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C2Fe1C141.8(5) C50Fe4C4941.1(5)
C2Fe1C340.6(4) C50Fe4C5140.3(4)
C2Fe1C468.7(5) C50Fe4C5268.4(5)
C2Fe1C568.7(5) C50Fe4C5368.4(5)
C2Fe1C6131.5(7) C50Fe4C54132.4(6)
C2Fe1C7108.5(5) C50Fe4C55108.1(6)
C2Fe1C8113.9(6) C50Fe4C56115.0(6)
C2Fe1C9143.5(7) C50Fe4C57146.4(6)
C2Fe1C10172.9(8) C50Fe4C58171.4(5)
C3Fe1C168.8(5) C51Fe4C4968.8(5)
C3Fe1C440.7(5) C51Fe4C5241.2(5)
C3Fe1C567.2(5) C51Fe4C5368.1(5)
C3Fe1C7131.9(7) C51Fe4C54169.4(7)
C3Fe1C8109.3(6) C51Fe4C56107.6(6)
C3Fe1C9114.1(6) C51Fe4C57114.6(5)
C4Fe1C168.3(4) C52Fe4C4968.6(5)
C4Fe1C7171.1(7) C52Fe4C54149.2(7)
C5Fe1C140.9(4) C53Fe4C4941.2(5)
C5Fe1C439.1(5) C53Fe4C5239.7(5)
C5Fe1C7148.8(6) C53Fe4C54118.9(6)
C5Fe1C8171.9(6) C53Fe4C56169.5(7)
C5Fe1C9134.8(6) C54Fe4C49110.6(5)
C6Fe1C1109.5(6) C55Fe4C49116.8(6)
C6Fe1C3169.8(8) C55Fe4C51129.0(7)
C6Fe1C4148.9(8) C55Fe4C52168.1(7)
C6Fe1C5118.5(7) C55Fe4C53150.9(6)
C6Fe1C739.0(6) C55Fe4C5441.1(6)
C6Fe1C866.1(6) C55Fe4C5639.2(6)
C6Fe1C968.6(6) C55Fe4C5768.1(6)
C6Fe1C1041.8(7) C55Fe4C5868.5(6)
C7Fe1C1115.7(5) C56Fe4C49147.6(7)
C8Fe1C1145.9(6) C56Fe4C52130.9(6)
C8Fe1C4133.6(6) C56Fe4C5466.9(6)
C8Fe1C738.9(5) C57Fe4C49171.2(6)
C9Fe1C1174.3(7) C57Fe4C52108.1(6)
C9Fe1C4110.4(5) C57Fe4C53131.2(6)
C9Fe1C766.4(5) C57Fe4C5467.8(6)
C9Fe1C838.9(6) C57Fe4C5640.6(6)
C10Fe1C1133.6(8) C58Fe4C49132.5(6)
C10Fe1C3146.4(8) C58Fe4C51148.0(6)
C10Fe1C4116.1(7) C58Fe4C52116.6(6)
C10Fe1C5111.3(6) C58Fe4C53110.4(6)
C10Fe1C767.5(6) C58Fe4C5440.0(5)
C10Fe1C867.1(7) C58Fe4C5667.8(6)
C10Fe1C941.4(7) C58Fe4C5740.8(5)
C1Si1C13109.9(6) C49Si4C59108.1(6)
C11Si1C1107.7(6) C60Si4C49107.3(5)
C11Si1C13108.4(7) C60Si4C59109.0(6)
C12Si1C1113.1(6) C61Si4C49114.4(6)
C12Si1C11110.2(7) C61Si4C59108.3(7)
C12Si1C13107.4(6) C61Si4C60109.6(7)
C15N1C14111.3(11) C63N4C62112.3(10)
C16N1C14110.4(10) C63N4C64110.6(11)
C16N1C15111.3(10) C64N4C62110.4(10)
Si1C1Fe1123.3(6) Si4C49Fe4125.5(6)
C2C1Fe167.1(6) C50C49Fe467.7(6)
C2C1Si1132.1(9) C50C49Si4133.2(10)
C5C1Fe168.4(6) C50C49C53104.9(10)
C5C1Si1123.2(10) C53C49Fe468.4(6)
C5C1C2104.4(10) C53C49Si4121.8(10)
C1C2Fe171.1(7) C49C50Fe471.1(7)
C1C2C14127.0(11) C49C50C62126.1(11)
C3C2Fe170.1(7) C51C50Fe470.5(7)
C3C2C1108.0(11) C51C50C49109.8(12)
C3C2C14125.0(12) C51C50C62124.1(12)
C14C2Fe1124.8(8) C62C50Fe4123.2(8)
C2C3Fe169.3(7) C50C51Fe469.2(7)
C2C3C4108.9(13) C50C51C52107.5(12)
C4C3Fe170.6(8) C52C51Fe469.7(7)
