mo_B0175_0m

Table 1 Crystal data and structure refinement for mo_B0175_0m.
Identification code mo_B0175_0m
Empirical formula C33H50Br2Fe2N2O3Si2Zn2
Formula weight 981.19
Temperature/K 100.01
Crystal system monoclinic
Space group P21/c
a/Å 17.5299(5)
b/Å 9.4853(3)
c/Å 23.4559(7)
α/° 90
β/° 103.372(2)
γ/° 90
Volume/Å3 3794.4(2)
Z 4
ρcalcg/cm3 1.718
μ/mm‑1 4.203
F(000) 1984.0
Crystal size/mm3 0.09 × 0.071 × 0.036
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.65 to 63.188
Index ranges -25 ≤ h ≤ 25, -11 ≤ k ≤ 13, -34 ≤ l ≤ 25
Reflections collected 43076
Independent reflections 12661 [Rint = 0.0594, Rsigma = 0.0669]
Data/restraints/parameters 12661/0/425
Goodness-of-fit on F2 1.018
Final R indexes [I>=2σ (I)] R1 = 0.0363, wR2 = 0.0671
Final R indexes [all data] R1 = 0.0729, wR2 = 0.0769
Largest diff. peak/hole / e Å-3 0.64/-0.79

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for mo_B0175_0m. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Br1990.4(2)7263.9(3)5855.9(2)22.96(6)
Zn1297.8(2)8566.3(3)5057.0(2)13.62(6)
Fe11187.5(2)9698.1(4)3108.1(2)15.81(7)
Si11439.3(3)10770.6(7)4610.6(3)14.66(13)
O1652.0(9)10430.1(16)4848.0(7)15.7(3)
N19.3(10)7376(2)4297.3(8)14.1(4)
C11479.7(12)9494(2)4011.7(10)14.0(4)
C2932.4(12)8429(2)3732.3(10)14.0(4)
C31281.7(13)7628(3)3341.5(10)16.8(5)
C42038.7(13)8189(3)3366.6(11)18.4(5)
C52160.6(13)9325(3)3772.3(10)16.4(5)
C6400.8(18)11299(3)2880.3(13)36.3(7)
C7154.4(15)10125(3)2524.4(12)29.9(6)
C8738.9(16)9793(3)2223.6(12)31.3(6)
C91353.2(17)10774(4)2391.9(14)43.6(9)
C101146(2)11714(3)2802.6(14)45.4(9)
C111447.1(15)12619(3)4352.0(12)26.6(6)
C122332.8(13)10445(3)5196.8(11)25.2(6)
C1397.2(12)8229(3)3778.3(10)15.3(5)
C14467.1(14)6042(2)4332.0(11)19.2(5)
C15-834.7(13)6998(3)4203.7(11)19.3(5)
Br26169.0(2)7729.1(3)5711.5(2)23.24(6)
Zn25308.6(2)6415.5(3)4997.0(2)13.07(6)
Fe26293.8(2)5580.5(4)3063.8(2)16.02(7)
Si26310.4(3)4033.5(7)4482.8(3)13.70(13)
O25599.0(9)4509.0(16)4785.5(7)15.4(3)
N24908(1)7515(2)4224.2(8)14.6(4)
C166444.8(13)5468(2)3966.3(10)15.8(5)
C175915.1(12)6586(2)3710.7(10)14.9(4)
C186314.6(13)7547(3)3413.8(10)17.2(5)
C197096.0(13)7040(3)3474.2(10)17.9(5)
C207173.5(13)5774(3)3807.7(10)16.6(5)
C215795.2(19)3756(3)2702.2(13)37.2(8)
C225317.7(15)4920(4)2467.2(13)36.2(8)
C235767.5(15)5812(3)2191.5(12)29.4(6)
C246518.1(15)5208(3)2257.6(11)24.9(6)
C256539.7(17)3937(3)2572.9(12)30.2(6)
C267264.8(13)3912(3)5034.0(11)22.3(5)
C276073.4(15)2278(3)4130.2(12)23.9(5)
C285060.9(12)6709(3)3712.4(11)17.0(5)
C295265.9(14)8948(2)4245.4(11)20.8(5)
