2870_twin1_hklf4

Table 1 Crystal data and structure refinement for 2870_twin1_hklf4.
Identification code 2870_twin1_hklf4
Empirical formula C50H55Cl4Fe2N2O2Si2Zn
Formula weight 1091.01
Temperature/K 173
Crystal system triclinic
Space group P-1
a/Å 14.1820(10)
b/Å 16.7847(11)
c/Å 21.5947(15)
α/° 77.232(6)
β/° 83.623(6)
γ/° 89.793(6)
Volume/Å3 4981.1(6)
Z 4
ρcalcg/cm3 1.452
μ/mm‑1 1.353
F(000) 2252.0
Crystal size/mm3 0.2 × 0.2 × 0.2
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.58 to 52
Index ranges -17 ≤ h ≤ 17, -20 ≤ k ≤ 20, -26 ≤ l ≤ 26
Reflections collected 22949
Independent reflections 22949 [Rint = ?, Rsigma = 0.1270]
Data/restraints/parameters 22949/48/1165
Goodness-of-fit on F2 0.898
Final R indexes [I>=2σ (I)] R1 = 0.0520, wR2 = 0.0853
Final R indexes [all data] R1 = 0.0971, wR2 = 0.0945
Largest diff. peak/hole / e Å-3 0.82/-0.95

