mo_B0273_0m_4

Table 1 Crystal data and structure refinement for mo_B0273_0m_4.
Identification code mo_B0273_0m_4
Empirical formula C36H60Br2Fe2N2O2Si4Zn2
Formula weight 1067.48
Temperature/K 99.99
Crystal system triclinic
Space group P-1
a/Å 9.606(3)
b/Å 14.581(6)
c/Å 15.922(6)
α/° 88.661(11)
β/° 86.404(8)
γ/° 77.905(11)
Volume/Å3 2176.1(13)
Z 2
ρcalcg/cm3 1.629
μ/mm‑1 3.722
F(000) 1088.0
Crystal size/mm3 0.157 × 0.143 × 0.08
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.344 to 51.996
Index ranges -11 ≤ h ≤ 11, -17 ≤ k ≤ 17, 0 ≤ l ≤ 19
Reflections collected 11416
Independent reflections 11416 [Rint = ?, Rsigma = 0.0452]
Data/restraints/parameters 11416/0/467
Goodness-of-fit on F2 1.171
Final R indexes [I>=2σ (I)] R1 = 0.0482, wR2 = 0.0923
Final R indexes [all data] R1 = 0.0643, wR2 = 0.1001
Largest diff. peak/hole / e Å-3 0.59/-0.94

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for mo_B0273_0m_4. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Br18148.3(7)-1123.0(5)3882.4(4)20.70(17)
Zn16215.3(8)-3.6(5)4417.0(5)11.34(16)
Fe14729.8(10)1041.1(6)1543.3(6)12.6(2)
Si13344.7(18)144.6(12)3485.0(11)12.2(4)
Si28398.9(19)1053.6(13)1486.1(11)15.1(4)
O14175(4)-10(3)4359(3)14.3(9)
N16389(5)1342(4)4049(3)12.5(11)
C14750(6)271(4)2647(4)11.2(13)
C25767(6)881(4)2624(4)11.8(13)
C36778(6)650(4)1912(4)11.9(13)
C46377(7)-121(4)1504(4)15.0(14)
C55155(7)-338(4)1943(4)14.1(14)
C62689(7)1798(5)1422(4)21.5(16)
C73647(7)2412(5)1467(4)18.7(15)
C84682(7)2192(5)784(4)20.5(15)
C94373(7)1461(5)327(4)18.6(15)
C103145(7)1204(5)723(4)22.1(16)
C112698(7)-935(4)3243(4)18.1(14)
C121811(7)1149(5)3601(4)19.2(15)
C135670(6)1646(4)3245(4)11.1(13)
C145713(7)2015(4)4713(4)16.4(14)
C157925(6)1351(4)3945(4)14.2(13)
C168489(7)2255(5)1818(4)20.0(15)
C179967(7)153(5)1819(4)18.6(15)
C188469(7)1050(5)311(4)20.8(15)
Br212679.5(8)-6274.1(5)3632.2(4)23.36(17)
Zn211077.8(8)-5070.3(5)4320.6(5)12.26(17)
Fe28954.2(10)-3786.4(6)1634.6(6)13.7(2)
Si37960.1(18)-4664.0(12)3649.1(11)12.2(4)
Si412639.4(19)-3955.9(13)1207.1(12)17.2(4)
O28987(4)-4934(3)4437(3)13.1(9)
N211376(5)-3758(3)3921(3)12.9(11)
C199201(6)-4618(4)2699(4)12.7(13)
C2010311(6)-4086(4)2585(4)12.8(13)
C2111078(7)-4316(4)1782(4)13.7(13)
C2210432(7)-4999(4)1417(4)18.2(14)
C239306(7)-5180(4)1970(4)15.5(14)
C246866(8)-3090(6)1623(5)31.0(18)
C257763(9)-2461(5)1807(5)33(2)