C304044.9(13)7695(3)4124.7(11)22.4(5)
O36665.4(15)523(3)2736.6(16)81.2(10)
C317104(3)-542(4)1973.4(19)80.2(15)
C327214.7(18)113(3)2543.6(16)42.5(8)
C338024.2(18)245(4)2900.6(16)45.7(8)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for mo_B0175_0m. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Br124.88(12)22.73(13)19.16(13)4.19(10)0.75(9)1.99(11)
Zn113.37(11)12.87(13)15.17(14)-0.44(10)4.45(10)-0.45(10)
Fe115.26(14)18.49(17)13.67(18)2.94(13)3.34(12)-1.35(13)
Si113.1(3)14.0(3)18.1(3)-2.7(3)6.1(2)-2.8(3)
O114.6(7)13.5(8)20.8(9)-0.8(6)7.7(6)-1.9(6)
N113.7(8)14.9(10)13.8(10)0.6(7)3.4(7)-1.9(8)
C112.4(9)12.2(11)16.8(12)3.0(9)2.0(8)-1.0(8)
C212.7(9)14.9(11)14.2(12)0.8(9)2.3(8)-1.7(9)
C318.6(10)16.6(11)16.1(12)0.6(9)5.7(9)-1(1)
C415.9(10)20.7(12)20.5(13)-0.8(10)7.8(9)1.9(10)
C513.5(9)19.9(12)15.3(12)2.0(9)2.5(8)-1.0(9)
C645.3(17)34.4(17)27.4(17)10.6(13)4.8(13)17.9(15)
C720.5(12)37.1(16)28.5(16)13.1(13)-1.6(11)0.1(12)
C836.2(14)38.3(17)16.8(14)5.1(12)0.5(11)6.6(14)
C925.8(13)74(3)30.4(18)32.5(17)4.7(12)-0.7(16)
C1059(2)26.9(16)36.5(19)18.6(14)-17.4(16)-14.4(16)
C1132.5(13)17.8(13)35.4(17)-2.0(11)20.2(12)-3.8(11)
C1217.2(11)36.2(16)21.7(14)-9.6(11)3.7(10)-3.8(11)
C1313.4(9)17.4(11)14.6(12)0.5(9)2.5(8)-1.0(9)
C1423.8(11)14.4(11)20.8(13)1.1(9)7.8(10)0.9(10)
C1516.7(10)19.0(12)23.7(14)-2.7(10)7.6(9)-5.9(10)
Br220.56(11)26.05(13)21.43(14)-5.29(10)1.47(9)-6.56(11)
Zn212.90(11)11.79(13)14.86(14)0.49(10)3.92(10)-0.39(10)
Fe215.10(14)19.52(17)13.95(18)-3.07(13)4.42(12)-0.34(14)
Si212.1(3)12.3(3)17.3(3)0.3(2)4.5(2)0.5(2)
O215.2(7)12.3(8)20.4(9)0.2(6)7.8(6)-0.5(6)
N214.1(8)14.7(10)15.5(10)1.0(7)4.5(7)0.6(8)
C1616.5(10)15.6(12)15.2(12)-3.5(9)3.5(9)-0.5(9)
C1716(1)16.4(11)12.6(11)-1.7(9)3.9(8)-0.2(9)
C1818.3(10)16.4(12)17.0(12)0.7(9)4.5(9)-1.0(9)
C1916.5(10)19.5(12)18.7(13)0.2(9)6.2(9)-1.7(10)
C2014.8(10)18.5(12)16.9(12)-1.1(9)4.5(9)-0.3(9)
C2157.5(19)34.9(17)21.9(16)-12.9(12)14.3(14)-24.8(16)
C2220.3(12)62(2)25.5(16)-24.9(15)4.4(11)-9.9(14)
C2329.4(13)37.3(16)18.7(14)-6.8(12)0.0(11)3.9(13)
C2426.2(12)33.2(15)17.6(14)-6.1(11)10(1)-2.3(12)
C2540.7(15)27.8(15)20.8(15)-11.4(11)4.7(12)5.9(13)
C2616.1(10)26.0(13)24.9(14)7.1(11)4.6(10)0.5(10)
C2726.4(12)16.3(12)31.0(15)-1.9(11)10.3(11)-0.6(11)
C2815.6(10)18.1(12)16.8(12)-0.7(9)2.7(9)1.2(9)
C2928.5(12)14.3(11)20.5(13)1.2(9)7.5(10)1.4(10)
C3016.1(10)28.8(14)23.7(14)4.8(11)7.3(10)6.5(11)
O351.9(15)45.7(17)161(3)23.7(18)55.4(19)7.5(14)
C3186(3)49(2)77(3)-16(2)-41(2)14(2)
C3236.1(15)19.4(14)71(3)5.7(15)11.8(16)-3.5(14)
C3344.6(18)43.7(19)47(2)1.8(16)7.4(15)-13.1(17)

