mo_B0433_0m

Table 1 Crystal data and structure refinement for mo_B0433_0m.
Identification code mo_B0433_0m
Empirical formula C33.82H53.3Cl2Fe2N2O3Si2Zn2
Formula weight 905.47
Temperature/K 100.01
Crystal system monoclinic
Space group P21
a/Å 13.9663(10)
b/Å 15.8280(11)
c/Å 18.8751(13)
α/° 90
β/° 105.280(3)
γ/° 90
Volume/Å3 4025.0(5)
Z 4
ρcalcg/cm3 1.494
μ/mm‑1 2.110
F(000) 1873.0
Crystal size/mm3 0.617 × 0.211 × 0.076
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.934 to 55.998
Index ranges -18 ≤ h ≤ 18, -20 ≤ k ≤ 20, -24 ≤ l ≤ 24
Reflections collected 71783
Independent reflections 19405 [Rint = 0.0251, Rsigma = 0.0249]
Data/restraints/parameters 19405/1/906
Goodness-of-fit on F2 1.028
Final R indexes [I>=2σ (I)] R1 = 0.0217, wR2 = 0.0531
Final R indexes [all data] R1 = 0.0233, wR2 = 0.0538
Largest diff. peak/hole / e Å-3 0.62/-0.35
Flack parameter-0.001(3)