C268758(8)-2474(5)1116(5)27.6(18)
C278492(8)-3093(5)518(4)26.4(17)
C287322(8)-3470(5)828(5)25.9(17)
C296954(7)-5594(5)3467(4)22.9(16)
C306647(7)-3553(4)3884(5)19.5(15)
C3110495(6)-3373(4)3204(4)11.1(13)
C3212919(7)-3848(5)3679(5)23.8(16)
C3311011(8)-3092(4)4633(4)19.2(15)
C3412943(7)-2791(4)1525(4)19.4(15)
C3512334(8)-3875(5)62(4)26.0(17)
C3614246(7)-4903(5)1379(5)27.8(17)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for mo_B0273_0m_4. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Br120.9(4)14.4(3)23.1(4)-2.0(3)2.9(3)3.6(3)
Zn110.8(3)11.5(4)11.4(4)0.6(3)0.1(3)-2.1(3)
Fe113.7(5)13.6(5)10.6(5)0.8(4)-1.9(4)-2.9(4)
Si112.3(8)14.0(9)11.5(9)1.2(7)-1.7(7)-4.9(7)
Si214.6(9)16.4(9)14.2(9)0.0(7)1.1(7)-3.5(7)
O115(2)16(2)12(2)5.2(19)-0.8(19)-6.4(18)
N111(3)12(3)15(3)-2(2)-2(2)-4(2)
C111(3)10(3)13(3)-1(2)-4(2)-1(2)
C213(3)12(3)10(3)4(3)-6(2)-3(3)
C313(3)12(3)8(3)5(2)-4(2)4(2)
C419(3)12(3)12(3)5(3)-3(3)1(3)
C518(3)10(3)15(3)-4(3)-7(3)-5(3)
C617(3)30(4)16(4)11(3)-7(3)1(3)
C726(4)17(4)11(3)0(3)-4(3)2(3)
C819(4)21(4)21(4)6(3)-7(3)-3(3)
C925(4)24(4)9(3)5(3)-6(3)-8(3)
C1026(4)28(4)16(4)6(3)-12(3)-13(3)
C1120(3)17(3)19(4)3(3)-3(3)-10(3)
C1214(3)24(4)19(4)4(3)-2(3)-3(3)
C138(3)11(3)12(3)2(3)-1(2)0(2)
C1426(4)11(3)12(3)-1(3)0(3)-2(3)
C1516(3)13(3)14(3)2(3)-1(3)-5(3)
C1618(3)23(4)19(4)2(3)2(3)-4(3)
C1714(3)19(4)22(4)-1(3)4(3)-4(3)
C1819(3)23(4)20(4)1(3)3(3)-5(3)
Br225.8(4)16.0(3)23.4(4)-2.7(3)3.6(3)5.6(3)
Zn211.2(4)11.4(4)13.4(4)0.4(3)0.5(3)-1.2(3)
Fe215.1(5)13.2(5)12.7(5)0.9(4)-2.9(4)-2.2(4)
Si312.3(8)12.6(9)12.3(9)1.1(7)-1.4(7)-3.6(7)
Si415.3(9)16.3(10)19.2(10)0.2(8)4.0(7)-3.3(7)
O214(2)9(2)16(2)0.2(19)-1.2(19)-0.6(17)
N213(3)12(3)14(3)2(2)-1(2)-4(2)
C1913(3)11(3)13(3)4(2)-1(3)3(3)
C209(3)11(3)16(3)2(3)2(2)3(2)
C2119(3)10(3)12(3)3(3)-1(3)-4(3)
C2226(4)11(3)17(4)-1(3)-2(3)0(3)
C2321(3)9(3)17(3)-1(3)-6(3)-3(3)
C2419(4)41(5)27(4)9(4)-5(3)7(3)
C2548(5)17(4)27(4)-2(3)-23(4)13(4)
C2628(4)16(4)40(5)12(3)-18(4)-5(3)
C2734(4)29(4)13(4)8(3)-7(3)3(3)
C2825(4)24(4)30(4)6(3)-10(3)-7(3)
C2923(4)27(4)21(4)3(3)-5(3)-13(3)
C3010(3)19(4)28(4)1(3)1(3)0(3)
C319(3)9(3)14(3)4(3)-2(2)1(2)
C3212(3)27(4)34(4)6(3)-6(3)-7(3)
C3333(4)12(3)15(3)-1(3)-6(3)-7(3)
C3423(4)18(4)18(4)3(3)4(3)-8(3)
C3529(4)30(4)19(4)0(3)11(3)-10(3)
C3617(4)22(4)41(5)0(3)6(3)1(3)

 

Table 4 Bond Lengths for mo_B0273_0m_4.