 

Table 4 Bond Lengths for mo_B0175_0m.
AtomAtomLength/Å AtomAtomLength/Å
Br1Zn12.3365(4) Zn2O21.9729(16)
Zn1Zn112.9034(5) Zn2O221.9839(15)
Zn1O11.9728(16) Zn2N22.0681(19)
Zn1O111.9747(15) Fe2C162.075(2)
Zn1N12.0710(19) Fe2C172.030(2)
Fe1C12.071(2) Fe2C182.035(2)
Fe1C22.024(2) Fe2C192.048(2)
Fe1C32.035(2) Fe2C202.052(2)
Fe1C42.055(2) Fe2C212.034(3)
Fe1C52.057(2) Fe2C222.042(3)
Fe1C62.037(3) Fe2C232.052(3)
Fe1C72.042(3) Fe2C242.049(3)
Fe1C82.044(3) Fe2C252.042(3)
Fe1C92.043(3) Si2O21.6346(16)
Fe1C102.038(3) Si2C161.873(2)
Si1O11.6354(15) Si2C261.866(2)
Si1C11.868(2) Si2C271.863(3)
Si1C111.857(3) O2Zn221.9839(15)
Si1C121.856(3) N2C281.499(3)
O1Zn111.9747(15) N2C291.494(3)
N1C131.499(3) N2C301.486(3)
N1C141.491(3) C16C171.445(3)
N1C151.489(3) C16C201.440(3)
C1C21.442(3) C17C181.426(3)
C1C51.441(3) C17C281.503(3)
C2C31.433(3) C18C191.427(3)
C2C131.505(3) C19C201.422(3)
C3C41.418(3) C21C221.418(5)
C4C51.421(3) C21C251.417(4)
C6C71.399(4) C22C231.411(4)
C6C101.417(5) C23C241.410(4)
C7C81.407(4) C24C251.410(4)
C8C91.409(4) O3C321.219(4)
C9C101.420(5) C31C321.447(5)
Br2Zn22.3381(4) C32C331.477(4)
Zn2Zn222.8963(5)    

1-X,2-Y,1-Z; 21-X,1-Y,1-Z

 