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for mo_B0433_0m. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Zn14620.2(2)4969.6(2)6472.3(2)17.01(7)
Zn24511.6(2)3637.4(2)5395.1(2)19.22(7)
Fe11563.2(3)4826.9(3)7406.5(2)20.47(9)
Fe27838.5(3)6566.8(3)6819.5(2)18.84(8)
Cl14674.0(6)2289.3(5)5753.7(4)27.60(16)
Cl24302.7(6)3858.2(4)4201.8(4)24.43(15)
Si12432.2(6)4180.8(6)5886.8(4)23.05(17)
Si26697.3(6)4622.2(5)6074.9(4)20.58(16)
O13577.7(16)4271.3(13)5836.4(11)23.4(4)
O25538.6(15)4386.0(13)6016.0(11)20.9(4)
N14802.8(18)4574.5(15)7540.0(13)19.1(5)
N24550.9(17)6221.0(15)6187.2(13)19.4(5)
C12363(2)4931.6(18)6639.3(15)19.6(5)
C23013(2)4916.7(18)7376.7(15)19.6(5)
C32756(2)5605(2)7781.0(17)25.2(6)
C41969(2)6063(2)7308.3(18)27.6(6)
C51726(2)5651.2(19)6611.7(17)24.2(6)
C6549(3)3873(2)7099(2)34.9(8)
C71304(3)3639(3)7716(3)58.9(14)
C81292(4)4218(5)8278(2)71.1(19)
C9540(4)4809(3)8006(3)59.5(14)
C1088(3)4594(2)7281(2)36.0(8)
C112193(3)3052(2)6087(2)35.0(8)
C121516(3)4509(3)5030.9(18)39.1(9)
C133822(2)4281.1(19)7650.0(16)20.9(6)
C145231(2)5233.1(19)8087.4(15)23.5(6)
C155488(2)3836.1(19)7667.3(18)25.2(6)
C166972(2)5502.4(18)6765.2(15)18.4(5)
C176394(2)6262.3(18)6725.7(15)18.4(5)
C186784(2)6750.2(19)7376.2(16)22.3(6)
C197597(2)6304(2)7822.0(16)24.0(6)
C207721(2)5537.3(19)7455.2(16)22.2(6)
C217895(3)7108(2)5847.8(19)35.3(8)
C228059(2)7727(2)6409(2)31.6(7)
C238908(2)7489(2)6966(2)29.3(7)
C249280(2)6720(2)6755(2)29.7(7)
C258652(3)6483(2)6062(2)33.9(8)
C267519(3)3703(2)6426(2)35.4(8)
C276835(3)4914(2)5153.2(18)33.5(7)
C285540(2)6507.4(18)6090.9(16)20.3(5)
C294245(2)6790.4(19)6715.6(17)24.9(6)
C303812(2)6297(2)5459.7(17)27.4(7)
Zn34889.9(2)5146.8(2)1457.0(2)15.68(6)
Zn44399.4(2)3538.6(2)728.2(2)17.61(7)
Fe32196.9(3)6110.8(3)2578.1(2)18.00(8)
Fe48087.1(3)6181.8(3)1004.1(2)20.40(8)
Cl34609.8(6)2277.3(5)1251.1(4)26.86(16)
Cl43799.5(6)3638.4(5)-489.6(4)25.74(14)
Si32609.8(6)4638.8(5)1235.6(4)19.19(15)
Si46752.8(6)4218.3(5)1046.9(4)18.81(15)
O33722.5(15)4414.2(12)1177.4(11)20.2(4)
O45604.6(15)4252.6(13)1085.5(11)19.8(4)
N35236.7(18)5232.2(16)2571.8(12)19.2(5)
N44843.0(17)6168.4(15)787.9(12)17.8(4)
C312761(2)5667.3(18)1740.7(15)18.5(5)
C323541(2)5878.1(18)2391.3(15)18.3(5)
C333453(2)6751.2(19)2562.2(16)21.0(6)
C342627(2)7091.9(18)2026.3(16)22.3(6)
C352204(2)6435.2(18)1526.2(16)21.8(6)
C361356(3)5189(2)2898(2)32.7(7)
C372154(3)5429(2)3492.0(18)29.9(7)
C382069(2)6306(2)3617.1(17)28.6(7)
C391211(2)6608(2)3097.1(18)29.1(7)
C40767(2)5925(2)2649.6(19)30.0(7)
C411739(2)4792(2)310.7(18)31.1(7)
C422140(3)3756(2)1696.2(19)29.6(7)
C434293(2)5269.1(18)2821.9(15)19.8(5)
C445881(2)5962(2)2883.6(16)26.7(6)
C455769(2)4439(2)2862.6(17)27.4(7)
C467233(2)5293.6(17)1362.8(15)17.9(5)
C476700(2)6082.4(18)1146.3(15)18.1(5)
C487238(2)6752.2(19)1584.1(16)21.9(6)
C498095(2)6395.7(19)2073.9(17)24.8(6)
C508096(2)5512.2(19)1941.3(16)22.5(6)
C517910(3)6505(2)-73.4(19)33.6(7)
C528423(3)7149(2)396(2)35.4(8)
C539304(3)6797(2)855(2)36.5(8)
C549334(2)5924(2)666(2)33.0(7)
C558473(3)5750(2)92.4(19)31.2(7)
C566807(3)3955(2)97.7(18)31.3(7)
C577489(3)3410(2)1683(2)31.8(7)
C585777(2)6178.9(18)529.4(15)18.5(5)
C593988(2)6089(2)124.4(16)24.6(6)
C604743(2)6986.0(18)1149.2(18)23.7(6)
O5-1073(3)4100(4)4426(2)92.7(15)
C61-1009(7)5595(6)4113(5)115(3)
C62-997(5)4638(7)3842(3)114(3)
C63-1045(8)3222(6)4235(5)120(3)
C64-1053(8)2718(7)4900(5)133(4)
O6-897(3)2822(3)-40(2)34.6(11)
C65-793(10)1786(6)890(5)82(3)
C66-347(8)2579(6)683(6)42(2)
C67-499(9)3554(7)-231(7)31.0(19)
C68-1083(5)3825(4)-1011(3)40.3(15)
O7-395(7)3703(7)987(6)68(3)
C69-440(20)2238(16)719(17)81(8)
C70-485(9)3167(10)512(10)57(4)
C71-731(18)3450(20)-347(18)71(11)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for mo_B0433_0m. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Zn119.24(15)16.10(15)16.83(14)-0.99(12)6.76(11)-1.53(12)
Zn223.84(17)17.56(15)17.98(14)-2.69(12)8.52(12)-3.15(13)
Fe118.3(2)24.3(2)20.28(18)0.16(16)7.65(15)0.75(16)
Fe216.80(19)17.98(19)22.01(19)1.70(15)5.61(15)-1.27(15)
Cl140.4(4)20.5(3)20.3(3)3.0(3)5.2(3)-3.5(3)
Cl231.8(4)22.2(3)19.6(3)3.5(3)7.3(3)-1.1(3)
Si121.6(4)28.7(4)20.7(4)-5.9(3)8.8(3)-6.7(3)
Si221.1(4)18.9(4)24.6(4)-2.9(3)11.0(3)-2.0(3)
O121.8(10)25.8(11)25.1(10)-9.3(9)10.6(8)-6.0(9)