AtomAtomLength/Å AtomAtomLength/Å
Br1Zn12.3308(11) Br2Zn22.3231(11)
Zn1Zn112.8889(16) Zn2Zn222.8794(16)
Zn1O111.961(4) Zn2O21.973(4)
Zn1O11.970(4) Zn2O221.976(4)
Zn1N12.072(5) Zn2N22.073(5)
Fe1C12.062(6) Fe2C192.058(6)
Fe1C22.027(6) Fe2C202.039(6)
Fe1C32.049(6) Fe2C212.051(6)
Fe1C42.061(6) Fe2C222.044(7)
Fe1C52.060(6) Fe2C232.053(6)
Fe1C62.056(6) Fe2C242.051(7)
Fe1C72.055(7) Fe2C252.044(7)
Fe1C82.040(7) Fe2C262.043(7)
Fe1C92.045(6) Fe2C272.052(7)
Fe1C102.040(7) Fe2C282.060(7)
Si1O11.635(4) Si3O21.634(4)
Si1C11.872(6) Si3C191.875(6)
Si1C111.866(6) Si3C291.860(7)
Si1C121.850(7) Si3C301.862(6)
Si2C31.861(6) Si4C211.870(7)
Si2C161.862(7) Si4C341.869(7)
Si2C171.874(7) Si4C351.861(7)
Si2C181.868(7) Si4C361.872(7)
O1Zn111.961(4) O2Zn221.976(4)
N1C131.507(8) N2C311.492(7)
N1C141.482(8) N2C321.488(8)
N1C151.477(8) N2C331.487(8)
C1C21.451(8) C19C201.446(9)
C1C51.430(8) C19C231.423(8)
C2C31.444(9) C20C211.445(9)
C2C131.492(8) C20C311.493(8)
C3C41.442(9) C21C221.430(9)
C4C51.417(9) C22C231.416(9)
C6C71.417(10) C24C251.429(11)
C6C101.416(10) C24C281.400(11)
C7C81.422(9) C25C261.408(11)
C8C91.397(9) C26C271.400(10)
C9C101.418(9) C27C281.409(10)

11-X,-Y,1-Z; 22-X,-1-Y,1-Z

 

Table 5 Bond Angles for mo_B0273_0m_4.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
Br1Zn1Zn11136.20(5) Br2Zn2Zn22136.25(5)
O1Zn1Br1127.29(13) O22Zn2Br2117.75(13)
O11Zn1Br1117.04(13) O2Zn2Br2126.00(12)
O1Zn1Zn1142.59(13) O2Zn2Zn2243.23(12)
O11Zn1Zn1142.82(12) O22Zn2Zn2243.15(12)
O11Zn1O185.41(18) O2Zn2O2286.38(18)
O11Zn1N1107.13(19) O22Zn2N2106.51(19)
O1Zn1N1104.62(18) O2Zn2N2104.39(18)
N1Zn1Br1111.64(14) N2Zn2Br2112.11(15)
N1Zn1Zn11111.84(15) N2Zn2Zn22111.43(15)
C2Fe1C141.6(2) C19Fe2C28131.6(3)
C2Fe1C341.5(2) C20Fe2C1941.3(2)
C2Fe1C468.5(2) C20Fe2C2141.4(2)
C2Fe1C568.5(2) C20Fe2C2268.4(3)
C2Fe1C6125.1(3) C20Fe2C2368.3(2)
C2Fe1C7107.9(3) C20Fe2C24131.7(3)
C2Fe1C8121.7(3) C20Fe2C25108.3(3)
C2Fe1C9156.3(3) C20Fe2C26115.6(3)
C2Fe1C10161.6(3) C20Fe2C27147.5(3)
C3Fe1C170.3(2) C20Fe2C28170.6(3)