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for 2870_twin1_hklf4. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Zn1-2530.2(5)6045.4(4)4720.2(3)21.17(18)
Cl1-2305.1(11)6046.2(9)3651.5(7)25.7(4)
Cl2-4075.5(11)5730.1(10)5110.1(8)33.1(4)
Cl3-2127.8(14)7237.9(9)4928.1(8)39.8(5)
Cl4-1565.2(11)5044.9(9)5157.2(7)23.8(4)
Zn2-17489.5(5)9100.9(4)4726.3(3)21.75(18)
Cl5-17267.8(12)9683.3(9)3656.8(7)26.9(4)
Cl6-19042.1(11)9199.8(11)5106.0(8)34.8(4)
Cl7-16562.6(11)9883.8(8)5162.9(7)23.7(4)
Cl8-17062.3(13)7793.8(9)4955.5(8)37.8(5)
Fe1-4185.5(6)8548.2(5)2899.9(4)16.6(2)
Si1-3933.3(12)7050.5(9)1993.5(8)15.6(4)
O1-3174(3)6437(2)2367.9(19)22.8(10)
N1-5340(4)6093(3)3886(2)18.9(12)
C1-4637(4)7637(3)2501(3)13.8(14)
C2-4977(4)7509(3)3176(3)11.6(14)
C3-5536(4)8177(3)3286(3)15.5(14)
C4-5552(4)8740(3)2694(3)17.2(14)
C5-5010(4)8415(3)2227(3)16.9(14)
C6-2742(4)8534(4)2867(4)32.2(17)
C7-3148(5)8480(4)3491(4)34.6(18)
C8-3693(5)9183(4)3494(3)31.7(17)
C9-3627(4)9671(4)2881(3)26.0(15)
C10-3039(4)9259(4)2485(3)32.2(17)
C11-4701(4)6853(3)3718(3)17.2(14)
C12-5174(6)5578(4)3414(3)51(2)
C13-6354(5)6273(4)4014(4)54(2)
C14-4774(4)6419(3)1670(3)17.4(15)
C15-4473(5)5738(4)1448(3)23.1(16)
C16-5062(5)5336(4)1137(3)29.5(18)
C17-5959(5)5611(4)1055(3)34.5(19)
C18-6276(5)6268(4)1281(3)34.2(18)
C19-5680(4)6674(4)1594(3)22.6(15)
C20-3291(4)7767(3)1293(3)21.6(15)
C21-3714(6)8031(5)739(3)54(2)
C22-3272(8)8607(5)223(4)80(3)
C23-2399(8)8931(5)265(4)63(3)
C24-1980(6)8687(5)798(4)52(2)
C25-2412(5)8111(4)1308(3)37.0(19)
Fe2-9189.1(6)7641.8(5)2940.8(4)15.2(2)
Si2-8942.0(12)9604.1(9)2008.3(8)16.0(4)
O2-8173(3)9994(2)2382.9(18)20.7(10)
N2-10382(4)9547(3)3899(2)16.8(12)
C26-9680(4)8753(3)2523(3)14.2(14)
C27-9990(4)8527(3)3211(3)13.3(14)
C28-10526(4)7783(3)3328(3)17.7(14)
C29-10557(4)7545(3)2745(3)18.1(15)
C30-10047(4)8125(3)2265(3)18.7(15)
C31-7750(4)7717(4)2883(4)32.5(18)
C32-8131(5)7444(4)3518(3)28.9(17)
C33-8641(5)6710(4)3564(3)31.8(18)
C34-8574(4)6536(3)2956(3)24.0(16)
C35-8022(4)7169(4)2522(3)28.9(17)
C36-9692(4)8903(3)3732(3)20.0(15)
C37A-11240(20)9076(17)4326(19)53(9)
C37B-11385(9)9349(8)3953(8)28(4)
C38A-10840(30)10124(16)3361(14)78(13)
C38B-10111(10)10344(5)3427(5)19(4)
C39-9723(5)10446(3)1670(3)19.6(15)
C40-10694(5)10329(4)1706(3)26.6(17)
C41-11275(5)10935(4)1420(3)42(2)
C42-10888(5)11682(4)1088(3)33.4(19)
C43-9933(5)11819(4)1039(3)35.3(19)
C44-9353(5)11207(4)1326(3)30.4(18)
C45-8339(5)9225(3)1320(3)24.6(16)
C46-8833(6)9165(4)812(3)39(2)
C47-8435(7)8853(5)307(4)62(3)
C48-7513(8)8604(5)291(4)66(3)
C49-6995(6)8659(4)780(4)57(3)
C50-7406(5)8972(4)1292(3)35.5(19)
Fe3-1802.9(6)2600.4(5)2836.4(4)17.8(2)
Si3-1636.8(12)4580.3(9)1996.3(8)15.8(4)
O3-2604(3)4847(2)2375.9(19)24.6(11)
N3-875(3)4227(3)4023(2)17.8(12)
C51-1103(4)3696(3)2502(3)12.2(13)
C52-1120(4)3412(3)3195(3)12.0(13)
C53-672(4)2642(3)3317(3)15.0(14)
C54-363(4)2436(3)2738(3)23.3(15)
C55-624(4)3075(3)2236(3)13.3(13)
C56-3190(5)2781(4)2687(3)30.1(17)
C57-3117(5)2440(4)3330(3)35.2(18)
C58-2674(5)1675(4)3377(3)31.5(17)
C59-2449(4)1550(4)2751(3)25.6(15)
C60-2778(4)2230(4)2334(3)26.6(16)
C61-1583(4)3835(3)3686(3)18.4(14)
C62-375(4)3602(3)4460(3)25.5(16)
C63-203(4)4800(3)3574(3)25.7(16)
C64-759(4)5452(3)1720(3)17.6(14)
C65196(4)5352(4)1813(3)22.0(16)
C66847(5)5974(4)1556(3)27.9(17)
C67577(5)6708(4)1220(3)29.2(18)
C68-354(5)6821(4)1121(3)30.0(18)
C69-1012(5)6217(4)1374(3)27.5(17)
C70-1898(5)4275(3)1244(3)22.3(16)
C71-1155(5)4263(4)762(3)25.7(16)
C72-1299(6)3998(4)218(3)40(2)
C73-2189(6)3745(4)144(3)39(2)
C74-2938(6)3767(4)594(3)42(2)
C75-2786(5)4028(3)1141(3)27.8(17)
Fe4-16794.9(6)13643.9(5)2839.6(4)17.6(2)
Si4-16667.2(12)12081.4(10)2040.3(8)17.2(4)
O4-17603(3)11580(2)2440.8(19)25.7(11)
N4-15865(4)11346(3)4037(2)21.4(13)
C76-16128(4)12695(3)2526(3)13.6(14)
C77-16133(4)12611(3)3214(3)14.3(14)
C78-15654(4)13304(3)3331(3)14.9(14)
C79-15357(4)13818(4)2721(3)26.4(17)
C80-15637(4)13461(3)2242(3)18.5(15)
C81-18191(5)13586(4)2724(4)33.0(19)
C82-18086(5)13618(4)3363(3)32.7(18)
C83-17592(5)14336(4)3357(3)30.9(18)
C84-17399(5)14761(4)2705(3)34.0(18)
C85-17760(4)14294(4)2314(3)27.9(17)
C86-16578(4)11920(3)3716(3)20.1(15)
C87-15200(4)11024(3)3577(3)26.9(17)
C88-15340(4)11721(4)4472(3)29.0(17)
C89-15759(4)11401(3)1746(3)20.4(15)
C90-14799(5)11564(4)1720(3)36.8(19)
C91-14113(5)11153(4)1415(4)47(2)
C92-14377(5)10539(4)1130(3)34.1(18)
C93-15325(5)10355(4)1161(3)27.7(17)
C94-15997(5)10783(3)1453(3)24.3(16)
C95-17011(5)12790(3)1309(3)19.6(15)
C96-17939(5)13050(4)1246(3)31.5(18)
C97-18161(6)13607(4)710(4)48(2)
C98-17474(7)13926(5)226(4)54(2)
C99-16548(7)13675(5)268(4)60(3)
C100-16334(5)13102(4)804(3)39.2(19)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for 2870_twin1_hklf4. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Zn122.0(4)20.8(4)19.4(4)-1.8(4)-2.2(4)1.2(3)