Table 5 Bond Angles for mo_B0175_0m.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
Br1Zn1Zn11132.710(17) O2Zn2Br2120.50(5)
O11Zn1Br1117.37(5) O2Zn2Zn2243.10(4)
O1Zn1Br1122.55(5) O22Zn2Zn2242.80(4)
O1Zn1Zn1142.67(4) O2Zn2O2285.90(6)
O11Zn1Zn1142.62(5) O22Zn2N2108.56(7)
O1Zn1O1185.30(6) O2Zn2N2107.26(7)
O1Zn1N1107.63(7) N2Zn2Br2113.06(5)
O11Zn1N1108.38(7) N2Zn2Zn22114.84(5)
N1Zn1Br1112.33(5) C17Fe2C1641.22(9)
N1Zn1Zn11114.86(5) C17Fe2C1841.07(9)
C2Fe1C141.21(9) C17Fe2C1968.81(9)
C2Fe1C341.34(9) C17Fe2C2068.50(9)
C2Fe1C468.85(9) C17Fe2C21121.90(11)
C2Fe1C568.47(9) C17Fe2C22106.82(10)
C2Fe1C6112.55(11) C17Fe2C23123.08(10)
C2Fe1C7107.02(10) C17Fe2C24159.51(10)
C2Fe1C8131.55(11) C17Fe2C25158.18(11)
C2Fe1C9171.61(13) C18Fe2C1669.47(9)
C2Fe1C10144.78(13) C18Fe2C1940.93(9)
C3Fe1C169.45(9) C18Fe2C2068.59(9)
C3Fe1C440.57(9) C18Fe2C22119.45(11)
C3Fe1C568.21(9) C18Fe2C23105.43(11)
C3Fe1C6142.88(11) C18Fe2C24122.75(11)
C3Fe1C7112.06(11) C18Fe2C25160.17(11)
C3Fe1C8107.69(11) C19Fe2C1669.11(9)
C3Fe1C9133.25(13) C19Fe2C2040.58(9)
C3Fe1C10173.88(13) C19Fe2C23119.86(11)
C4Fe1C169.03(9) C19Fe2C24107.03(10)
C4Fe1C540.41(9) C20Fe2C1640.85(8)
C5Fe1C140.85(8) C20Fe2C23156.08(10)
C6Fe1C1109.29(11) C21Fe2C16108.84(11)
C6Fe1C4175.91(12) C21Fe2C18156.10(11)
C6Fe1C5135.99(12) C21Fe2C19162.45(12)
C6Fe1C740.10(12) C21Fe2C20126.64(12)
C6Fe1C867.83(12) C21Fe2C2240.71(13)
C6Fe1C968.19(13) C21Fe2C2367.95(13)
C6Fe1C1040.69(13) C21Fe2C2467.92(11)
C7Fe1C1132.51(10) C21Fe2C2540.69(12)
C7Fe1C4143.74(11) C22Fe2C16124.91(11)
C7Fe1C5173.25(11) C22Fe2C19154.80(12)
C7Fe1C840.30(11) C22Fe2C20162.89(12)
C7Fe1C967.82(11) C22Fe2C2340.32(12)
C8Fe1C1171.51(10) C22Fe2C2467.92(11)
C8Fe1C4114.38(11) C22Fe2C2568.42(12)
C8Fe1C5146.44(10) C23Fe2C16160.84(10)
C9Fe1C1147.10(12) C24Fe2C16157.87(10)
C9Fe1C4111.04(12) C24Fe2C20122.22(10)
C9Fe1C5117.25(10) C24Fe2C2340.23(10)
C9Fe1C840.33(12) C25Fe2C16122.84(11)
C10Fe1C1115.34(12) C25Fe2C19124.71(11)
C10Fe1C4136.19(12) C25Fe2C20109.43(11)
C10Fe1C5112.55(11) C25Fe2C2367.95(11)
C10Fe1C767.95(12) C25Fe2C2440.33(11)
C10Fe1C868.13(13) O2Si2C16107.65(9)
C10Fe1C940.72(14) O2Si2C26111.58(10)
O1Si1C1108.05(9) O2Si2C27108.98(10)
O1Si1C11111.61(10) C26Si2C16105.44(11)
O1Si1C12110.43(10) C27Si2C16114.24(11)
C11Si1C1111.23(11) C27Si2C26108.95(12)
C12Si1C1106.08(11) Zn2O2Zn2294.10(6)
C12Si1C11109.30(13) Si2O2Zn2129.00(9)
Zn1O1Zn1194.70(6) Si2O2Zn22136.67(10)
Si1O1Zn1126.90(9) C28N2Zn2110.96(14)
Si1O1Zn11138.00(10) C29N2Zn2112.02(14)
C13N1Zn1110.74(14) C29N2C28109.83(18)
C14N1Zn1113.24(14) C30N2Zn2108.83(14)
C14N1C13110.32(17) C30N2C28107.29(18)
C15N1Zn1107.15(14) C30N2C29107.75(18)
C15N1C13107.19(17) Si2C16Fe2133.80(12)
C15N1C14107.93(18) C17C16Fe267.72(13)
Si1C1Fe1131.70(12) C17C16Si2129.54(16)
C2C1Fe167.63(13) C20C16Fe268.75(13)
C2C1Si1131.20(16) C20C16Si2124.44(17)
C5C1Fe169.07(13) C20C16C17105.5(2)
C5C1Si1122.96(17) C16C17Fe271.06(13)
C5C1C2105.6(2) C16C17C28126.9(2)
C1C2Fe171.16(13) C18C17Fe269.67(13)
C1C2C13127.7(2) C18C17C16109.32(19)
C3C2Fe169.75(13) C18C17C28123.6(2)
C3C2C1108.93(19) C28C17Fe2122.47(16)
C3C2C13123.1(2) C17C18Fe269.26(13)
C13C2Fe1120.56(15) C17C18C19107.7(2)
C2C3Fe168.91(13) C19C18Fe270.02(14)
C4C3Fe170.49(14) C18C19Fe269.05(13)
C4C3C2108.0(2) C20C19Fe269.87(13)
C3C4Fe168.94(13) C20C19C18107.9(2)
C3C4C5107.9(2) C16C20Fe270.40(13)
C5C4Fe169.86(13) C19C20Fe269.55(13)
C1C5Fe170.09(13) C19C20C16109.6(2)
C4C5Fe169.72(13) C22C21Fe269.98(16)
C4C5C1109.6(2) C25C21Fe269.99(16)
C7C6Fe170.14(16) C25C21C22108.2(3)
C7C6C10108.2(3) C21C22Fe269.32(16)
C10C6Fe169.66(17) C23C22Fe270.22(15)
C6C7Fe169.76(16) C23C22C21107.6(2)
C6C7C8108.5(3) C22C23Fe269.46(16)
C8C7Fe169.90(15) C24C23Fe269.76(15)
C7C8Fe169.80(16) C24C23C22108.2(3)
C7C8C9108.1(3) C23C24Fe270.01(15)
C9C8Fe169.81(16) C23C24C25108.4(2)
C8C9Fe169.86(16) C25C24Fe269.58(15)
C8C9C10107.8(3) C21C25Fe269.32(16)
C10C9Fe169.43(17) C24C25Fe270.09(15)
C6C10Fe169.65(16) C24C25C21107.5(3)
C6C10C9107.5(3) N2C28C17113.87(19)
C9C10Fe169.85(18) O3C32C31122.2(4)
N1C13C2114.25(18) O3C32C33120.0(4)
Br2Zn2Zn22132.096(17) C31C32C33117.8(3)
O22Zn2Br2118.29(5)     