C3Fe1C441.1(2) C21Fe2C1970.0(2)
C3Fe1C569.1(2) C21Fe2C2368.9(3)
C3Fe1C6161.2(3) C21Fe2C27115.3(3)
C3Fe1C7123.7(3) C21Fe2C28147.6(3)
C4Fe1C168.6(2) C22Fe2C1968.6(3)
C5Fe1C140.6(2) C22Fe2C2140.9(2)
C5Fe1C440.2(2) C22Fe2C2340.4(3)
C6Fe1C1108.1(3) C22Fe2C24148.1(3)
C6Fe1C4157.1(3) C22Fe2C27109.8(3)
C6Fe1C5122.6(3) C22Fe2C28117.0(3)
C7Fe1C1122.1(2) C23Fe2C1940.5(2)
C7Fe1C4160.8(3) C23Fe2C28110.3(3)
C7Fe1C5157.8(3) C24Fe2C19108.7(3)
C7Fe1C640.3(3) C24Fe2C21170.6(3)
C8Fe1C1157.9(3) C24Fe2C23116.5(3)
C8Fe1C3106.3(3) C24Fe2C2767.5(3)
C8Fe1C4123.9(3) C24Fe2C2839.8(3)
C8Fe1C5160.1(3) C25Fe2C19115.5(3)
C8Fe1C667.8(3) C25Fe2C21130.6(3)
C8Fe1C740.6(3) C25Fe2C22170.1(3)
C8Fe1C940.0(3) C25Fe2C23148.2(3)
C9Fe1C1160.6(3) C25Fe2C2440.9(3)
C9Fe1C3119.8(3) C25Fe2C2767.6(3)
C9Fe1C4107.2(3) C25Fe2C2867.7(3)
C9Fe1C5124.2(3) C26Fe2C19147.7(3)
C9Fe1C667.9(3) C26Fe2C21107.9(3)
C9Fe1C768.0(3) C26Fe2C22131.7(3)
C10Fe1C1124.1(3) C26Fe2C23170.7(3)
C10Fe1C3155.8(3) C26Fe2C2467.9(3)
C10Fe1C4121.3(3) C26Fe2C2540.3(3)
C10Fe1C5108.0(3) C26Fe2C2740.0(3)
C10Fe1C640.4(3) C26Fe2C2867.4(3)
C10Fe1C768.1(3) C27Fe2C19170.7(3)
C10Fe1C867.8(3) C27Fe2C23132.6(3)
C10Fe1C940.6(3) C27Fe2C2840.1(3)
O1Si1C1105.0(2) O2Si3C19105.4(3)
O1Si1C11109.8(3) O2Si3C29111.5(3)
O1Si1C12109.5(3) O2Si3C30109.3(3)
C11Si1C1107.0(3) C29Si3C19107.3(3)
C12Si1C1115.9(3) C29Si3C30108.1(3)
C12Si1C11109.6(3) C30Si3C19115.1(3)
C3Si2C16114.2(3) C21Si4C36107.4(3)
C3Si2C17106.4(3) C34Si4C21114.2(3)
C3Si2C18109.6(3) C34Si4C36110.8(3)
C16Si2C17111.9(3) C35Si4C21108.7(3)
C16Si2C18107.6(3) C35Si4C34107.0(3)
C18Si2C17107.0(3) C35Si4C36108.6(3)
Zn11O1Zn194.59(18) Zn2O2Zn2293.62(18)
Si1O1Zn11140.8(3) Si3O2Zn2123.2(2)
Si1O1Zn1123.4(2) Si3O2Zn22141.4(3)
C13N1Zn1112.3(4) C31N2Zn2113.0(4)
C14N1Zn1109.7(4) C32N2Zn2107.4(4)
C14N1C13107.8(5) C32N2C31110.5(5)
C15N1Zn1107.3(4) C33N2Zn2109.4(4)
C15N1C13110.5(5) C33N2C31108.7(5)
C15N1C14109.1(5) C33N2C32107.6(5)
Si1C1Fe1133.4(3) Si3C19Fe2130.6(3)
C2C1Fe167.9(3) C20C19Fe268.6(3)