C3C4Fe168.7(7) C51C52Fe469.1(8)
C5C4Fe170.1(7) C53C52Fe469.9(7)
C5C4C3107.7(12) C53C52C51107.9(13)
C1C5Fe170.7(7) C49C53Fe470.4(7)
C4C5Fe170.8(8) C52C53Fe470.4(7)
C4C5C1110.9(13) C52C53C49109.9(13)
C7C6Fe171.8(9) C55C54Fe469.0(8)
C7C6C10108.0(16) C58C54Fe469.5(8)
C10C6Fe169.3(9) C58C54C55108.2(14)
C6C7Fe169.2(9) C54C55Fe469.9(8)
C6C7C8109.0(15) C56C55Fe470.7(9)
C8C7Fe170.3(8) C56C55C54107.2(16)
C7C8Fe170.8(9) C55C56Fe470.2(8)
C9C8Fe170.5(9) C55C56C57110.1(15)
C9C8C7110.7(16) C57C56Fe469.5(8)
C8C9Fe170.6(8) C56C57Fe469.8(8)
C8C9C10107.0(14) C56C57C58106.5(15)
C10C9Fe168.6(9) C58C57Fe469.5(8)
C6C10Fe169.0(9) C54C58Fe470.5(9)
C9C10Fe170.0(9) C54C58C57108.0(15)
C9C10C6105.3(15) C57C58Fe469.7(8)
C2C14N1111.8(10) C50C62N4115.8(10)
C17Fe2C2068.5(4) C65Fe5C6868.7(5)
C17Fe2C2140.2(5) C65Fe5C70110.4(5)
C17Fe2C22109.0(5) C65Fe5C72149.3(6)
C17Fe2C25149.4(6) C66Fe5C6540.7(4)
C18Fe2C1741.9(5) C66Fe5C6868.8(5)
C18Fe2C1941.3(4) C66Fe5C6968.4(5)
C18Fe2C2068.4(5) C66Fe5C70130.2(5)
C18Fe2C2168.2(5) C66Fe5C72115.1(5)
C18Fe2C22117.4(5) C66Fe5C74169.0(5)
C18Fe2C23108.1(5) C67Fe5C6569.3(4)
C18Fe2C24129.9(6) C67Fe5C6641.5(4)
C18Fe2C25168.1(6) C67Fe5C6840.8(5)
C18Fe2C26149.7(5) C67Fe5C6968.7(5)
C19Fe2C1770.1(5) C67Fe5C70167.4(6)
C19Fe2C2040.7(5) C67Fe5C71128.1(5)
C19Fe2C2168.3(5) C67Fe5C72105.1(5)
C19Fe2C22149.6(6) C67Fe5C73115.0(5)
C19Fe2C23116.5(6) C67Fe5C74149.0(5)
C19Fe2C24108.1(5) C68Fe5C72127.5(5)
C19Fe2C25129.5(5) C69Fe5C6540.8(4)
C19Fe2C26168.6(6) C69Fe5C6840.5(4)
C20Fe2C25109.5(5) C69Fe5C70119.8(5)
C21Fe2C2040.1(4) C69Fe5C72166.9(5)
C21Fe2C25118.3(6) C69Fe5C74109.8(5)
C22Fe2C20169.1(6) C70Fe5C68151.5(6)
C22Fe2C21131.5(6) C70Fe5C7268.5(5)
C22Fe2C2566.9(5) C71Fe5C65117.8(5)
C23Fe2C17130.0(6) C71Fe5C66107.8(5)
C23Fe2C20149.8(6) C71Fe5C68166.5(5)
C23Fe2C21168.7(6) C71Fe5C69151.7(5)
C23Fe2C2239.7(5) C71Fe5C7040.2(5)
C23Fe2C2567.4(5) C71Fe5C7241.0(5)
C23Fe2C2667.0(6) C71Fe5C7468.2(5)
C24Fe2C17169.1(6) C73Fe5C65169.7(6)
C24Fe2C20117.6(5) C73Fe5C66148.3(5)
C24Fe2C21150.0(6) C73Fe5C68108.0(5)
C24Fe2C2266.7(5) C73Fe5C69130.5(6)
C24Fe2C2340.4(5) C73Fe5C7067.6(5)
C24Fe2C2539.7(5) C73Fe5C7167.7(5)
C24Fe2C2666.9(5) C73Fe5C7240.4(5)
C26Fe2C17116.8(5) C73Fe5C7441.0(5)
C26Fe2C20131.2(6) C74Fe5C65131.1(5)
C26Fe2C21110.4(5) C74Fe5C68117.5(6)
C26Fe2C2239.5(5) C74Fe5C7040.4(5)
C26Fe2C2540.3(5) C74Fe5C7269.1(5)
C17Si2C27105.8(7) C75Si5C65106.9(6)
C17Si2C28113.8(7) C76Si5C65108.3(6)