O221.4(10)20.4(10)23.2(10)-5.9(8)9.6(8)-3.3(8)
N118.8(12)18.0(11)21.2(11)1.3(9)6.6(9)1.5(9)
N217.4(11)19.0(11)20.5(11)2.3(9)2.6(9)-1.0(9)
C119.5(13)20.0(13)20.4(12)-1.0(11)7.1(10)-4.0(11)
C219.2(13)21.0(13)20.0(12)-1.5(11)7.5(10)-1.0(11)
C323.5(15)29.1(16)24.5(14)-8.4(12)9.0(12)-1.0(12)
C425.5(15)20.9(14)39.2(17)-5.4(13)13.5(13)-0.3(12)
C522.8(15)22.6(14)27.7(15)4.7(12)7.8(12)0.5(12)
C633.4(18)31.3(17)45.6(19)-6.9(15)20.1(16)-9.4(14)
C729(2)44(2)108(4)48(3)27(2)9.9(18)
C846(3)133(5)31(2)28(3)3.6(18)-40(3)
C957(3)76(3)65(3)-36(3)49(2)-32(3)
C1020.4(16)32.3(17)57(2)9.6(16)14.0(15)1.6(13)
C1137.8(19)28.6(17)46(2)-14.2(15)24.1(16)-13.6(15)
C1229.2(18)68(3)20.0(15)-3.5(16)5.9(13)-12.1(17)
C1320.5(14)23.8(14)19.8(13)3.5(11)7.5(11)-0.9(11)
C1425.4(15)25.2(15)19.4(13)-0.6(11)4.9(11)-1.8(12)
C1522.9(15)22.6(14)31.8(15)7.0(12)9.9(12)4.9(12)
C1617.5(13)18.5(13)19.4(13)2.3(10)5.3(10)0(1)
C1717.7(13)18.0(13)20.2(13)1.7(10)6.2(10)-1.7(10)
C1821.2(14)22.3(14)25.0(14)-2.8(11)9.1(11)-1.7(11)
C1921.7(14)28.3(15)21.8(13)-2.1(11)5.7(11)-6.3(12)
C2020.2(14)24.2(14)21.6(14)6.5(11)4.4(11)1.0(11)
C2129.0(18)48(2)28.7(16)13.5(15)6.6(13)-11.9(16)
C2225.8(16)24.9(15)47(2)14.3(14)14.1(14)0.6(13)
C2323.3(16)24.5(15)40.2(18)0.7(13)8.5(13)-7.9(12)
C2421.4(15)26.3(16)43.4(19)5.6(14)12.1(14)-0.5(12)
C2537.1(19)33.2(17)40.8(18)-4.9(15)26.6(16)-10.8(15)
C2628.2(17)25.3(16)55(2)-6.9(15)14.5(15)1.5(14)
C2738.3(19)39.2(19)28.6(15)-9.6(14)18.9(14)-12.7(15)
C2817.9(13)19.9(13)23.5(13)4.7(11)6.2(11)-0.9(11)
C2923.3(15)21.7(14)31.5(16)1.7(12)10.1(12)2.8(11)
C3021.7(15)32.5(17)24.3(14)8.4(12)-0.3(12)-2.5(12)
Zn317.58(15)14.53(14)15.36(14)0.19(11)5.08(11)-0.29(11)
Zn421.38(16)14.96(14)17.21(14)-1.20(12)6.36(12)-1.72(12)
Fe317.31(19)18.35(18)19.01(18)1.52(15)5.94(15)1.65(15)
Fe416.18(19)19.21(19)26.5(2)2.79(16)6.92(15)-0.09(16)
Cl340.1(4)18.3(3)21.5(3)3.4(3)7.1(3)-0.9(3)
Cl435.1(4)24.5(3)16.9(3)-0.1(3)5.6(3)0.1(3)
Si317.8(4)19.2(4)21.1(4)-2.3(3)6.0(3)-1.8(3)
Si418.4(4)16.2(3)22.3(4)-1.0(3)6.4(3)1.1(3)
O320.7(10)17.9(10)23.4(10)-3.7(8)8.6(8)-3.4(8)
O420.5(10)16.5(9)24.2(10)-2.2(8)9.2(8)-2.2(8)
N317.6(11)23.7(12)16.6(10)1.3(9)5.0(9)2.2(9)
N416.5(11)17.3(11)19.8(11)2.5(9)5.1(9)1.5(9)
C3118.2(13)20.4(13)17.8(12)1.7(10)6.6(10)-0.2(11)
C3219.0(13)19.9(13)17.7(12)1.3(10)8.2(10)-1(1)
C3322.0(14)22.4(14)20.2(13)-0.2(11)8.5(11)-3.5(11)
C3428.5(16)17.3(13)23.2(14)2.1(11)10.5(12)1.7(12)
C3526.0(15)20.0(13)19.7(13)4.1(11)6.6(11)1.4(11)
C3638.3(19)26.3(16)42.0(18)-1.2(14)25.8(15)-5.4(14)
C3729.0(17)36.0(17)29.9(16)12.3(14)16.9(13)8.4(14)
C3828.5(16)37.1(18)22.0(14)0.3(13)10.1(12)-1.5(14)
C3927.5(16)29.3(16)34.7(16)2.9(14)15.3(13)7.5(13)
C4018.3(14)40.3(19)32.8(16)1.9(14)9.0(12)-2.1(13)
C4123.9(16)39.6(18)27.0(15)-8.3(14)1.8(12)2.1(14)
C4232.3(17)22.9(15)39.3(18)-3.4(13)19.5(14)-6.7(13)
C4319.2(13)23.9(14)17.6(12)2.3(11)7.2(10)1.7(11)
C4423.1(15)35.4(17)20.6(14)-7.8(12)3.6(11)-3.9(13)
C4527.3(16)33.9(17)21.9(14)8.0(12)7.9(12)12.3(13)
C4619.0(13)17.7(13)18.0(12)1.2(10)6.3(10)1.4(10)
C4718.3(13)18.8(13)18.9(12)1.2(11)8(1)-0.7(11)
C4820.1(14)19.0(13)26.8(14)-1.6(11)6.3(11)-1.2(11)
C4921.9(15)23.9(15)26.1(14)-2.3(12)2.1(12)-3.2(11)
C5021.2(14)22.1(14)23.2(14)1.9(11)4.3(11)-0.3(11)
C5126.1(17)47(2)32.2(17)12.3(15)15.3(13)1.9(15)
C5233.4(18)27.7(16)54(2)13.5(16)26.9(16)1.2(14)
C5326.2(18)37.3(19)49(2)5.2(16)15.3(15)-7.8(14)
C5420.2(15)36.7(18)47(2)8.4(15)18.3(14)5.1(13)
C5531.3(18)33.7(17)34.9(17)0.5(14)19.9(14)-1.0(14)
C5628.4(17)37.1(18)32.0(16)-12.6(14)14.4(14)-3.3(14)
C5731.1(17)21.8(15)41.4(18)4.7(13)7.8(14)5.7(13)
C5817.7(13)19.2(12)19.2(12)3.0(11)6(1)1.7(11)
C5920.5(14)29.2(15)22.6(14)7.3(12)3.3(11)0.6(12)
C6026.6(16)16.1(13)32.3(16)3.4(12)14.6(13)2.8(11)
O561(3)150(5)73(3)10(3)27(2)-6(3)
C61140(7)124(7)95(5)36(5)55(5)47(6)
C6267(4)225(11)45(3)20(5)5(3)-14(5)
C63161(8)110(6)97(6)-50(5)52(6)-45(6)
C64180(10)147(8)95(6)-21(6)76(6)-43(7)
O630(2)33(2)41(2)-9.7(18)11.3(17)-6.0(17)
C65155(11)43(5)54(5)1(4)37(6)-9(6)
C6646(4)42(6)37(4)-9(4)10(3)-8(4)
C6719(5)33(4)39(4)-12(3)5(4)1(3)
C6842(3)42(3)41(3)-3(3)18(3)-2(3)
O740(5)70(7)95(8)-44(6)19(5)-12(5)
C69104(17)60(17)91(16)-28(15)48(13)-27(15)
C7024(6)44(8)105(12)-35(9)18(6)-7(5)
C7116(10)100(20)87(18)-59(14)2(9)2(10)