1-X,2-Y,1-Z; 21-X,1-Y,1-Z

 

Table 6 Torsion Angles for mo_B0175_0m.
ABCDAngle/˚ ABCDAngle/˚
Zn1N1C13C276.4(2) Zn2N2C28C17-68.1(2)
Fe1C1C2C359.76(16) Fe2C16C17C18-59.37(16)
Fe1C1C2C13-114.5(2) Fe2C16C17C28116.9(2)
Fe1C1C5C4-58.64(17) Fe2C16C20C1958.66(17)
Fe1C2C3C459.91(17) Fe2C17C18C19-59.70(17)
Fe1C2C13N1-174.24(15) Fe2C17C28N2-178.95(15)
Fe1C3C4C559.23(17) Fe2C18C19C20-59.30(17)
Fe1C4C5C158.86(16) Fe2C19C20C16-59.18(17)
Fe1C6C7C8-59.38(19) Fe2C21C22C2360.03(19)
Fe1C6C10C959.9(2) Fe2C21C25C24-59.92(19)
Fe1C7C8C9-59.6(2) Fe2C22C23C2459.21(19)
Fe1C8C9C10-59.3(2) Fe2C23C24C2559.18(19)
Fe1C9C10C6-59.7(2) Fe2C24C25C2159.44(18)
Si1C1C2Fe1126.6(2) Si2C16C17Fe2-129.2(2)
Si1C1C2C3-173.67(18) Si2C16C17C18171.45(18)
Si1C1C2C1312.0(4) Si2C16C17C28-12.3(4)
Si1C1C5Fe1-126.93(17) Si2C16C20Fe2129.33(18)
Si1C1C5C4174.42(17) Si2C16C20C19-172.01(17)
O1Si1C1Fe1100.75(15) O2Si2C16Fe2-114.84(15)
O1Si1C1C24.9(2) O2Si2C16C17-18.5(2)
O1Si1C1C5-168.83(18) O2Si2C16C20152.37(19)
C1Si1O1Zn11-123.02(15) C16Si2O2Zn22139.24(14)
C1Si1O1Zn147.76(14) C16Si2O2Zn2-33.76(15)
C1C2C3Fe1-60.63(16) C16C17C18Fe260.22(16)
C1C2C3C4-0.7(3) C16C17C18C190.5(3)
C1C2C13N1-85.2(3) C16C17C28N291.2(3)
C2C1C5Fe157.99(15) C17C16C20Fe2-57.97(15)
C2C1C5C4-0.6(3) C17C16C20C190.7(3)
C2C3C4Fe1-58.91(16) C17C18C19Fe259.22(16)
C2C3C4C50.3(3) C17C18C19C20-0.1(3)
C3C2C13N1101.2(3) C18C17C28N2-93.0(3)
C3C4C5Fe1-58.65(17) C18C19C20Fe258.79(17)
C3C4C5C10.2(3) C18C19C20C16-0.4(3)
C5C1C2Fe1-58.92(15) C20C16C17Fe258.63(16)
C5C1C2C30.8(3) C20C16C17C18-0.7(3)
C5C1C2C13-173.5(2) C20C16C17C28175.5(2)
C6C7C8Fe159.29(19) C21C22C23Fe2-59.46(19)
C6C7C8C9-0.3(3) C21C22C23C24-0.2(3)
C7C6C10Fe1-59.8(2) C22C21C25Fe259.77(19)
C7C6C10C90.0(3) C22C21C25C24-0.2(3)
C7C8C9Fe159.55(19) C22C23C24Fe2-59.02(19)
C7C8C9C100.3(3) C22C23C24C250.2(3)
C8C9C10Fe159.5(2) C23C24C25Fe2-59.44(18)
C8C9C10C6-0.2(3) C23C24C25C210.0(3)
C10C6C7Fe159.5(2) C25C21C22Fe2-59.78(19)
C10C6C7C80.1(3) C25C21C22C230.2(3)
C11Si1O1Zn1170.35(13) C26Si2O2Zn281.47(15)
C11Si1O1Zn11-0.42(19) C26Si2O2Zn22-105.52(16)
C11Si1C1Fe1-22.08(18) C26Si2C16Fe2125.93(16)
C11Si1C1C2-118.0(2) C26Si2C16C17-137.7(2)
C11Si1C1C568.3(2) C26Si2C16C2033.1(2)
C12Si1O1Zn1-67.85(15) C27Si2O2Zn2214.83(18)
C12Si1O1Zn11121.38(16) C27Si2O2Zn2-158.17(13)
C12Si1C1Fe1-140.83(15) C27Si2C16Fe26.3(2)
C12Si1C1C2123.3(2) C27Si2C16C17102.7(2)
C12Si1C1C5-50.4(2) C27Si2C16C20-86.5(2)
C13C2C3Fe1114.0(2) C28C17C18Fe2-116.2(2)
C13C2C3C4173.9(2) C28C17C18C19-175.9(2)
C14N1C13C2-49.8(3) C29N2C28C1756.3(2)
C15N1C13C2-167.05(19) C30N2C28C17173.1(2)