C28Si2C27111.9(8) C76Si5C75111.0(6)
C29Si2C17109.5(6) C77Si5C65114.3(5)
C29Si2C27109.6(8) C77Si5C75107.7(6)
C29Si2C28106.2(7) C77Si5C76108.6(6)
C31N2C30112.5(10) C79N5C78112.7(9)
C32N2C30110.0(9) C80N5C78108.8(9)
C32N2C31112.6(10) C80N5C79111.0(9)
Si2C17Fe2126.2(6) Si5C65Fe5127.7(6)
C18C17Fe267.5(7) C66C65Fe569.3(6)
C18C17Si2131.9(10) C66C65Si5129.1(10)
C21C17Fe270.1(7) C66C65C69107.4(10)
C21C17Si2122.6(11) C69C65Fe569.4(6)
C21C17C18105.5(10) C69C65Si5123.5(9)
C17C18Fe270.6(8) C65C66Fe570.0(7)
C17C18C30127.4(11) C65C66C67108.2(11)
C19C18Fe270.2(7) C65C66C78129.3(11)
C19C18C17109.2(12) C67C66Fe569.0(7)
C19C18C30123.4(12) C67C66C78122.3(11)
C30C18Fe2123.8(8) C78C66Fe5122.8(8)
C18C19Fe268.4(7) C66C67Fe569.6(7)
C18C19C20106.9(11) C68C67Fe570.3(7)
C20C19Fe270.9(7) C68C67C66107.3(11)
C19C20Fe268.3(7) C67C68Fe568.9(7)
C21C20Fe269.6(7) C69C68Fe569.5(7)
C21C20C19108.0(11) C69C68C67108.2(12)
C17C21Fe269.6(7) C65C69Fe569.8(6)
C17C21C20110.4(13) C68C69Fe570.0(6)
C20C21Fe270.4(7) C68C69C65108.8(12)
C23C22Fe269.7(7) C71C70Fe569.5(7)
C26C22Fe270.1(7) C71C70C74108.9(12)
C26C22C23108.9(12) C74C70Fe569.7(7)
C22C23Fe270.7(8) C70C71Fe570.3(7)
C22C23C24107.2(13) C70C71C72109.2(13)
C24C23Fe269.7(7) C72C71Fe570.6(7)
C23C24Fe269.9(7) C71C72Fe568.4(7)
C25C24Fe271.5(8) C73C72Fe568.5(7)
C25C24C23109.0(12) C73C72C71105.2(12)
C24C25Fe268.9(7) C72C73Fe571.1(7)
C24C25C26106.5(12) C72C73C74110.4(13)
C26C25Fe269.0(7) C74C73Fe570.0(7)
C22C26Fe270.4(8) C70C74Fe569.9(8)
C22C26C25108.3(13) C70C74C73106.3(13)
C25C26Fe270.7(7) C73C74Fe569.1(8)
C18C30N2112.2(10) C66C78N5116.8(9)
C33Fe3C40166.4(6) C81Fe6C86107.1(5)
C34Fe3C3341.6(5) C82Fe6C8141.8(5)
C34Fe3C3668.4(5) C82Fe6C8340.5(4)
C34Fe3C3767.9(5) C82Fe6C8468.0(5)
C34Fe3C38118.4(5) C82Fe6C86121.1(5)
C34Fe3C39108.3(5) C82Fe6C87108.3(5)
C34Fe3C40128.7(5) C82Fe6C88126.4(6)
C34Fe3C41166.2(5) C82Fe6C89163.3(5)
C35Fe3C3369.5(5) C82Fe6C90154.6(5)
C35Fe3C3440.8(4) C83Fe6C8170.1(5)
C35Fe3C3640.2(5) C83Fe6C8440.2(5)
C35Fe3C3767.5(5) C83Fe6C86155.0(6)
C35Fe3C38152.6(6) C83Fe6C89125.5(5)
C35Fe3C39119.3(5) C84Fe6C8170.1(5)
C35Fe3C40109.1(5) C84Fe6C86164.0(6)
C35Fe3C41127.8(5) C85Fe6C8141.2(5)
C36Fe3C3369.3(5) C85Fe6C8268.4(5)
C36Fe3C40118.9(5) C85Fe6C8368.7(5)
C37Fe3C3340.6(5) C85Fe6C8441.4(5)
C37Fe3C3640.4(4) C85Fe6C86126.5(5)
C37Fe3C38128.1(5) C85Fe6C87163.9(5)
C37Fe3C39165.8(5) C85Fe6C88154.1(5)
C37Fe3C40152.4(5) C85Fe6C89119.0(6)
C38Fe3C33106.8(5) C85Fe6C90107.5(6)