 

Table 4 Bond Lengths for mo_B0433_0m.
AtomAtomLength/Å AtomAtomLength/Å
Zn1Zn22.9052(5) Zn4Cl42.2350(7)
Zn1O11.965(2) Zn4O31.989(2)
Zn1O21.955(2) Zn4O41.992(2)
Zn1N12.061(2) Fe3C312.066(3)
Zn1N22.048(2) Fe3C322.033(3)
Zn2Cl12.2320(8) Fe3C332.033(3)
Zn2Cl22.2213(8) Fe3C342.046(3)
Zn2O11.994(2) Fe3C352.053(3)
Zn2O21.987(2) Fe3C362.061(3)
Fe1C12.056(3) Fe3C372.049(3)
Fe1C22.045(3) Fe3C382.039(3)
Fe1C32.042(3) Fe3C392.046(3)
Fe1C42.059(3) Fe3C402.058(3)
Fe1C52.046(3) Fe4C462.070(3)
Fe1C62.047(3) Fe4C472.030(3)
Fe1C72.030(4) Fe4C482.026(3)
Fe1C82.026(4) Fe4C492.045(3)
Fe1C92.043(4) Fe4C502.059(3)
Fe1C102.045(3) Fe4C512.048(3)
Fe2C162.061(3) Fe4C522.040(3)
Fe2C172.036(3) Fe4C532.042(3)
Fe2C182.043(3) Fe4C542.047(3)
Fe2C192.050(3) Fe4C552.051(3)
Fe2C202.055(3) Si3O31.626(2)
Fe2C212.045(3) Si3C311.870(3)
Fe2C222.048(3) Si3C411.862(3)
Fe2C232.055(3) Si3C421.855(3)
Fe2C242.063(3) Si4O41.625(2)
Fe2C252.053(3) Si4C461.868(3)
Si1O11.634(2) Si4C561.860(3)
Si1C11.874(3) Si4C571.866(3)
Si1C111.874(4) N3C431.513(4)
Si1C121.851(4) N3C441.487(4)
Si2O21.636(2) N3C451.488(4)
Si2C161.877(3) N4C581.509(4)
Si2C261.864(4) N4C591.490(4)
Si2C271.858(3) N4C601.486(4)
N1C131.511(4) C31C321.450(4)
N1C141.479(4) C31C351.442(4)
N1C151.490(4) C32C331.432(4)
N2C281.510(4) C32C431.498(4)
N2C291.488(4) C33C341.424(4)
N2C301.490(4) C34C351.424(4)
C1C21.447(4) C36C371.410(5)
C1C51.438(4) C36C401.432(5)
C2C31.428(4) C37C381.418(5)
C2C131.500(4) C38C391.417(5)
C3C41.419(5) C39C401.410(5)
C4C51.426(4) C46C471.456(4)
C6C71.401(6) C46C501.440(4)
C6C101.396(5) C47C481.429(4)
C7C81.404(8) C47C581.500(4)
C8C91.399(8) C48C491.422(4)
C9C101.390(6) C49C501.421(4)
C16C171.439(4) C51C521.416(5)
C16C201.441(4) C51C551.419(5)
C17C181.431(4) C52C531.419(5)
C17C281.502(4) C53C541.429(5)
C18C191.412(4) C54C551.417(5)
C19C201.430(4) O5C621.418(8)
C21C221.416(5) O5C631.439(9)
C21C251.427(5) C61C621.600(12)
C22C231.413(5) C63C641.490(12)
C23C241.421(5) O6C661.431(11)
C24C251.421(5) O6C671.374(12)
Zn3Zn42.8886(5) C65C661.498(12)
Zn3O31.956(2) C67C681.544(12)
Zn3O41.965(2) O7C701.216(16)
Zn3N32.036(2) C69C701.52(3)
Zn3N42.042(2) C70C711.63(4)
Zn4Cl32.2121(8)    