Cl125.6(10)33.6(10)18.4(9)-6.1(7)-4.6(7)4.6(8)
Cl222.9(10)44(1)24.5(10)8.8(8)-1.8(8)-2.0(8)
Cl367.0(14)25.4(9)27.7(11)-10.3(8)0.5(9)-2.2(9)
Cl428.3(10)24.7(8)20.1(9)-6.6(7)-6.7(7)8.4(7)
Zn223.2(5)23.2(4)20.0(4)-7.0(4)-2.7(4)-1.4(3)
Cl526.8(10)32.8(10)19.9(10)-2.4(7)-4.8(8)-1.2(8)
Cl621.2(9)58.8(12)30.4(11)-23.2(9)-2.3(8)-0.4(8)
Cl726.0(9)22.5(8)22.0(9)-1.2(7)-7.3(8)-7.2(7)
Cl863.4(14)22.0(9)27.6(10)-3.2(7)-8.4(9)-0.2(9)
Fe114.5(5)13.6(5)22.8(6)-5.5(4)-3.7(4)-1.2(4)
Si117.8(10)15.0(9)14.4(10)-4.0(7)-1.9(8)-2.1(8)
O123(3)21(2)22(3)-1.9(19)0(2)4.7(19)
N130(3)10(3)14(3)1(2)1(2)5(2)
C112(3)12(3)18(4)-4(3)-3(3)-1(3)
C29(3)9(3)16(4)-1(3)-1(3)-1(3)
C34(3)17(3)28(4)-12(3)4(3)-1(3)
C410(3)15(3)29(4)-6(3)-7(3)3(3)
C514(4)17(3)19(4)-2(3)-4(3)-4(3)
C610(4)36(4)58(5)-22(4)-15(4)1(3)
C728(4)33(4)46(4)-4(3)-25(4)-6(3)
C831(4)31(4)44(4)-26(3)-17(3)-3(3)
C926.4(18)24.1(17)28.2(18)-6.8(11)-3.3(11)0.2(10)
C1017(4)30(4)46(4)-5(3)2(3)-13(3)
C1116(4)18(3)18(4)-4(3)-4(3)-1(3)
C1296(7)31(4)22(4)-9(3)10(4)-27(4)
C1317(4)33(4)93(7)14(4)14(4)0(3)
C1427(4)12(3)10(3)2(3)4(3)-2(3)
C1527(4)21(4)22(4)-4(3)-8(3)-4(3)
C1650(5)9(3)31(4)-7(3)-6(4)2(3)
C1743(5)38(5)24(4)-9(3)-3(4)-18(4)
C1827(4)49(5)30(4)-16(4)-3(3)-2(4)
C1920(4)27(4)24(4)-13(3)-2(3)4(3)
C2022(4)15(3)27(4)-5(3)5(3)3(3)
C2160(6)70(6)23(5)8(4)-7(4)-26(5)
C22110(9)73(7)41(6)21(5)-8(6)-27(6)
C2387(8)44(5)44(6)3(5)29(6)-16(5)
C2439(5)48(5)62(7)-11(5)19(5)-18(4)
C2539(5)40(4)25(4)3(3)2(4)-10(4)
Fe213.2(5)13.0(4)19.6(5)-3.4(4)-3.3(4)0.0(4)
Si216.7(10)12.9(9)18(1)-3.0(7)-1.1(8)-4.0(8)
O215(2)26(2)19(2)0.9(19)-0.5(19)-4.8(19)
N224(3)14(3)13(3)-6(2)3(2)-8(2)
C268(3)13(3)20(4)-2(3)2(3)1(3)
C276(3)15(3)18(4)-2(3)-2(3)4(3)
C2818(4)17(3)19(4)-5(3)-1(3)-3(3)
C297(3)11(3)38(4)-11(3)-3(3)-6(3)
C3014(4)22(4)24(4)-12(3)-3(3)3(3)
C3112(4)28(4)61(6)-14(4)-10(4)4(3)
C3226(4)33(4)36(5)-17(3)-18(4)20(3)
C3336(5)17(4)41(5)3(3)-16(4)16(3)
C3425(4)13(3)37(4)-10(3)-7(3)9(3)
C3516(4)36(4)34(4)-8(3)1(3)8(3)
C3621(4)22(3)22(4)-16(3)-1(3)2(3)
C37A42(17)50(20)90(30)-48(18)-22(18)-9(14)
C37B23(7)28(8)39(9)-20(7)-7(7)6(6)
C38A100(30)42(17)110(30)-32(17)-50(20)60(20)
C38B27(8)14(5)14(6)1(4)6(5)10(5)
C3931(4)19(3)13(4)-8(3)-11(3)1(3)
C4031(4)20(4)27(4)2(3)-10(3)0(3)
C4138(5)42(5)48(5)-8(4)-14(4)3(4)
C4245(5)22(4)35(5)-5(3)-18(4)10(4)
C4355(6)12(4)38(5)2(3)-17(4)-3(4)
C4428(4)25(4)37(5)1(3)-10(4)-6(3)
C4532(4)12(3)26(4)0(3)4(3)-6(3)
C4651(5)39(5)23(4)-5(3)9(4)-13(4)
C4797(9)52(6)34(5)-19(4)24(5)-32(6)
C48104(9)40(5)48(6)-28(5)49(6)-31(6)
C4964(7)29(5)68(7)-12(4)43(5)7(4)
C5043(5)23(4)35(5)-7(3)18(4)-5(3)
Fe318.8(6)14.5(5)20.4(6)-4.6(4)-1.6(4)-6.1(4)
Si317.9(10)13.0(9)17.3(10)-4.3(7)-3.5(8)1.8(7)
O317(3)27(2)33(3)-12(2)-7(2)-4(2)
N318(3)17(3)21(3)-8(2)-6(2)4(2)
C5112.4(16)11.9(15)12.9(16)-3.8(10)-1.8(10)-2.1(10)
C527(3)16(3)16(3)-8(3)1(3)-4(2)
C5316(4)11(3)18(3)-1(2)-1(3)-4(3)
C5431(4)10(3)30(4)-5(3)-7(3)4(3)
C5518(4)8(3)15(3)-5(2)1(3)-5(3)
C5630(5)23(4)39(4)-6(3)-8(3)-17(3)
C5731(5)47(4)28(4)-15(3)6(4)-19(4)
C5832(5)30(4)27(4)4(3)-1(3)-25(3)
C5926.8(18)24.7(17)26.4(18)-7.8(11)-3.3(11)-2.4(10)
C6020(4)32(4)29(4)-7(3)-6(3)-16(3)
C6117(4)16(3)23(4)-3(3)-7(3)-3(3)
C6228(4)34(4)12(4)-2(3)1(3)-5(3)
C6324(4)22(4)32(4)-9(3)-1(3)-9(3)
C6424(4)16(3)14(4)-8(3)1(3)-5(3)
C6526(4)18(3)22(4)-3(3)-7(3)2(3)
C6627(4)27(4)26(4)1(3)-2(3)-3(3)
C6735(5)23(4)27(4)-9(3)11(4)-15(3)
C6845(5)5(3)37(5)-1(3)-1(4)8(3)
C6927(4)24(4)32(4)-6(3)-3(3)2(3)
C7029(4)12(3)28(4)-3(3)-9(3)1(3)
C7127(4)34(4)20(4)-9(3)-9(3)6(3)
C7246(5)49(5)29(5)-11(4)-16(4)20(4)
C7371(6)33(4)23(4)-18(3)-24(4)15(4)
C7446(6)42(5)43(5)-11(4)-27(4)-2(4)
C7533(4)21(4)29(4)-1(3)-14(3)7(3)
Fe418.6(6)13.9(5)20.0(5)-3.4(4)-1.3(4)4.3(4)
Si420(1)13.9(9)17.1(10)-2.4(7)-1.9(8)1.3(8)
O419(3)22(2)31(3)5(2)-6(2)3(2)
N426(3)16(3)19(3)3(2)-6(2)1(2)
C768(3)16(3)18(4)-7(3)-1(3)9(3)
C7712(3)11(3)19(4)-2(3)1(3)4(3)
C7816(4)23(3)10(3)-8(3)-7(3)4(3)
C7927(4)18(4)33(4)-6(3)0(3)-5(3)
C8021(4)17(3)18(4)-3(3)-2(3)1(3)
C8123(4)19(4)59(6)-12(4)-9(4)8(3)
C8223(4)41(4)27(5)4(3)1(3)17(3)
C8325(4)33(4)37(5)-15(4)-1(3)15(3)
C8435(5)24(4)45(5)-10(3)-6(4)16(3)
C8524(4)33(4)27(4)-4(3)-8(3)13(3)
C8613(3)22(3)24(4)-3(3)-1(3)1(3)
C8724(4)22(4)33(4)-6(3)3(3)3(3)
C8827(4)32(4)22(4)8(3)-9(3)-2(3)
C8921(4)17(3)22(4)-2(3)-2(3)-2(3)
C9022(4)46(5)53(5)-32(4)-9(4)1(4)
C9111(4)62(5)81(7)-48(5)-1(4)6(4)
C9225(5)42(5)40(5)-21(4)-3(4)14(4)
C9340(5)20(4)26(4)-9(3)-11(3)6(3)
C9422(4)20(4)29(4)-1(3)1(3)1(3)
C9525(4)13(3)23(4)-6(3)-7(3)-2(3)
C9639(5)26(4)29(4)3(3)-18(4)-4(3)
C9762(6)28(4)57(6)-1(4)-35(5)2(4)
C9882(8)36(5)44(6)6(4)-33(5)-6(5)
C9988(8)49(5)30(5)14(4)-2(5)-17(5)
C10040(5)49(5)24(4)-1(4)-1(4)-1(4)