C38Fe3C36165.8(6) C87Fe6C81125.8(5)
C38Fe3C3940.4(5) C87Fe6C83119.8(5)
C38Fe3C4067.9(5) C87Fe6C84153.5(5)
C39Fe3C33127.5(5) C87Fe6C8640.6(5)
C39Fe3C36152.5(5) C87Fe6C8968.8(5)
C39Fe3C4040.5(5) C87Fe6C9068.3(5)
C41Fe3C33150.9(6) C88Fe6C81163.8(6)
C41Fe3C36107.7(5) C88Fe6C83107.6(5)
C41Fe3C37118.4(6) C88Fe6C84119.2(5)
C41Fe3C3868.7(5) C88Fe6C8667.7(5)
C41Fe3C3968.6(5) C88Fe6C8740.4(5)
C41Fe3C4040.4(5) C88Fe6C8940.9(5)
C42Fe3C33116.5(5) C88Fe6C9068.4(5)
C42Fe3C34151.4(5) C89Fe6C81153.3(6)
C42Fe3C35166.1(5) C89Fe6C84106.7(5)
C42Fe3C36128.1(6) C89Fe6C8668.2(5)
C42Fe3C37108.2(5) C90Fe6C81118.3(5)
C42Fe3C3840.3(5) C90Fe6C83163.5(5)
C42Fe3C3968.1(6) C90Fe6C84126.4(6)
C42Fe3C4068.2(5) C90Fe6C8639.9(5)
C42Fe3C4141.4(5) C90Fe6C8941.2(5)
C33Si3C43109.8(6) C81Si6C91109.8(6)
C33Si3C44106.0(6) C81Si6C92113.2(6)
C43Si3C44106.1(7) C81Si6C93105.9(6)
C45Si3C33115.0(6) C92Si6C91107.2(6)
C45Si3C43106.9(6) C92Si6C93112.2(7)
C45Si3C44112.7(6) C93Si6C91108.4(7)
C47N3C46112.2(9) C94N6C96110.4(10)
C47N3C48111.7(10) C95N6C94110.7(9)
C48N3C46111.9(10) C95N6C96112.4(10)
Si3C33Fe3128.1(6) Si6C81Fe6128.6(6)
C34C33Fe368.6(6) C82C81Fe668.4(6)
C34C33Si3133.2(10) C82C81Si6134.9(10)
C37C33Fe369.3(7) C85C81Fe668.3(6)
C37C33Si3121.9(10) C85C81Si6121.1(11)
C37C33C34104.8(10) C85C81C82104.0(10)
C33C34Fe369.8(7) C81C82Fe669.8(7)
C33C34C46128.4(10) C81C82C94126.2(10)
C35C34Fe369.4(7) C83C82Fe670.3(7)
C35C34C33108.4(11) C83C82C81110.4(11)
C35C34C46123.3(11) C83C82C94123.4(11)
C46C34Fe3126.0(8) C94C82Fe6126.5(8)
C34C35Fe369.8(6) C82C83Fe669.3(6)
C36C35Fe370.7(7) C84C83Fe670.1(7)
C36C35C34109.0(11) C84C83C82108.2(11)
C35C36Fe369.1(7) C83C84Fe669.7(7)
C35C36C37106.8(11) C83C84C85107.4(11)
C37C36Fe369.4(7) C85C84Fe668.3(7)
C33C37Fe370.1(7) C81C85Fe670.5(7)
C36C37Fe370.1(7) C81C85C84110.1(13)
C36C37C33110.9(12) C84C85Fe670.3(7)
C39C38Fe370.0(7) C87C86Fe669.2(7)
C42C38Fe369.3(7) C90C86Fe669.6(7)
C42C38C39108.3(11) C90C86C87108.8(12)
C38C39Fe369.6(7) C86C87Fe670.2(7)
C38C39C40107.8(13) C88C87Fe669.7(7)
C40C39Fe370.1(7) C88C87C86107.4(13)
C39C40Fe369.4(6) C87C88Fe669.9(7)
C41C40Fe369.1(7) C87C88C89109.1(12)
C41C40C39108.6(11) C89C88Fe670.0(8)
C40C41Fe370.4(7) C88C89Fe669.1(8)
C40C41C42106.8(12) C88C89C90106.3(12)
C42C41Fe368.9(7) C90C89Fe669.2(7)
C38C42Fe370.5(8) C86C90Fe670.5(8)
C38C42C41108.5(13) C86C90C89108.4(13)
C41C42Fe369.7(7) C89C90Fe669.6(7)
C34C46N3112.6(10) C82C94N6111.5(9)