 

Table 5 Bond Angles for mo_B0433_0m.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
O1Zn1Zn243.17(6) O4Zn3N3114.32(9)
O1Zn1N1107.91(9) O4Zn3N4106.63(9)
O1Zn1N2114.04(9) N3Zn3Zn4120.85(7)
O2Zn1Zn242.95(6) N3Zn3N4123.15(10)
O2Zn1O186.08(9) N4Zn3Zn4116.00(7)
O2Zn1N1111.16(9) Cl3Zn4Zn3126.58(2)
O2Zn1N2109.40(9) Cl3Zn4Cl4119.50(3)
N1Zn1Zn2115.74(7) Cl4Zn4Zn3113.89(2)
N2Zn1Zn2121.86(7) O3Zn4Zn342.50(6)
N2Zn1N1122.38(10) O3Zn4Cl3117.45(6)
Cl1Zn2Zn1119.95(2) O3Zn4Cl4107.32(6)
Cl2Zn2Zn1124.34(2) O3Zn4O485.10(8)
Cl2Zn2Cl1115.70(3) O4Zn4Zn342.74(6)
O1Zn2Zn142.40(6) O4Zn4Cl3111.10(6)
O1Zn2Cl1112.33(7) O4Zn4Cl4111.25(6)
O1Zn2Cl2114.76(7) C32Fe3C3141.42(11)
O2Zn2Zn142.10(6) C32Fe3C3468.95(12)
O2Zn2Cl1113.04(6) C32Fe3C3568.75(12)
O2Zn2Cl2112.69(6) C32Fe3C36123.10(13)
O2Zn2O184.46(8) C32Fe3C37106.48(12)
C1Fe1C469.28(12) C32Fe3C38120.87(12)
C2Fe1C141.34(11) C32Fe3C39157.15(13)
C2Fe1C468.49(12) C32Fe3C40160.38(13)
C2Fe1C568.49(12) C33Fe3C3169.74(11)
C2Fe1C6131.28(13) C33Fe3C3241.24(12)
C2Fe1C10169.75(14) C33Fe3C3440.87(12)
C3Fe1C169.50(12) C33Fe3C3568.72(12)
C3Fe1C240.92(12) C33Fe3C36156.64(14)
C3Fe1C440.48(13) C33Fe3C37119.45(13)
C3Fe1C568.35(13) C33Fe3C38103.48(13)
C3Fe1C6169.55(14) C33Fe3C39120.50(13)
C3Fe1C9116.26(15) C33Fe3C40158.15(13)
C3Fe1C10148.68(14) C34Fe3C3169.28(11)
C5Fe1C141.05(12) C34Fe3C3540.64(12)
C5Fe1C440.66(13) C34Fe3C36162.34(14)
C5Fe1C6117.67(14) C34Fe3C37154.94(14)
C6Fe1C1108.88(13) C34Fe3C40124.20(13)
C6Fe1C4149.49(15) C35Fe3C3140.99(11)
C7Fe1C1116.67(18) C35Fe3C36127.48(13)
C7Fe1C2108.97(14) C35Fe3C40110.56(13)
C7Fe1C3130.52(17) C36Fe3C31110.17(12)
C7Fe1C4168.6(2) C37Fe3C31124.52(12)
C7Fe1C5149.9(2) C37Fe3C35162.63(13)
C7Fe1C640.21(18) C37Fe3C3640.12(14)
C7Fe1C967.9(2) C37Fe3C4068.00(13)
C7Fe1C1067.40(15) C38Fe3C31159.23(13)
C8Fe1C1149.6(2) C38Fe3C34119.11(13)
C8Fe1C2116.98(17) C38Fe3C35156.36(13)
C8Fe1C3108.43(17) C38Fe3C3667.96(14)
C8Fe1C4129.8(2) C38Fe3C3740.60(14)
C8Fe1C5168.4(2) C38Fe3C3940.60(13)
C8Fe1C667.41(19) C38Fe3C4068.05(14)
C8Fe1C740.5(2) C39Fe3C31159.63(12)
C8Fe1C940.2(2) C39Fe3C34106.08(13)
C8Fe1C1067.04(18) C39Fe3C35122.83(13)
C9Fe1C1168.65(19) C39Fe3C3667.95(14)
C9Fe1C2149.10(17) C39Fe3C3768.09(13)
C9Fe1C4108.20(17) C39Fe3C4040.20(14)
C9Fe1C5130.1(2) C40Fe3C31125.02(13)
C9Fe1C667.31(16) C40Fe3C3640.69(14)
C9Fe1C1039.76(18) C47Fe4C4641.57(11)
C10Fe1C1130.62(14) C47Fe4C4968.84(12)
C10Fe1C4117.00(14) C47Fe4C5068.71(11)
C10Fe1C5109.47(14) C47Fe4C51106.33(12)
C10Fe1C639.91(15) C47Fe4C52120.08(13)
C16Fe2C24131.49(12) C47Fe4C53155.95(14)
C17Fe2C1641.13(11) C47Fe4C54160.94(14)
C17Fe2C1841.08(11) C47Fe4C55123.76(13)
C17Fe2C1968.41(12) C48Fe4C4669.87(11)
C17Fe2C2068.51(11) C48Fe4C4741.26(11)
C17Fe2C21107.03(13) C48Fe4C4940.89(12)
C17Fe2C22115.07(13) C48Fe4C5068.73(12)
C17Fe2C23148.05(13) C48Fe4C51119.40(13)
C17Fe2C24169.33(13) C48Fe4C52102.92(13)
C17Fe2C25129.95(13) C48Fe4C53119.32(14)
C18Fe2C1669.40(12) C48Fe4C54157.57(14)
C18Fe2C1940.36(12) C48Fe4C55157.29(13)
C18Fe2C2068.49(12) C49Fe4C4669.07(11)
C18Fe2C21127.25(14) C49Fe4C5040.50(12)
C18Fe2C22105.54(13) C49Fe4C51155.14(14)
C18Fe2C23115.28(13) C49Fe4C54123.86(14)
C18Fe2C24149.39(13) C49Fe4C55161.70(14)
C18Fe2C25167.00(14) C50Fe4C4640.81(11)
C19Fe2C1669.06(12) C51Fe4C46124.43(13)
C19Fe2C2040.75(12) C51Fe4C50162.44(14)
C19Fe2C23108.10(13) C51Fe4C5540.52(14)
C19Fe2C24118.59(13) C52Fe4C46158.63(13)
C19Fe2C25152.38(15) C52Fe4C49119.27(14)
C20Fe2C1640.98(11) C52Fe4C50156.74(15)
C20Fe2C24110.89(13) C52Fe4C5140.52(16)
C21Fe2C16117.33(13) C52Fe4C5340.68(15)
C21Fe2C19165.36(15) C52Fe4C5468.53(14)
C21Fe2C20152.10(14) C52Fe4C5568.19(15)
C21Fe2C2240.48(15) C53Fe4C46160.32(13)
C21Fe2C2367.93(14) C53Fe4C49105.65(15)
C21Fe2C2468.22(14) C53Fe4C50123.16(14)
C21Fe2C2540.76(16) C53Fe4C5168.33(15)
C22Fe2C16149.21(13) C53Fe4C5440.92(15)
C22Fe2C19127.53(14) C53Fe4C5568.33(15)
C22Fe2C20167.12(14) C54Fe4C46125.28(13)
C22Fe2C2340.30(13) C54Fe4C50110.59(13)
C22Fe2C2468.04(13) C54Fe4C5168.30(14)
C22Fe2C2568.16(15) C54Fe4C5540.46(14)
C23Fe2C16169.74(12) C55Fe4C46110.45(13)
C23Fe2C20130.65(13) C55Fe4C50127.25(13)
C23Fe2C2440.38(13) O3Si3C31104.09(12)