 

Table 4 Bond Lengths for 2870_twin1_hklf4.
AtomAtomLength/Å AtomAtomLength/Å
Zn1Cl12.2945(17) C45C501.387(9)
Zn1Cl22.2803(18) C46C471.377(9)
Zn1Cl32.2380(17) C47C481.371(12)
Zn1Cl42.2713(17) C48C491.370(12)
Zn2Cl52.2880(17) C49C501.398(9)
Zn2Cl62.2821(18) Fe3C512.042(5)
Zn2Cl72.2774(16) Fe3C522.011(5)
Zn2Cl82.2394(17) Fe3C532.015(6)
Fe1C12.053(5) Fe3C542.054(6)
Fe1C22.019(5) Fe3C552.046(6)
Fe1C32.045(6) Fe3C562.040(7)
Fe1C42.045(6) Fe3C572.030(7)
Fe1C52.013(6) Fe3C582.051(6)
Fe1C62.041(6) Fe3C592.047(6)
Fe1C72.040(6) Fe3C602.028(6)
Fe1C82.022(6) Si3O31.632(4)
Fe1C92.040(6) Si3C511.852(6)
Fe1C102.024(6) Si3C641.876(6)
Si1O11.641(4) Si3C701.882(6)
Si1C11.843(6) N3C611.533(7)
Si1C141.886(6) N3C621.483(7)
Si1C201.862(6) N3C631.473(7)
N1C111.522(6) C51C521.464(7)
N1C121.476(7) C51C551.433(7)
N1C131.477(7) C52C531.424(7)
C1C21.452(7) C52C611.497(7)
C1C51.436(7) C53C541.395(8)
C2C31.421(7) C54C551.427(8)
C2C111.505(7) C56C571.397(9)
C3C41.416(8) C56C601.410(8)
C4C51.406(7) C57C581.417(9)
C6C71.391(9) C58C591.416(8)
C6C101.404(8) C59C601.403(8)
C7C81.410(8) C64C651.395(8)
C8C91.389(9) C64C691.403(8)
C9C101.416(8) C65C661.376(8)
C14C151.386(8) C66C671.363(8)
C14C191.369(8) C67C681.367(9)
C15C161.392(8) C68C691.360(8)
C16C171.369(9) C70C711.401(8)
C17C181.360(8) C70C751.384(8)
C18C191.404(8) C71C721.380(8)
C20C211.382(9) C72C731.371(9)
C20C251.383(9) C73C741.365(9)
C21C221.396(10) C74C751.385(9)
C22C231.375(12) Fe4C762.055(5)
C23C241.338(11) Fe4C772.021(5)
C24C251.382(9) Fe4C782.044(6)
Fe2C262.042(5) Fe4C792.042(6)
Fe2C272.016(5) Fe4C802.040(6)
Fe2C282.022(6) Fe4C812.029(7)
Fe2C292.046(6) Fe4C822.038(7)
Fe2C302.033(6) Fe4C832.041(6)
Fe2C312.034(6) Fe4C842.037(6)
Fe2C322.035(6) Fe4C852.035(6)
Fe2C332.039(6) Si4O41.629(4)
Fe2C342.045(5) Si4C761.847(6)
Fe2C352.041(6) Si4C891.871(6)
Si2O21.646(4) Si4C951.867(6)
Si2C261.853(6) N4C861.512(7)
Si2C391.864(6) N4C871.482(7)
Si2C451.865(7) N4C881.502(7)
N2C361.530(7) C76C771.460(7)
N2C37A1.55(3) C76C801.444(7)
N2C37B1.449(14) C77C781.433(7)
N2C38A1.54(2) C77C861.491(7)
N2C38B1.515(10) C78C791.427(8)
C26C271.467(7) C79C801.400(8)
C26C301.422(7) C81C821.417(9)
C27C281.425(7) C81C851.412(8)
C27C361.507(7) C82C831.394(8)
C28C291.407(8) C83C841.428(9)
C29C301.395(8) C84C851.410(8)
C31C321.394(9) C89C901.384(8)
C31C351.411(8) C89C941.391(8)
C32C331.411(8) C90C911.384(8)
C33C341.399(9) C91C921.385(8)
C34C351.425(8) C92C931.372(8)
C39C401.383(8) C93C941.374(8)
C39C441.401(8) C95C961.397(8)
C40C411.388(8) C95C1001.382(8)
C41C421.383(9) C96C971.383(9)
C42C431.364(9) C97C981.364(10)
C43C441.394(8) C98C991.384(11)
C45C461.389(9) C99C1001.394(10)