1-X,2-Y,1-Z; 21-X,1-Y,1-Z

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for mo_B0175_0m.
AtomxyzU(eq)
H310476857310720
H424007863315022
H526219887387120
H611711740313144
H7-3269634249136
H87229040195438
H9182210802225552
H10145212481299155
H11A93412850410040
H11B185312727413040
H11C155813256469040
H12A236511145550938
H12B279710520503338
H12C23089498535838
H13A-1429167379918
H13B-1987760341718
H14A10276263440429
H14B3055526396229
H14C3705460465329
H15A-9136426453329
H15B-9976458383929
H15C-11497860417729
H1861008376321221
H1974947471331921
H2076355217391020
H2156422987291045
H2247905072249143
H2355956671199535
H2469385592211430
H2569743315267936
H26A73604792525934
H26B76893758483234
H26C72473124530134
H27A61121554443336
H27B64452064388736
H27C55392293388436
H28A47847180334620
H28B48395750371420
H29A51209503455631
H29B50759421386831
H29C58388862432631
H30A37936767409934
H30B38498212375834
H30C39248225445134
H31A7151-15682020120
H31B7505-1981777120
H31C6583-3061737120
H33A82891023275169
H33B8309-635287969
H33C8011434330969

Experimental

Single crystals of C33H50Br2Fe2N2O3Si2Zn2 [mo_B0175_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 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 [mo_B0175_0m]

Crystal Data for C33H50Br2Fe2N2O3Si2Zn2 (=981.19 g/mol): monoclinic, space group P21/c (no. 14), a = 17.5299(5) Å, b = 9.4853(3) Å, c = 23.4559(7) Å, β = 103.372(2)°, = 3794.4(2) Å3, Z = 4, T = 100.01 K, μ(MoKα) = 4.203 mm-1, Dcalc = 1.718 g/cm3, 43076 reflections measured (4.65° ≤ 2Θ ≤ 63.188°), 12661 unique (Rint = 0.0594, Rsigma = 0.0669) which were used in all calculations. The final R1 was 0.0363 (I > 2σ(I)) and wR2 was 0.0769 (all data).

Refinement model description

Number of restraints - 0, 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.a Secondary CH2 refined with riding coordinates:
C13(H13A,H13B), C28(H28A,H28B)
2.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)
2.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), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C)

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.