C25Fe2C16109.78(13) O3Si3C41111.40(14)
C25Fe2C20119.98(14) O3Si3C42109.25(14)
C25Fe2C2367.86(14) C41Si3C31108.82(14)
C25Fe2C2440.38(14) C42Si3C31115.04(14)
O1Si1C1103.60(12) C42Si3C41108.25(17)
O1Si1C11108.94(15) O4Si4C46103.33(12)
O1Si1C12112.75(14) O4Si4C56109.96(13)
C1Si1C11113.83(14) O4Si4C57112.15(14)
C12Si1C1108.76(16) C56Si4C46114.17(15)
C12Si1C11108.97(19) C56Si4C57108.07(17)
O2Si2C16103.55(12) C57Si4C46109.19(14)
O2Si2C26110.58(14) Zn3O3Zn494.13(9)
O2Si2C27109.73(14) Si3O3Zn3126.55(12)
C26Si2C16109.78(15) Si3O3Zn4138.71(12)
C27Si2C16114.39(15) Zn3O4Zn493.79(9)
C27Si2C26108.74(18) Si4O4Zn3129.80(12)
Zn1O1Zn294.43(9) Si4O4Zn4136.20(12)
Si1O1Zn1126.38(12) C43N3Zn3109.60(16)
Si1O1Zn2137.62(12) C44N3Zn3114.52(18)
Zn1O2Zn294.94(9) C44N3C43109.4(2)
Si2O2Zn1127.89(12) C44N3C45108.5(2)
Si2O2Zn2136.36(12) C45N3Zn3106.55(18)
C13N1Zn1110.15(17) C45N3C43108.0(2)
C14N1Zn1113.11(18) C58N4Zn3108.61(16)
C14N1C13109.6(2) C59N4Zn3109.95(18)
C14N1C15108.4(2) C59N4C58107.4(2)
C15N1Zn1107.73(18) C60N4Zn3113.40(17)
C15N1C13107.7(2) C60N4C58109.4(2)
C28N2Zn1109.92(17) C60N4C59107.9(2)
C29N2Zn1114.31(18) Si3C31Fe3132.17(15)
C29N2C28109.4(2) C32C31Fe368.07(16)
C29N2C30108.5(2) C32C31Si3126.2(2)
C30N2Zn1107.05(18) C35C31Fe369.04(16)
C30N2C28107.4(2) C35C31Si3127.6(2)
Si1C1Fe1128.96(15) C35C31C32105.8(2)
C2C1Fe168.92(16) C31C32Fe370.51(16)
C2C1Si1125.1(2) C31C32C43125.1(3)
C5C1Fe169.10(16) C33C32Fe369.38(17)
C5C1Si1129.0(2) C33C32C31108.8(2)
C5C1C2105.8(2) C33C32C43126.1(3)
C1C2Fe169.75(16) C43C32Fe3124.77(19)
C1C2C13124.5(3) C32C33Fe369.38(16)
C3C2Fe169.44(17) C34C33Fe370.07(17)
C3C2C1108.6(3) C34C33C32107.9(3)
C3C2C13126.9(3) C33C34Fe369.06(16)
C13C2Fe1127.3(2) C35C34Fe369.95(17)
C2C3Fe169.65(17) C35C34C33108.1(3)
C4C3Fe170.42(18) C31C35Fe369.97(16)
C4C3C2108.4(3) C34C35Fe369.41(17)
C3C4Fe169.10(18) C34C35C31109.3(3)
C3C4C5107.6(3) C37C36Fe369.48(19)
C5C4Fe169.15(18) C37C36C40107.8(3)
C1C5Fe169.85(16) C40C36Fe369.55(19)
C4C5Fe170.19(18) C36C37Fe370.39(19)
C4C5C1109.5(3) C36C37C38108.2(3)
C7C6Fe169.2(2) C38C37Fe369.32(18)
C10C6Fe170.0(2) C37C38Fe370.08(18)
C10C6C7107.8(4) C39C38Fe369.96(18)
C6C7Fe170.5(2) C39C38C37107.9(3)
C6C7C8107.4(4) C38C39Fe369.44(18)
C8C7Fe169.6(3) C40C39Fe370.36(19)
C7C8Fe169.9(2) C40C39C38108.3(3)
C9C8Fe170.5(3) C36C40Fe369.76(18)
C9C8C7108.5(4) C39C40Fe369.44(18)
C8C9Fe169.3(2) C39C40C36107.7(3)
C10C9Fe170.2(2) C32C43N3113.5(2)
C10C9C8107.4(4) Si4C46Fe4134.72(15)
C6C10Fe170.1(2) C47C46Fe467.76(15)
C9C10Fe170.0(2) C47C46Si4125.3(2)
C9C10C6108.9(4) C50C46Fe469.20(16)
C2C13N1112.0(2) C50C46Si4128.3(2)
Si2C16Fe2130.62(15) C50C46C47105.7(2)
C17C16Fe268.49(16) C46C47Fe470.67(16)
C17C16Si2125.1(2) C46C47C58125.2(3)
C17C16C20106.2(2) C48C47Fe469.22(17)
C20C16Fe269.30(16) C48C47C46108.8(2)
C20C16Si2128.5(2) C48C47C58125.9(3)
C16C17Fe270.39(16) C58C47Fe4122.97(19)
C16C17C28125.0(3) C47C48Fe469.52(16)
C18C17Fe269.72(17) C49C48Fe470.25(18)
C18C17C16109.0(2) C49C48C47107.8(3)
C18C17C28126.0(3) C48C49Fe468.86(18)
C28C17Fe2124.7(2) C50C49Fe470.30(18)
C17C18Fe269.20(17) C50C49C48108.4(3)
C19C18Fe270.11(18) C46C50Fe469.99(16)
C19C18C17107.8(3) C49C50Fe469.20(18)
C18C19Fe269.53(17) C49C50C46109.3(3)
C18C19C20108.5(3) C52C51Fe469.5(2)
C20C19Fe269.82(17) C52C51C55108.0(3)
C16C20Fe269.72(16) C55C51Fe469.87(19)
C19C20Fe269.43(17) C51C52Fe470.03(19)
C19C20C16108.6(3) C51C52C53108.2(3)
C22C21Fe269.87(19) C53C52Fe469.7(2)
C22C21C25107.8(3) C52C53Fe469.60(19)
C25C21Fe269.91(19) C52C53C54107.8(3)
C21C22Fe269.65(19) C54C53Fe469.72(19)
C23C22Fe270.12(18) C53C54Fe469.4(2)
C23C22C21108.1(3) C55C54Fe469.94(19)
C22C23Fe269.58(18) C55C54C53107.7(3)
C22C23C24108.5(3) C51C55Fe469.61(19)
C24C23Fe270.13(18) C54C55Fe469.6(2)
C23C24Fe269.49(18) C54C55C51108.3(3)
C25C24Fe269.40(19) C47C58N4112.8(2)
C25C24C23107.6(3) C62O5C63111.9(6)
C21C25Fe269.33(19) O5C62C61108.2(6)
C24C25Fe270.22(19) O5C63C64107.5(6)
C24C25C21108.0(3) C67O6C66108.9(7)
C17C28N2112.7(2) O6C66C65108.5(8)
O3Zn3Zn443.37(6) O6C67C68109.6(8)
O3Zn3O486.70(8) O7C70C69120(2)
O3Zn3N3105.82(9) O7C70C71119.6(19)
O3Zn3N4114.45(9) C69C70C71120.5(19)
O4Zn3Zn443.47(6)     