 

Table 6 Hydrogen Bonds for 3239.
DHAd(D-H)/Åd(H-A)/Åd(D-A)/ÅD-H-A/°
N1H1Cl11.002.153.129(11)165.3
N2H2Cl11.002.103.073(10)165.2
N3H3ACl31.002.083.043(9)161.7
N4H4ACl211.002.083.008(10)154.0
N5H5ACl51.002.173.054(9)146.8
N6H6ACl411.002.113.080(9)163.2

1-1+X,+Y,+Z

 

Table 7 Torsion Angles for 3239.
ABCDAngle/˚ ABCDAngle/˚
Fe1C1C2C3-60.7(8) Fe4C49C50C51-60.1(8)
Fe1C1C2C14119.9(12) Fe4C49C50C62117.9(11)
Fe1C1C5C459.5(9) Fe4C49C53C5259.6(8)
Fe1C2C3C4-59.7(9) Fe4C50C51C52-59.4(8)
Fe1C2C14N1-153.8(8) Fe4C50C62N4-165.7(8)
Fe1C3C4C5-59.4(9) Fe4C51C52C53-59.3(9)
Fe1C4C5C1-59.4(8) Fe4C52C53C49-59.6(8)
Fe1C6C7C859.2(10) Fe4C54C55C5661.2(9)
Fe1C6C10C9-61.0(10) Fe4C54C58C57-59.9(9)
Fe1C7C8C959.4(10) Fe4C55C56C5758.2(10)
Fe1C8C9C1059.2(10) Fe4C56C57C5860.1(9)
Fe1C9C10C660.3(10) Fe4C57C58C5460.4(9)
Si1C1C2Fe1-114.9(10) Si4C49C50Fe4-118.5(10)
Si1C1C2C3-175.6(9) Si4C49C50C51-178.6(9)
Si1C1C2C144.9(19) Si4C49C50C62-0.6(18)
Si1C1C5Fe1116.6(9) Si4C49C53Fe4119.3(8)
Si1C1C5C4176.1(8) Si4C49C53C52178.9(8)
C1C2C3Fe161.3(8) C49C50C51Fe460.5(8)
C1C2C3C41.7(13) C49C50C51C521.1(13)
C1C2C14N1114.4(13) C49C50C62N4104.3(13)
C2C1C5Fe1-57.7(8) C50C49C53Fe4-58.2(7)
C2C1C5C41.8(13) C50C49C53C521.4(13)
C2C3C4Fe158.9(8) C50C51C52Fe459.1(8)
C2C3C4C5-0.6(14) C50C51C52C53-0.2(14)
C3C2C14N1-64.9(15) C51C50C62N4-77.9(14)
C3C4C5Fe158.6(9) C51C52C53Fe458.8(9)
C3C4C5C1-0.8(14) C51C52C53C49-0.7(14)
C5C1C2Fe158.6(8) C53C49C50Fe458.6(7)
C5C1C2C3-2.1(13) C53C49C50C51-1.5(12)
C5C1C2C14178.5(10) C53C49C50C62176.5(10)
C6C7C8Fe1-58.5(11) C54C55C56Fe4-60.7(9)
C6C7C8C90.8(17) C54C55C56C57-2.6(16)
C7C6C10Fe161.7(11) C55C54C58Fe458.3(9)
C7C6C10C90.6(17) C55C54C58C57-1.6(15)
C7C8C9Fe1-59.5(10) C55C56C57Fe4-58.5(10)
C7C8C9C10-0.4(17) C55C56C57C581.6(15)
C8C9C10Fe1-60.5(10) C56C57C58Fe4-60.3(9)
C8C9C10C6-0.2(17) C56C57C58C540.1(15)
C10C6C7Fe1-60.1(11) C58C54C55Fe4-58.6(9)
C10C6C7C8-0.9(17) C58C54C55C562.6(15)
C11Si1C1Fe168.8(9) C59Si4C49Fe469.7(9)
C11Si1C1C2156.9(11) C59Si4C49C50161.5(11)
C11Si1C1C5-15.6(11) C59Si4C49C53-15.2(11)
C12Si1C1Fe1-53.2(10) C60Si4C49Fe4-172.9(8)
C12Si1C1C234.8(14) C60Si4C49C50-81.1(12)
C12Si1C1C5-137.7(10) C60Si4C49C53102.2(10)
C13Si1C1Fe1-173.3(8) C61Si4C49Fe4-51.1(11)
C13Si1C1C2-85.2(13) C61Si4C49C5040.7(14)
C13Si1C1C5102.3(11) C61Si4C49C53-135.9(10)
C14C2C3Fe1-119.2(11) C62C50C51Fe4-117.5(11)
C14C2C3C4-178.9(11) C62C50C51C52-177.0(10)
C15N1C14C2-66.9(14) C63N4C62C5056.5(14)
C16N1C14C2168.9(10) C64N4C62C50-179.5(10)
Fe2C17C18C19-59.9(8) Fe5C65C66C67-58.5(8)
Fe2C17C18C30118.2(12) Fe5C65C66C78116.5(12)
Fe2C17C21C2058.7(8) Fe5C65C69C6859.4(8)
Fe2C18C19C20-60.8(8) Fe5C66C67C68-60.4(8)
Fe2C18C30N2-159.6(8) Fe5C66C78N5-162.8(7)
Fe2C19C20C21-58.4(8) Fe5C67C68C69-58.5(8)
Fe2C20C21C17-58.2(8) Fe5C68C69C65-59.2(8)
Fe2C22C23C2460.5(8) Fe5C70C71C7260.1(8)
Fe2C22C26C25-60.9(9) Fe5C70C74C73-59.8(8)
Fe2C23C24C2561.0(9) Fe5C71C72C7358.9(8)
Fe2C24C25C2659.0(9) Fe5C72C73C7459.1(9)
Fe2C25C26C2260.7(9) Fe5C73C74C7060.4(8)
Si2C17C18Fe2-119.2(11) Si5C65C66Fe5-122.4(9)
Si2C17C18C19-179.1(9) Si5C65C66C67179.1(8)
Si2C17C18C30-1(2) Si5C65C66C78-5.9(18)
Si2C17C21Fe2121.0(9) Si5C65C69Fe5122.3(8)
Si2C17C21C20179.7(8) Si5C65C69C68-178.4(8)
C17C18C19Fe260.1(8) C65C66C67Fe559.1(8)
C17C18C19C20-0.7(13) C65C66C67C68-1.3(13)
C17C18C30N2109.9(14) C65C66C78N5107.2(13)
C18C17C21Fe2-58.5(8) C66C65C69Fe5-59.1(8)
C18C17C21C200.1(13) C66C65C69C680.2(13)
C18C19C20Fe259.2(8) C66C67C68Fe559.9(8)
C18C19C20C210.8(13) C66C67C68C691.4(13)