 

Table 5 Bond Angles for 2870_twin1_hklf4.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
Cl2Zn1Cl1109.94(7) C50C45Si2123.1(5)
Cl3Zn1Cl1112.94(6) C50C45C46116.8(6)
Cl3Zn1Cl2109.34(7) C47C46C45122.4(8)
Cl3Zn1Cl4110.49(7) C48C47C46119.6(9)
Cl4Zn1Cl1103.36(6) C49C48C47120.0(8)
Cl4Zn1Cl2110.66(6) C48C49C50119.9(8)
Cl6Zn2Cl5109.56(7) C45C50C49121.2(8)
Cl7Zn2Cl5103.77(6) C51Fe3C5469.6(2)
Cl7Zn2Cl6109.71(6) C51Fe3C5541.0(2)
Cl8Zn2Cl5113.13(6) C51Fe3C58162.9(2)
Cl8Zn2Cl6109.66(7) C51Fe3C59154.9(2)
Cl8Zn2Cl7110.84(7) C52Fe3C5142.3(2)
C2Fe1C141.8(2) C52Fe3C5341.4(2)
C2Fe1C340.9(2) C52Fe3C5468.9(2)
C2Fe1C468.7(2) C52Fe3C5569.1(2)
C2Fe1C6121.4(2) C52Fe3C56119.2(2)
C2Fe1C7108.0(2) C52Fe3C57106.1(2)
C2Fe1C8125.4(3) C52Fe3C58124.3(2)
C2Fe1C9161.4(2) C52Fe3C59161.8(2)
C2Fe1C10156.3(2) C52Fe3C60155.4(2)
C3Fe1C170.0(2) C53Fe3C5170.4(2)
C3Fe1C440.5(2) C53Fe3C5440.1(2)
C4Fe1C169.8(2) C53Fe3C5568.3(2)
C5Fe1C141.4(2) C53Fe3C56153.8(2)
C5Fe1C268.6(2) C53Fe3C57118.9(3)
C5Fe1C368.1(2) C53Fe3C58106.3(2)
C5Fe1C440.5(2) C53Fe3C59124.7(2)
C5Fe1C6129.2(3) C53Fe3C60162.8(2)
C5Fe1C7165.8(3) C55Fe3C5440.7(2)
C5Fe1C8152.6(2) C55Fe3C58154.6(2)
C5Fe1C9119.5(2) C55Fe3C59120.9(2)
C5Fe1C10109.5(3) C56Fe3C51107.2(2)
C6Fe1C1109.3(2) C56Fe3C54165.2(3)
C6Fe1C3154.4(3) C56Fe3C55127.7(2)
C6Fe1C4164.9(3) C56Fe3C5867.9(3)
C7Fe1C1127.0(2) C56Fe3C5968.5(2)
C7Fe1C3118.9(3) C57Fe3C51125.2(2)
C7Fe1C4152.5(3) C57Fe3C54153.4(3)
C7Fe1C639.9(3) C57Fe3C55164.0(3)
C8Fe1C1164.2(2) C57Fe3C5640.1(3)
C8Fe1C3105.9(3) C57Fe3C5840.6(2)
C8Fe1C4117.6(2) C57Fe3C5968.4(3)
C8Fe1C667.4(3) C58Fe3C54119.3(3)
C8Fe1C740.6(2) C59Fe3C54107.8(2)
C8Fe1C940.0(2) C59Fe3C5840.4(2)
C8Fe1C1067.6(3) C60Fe3C51120.5(2)
C9Fe1C1154.9(2) C60Fe3C54127.6(3)
C9Fe1C3123.7(2) C60Fe3C55110.1(2)
C9Fe1C4105.9(2) C60Fe3C5640.6(2)
C9Fe1C668.1(3) C60Fe3C5767.5(3)
C9Fe1C768.2(3) C60Fe3C5867.3(3)
C10Fe1C1120.8(3) C60Fe3C5940.3(2)
C10Fe1C3162.1(2) O3Si3C51110.5(2)
C10Fe1C4126.2(3) O3Si3C64111.8(2)
C10Fe1C640.4(2) O3Si3C70110.8(3)
C10Fe1C767.8(3) C51Si3C64110.9(3)
C10Fe1C940.8(2) C51Si3C70107.8(2)
O1Si1C1114.0(2) C64Si3C70104.9(3)
O1Si1C14108.4(2) C62N3C61111.5(4)
O1Si1C20109.5(3) C63N3C61112.9(5)
C1Si1C14108.4(3) C63N3C62111.6(5)
C1Si1C20109.5(3) Si3C51Fe3122.5(3)
C20Si1C14106.9(3) C52C51Fe367.7(3)
C12N1C11112.3(5) C52C51Si3132.7(4)
C12N1C13112.3(6) C55C51Fe369.7(3)
C13N1C11113.1(4) C55C51Si3121.9(4)
Si1C1Fe1128.4(3) C55C51C52105.1(5)
C2C1Fe167.8(3) C51C52Fe370.0(3)
C2C1Si1135.6(4) C51C52C61125.7(5)
C5C1Fe167.8(3) C53C52Fe369.5(3)
C5C1Si1120.7(4) C53C52C51108.1(5)
C5C1C2103.7(5) C53C52C61126.1(5)
C1C2Fe170.4(3) C61C52Fe3123.3(4)
C1C2C11128.0(5) C52C53Fe369.1(3)
C3C2Fe170.5(3) C54C53Fe371.4(4)
C3C2C1109.8(5) C54C53C52109.2(5)
C3C2C11121.7(5) C53C54Fe368.5(3)
C11C2Fe1118.9(4) C53C54C55107.8(5)
C2C3Fe168.5(3) C55C54Fe369.4(3)
C4C3Fe169.8(3) C51C55Fe369.3(3)
C4C3C2107.9(5) C54C55Fe369.9(3)
C3C4Fe169.7(3) C54C55C51109.8(5)
C5C4Fe168.5(3) C57C56Fe369.6(4)
C5C4C3107.4(5) C57C56C60107.0(6)
C1C5Fe170.8(3) C60C56Fe369.3(4)
C4C5Fe171.0(3) C56C57Fe370.3(4)
C4C5C1111.3(5) C56C57C58108.6(6)
C7C6Fe170.1(4) C58C57Fe370.4(4)
C7C6C10108.3(6) C57C58Fe368.9(4)
C10C6Fe169.2(4) C59C58Fe369.6(4)
C6C7Fe170.1(4) C59C58C57108.0(6)
C6C7C8107.2(6) C58C59Fe369.9(3)
C8C7Fe169.0(4) C60C59Fe369.2(3)
C7C8Fe170.4(4) C60C59C58106.6(6)
C9C8Fe170.7(4) C56C60Fe370.2(4)
C9C8C7109.5(6) C59C60Fe370.6(4)
C8C9Fe169.3(3) C59C60C56109.8(6)
C8C9C10106.6(6) C52C61N3113.5(5)
C10C9Fe169.0(3) C65C64Si3121.1(4)
C6C10Fe170.4(4) C65C64C69116.7(6)
C6C10C9108.3(6) C69C64Si3122.1(5)
C9C10Fe170.2(4) C66C65C64120.5(6)
C2C11N1114.8(5) C67C66C65121.2(6)
C15C14Si1121.5(5) C66C67C68119.4(6)
C19C14Si1120.0(4) C69C68C67120.4(6)
C19C14C15118.2(6) C68C69C64121.8(6)
C14C15C16121.2(6) C71C70Si3119.3(5)
C17C16C15119.6(6) C75C70Si3123.9(5)
C18C17C16120.2(6) C75C70C71116.8(6)
C17C18C19120.2(7) C72C71C70121.5(7)
C14C19C18120.6(6) C73C72C71119.5(7)
C21C20Si1120.6(5) C74C73C72120.9(7)