C2C1Si1129.0(5) C20C19Si3127.9(5)
C5C1Fe169.7(4) C23C19Fe269.6(4)
C5C1Si1124.5(5) C23C19Si3125.5(5)
C5C1C2106.0(5) C23C19C20106.4(5)
C1C2Fe170.5(3) C19C20Fe270.0(3)
C1C2C13122.3(5) C19C20C31122.3(5)
C3C2Fe170.1(3) C21C20Fe269.8(4)
C3C2C1109.7(5) C21C20C19109.2(5)
C3C2C13128.0(6) C21C20C31128.4(6)
C13C2Fe1123.6(4) C31C20Fe2123.0(4)
Si2C3Fe1128.6(3) Si4C21Fe2127.7(3)
C2C3Fe168.4(3) C20C21Fe268.9(3)
C2C3Si2135.8(5) C20C21Si4134.8(5)
C4C3Fe169.9(3) C22C21Fe269.3(4)
C4C3Si2118.4(5) C22C21Si4119.3(5)
C4C3C2105.7(5) C22C21C20105.9(5)
C3C4Fe169.0(3) C21C22Fe269.8(4)
C5C4Fe169.9(4) C23C22Fe270.1(4)
C5C4C3109.2(6) C23C22C21109.4(6)
C1C5Fe169.8(4) C19C23Fe269.9(3)
C4C5Fe169.9(4) C22C23Fe269.4(4)
C4C5C1109.4(5) C22C23C19109.1(6)
C7C6Fe169.8(4) C25C24Fe269.3(4)
C10C6Fe169.2(4) C28C24Fe270.4(4)
C10C6C7108.1(6) C28C24C25107.7(7)
C6C7Fe169.9(4) C24C25Fe269.8(4)
C6C7C8107.2(6) C26C25Fe269.8(4)
C8C7Fe169.1(4) C26C25C24107.4(7)
C7C8Fe170.3(4) C25C26Fe269.9(4)
C9C8Fe170.2(4) C27C26Fe270.3(4)
C9C8C7108.9(6) C27C26C25108.4(7)
C8C9Fe169.8(4) C26C27Fe269.7(4)
C8C9C10108.0(6) C26C27C28108.2(7)
C10C9Fe169.5(4) C28C27Fe270.3(4)
C6C10Fe170.4(4) C24C28Fe269.7(4)
C6C10C9107.9(6) C24C28C27108.3(7)
C9C10Fe169.9(4) C27C28Fe269.6(4)
C2C13N1114.5(5) N2C31C20114.8(5)

11-X,-Y,1-Z; 22-X,-1-Y,1-Z

 

Table 6 Torsion Angles for mo_B0273_0m_4.
ABCDAngle/˚ ABCDAngle/˚
Zn1N1C13C2-35.2(6) Zn2N2C31C20-36.1(6)
Fe1C1C2C3-59.3(4) Fe2C19C20C21-58.9(4)
Fe1C1C2C13118.1(6) Fe2C19C20C31117.2(6)
Fe1C1C5C458.8(4) Fe2C19C23C2258.5(5)
Fe1C2C3Si2123.7(6) Fe2C20C21Si4122.7(6)
Fe1C2C3C4-60.3(4) Fe2C20C21C22-59.7(4)
Fe1C2C13N1173.2(4) Fe2C20C31N2171.7(4)
Fe1C3C4C5-58.4(4) Fe2C21C22C23-59.1(5)
Fe1C4C5C1-58.7(4) Fe2C22C23C19-58.8(4)
Fe1C6C7C859.3(4) Fe2C24C25C2660.0(5)
Fe1C6C10C9-60.1(5) Fe2C24C28C27-59.1(5)
Fe1C7C8C959.8(5) Fe2C25C26C2760.0(5)
Fe1C8C9C1059.2(5) Fe2C26C27C2860.0(5)
Fe1C9C10C660.4(5) Fe2C27C28C2459.2(5)
Si1C1C2Fe1-128.8(5) Si3C19C20Fe2-125.6(5)
Si1C1C2C3171.9(4) Si3C19C20C21175.5(4)