C19C18C30N2-72.3(14) C67C66C78N5-78.4(13)
C19C20C21Fe257.6(8) C67C68C69Fe558.2(8)
C19C20C21C17-0.6(13) C67C68C69C65-1.0(13)
C21C17C18Fe260.2(8) C69C65C66Fe559.1(8)
C21C17C18C190.4(13) C69C65C66C670.6(12)
C21C17C18C30178.5(11) C69C65C66C78175.6(11)
C22C23C24Fe2-61.1(9) C70C71C72Fe5-59.9(9)
C22C23C24C25-0.1(15) C70C71C72C73-1.0(13)
C23C22C26Fe259.0(9) C71C70C74Fe558.6(8)
C23C22C26C25-1.9(15) C71C70C74C73-1.2(13)
C23C24C25Fe2-60.0(9) C71C72C73Fe5-58.9(8)
C23C24C25C26-1.0(15) C71C72C73C740.3(14)
C24C25C26Fe2-58.9(9) C72C73C74Fe5-59.8(9)
C24C25C26C221.8(15) C72C73C74C700.5(14)
C26C22C23Fe2-59.3(9) C74C70C71Fe5-58.7(8)
C26C22C23C241.2(14) C74C70C71C721.4(14)
C27Si2C17Fe261.2(11) C75Si5C65Fe584.0(9)
C27Si2C17C18152.4(12) C75Si5C65C66177.0(10)
C27Si2C17C21-27.0(12) C75Si5C65C69-4.7(11)
C28Si2C17Fe2-62.1(12) C76Si5C65Fe5-156.3(8)
C28Si2C17C1829.1(15) C76Si5C65C66-63.2(11)
C28Si2C17C21-150.3(11) C76Si5C65C69115.1(10)
C29Si2C17Fe2179.3(9) C77Si5C65Fe5-35.0(11)
C29Si2C17C18-89.5(13) C77Si5C65C6658.0(12)
C29Si2C17C2191.1(12) C77Si5C65C69-123.7(10)
C30C18C19Fe2-118.1(11) C78C66C67Fe5-116.3(10)
C30C18C19C20-178.9(10) C78C66C67C68-176.7(10)
C31N2C30C18-60.8(13) C79N5C78C6658.9(12)
C32N2C30C18172.8(11) C80N5C78C66-177.6(9)
Fe3C33C34C35-58.8(8) Fe6C81C82C83-58.7(8)
Fe3C33C34C46120.5(12) Fe6C81C82C94121.1(11)
Fe3C33C37C3658.3(8) Fe6C81C85C8459.3(8)
Fe3C34C35C36-60.0(8) Fe6C82C83C84-59.5(8)
Fe3C34C46N3-154.5(7) Fe6C82C94N6-149.5(8)
Fe3C35C36C37-59.4(8) Fe6C83C84C85-58.1(8)
Fe3C36C37C33-58.3(9) Fe6C84C85C81-59.4(8)
Fe3C38C39C4059.9(8) Fe6C86C87C8860.1(8)
Fe3C38C42C41-59.6(8) Fe6C86C90C89-59.6(8)
Fe3C39C40C4158.1(8) Fe6C87C88C8959.1(9)
Fe3C40C41C4259.6(8) Fe6C88C89C9059.5(8)
Fe3C41C42C3860.0(9) Fe6C89C90C8660.1(9)
Si3C33C34Fe3-122.7(11) Si6C81C82Fe6-123.5(11)
Si3C33C34C35178.5(9) Si6C81C82C83177.8(9)
Si3C33C34C46-2(2) Si6C81C82C94-2.3(19)
Si3C33C37Fe3122.8(9) Si6C81C85Fe6122.9(8)
Si3C33C37C36-178.9(8) Si6C81C85C84-177.8(8)
C33C34C35Fe359.1(8) C81C82C83Fe658.4(8)
C33C34C35C36-0.9(13) C81C82C83C84-1.0(13)
C33C34C46N3113.7(12) C81C82C94N6119.9(11)
C34C33C37Fe3-59.7(8) C82C81C85Fe6-59.5(7)
C34C33C37C36-1.4(13) C82C81C85C84-0.2(13)
C34C35C36Fe359.5(8) C82C83C84Fe659.0(8)
C34C35C36C370.0(13) C82C83C84C850.9(13)
C35C34C46N3-67.0(14) C83C82C94N6-60.3(14)
C35C36C37Fe359.2(8) C83C84C85Fe659.0(8)
C35C36C37C330.9(13) C83C84C85C81-0.4(14)
C37C33C34Fe360.2(8) C85C81C82Fe659.4(8)
C37C33C34C351.4(13) C85C81C82C830.8(13)
C37C33C34C46-179.3(11) C85C81C82C94-179.4(10)
C38C39C40Fe3-59.6(8) C86C87C88Fe6-60.4(8)
C38C39C40C41-1.5(14) C86C87C88C89-1.3(14)
C39C38C42Fe359.2(9) C87C86C90Fe658.1(9)
C39C38C42C41-0.4(14) C87C86C90C89-1.5(14)
C39C40C41Fe3-58.3(8) C87C88C89Fe6-59.1(8)
C39C40C41C421.3(13) C87C88C89C900.4(14)
C40C41C42Fe3-60.6(8) C88C89C90Fe6-59.5(9)
C40C41C42C38-0.6(14) C88C89C90C860.7(14)
C42C38C39Fe3-58.8(9) C90C86C87Fe6-58.4(9)
C42C38C39C401.1(14) C90C86C87C881.7(14)
C43Si3C33Fe342.9(11) C91Si6C81Fe643.3(11)
C43Si3C33C34138.6(12) C91Si6C81C82140.7(12)
C43Si3C33C37-44.7(12) C91Si6C81C85-42.6(11)
C44Si3C33Fe3157.1(9) C92Si6C81Fe6-76.5(11)
C44Si3C33C34-107.2(12) C92Si6C81C8220.9(14)
C44Si3C33C3769.5(11) C92Si6C81C85-162.4(10)
C45Si3C33Fe3-77.6(10) C93Si6C81Fe6160.2(9)
C45Si3C33C3418.1(14) C93Si6C81C82-102.4(13)
C45Si3C33C37-165.2(10) C93Si6C81C8574.3(11)
C46C34C35Fe3-120.3(11) C94C82C83Fe6-121.4(11)
C46C34C35C36179.7(10) C94C82C83C84179.1(10)
C47N3C46C34-60.6(13) C95N6C94C82-61.9(12)
C48N3C46C34172.8(9) C96N6C94C82172.9(9)