C21C20C25116.3(6) C73C74C75119.2(7)
C25C20Si1123.0(5) C70C75C74122.1(7)
C20C21C22121.7(8) C77Fe4C7642.0(2)
C23C22C21119.6(9) C77Fe4C7841.3(2)
C24C23C22119.7(8) C77Fe4C7968.8(2)
C23C24C25120.8(8) C77Fe4C8069.1(2)
C24C25C20121.9(7) C77Fe4C81119.3(2)
C26Fe2C2969.0(2) C77Fe4C82107.0(2)
C26Fe2C34155.5(2) C77Fe4C83125.1(3)
C27Fe2C2642.4(2) C77Fe4C84163.5(3)
C27Fe2C2841.3(2) C77Fe4C85154.0(2)
C27Fe2C2969.1(2) C78Fe4C7670.3(2)
C27Fe2C3069.2(2) C79Fe4C7669.2(2)
C27Fe2C31120.3(2) C79Fe4C7840.9(2)
C27Fe2C32106.3(2) C80Fe4C7641.3(2)
C27Fe2C33123.9(3) C80Fe4C7868.7(2)
C27Fe2C34161.0(2) C80Fe4C7940.1(2)
C27Fe2C35155.8(2) C80Fe4C83152.5(2)
C28Fe2C2669.9(2) C81Fe4C76108.3(2)
C28Fe2C2940.5(2) C81Fe4C78152.6(3)
C28Fe2C3068.0(2) C81Fe4C79166.0(3)
C28Fe2C31154.6(3) C81Fe4C80129.2(3)
C28Fe2C32119.1(3) C81Fe4C8240.8(3)
C28Fe2C33106.1(3) C81Fe4C8368.2(3)
C28Fe2C34124.2(2) C81Fe4C8467.8(3)
C28Fe2C35162.2(2) C81Fe4C8540.6(2)
C30Fe2C2640.8(2) C82Fe4C76127.6(3)
C30Fe2C2940.0(2) C82Fe4C78117.2(3)
C30Fe2C31128.4(3) C82Fe4C79151.5(3)
C30Fe2C32164.5(3) C82Fe4C80166.9(3)
C30Fe2C33154.2(2) C82Fe4C8340.0(2)
C30Fe2C34121.1(2) C83Fe4C76164.3(3)
C30Fe2C35109.4(3) C83Fe4C78105.3(3)
C31Fe2C26108.7(2) C83Fe4C79117.9(3)
C31Fe2C29164.4(3) C84Fe4C76153.4(3)
C31Fe2C3240.1(3) C84Fe4C78125.7(3)
C31Fe2C3367.6(3) C84Fe4C79107.9(3)
C31Fe2C3467.8(2) C84Fe4C80119.5(3)
C31Fe2C3540.5(2) C84Fe4C8267.8(3)
C32Fe2C26126.0(2) C84Fe4C8341.0(2)
C32Fe2C29153.7(3) C85Fe4C76119.1(2)
C32Fe2C3340.5(2) C85Fe4C78164.1(2)
C32Fe2C3467.9(2) C85Fe4C79127.5(3)
C32Fe2C3568.3(3) C85Fe4C80109.1(3)
C33Fe2C26163.1(2) C85Fe4C8268.6(3)
C33Fe2C29119.2(3) C85Fe4C8369.0(3)
C33Fe2C3440.1(2) C85Fe4C8440.5(2)
C33Fe2C3568.2(3) O4Si4C76110.7(2)
C34Fe2C29107.6(2) O4Si4C89112.7(2)
C35Fe2C26120.5(2) O4Si4C95109.6(3)
C35Fe2C29126.3(2) C76Si4C89109.9(3)
C35Fe2C3440.8(2) C76Si4C95108.2(3)
O2Si2C26114.1(2) C95Si4C89105.6(3)
O2Si2C39107.3(2) C87N4C86112.9(5)
O2Si2C45111.4(3) C87N4C88111.3(5)
C26Si2C39109.4(3) C88N4C86112.1(4)
C26Si2C45107.7(3) Si4C76Fe4123.7(3)
C39Si2C45106.8(3) C77C76Fe467.8(3)
C36N2C37A106.5(11) C77C76Si4133.0(4)
C36N2C38A119.5(11) C80C76Fe468.8(3)
C37BN2C36116.9(6) C80C76Si4121.9(4)
C37BN2C38B112.7(7) C80C76C77104.9(5)
C38AN2C37A103.5(15) C76C77Fe470.2(3)
C38BN2C36107.3(5) C76C77C86125.3(5)
Si2C26Fe2125.3(3) C78C77Fe470.2(3)
C27C26Fe267.9(3) C78C77C76109.3(5)
C27C26Si2133.4(4) C78C77C86125.4(5)
C30C26Fe269.2(3) C86C77Fe4125.1(4)
C30C26Si2121.1(4) C77C78Fe468.5(3)
C30C26C27105.4(5) C79C78Fe469.5(3)
C26C27Fe269.8(3) C79C78C77106.7(5)
C26C27C36128.5(5) C78C79Fe469.6(3)
C28C27Fe269.5(3) C80C79Fe469.9(4)
C28C27C26107.2(5) C80C79C78109.3(5)
C28C27C36123.7(5) C76C80Fe469.9(3)
C36C27Fe2118.6(4) C79C80Fe470.0(4)
C27C28Fe269.1(3) C79C80C76109.8(5)
C29C28Fe270.7(3) C82C81Fe469.9(4)
C29C28C27108.8(5) C85C81Fe469.9(4)
C28C29Fe268.8(3) C85C81C82108.5(6)
C30C29Fe269.5(3) C81C82Fe469.3(4)
C30C29C28108.0(5) C83C82Fe470.1(4)
C26C30Fe269.9(3) C83C82C81108.5(6)
C29C30Fe270.5(3) C82C83Fe469.9(4)
C29C30C26110.5(5) C82C83C84107.2(6)
C32C31Fe270.0(4) C84C83Fe469.4(4)
C32C31C35109.2(6) C83C84Fe469.7(4)
C35C31Fe270.0(4) C85C84Fe469.7(3)
C31C32Fe269.9(4) C85C84C83108.8(6)
C31C32C33107.6(6) C81C85Fe469.5(4)
C33C32Fe269.9(4) C84C85Fe469.8(4)
C32C33Fe269.6(3) C84C85C81106.9(6)
C34C33Fe270.2(4) C77C86N4113.4(5)
C34C33C32108.3(6) C90C89Si4121.2(5)
C33C34Fe269.7(3) C90C89C94115.7(6)
C33C34C35108.1(6) C94C89Si4122.3(5)
C35C34Fe269.4(3) C91C90C89122.7(6)
C31C35Fe269.5(4) C90C91C92119.9(7)
C31C35C34106.6(6) C93C92C91118.5(6)
C34C35Fe269.8(3) C92C93C94120.7(6)
C27C36N2112.7(5) C93C94C89122.4(6)
C40C39Si2121.4(5) C96C95Si4123.0(5)
C40C39C44116.6(6) C100C95Si4120.3(5)
C44C39Si2121.8(5) C100C95C96116.6(6)
C39C40C41121.9(6) C97C96C95121.5(7)
C42C41C40120.0(7) C98C97C96120.7(8)
C43C42C41119.8(7) C97C98C99119.4(8)
C42C43C44119.8(6) C98C99C100119.4(8)
C43C44C39121.8(6) C95C100C99122.2(8)
C46C45Si2120.1(5)     