 

Table 6 Torsion Angles for mo_B0433_0m.
ABCDAngle/˚ ABCDAngle/˚
Zn1N1C13C2-50.2(3) Fe3C31C32C33-59.0(2)
Zn1N2C28C17-49.5(3) Fe3C31C32C43119.4(3)
Fe1C1C2C3-58.7(2) Fe3C31C35C3458.4(2)
Fe1C1C2C13122.0(3) Fe3C32C33C34-59.7(2)
Fe1C1C5C459.1(2) Fe3C32C43N3-179.04(18)
Fe1C2C3C4-60.0(2) Fe3C33C34C35-59.2(2)
Fe1C2C13N1-179.43(19) Fe3C34C35C31-58.7(2)
Fe1C3C4C5-58.6(2) Fe3C36C37C3859.2(2)
Fe1C4C5C1-58.9(2) Fe3C36C40C39-59.3(2)
Fe1C6C7C860.2(3) Fe3C37C38C3960.0(2)
Fe1C6C10C9-59.5(3) Fe3C38C39C4059.8(2)
Fe1C7C8C960.2(3) Fe3C39C40C3659.5(2)
Fe1C8C9C1060.1(3) Fe4C46C47C48-58.9(2)
Fe1C9C10C659.6(3) Fe4C46C47C58117.3(3)
Fe2C16C17C18-59.2(2) Fe4C46C50C4958.1(2)
Fe2C16C17C28119.2(3) Fe4C47C48C49-60.1(2)
Fe2C16C20C1958.7(2) Fe4C47C58N4-173.99(19)
Fe2C17C18C19-59.7(2) Fe4C48C49C50-59.3(2)
Fe2C17C28N2-177.80(19) Fe4C49C50C46-58.6(2)
Fe2C18C19C20-59.1(2) Fe4C51C52C5359.5(2)
Fe2C19C20C16-58.9(2) Fe4C51C55C54-59.0(2)
Fe2C21C22C2359.8(2) Fe4C52C53C5459.5(2)
Fe2C21C25C24-59.8(2) Fe4C53C54C5559.7(2)
Fe2C22C23C2459.6(2) Fe4C54C55C5159.1(2)
Fe2C23C24C2559.2(2) Si3C31C32Fe3-127.0(2)
Fe2C24C25C2159.2(2) Si3C31C32C33174.0(2)
Si1C1C2Fe1-123.6(2) Si3C31C32C43-7.6(4)
Si1C1C2C3177.7(2) Si3C31C35Fe3127.8(2)
Si1C1C2C13-1.5(4) Si3C31C35C34-173.8(2)
Si1C1C5Fe1123.8(2) Si4C46C47Fe4-129.9(2)
Si1C1C5C4-177.0(2) Si4C46C47C48171.2(2)
Si2C16C17Fe2-125.3(2) Si4C46C47C58-12.7(4)
Si2C16C17C18175.4(2) Si4C46C50Fe4131.2(2)
Si2C16C17C28-6.1(4) Si4C46C50C49-170.6(2)
Si2C16C20Fe2126.1(2) O3Si3C31Fe3-137.10(18)
Si2C16C20C19-175.2(2) O3Si3C31C32-44.9(3)
O1Si1C1Fe1-145.48(18) O3Si3C31C35127.8(3)
O1Si1C1C2-55.3(3) O4Si4C46Fe4-135.18(19)
O1Si1C1C5120.8(3) O4Si4C46C47-42.4(3)
O2Si2C16Fe2-143.75(18) O4Si4C46C50126.5(3)
O2Si2C16C17-53.0(3) C31Si3O3Zn3-7.54(18)
O2Si2C16C20121.2(3) C31Si3O3Zn4-176.09(18)
C1Si1O1Zn13.03(19) C31C32C33Fe359.7(2)
C1Si1O1Zn2164.77(18) C31C32C33C34-0.1(3)
C1C2C3Fe158.9(2) C31C32C43N391.5(3)
C1C2C3C4-1.1(3) C32C31C35Fe3-58.37(19)
C1C2C13N190.8(3) C32C31C35C340.0(3)
C2C1C5Fe1-59.44(19) C32C33C34Fe359.3(2)
C2C1C5C4-0.3(3) C32C33C34C350.1(3)
C2C3C4Fe159.5(2) C33C32C43N3-90.5(3)
C2C3C4C50.9(4) C33C34C35Fe358.7(2)
C3C2C13N1-88.3(3) C33C34C35C31-0.1(3)
C3C4C5Fe158.6(2) C35C31C32Fe359.00(19)
C3C4C5C1-0.4(4) C35C31C32C330.0(3)
C5C1C2Fe159.55(19) C35C31C32C43178.4(3)
C5C1C2C30.9(3) C36C37C38Fe3-59.9(2)
C5C1C2C13-178.4(3) C36C37C38C390.1(4)
C6C7C8Fe1-60.8(3) C37C36C40Fe359.1(2)
C6C7C8C9-0.6(5) C37C36C40C39-0.2(4)
C7C6C10Fe159.1(3) C37C38C39Fe3-60.1(2)
C7C6C10C9-0.4(4) C37C38C39C40-0.2(4)
C7C8C9Fe1-59.8(3) C38C39C40Fe3-59.3(2)
C7C8C9C100.3(5) C38C39C40C360.2(4)
C8C9C10Fe1-59.5(3) C40C36C37Fe3-59.2(2)
C8C9C10C60.1(4) C40C36C37C380.0(4)
C10C6C7Fe1-59.6(3) C41Si3O3Zn3109.56(18)
C10C6C7C80.6(4) C41Si3O3Zn4-59.0(2)
C11Si1O1Zn1-118.47(18) C41Si3C31Fe3104.0(2)
C11Si1O1Zn243.3(2) C41Si3C31C32-163.7(3)
C11Si1C1Fe1-27.3(3) C41Si3C31C358.9(3)
C11Si1C1C262.8(3) C42Si3O3Zn3-130.90(16)
C11Si1C1C5-121.0(3) C42Si3O3Zn460.6(2)
C12Si1O1Zn1120.4(2) C42Si3C31Fe3-17.6(3)
C12Si1O1Zn2-77.8(2) C42Si3C31C3274.6(3)
C12Si1C1Fe194.4(2) C42Si3C31C35-112.7(3)
C12Si1C1C2-175.5(2) C43C32C33Fe3-118.7(3)
C12Si1C1C50.6(3) C43C32C33C34-178.4(3)
C13C2C3Fe1-121.9(3) C44N3C43C3279.8(3)
C13C2C3C4178.1(3) C45N3C43C32-162.2(2)
C14N1C13C274.8(3) C46Si4O4Zn3-5.28(18)
C15N1C13C2-167.4(2) C46Si4O4Zn4167.92(17)
C16Si2O2Zn16.20(18) C46C47C48Fe459.8(2)
C16Si2O2Zn2173.20(17) C46C47C48C49-0.3(3)
C16C17C18Fe259.6(2) C46C47C58N497.5(3)
C16C17C18C19-0.1(3) C47C46C50Fe4-58.17(18)
C16C17C28N293.0(3) C47C46C50C490.0(3)
C17C16C20Fe2-58.82(19) C47C48C49Fe459.6(2)
C17C16C20C19-0.1(3) C47C48C49C500.3(4)
C17C18C19Fe259.2(2) C48C47C58N4-87.0(3)
C17C18C19C200.0(3) C48C49C50Fe458.5(2)
C18C17C28N2-88.9(3) C48C49C50C46-0.2(4)
C18C19C20Fe258.9(2) C50C46C47Fe459.1(2)
C18C19C20C160.0(3) C50C46C47C480.2(3)
C20C16C17Fe259.34(19) C50C46C47C58176.4(3)
C20C16C17C180.1(3) C51C52C53Fe4-59.7(2)
C20C16C17C28178.5(3) C51C52C53C54-0.2(4)
C21C22C23Fe2-59.5(2) C52C51C55Fe459.2(2)
C21C22C23C240.0(4) C52C51C55C540.1(4)
C22C21C25Fe259.8(2) C52C53C54Fe4-59.4(2)
C22C21C25C240.0(4) C52C53C54C550.3(4)
C22C23C24Fe2-59.2(2) C53C54C55Fe4-59.3(2)
C22C23C24C250.0(4) C53C54C55C51-0.2(4)
C23C24C25Fe2-59.2(2) C55C51C52Fe4-59.5(2)
C23C24C25C210.0(4) C55C51C52C530.0(4)
C25C21C22Fe2-59.8(2) C56Si4O4Zn3-127.55(18)
C25C21C22C230.0(4) C56Si4O4Zn445.7(2)
C26Si2O2Zn1123.74(18) C56Si4C46Fe4-15.8(3)
C26Si2O2Zn2-69.3(2) C56Si4C46C4777.0(3)
C26Si2C16Fe298.2(2) C56Si4C46C50-114.1(3)
C26Si2C16C17-171.1(2) C57Si4O4Zn3112.18(18)
C26Si2C16C203.1(3) C57Si4O4Zn4-74.6(2)
C27Si2O2Zn1-116.32(18) C57Si4C46Fe4105.3(2)
C27Si2O2Zn250.7(2) C57Si4C46C47-161.9(2)
C27Si2C16Fe2-24.4(3) C57Si4C46C507.0(3)
C27Si2C16C1766.3(3) C58C47C48Fe4-116.3(3)
C27Si2C16C20-119.4(3) C58C47C48C49-176.4(3)
C28C17C18Fe2-118.8(3) C59N4C58C47-168.5(2)
C28C17C18C19-178.5(3) C60N4C58C4774.6(3)
C29N2C28C1776.8(3) C62O5C63C64175.9(7)
C30N2C28C17-165.6(2) C63O5C62C61-178.7(7)
Zn3N3C43C32-46.5(3) C66O6C67C68179.9(8)
Zn3N4C58C47-49.7(3) C67O6C66C65179.4(9)