 

Table 8 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for 3239.
AtomxyzU(eq)
H180467207562646
H370267751652640
H466287750809842
H582027676925241
H696378850883085
H795638869717560
H878268945638660
H967378999750271
H1078558943909698
H11A101628173994676
H11B1098477581030476
H11C983576251019576
H12A112267843765683
H12B117688032864083
H12C108388333808683
H13A102966732902092
H13B114096933915492
H13C107726844815492
H14A97757685663039
H14B88797989602539
H15A89656465588292
H15B88816718682792
H15C98866765645592
H16A98647364509361
H16B87977555458461
H16C90546972460261
H252946899556138
H1967076339668236
H2075606424834131
H2162506545926439
H2242235308795347
H2350105216660351
H2468505141717547
H2571975189887652
H2655485323934551
H27A3813648010027129
H27B496564589995129
H27C427159849682129
H28A311659667547135
H28B261864997281135
H28C242162128162135
H29A36557405789492
H29B42337443892692
H29C30797308870292
H30A39346375642943
H30B47266107594343
H31A37287315627754
H31B44047621571754
H31C48837389668654
H32A32656732488678
H32B41606495449578
H32C39517083441078
H3A55025359422633
H3544504723312733
H3638444653143339
H375319476869638
H3873283695237245
H3964263639368043
H4046153463302638
H4143783448130743
H426082358491548
H43A78754181106369
H43B8095463744369
H43C6985444137169
H44A6835560463295
H44B8007566396495
H44C72755844160395
H45A84675111312465
H45B91334944241965
H45C85394534287165
H46A71904905374732
H46B63704608415432
H47A71105845371476
H47B62016117402976
H47C60195801310776
H48A74635413524372
H48B65855099552872
H48C65285696548872
H4A5885577460140
H5120175011282342
H5210415002119154
H53-79574097838
H5417666862138156
H5528736605288161
H5637615837259869
H573150555798063
H581899620322659
H59A-249680294373
H59B-11477054130873
H59C-1233648895773
H60A-16576080271968
H60B-16906645305968
H60C-9886246366868
H61A7756933370887
H61B967333307987
H61C10657116278287
H62A15136177400738
H62B23965789402838
H63A10814854404672
H63B13214812512972
H63C21924925459772
H64A15235543605683
H64B16786075562283
H64C25145654569183
H5A34673533587230
H6756144173760931
H6854054159925045
H6945483354951036
H7064032327894441
H7167632652748245
H7276033508777445
H7376913717945252
H74693429791016647
H75A42512338955778
H75B32362069910278
H75C32362647938178
H76A23222977729470
H76B21532385726270
H76C27202646655570
H77A45922131695470
H77B41201741755370
H77C51452012797270
H78A47552980643129
H78B55523410641229
H79A41274290640743
H79B38304322532443
H79C49644252581143
H80A37743587441952
H80B41433061487052
H80C49283492480352
H6A-14733973600638
H83-18994498724329
H84-16614494895640
H851834395960241
H8613285559809645
H87-1425617678040
H88-16775727743546
H89-11805704916150
H907045588955244
H91A30584548969859
H91B19994668993059
H91C24295016923659
H92A21614751726692
H92B21424171700292
H92C30834400767692
H93A26833517897199
H93B16363375835299
H93C17023536938799
H94A5144333647434
H94B-4284687615534
H95A2833388632258
H95B-8243176611658
H95C-4073460705158
H96A-9914270470166
H96B-10693674464766
H96C-83937490866