 

Table 6 Hydrogen Bonds for 2870_twin1_hklf4.
DHAd(D-H)/Åd(H-A)/Åd(D-A)/ÅD-H-A/°
N1H1ACl21.002.453.302(5)143.4
N1H1ACl211.002.723.385(5)124.1
N2H2ACl621.002.683.365(5)125.9
N2H2ACl631.002.533.342(5)138.6
N3H3BCl41.002.203.130(5)153.7

1-1-X,1-Y,1-Z; 2-3-X,2-Y,1-Z; 31+X,+Y,+Z

 

Table 7 Torsion Angles for 2870_twin1_hklf4.
ABCDAngle/˚ ABCDAngle/˚
Fe1C1C2C359.7(4) C50C45C46C471.3(10)
Fe1C1C2C11-111.9(6) Fe3C51C52C5359.2(4)
Fe1C1C5C4-59.6(4) Fe3C51C52C61-117.3(6)
Fe1C2C3C458.8(4) Fe3C51C55C54-58.3(4)
Fe1C2C11N1-179.7(3) Fe3C52C53C5460.4(4)
Fe1C3C4C558.3(4) Fe3C52C61N3163.4(4)
Fe1C4C5C159.5(4) Fe3C53C54C5558.3(4)
Fe1C6C7C8-59.3(4) Fe3C54C55C5157.9(4)
Fe1C6C10C960.3(4) Fe3C56C57C58-60.3(4)
Fe1C7C8C9-60.1(4) Fe3C56C60C5959.6(4)
Fe1C8C9C10-59.2(4) Fe3C57C58C59-58.8(4)
Fe1C9C10C6-60.4(4) Fe3C58C59C60-59.7(4)
Si1C1C2Fe1122.9(6) Fe3C59C60C56-59.4(4)
Si1C1C2C3-177.3(5) Si3C51C52Fe3114.3(5)
Si1C1C2C1111.0(10) Si3C51C52C53173.5(4)
Si1C1C5Fe1-122.6(4) Si3C51C52C61-3.0(9)
Si1C1C5C4177.8(4) Si3C51C55Fe3-116.4(4)
Si1C14C15C16-171.8(5) Si3C51C55C54-174.7(4)
Si1C14C19C18172.0(5) Si3C64C65C66174.0(5)
Si1C20C21C22175.8(6) Si3C64C69C68-173.4(5)
Si1C20C25C24-175.1(5) Si3C70C71C72176.2(5)
O1Si1C1Fe168.1(4) Si3C70C75C74-176.5(5)
O1Si1C1C2-28.9(7) O3Si3C51Fe360.3(4)
O1Si1C1C5153.0(4) O3Si3C51C52-28.2(6)
O1Si1C14C15-35.0(5) O3Si3C51C55145.2(4)
O1Si1C14C19151.3(5) O3Si3C64C65133.6(5)
O1Si1C20C21146.0(5) O3Si3C64C69-50.9(5)
O1Si1C20C25-39.1(6) O3Si3C70C71161.0(4)
C1Si1C14C15-159.2(5) O3Si3C70C75-21.5(6)
C1Si1C14C1927.1(6) C51Si3C64C659.8(6)
C1Si1C20C21-88.3(6) C51Si3C64C69-174.7(5)
C1Si1C20C2586.6(6) C51Si3C70C71-78.0(5)
C1C2C3Fe1-59.7(4) C51Si3C70C7599.5(5)
C1C2C3C4-0.8(6) C51C52C53Fe3-59.5(4)
C1C2C11N1-92.9(7) C51C52C53C540.9(6)
C2C1C5Fe158.8(4) C51C52C61N3-108.5(6)
C2C1C5C4-0.9(6) C52C51C55Fe358.7(4)
C2C3C4Fe1-58.1(4) C52C51C55C540.4(6)
C2C3C4C50.2(6) C52C53C54Fe3-59.0(4)
C3C2C11N196.4(6) C52C53C54C55-0.6(7)
C3C4C5Fe1-59.1(4) C53C52C61N375.7(7)
C3C4C5C10.4(7) C53C54C55Fe3-57.8(4)
C5C1C2Fe1-58.7(4) C53C54C55C510.1(7)
C5C1C2C31.0(6) C55C51C52Fe3-60.0(4)
C5C1C2C11-170.7(5) C55C51C52C53-0.8(6)
C6C7C8Fe160.0(4) C55C51C52C61-177.2(5)
C6C7C8C9-0.1(7) C56C57C58Fe360.2(4)
C7C6C10Fe1-59.3(4) C56C57C58C591.3(7)
C7C6C10C91.0(7) C57C56C60Fe3-59.6(4)
C7C8C9Fe159.9(4) C57C56C60C590.0(7)
C7C8C9C100.7(7) C57C58C59Fe358.4(4)
C8C9C10Fe159.4(4) C57C58C59C60-1.3(7)
C8C9C10C6-1.1(7) C58C59C60Fe360.2(4)
C10C6C7Fe158.7(4) C58C59C60C560.8(7)
C10C6C7C8-0.5(7) C60C56C57Fe359.5(4)
C11C2C3Fe1112.6(5) C60C56C57C58-0.8(7)
C11C2C3C4171.5(5) C61C52C53Fe3116.9(6)
C12N1C11C274.6(6) C61C52C53C54177.3(5)
C13N1C11C2-53.8(7) C62N3C61C52-71.0(6)
C14Si1C1Fe1-171.2(3) C63N3C61C5255.5(6)
C14Si1C1C291.9(6) C64Si3C51Fe3-175.2(3)
C14Si1C1C5-86.3(5) C64Si3C51C5296.3(6)
C14Si1C20C2128.8(6) C64Si3C51C55-90.3(5)
C14Si1C20C25-156.3(5) C64Si3C70C7140.3(5)
C14C15C16C17-0.8(9) C64Si3C70C75-142.2(5)
C15C14C19C18-1.9(9) C64C65C66C671.6(10)
C15C16C17C18-0.6(10) C65C64C69C682.3(9)
C16C17C18C190.7(10) C65C66C67C68-1.8(10)
C17C18C19C140.5(10) C66C67C68C692.3(10)
C19C14C15C162.0(9) C67C68C69C64-2.6(10)
C20Si1C1Fe1-54.9(5) C69C64C65C66-1.8(9)
C20Si1C1C2-151.9(6) C70Si3C51Fe3-60.9(4)
C20Si1C1C529.9(5) C70Si3C51C52-149.5(5)
C20Si1C14C1582.9(5) C70Si3C51C5524.0(5)
C20Si1C14C19-90.8(5) C70Si3C64C65-106.3(5)
C20C21C22C23-0.9(14) C70Si3C64C6969.2(5)
C21C20C25C240.0(10) C70C71C72C730.3(10)
C21C22C23C240.5(15) C71C70C75C741.0(9)
C22C23C24C250.2(14) C71C72C73C741.4(11)
C23C24C25C20-0.4(12) C72C73C74C75-1.8(11)
C25C20C21C220.6(11) C73C74C75C700.6(10)
Fe2C26C27C28-59.7(4) C75C70C71C72-1.5(9)
Fe2C26C27C36111.0(6) Fe4C76C77C78-59.5(4)
Fe2C26C30C2958.9(4) Fe4C76C77C86119.6(6)
Fe2C27C28C29-59.7(4) Fe4C76C80C7958.7(4)
Fe2C27C36N2-178.3(3) Fe4C77C78C79-59.2(4)
Fe2C28C29C30-58.6(4) Fe4C77C86N4-163.6(4)
Fe2C29C30C26-58.6(4) Fe4C78C79C80-58.8(4)
Fe2C31C32C3359.9(4) Fe4C79C80C76-58.7(4)
Fe2C31C35C34-60.2(4) Fe4C81C82C8359.3(4)
Fe2C32C33C3459.8(4) Fe4C81C85C84-60.0(4)
Fe2C33C34C3559.0(4) Fe4C82C83C8459.6(4)
Fe2C34C35C3160.0(4) Fe4C83C84C8558.8(4)
Si2C26C27Fe2-118.3(5) Fe4C84C85C8159.8(4)
Si2C26C27C28-178.0(4) Si4C76C77Fe4-116.0(5)
Si2C26C27C36-7.3(9) Si4C76C77C78-175.5(4)
Si2C26C30Fe2119.5(4) Si4C76C77C863.7(9)
Si2C26C30C29178.5(4) Si4C76C80Fe4117.4(4)
Si2C39C40C41-175.8(5) Si4C76C80C79176.1(4)
Si2C39C44C43175.9(5) Si4C89C90C91-169.6(6)
Si2C45C46C47-176.8(5) Si4C89C94C93171.1(5)
Si2C45C50C49177.2(5) Si4C95C96C97176.8(5)
O2Si2C26Fe2-65.9(4) Si4C95C100C99-175.7(6)
O2Si2C26C2726.1(6) O4Si4C76Fe4-64.1(4)
O2Si2C26C30-151.3(4) O4Si4C76C7725.9(6)
O2Si2C39C40-137.1(5) O4Si4C76C80-148.6(4)
O2Si2C39C4447.7(6) O4Si4C89C90-144.2(5)
O2Si2C45C46-155.6(5) O4Si4C89C9445.9(6)
O2Si2C45C5026.3(6) O4Si4C95C9620.6(6)
C26Si2C39C40-12.8(6) O4Si4C95C100-161.1(5)
C26Si2C39C44172.0(5) C76Si4C89C90-20.2(6)
C26Si2C45C4678.6(5) C76Si4C89C94169.8(5)
C26Si2C45C50-99.5(5) C76Si4C95C96-100.1(5)
C26C27C28Fe259.8(4) C76Si4C95C10078.1(6)
C26C27C28C290.1(6) C76C77C78Fe459.6(4)
C26C27C36N295.7(7) C76C77C78C790.3(6)
C27C26C30Fe2-58.5(4) C76C77C86N4106.9(6)
C27C26C30C290.4(6) C77C76C80Fe4-58.5(4)
C27C28C29Fe258.8(4) C77C76C80C790.3(6)
C27C28C29C300.2(7) C77C78C79Fe458.6(4)
C28C27C36N2-94.9(6) C77C78C79C80-0.1(7)
C28C29C30Fe258.2(4) C78C77C86N4-74.1(7)
C28C29C30C26-0.4(7) C78C79C80Fe458.6(4)
C30C26C27Fe259.4(4) C78C79C80C76-0.1(7)
C30C26C27C28-0.3(6) C80C76C77Fe459.2(4)
C30C26C27C36170.4(5) C80C76C77C78-0.3(6)
C31C32C33Fe2-60.0(4) C80C76C77C86178.8(5)
C31C32C33C34-0.2(7) C81C82C83Fe4-58.8(4)
C32C31C35Fe259.2(4) C81C82C83C840.8(7)
C32C31C35C34-1.0(7) C82C81C85Fe459.5(4)
C32C33C34Fe2-59.4(4) C82C81C85C84-0.5(7)
C32C33C34C35-0.4(7) C82C83C84Fe4-59.9(4)
C33C34C35Fe2-59.1(4) C82C83C84C85-1.1(7)
C33C34C35C310.8(7) C83C84C85Fe4-58.8(4)
C35C31C32Fe2-59.2(4) C83C84C85C811.0(7)
C35C31C32C330.8(7) C85C81C82Fe4-59.5(4)
C36C27C28Fe2-111.5(5) C85C81C82C83-0.2(7)
C36C27C28C29-171.2(5) C86C77C78Fe4-119.6(6)
C37AN2C36C2778.4(15) C86C77C78C79-178.9(5)
C37BN2C36C2743.5(10) C87N4C86C77-54.7(6)
C38AN2C36C27-38.1(19) C88N4C86C7771.9(6)
C38BN2C36C27-84.1(8) C89Si4C76Fe4170.7(3)
C39Si2C26Fe2173.9(3) C89Si4C76C77-99.3(6)
C39Si2C26C27-94.1(6) C89Si4C76C8086.2(5)
C39Si2C26C3088.5(5) C89Si4C95C96142.3(5)
C39Si2C45C46-38.8(6) C89Si4C95C100-39.4(6)
C39Si2C45C50143.1(5) C89C90C91C92-1.3(12)
C39C40C41C42-0.2(10) C90C89C94C930.6(9)
C40C39C44C430.5(10) C90C91C92C930.0(11)
C40C41C42C430.6(11) C91C92C93C941.6(10)
C41C42C43C44-0.5(11) C92C93C94C89-1.9(10)
C42C43C44C39-0.1(11) C94C89C90C911.0(10)
C44C39C40C41-0.4(9) C95Si4C76Fe455.9(4)
C45Si2C26Fe258.2(4) C95Si4C76C77145.9(5)
C45Si2C26C27150.2(6) C95Si4C76C80-28.6(5)
C45Si2C26C30-27.2(5) C95Si4C89C9096.2(6)
C45Si2C39C40103.5(5) C95Si4C89C94-73.8(5)
C45Si2C39C44-71.7(6) C95C96C97C98-0.4(11)
C45C46C47C48-1.2(11) C96C95C100C992.7(10)
C46C45C50C49-0.9(9) C96C97C98C991.3(12)
C46C47C48C490.7(12) C97C98C99C100-0.2(12)
C47C48C49C50-0.3(12) C98C99C100C95-1.9(12)
C48C49C50C450.4(11) C100C95C96C97-1.6(9)