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for mo_B0433_0m.
AtomxyzU(eq)
H330605733828130
H416606556743333
H512215825619429
H63803592663842
H717443174775071
H817214209876185
H93715273826871
H10-4484888696243
H11A24282681575253
H11B14792967601853
H11C25472918659653
H12A16385098492159
H12B8444456509459
H12C15814147462559
H13A36323741738625
H13B38994178817925
H14A58615430801035
H14B53484997858335
H14C47685709803335
H15A61334009760238
H15B52083388731638
H15C55753625816838
H1865397280748827
H1979956482828729
H2082155121763627
H2173747110540742
H2276668217641138
H2391847792740735
H2498466419702836
H2587245994578841
H26A75103583693453
H26B81993835641053
H26C72813207611953
H27A64774505478950
H27B75404911516250
H27C65605480502250
H28A56396257563524
H28B55327130603524
H29A36106598678737
H29B41727368652137
H29C47516781718737
H30A40045925510541
H30B37906883528941
H30C31556132550741
H3338717050296225
H3423997659200627
H3516436494111626
H3612314637269739
H3726625066376236
H3825106633398434
H399757173305735
H401825949225536
H41A1093498036547
H41B165842574047
H41C200752204047
H42A14293835164644
H42B24973746221844
H42C22453220146844
H43A39944698278024
H43B44635433334724
H44A64625969268440
H44B61005909341940
H44C55076488275340
H45A53773952263141
H45B58644413339541
H45C64174430275341
H4870557332155326
H4985836697243030
H5085905126219427
H5172976567-43640
H528213771940442
H5397887088122144
H549840553288640
H5583025219-14137
H56A64503425-5747
H56B750138918747
H56C64974410-23747
H57A74813543218848
H57B81753412164448
H57C71972850154948
H58A5747571517322
H58B5812671927222
H59A40115536-10437
H59B40266536-22737
H59C3366614426737
H60A41176993129136
H60B4747745180736
H60C52997054158836
H61A-90259773732173
H61B-48056764565173
H61C-165357194206173
H62A-156245383407136
H62B-37345223705136
H63A-43731004078143
H63B-163030783827143
H64A-67521964903199
H64B-173925784893199
H64C-75030485342199
H65A-6561314594124
H65B-15121858798124
H65C-50216661412124
H66A-3733034103750
H66B357248169350
H67A2073461-21837
H67B-531400612437
H68A-9713415-136960
H68B-8564384-112060
H68C-17933849-103860
H69A481952512121
H69B-10931981523121
H69C-24121831255121
H71A-13173148-631106
H71B-1633323-541106
H71C-8624063-386106

 

Table 8 Atomic Occupancy for mo_B0433_0m.
AtomOccupancy AtomOccupancy AtomOccupancy
O60.647(7) C650.647(7) H65A0.647(7)
H65B0.647(7) H65C0.647(7) C660.647(7)
H66A0.647(7) H66B0.647(7) C670.647(7)
H67A0.647(7) H67B0.647(7) C680.647(7)
H68A0.647(7) H68B0.647(7) H68C0.647(7)
O70.353(7) C690.353(7) H69A0.353(7)
H69B0.353(7) H69C0.353(7) C700.353(7)
C710.353(7) H71A0.353(7) H71B0.353(7)
H71C0.353(7)     

Experimental

Single crystals of C33.82H53.3Cl2Fe2N2O3Si2Zn2 [mo_B0433_0m] were []. A suitable crystal was selected and [] on a Bruker APEX-II CCD diffractometer. The crystal was kept at 100.01 K during data collection. Using Olex2 [1], the structure was solved with the ShelXT [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 [mo_B0433_0m]

Crystal Data for C33.8225H53.295Cl2Fe2N2O3Si2Zn2 (=905.47 g/mol): monoclinic, space group P21 (no. 4), a = 13.9663(10) Å, b = 15.8280(11) Å, c = 18.8751(13) Å, β = 105.280(3)°, = 4025.0(5) Å3, Z = 4, T = 100.01 K, μ(MoKα) = 2.110 mm-1, Dcalc = 1.494 g/cm3, 71783 reflections measured (4.934° ≤ 2Θ ≤ 55.998°), 19405 unique (Rint = 0.0251, Rsigma = 0.0249) which were used in all calculations. The final R1 was 0.0217 (I > 2σ(I)) and wR2 was 0.0538 (all data).

Refinement model description

Number of restraints - 1, number of constraints - unknown.

Details:

1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Others
Sof(O7)=Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=Sof(C70)=Sof(C71)=Sof(H71A)=
Sof(H71B)=Sof(H71C)=1-FVAR(1)
Sof(O6)=Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(H65C)=Sof(C66)=Sof(H66A)=Sof(H66B)=
Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
C13(H13A,H13B), C28(H28A,H28B), C43(H43A,H43B), C58(H58A,H58B), C62(H62A,
H62B), C63(H63A,H63B), C66(H66A,H66B), C67(H67A,H67B)
3.b Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C18(H18),
C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C33(H33),
C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40),
C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55)
3.c Idealised Me refined as rotating group:
C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
H15C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,
H30B,H30C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C),
C45(H45A,H45B,H45C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C59(H59A,H59B,
H59C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C64(H64A,H64B,H64C), C65(H65A,
H65B,H65C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C71(H71A,H71B,H71C)

This report has been created with Olex2, compiled on 2016.11.07 svn.r3352 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.