 

Table 9 Atomic Occupancy for 3239.
AtomOccupancy AtomOccupancy AtomOccupancy
Cl6A0.679(7) Cl6B0.321(7)   

Experimental

Single crystals of C96H156Cl6Fe6N6Si6 [3239] were []. A suitable crystal was selected and [] on a Xcalibur, Sapphire3 diffractometer. The crystal was kept at 173.15 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 [3239]

Crystal Data for C96H156Cl6Fe6N6Si6 (=2110.60 g/mol): monoclinic, space group P21 (no. 4), a = 13.7887(10) Å, b = 26.7489(19) Å, c = 15.0402(18) Å, β = 101.546(9)°, = 5435.1(8) Å3, Z = 2, T = 173.15 K, μ(MoKα) = 1.037 mm-1, Dcalc = 1.290 g/cm3, 44583 reflections measured (4.732° ≤ 2Θ ≤ 52°), 21323 unique (Rint = 0.0984, Rsigma = 0.1960) which were used in all calculations. The final R1 was 0.0765 (I > 2σ(I)) and wR2 was 0.1450 (all data).

Refinement model description

Number of restraints - 13, number of constraints - unknown.

Details:

1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All N(H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C22) ≈ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C23) ≈ Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
3. Others
Sof(Cl6A)=1-FVAR(1)
Sof(Cl6B)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
N1(H1), C5(H5), N2(H2), N3(H3A), N4(H4A), N5(H5A), C73(H73), N6(H6A)
4.b Secondary CH2 refined with riding coordinates:
C14(H14A,H14B), C30(H30A,H30B), C46(H46A,H46B), C62(H62A,H62B), C78(H78A,
H78B), C94(H94A,H94B)
4.c Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C19(H19), C20(H20),
C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C35(H35), C36(H36),
C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C51(H51),
C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C67(H67),
C68(H68), C69(H69), C70(H70), C71(H71), C72(H72), C74(H74), C83(H83),
C84(H84), C85(H85), C86(H86), C87(H87), C88(H88), C89(H89), C90(H90)
4.d Idealised Me refined as rotating group:
C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,
H15C), C16(H16A,H16B,H16C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,
H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C43(H43A,H43B,H43C),
C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C48(H48A,H48B,
H48C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C63(H63A,
H63B,H63C), C64(H64A,H64B,H64C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C),
C77(H77A,H77B,H77C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C91(H91A,H91B,
H91C), C92(H92A,H92B,H92C), C93(H93A,H93B,H93C), C95(H95A,H95B,H95C), C96(H96A,
H96B,H96C)

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.