 

Table 8 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for 2870_twin1_hklf4.
AtomxyzU(eq)
H1-34706057263734
H1A-51535760429723
H3-58458235368719
H4-58719245262521
H5-49048676178720
H6-23348147272339
H7-30728050384942
H8-40499305386038
H9-391910181275231
H10-28749442203739
H11A-47047085410121
H11B-40446690360521
H12A-45125409339076
H12B-53075890299476
H12C-55935094354476
H13A-65786590362281
H13B-64356588434781
H13C-67225761415881
H15-38545541150928
H16-4843487398235
H17-6362534183941
H18-69016453122841
H19-59097130175427
H21-4321781470965
H22-35738774-15696
H23-20969327-8376
H24-1378891382662
H25-20967947168044
H2-76219875225531
H2A-102519626432720
H2B-100679881415020
H28-108167496373321
H29-108717072268922
H30-99568104182622
H31-73688196271939
H32-80617706385835
H33-89736390394238
H34-88496075285229
H35-78677214207635
H37A-115878784407279
H37B-116629461449279
H37C-110148683468379
H37D-115509268354242
H37E-117549797407242
H37F-115318847428142
H38A-10346104153041117
H38B-11233105183541117
H38C-1124298043159117
H38D-949910543350929
H38E-1059710748347629
H38F-1006110256299129
H40-109719819193232
H41-1194010836145251
H42-112861209889640
H43-96631233080942
H44-868911309128837
H46-9468934581247
H47-87988810-2974
H48-72338394-5879
H49-6356848577069
H50-70419011162843
H3A-30694582231037
H3B-12534551429521
H53-5952320372918
H54-371956268628
H55-4993087179316
H56-34653288251836
H57-33292680367842
H58-25491310376138
H59-21371094263531
H60-27302308188332
H61A-19903435401122
H61B-19984263347822
H62A823326420838
H62B-8383201472438
H62C-393865473638
H63A-5565211330039
H63B2024501331039
H63C1925070381539
H653974851205526
H6614975891161534
H6710317138105635
H68-543732487436
H69-16596315131533
H71-538444081031
H72-7853992-10348
H73-22863552-22647
H74-3556360653450
H75-33084038145633
H4A-1743811140266738
H4B-1623510867431226
H78-1555413401373618
H79-1502214324265232
H80-1552113688179622
H81-1850013160259340
H82-1831313218373339
H83-1741714510371937
H84-1708015275255941
H85-1772114429186134
H86A-1700511608352024
H86B-1697012142404424
H87A-1479510618381140
H87B-1480511472330640
H87C-1556210768330940
H88A-1579611942476344
H88B-1491912161421744
H88C-1496411303472244
H90-1460311976192044
H91-1346111292140056
H92-139131025291941
H93-15518992697833
H94-1664910652145529
H96-1842912839157838
H97-188001377067958
H98-1763014316-13665
H99-1606313890-6771
H100-157001292182347

 

Table 9 Atomic Occupancy for 2870_twin1_hklf4.
AtomOccupancy AtomOccupancy AtomOccupancy
H2A0.65(2) H2B0.35(2) C37A0.35(2)
H37A0.35(2) H37B0.35(2) H37C0.35(2)
C37B0.65(2) H37D0.65(2) H37E0.65(2)
H37F0.65(2) C38A0.35(2) H38A0.35(2)
H38B0.35(2) H38C0.35(2) C38B0.65(2)
H38D0.65(2) H38E0.65(2) H38F0.65(2)

Experimental

Single crystals of C50H55Cl4Fe2N2O2Si2Zn [2870_twin1_hklf4] 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 XT [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. (2015). Acta Cryst. A71, 3-8.
  3. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Crystal structure determination of [2870_twin1_hklf4]

Crystal Data for C50H55Cl4Fe2N2O2Si2Zn (=1091.01 g/mol): triclinic, space group P-1 (no. 2), a = 14.1820(10) Å, b = 16.7847(11) Å, c = 21.5947(15) Å, α = 77.232(6)°, β = 83.623(6)°, γ = 89.793(6)°, = 4981.1(6) Å3, Z = 4, T = 173 K, μ(MoKα) = 1.353 mm-1, Dcalc = 1.452 g/cm3, 22949 reflections measured (4.58° ≤ 2Θ ≤ 52°), 22949 unique (Rint = ?, Rsigma = 0.1270) which were used in all calculations. The final R1 was 0.0520 (I > 2σ(I)) and wR2 was 0.0945 (all data).

Refinement model description

Number of restraints - 48, number of constraints - unknown.

Details:

1. Twinned data refinement
Scales: 0.4046(5) 0.5954(5)
2. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
At 1.5 times of:
All C(H,H,H) groups, All O(H) groups
3. Rigid bond restraints
C9, C6, C10, C8, C7
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
C54, C52, C55, C53, C51
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
C56, C59, C58, C60, C57
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(C59) ≈ Ueq, Uanis(C51) ≈ Ueq, Uanis(C9) ≈ Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.0001
5. Others
Sof(H2B)=Sof(C37A)=Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C38A)=Sof(H38A)=
Sof(H38B)=Sof(H38C)=1-FVAR(1)
Sof(H2A)=Sof(C37B)=Sof(H37D)=Sof(H37E)=Sof(H37F)=Sof(C38B)=Sof(H38D)=
Sof(H38E)=Sof(H38F)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
N1(H1A), N2(H2A), N2(H2B), N3(H3B), N4(H4B)
6.b Secondary CH2 refined with riding coordinates:
C11(H11A,H11B), C61(H61A,H61B), C86(H86A,H86B)
6.c Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C15(H15),
C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24),
C25(H25), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33),
C34(H34), C35(H35), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C46(H46),
C47(H47), C48(H48), C49(H49), C50(H50), C53(H53), C54(H54), C55(H55),
C56(H56), C57(H57), C58(H58), C59(H59), C60(H60), C65(H65), C66(H66), C67(H67),
C68(H68), C69(H69), C71(H71), C72(H72), C73(H73), C74(H74), C75(H75),
C78(H78), C79(H79), C80(H80), C81(H81), C82(H82), C83(H83), C84(H84), C85(H85),
C90(H90), C91(H91), C92(H92), C93(H93), C94(H94), C96(H96), C97(H97),
C98(H98), C99(H99), C100(H100)
6.d Tetrahedral OH refined with riding coordinates:
O1(H1), O2(H2), O3(H3A), O4(H4A)
6.e Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C37A(H37A,H37B,H37C), C37B(H37D,
H37E,H37F), C38A(H38A,H38B,H38C), C38B(H38D,H38E,H38F), C62(H62A,H62B,H62C),
C63(H63A,H63B,H63C), C87(H87A,H87B,H87C), C88(H88A,H88B,H88C)

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.