Si1C1C2C13-10.6(9) Si3C19C20C31-8.4(9)
Si1C1C5Fe1129.4(5) Si3C19C23Fe2126.0(5)
Si1C1C5C4-171.8(4) Si3C19C23C22-175.5(5)
Si2C3C4Fe1-123.8(4) Si4C21C22Fe2-122.5(4)
Si2C3C4C5177.8(4) Si4C21C22C23178.4(5)
O1Si1C1Fe1-146.4(4) O2Si3C19Fe2-146.7(4)
O1Si1C1C2-50.6(6) O2Si3C19C20-53.3(6)
O1Si1C1C5119.6(5) O2Si3C19C23120.6(5)
C1Si1O1Zn11.8(4) C19Si3O2Zn22163.7(4)
C1Si1O1Zn11165.8(4) C19Si3O2Zn23.9(4)
C1C2C3Fe159.5(4) C19C20C21Fe259.1(4)
C1C2C3Si2-176.7(5) C19C20C21Si4-178.2(5)
C1C2C3C4-0.8(7) C19C20C21C22-0.6(7)
C1C2C13N186.3(7) C19C20C31N285.7(7)
C2C1C5Fe1-58.5(4) C20C19C23Fe2-59.0(4)
C2C1C5C40.3(7) C20C19C23C22-0.5(7)
C2C3C4Fe159.4(4) C20C21C22Fe259.4(4)
C2C3C4C51.0(7) C20C21C22C230.3(7)
C3C2C13N1-96.8(7) C21C20C31N2-99.0(7)
C3C4C5Fe157.9(4) C21C22C23Fe258.9(4)
C3C4C5C1-0.8(7) C21C22C23C190.1(7)
C5C1C2Fe159.6(4) C23C19C20Fe259.6(4)
C5C1C2C30.3(7) C23C19C20C210.7(7)
C5C1C2C13177.7(5) C23C19C20C31176.8(5)
C6C7C8Fe1-59.8(4) C24C25C26Fe2-60.0(5)
C6C7C8C90.0(7) C24C25C26C270.0(8)
C7C6C10Fe159.1(4) C25C24C28Fe259.5(5)
C7C6C10C9-1.0(7) C25C24C28C270.4(8)
C7C8C9Fe1-59.9(5) C25C26C27Fe2-59.7(5)
C7C8C9C10-0.7(8) C25C26C27C280.3(8)
C8C9C10Fe1-59.4(5) C26C27C28Fe2-59.6(5)
C8C9C10C61.0(8) C26C27C28C24-0.4(8)
C10C6C7Fe1-58.7(5) C28C24C25Fe2-60.2(5)
C10C6C7C80.6(7) C28C24C25C26-0.2(8)
C11Si1O1Zn1116.4(3) C29Si3O2Zn22-80.1(5)
C11Si1O1Zn11-79.6(5) C29Si3O2Zn2120.0(3)
C11Si1C1Fe197.0(5) C29Si3C19Fe294.3(5)
C11Si1C1C2-167.3(5) C29Si3C19C20-172.3(5)
C11Si1C1C53.0(6) C29Si3C19C231.6(6)
C12Si1O1Zn1-123.3(3) C30Si3O2Zn2239.4(5)
C12Si1O1Zn1140.8(5) C30Si3O2Zn2-120.5(3)
C12Si1C1Fe1-25.6(6) C30Si3C19Fe2-26.1(6)
C12Si1C1C270.2(6) C30Si3C19C2067.3(6)
C12Si1C1C5-119.5(5) C30Si3C19C23-118.8(5)
C13C2C3Fe1-117.7(6) C31C20C21Fe2-116.7(6)
C13C2C3Si26.0(10) C31C20C21Si46.0(10)
C13C2C3C4-178.0(6) C31C20C21C22-176.4(6)
C14N1C13C2-156.2(5) C32N2C31C2084.3(6)
C15N1C13C284.6(6) C33N2C31C20-157.8(5)
C16Si2C3Fe175.2(5) C34Si4C21Fe273.0(5)
C16Si2C3C2-23.2(7) C34Si4C21C20-24.2(7)
C16Si2C3C4161.2(5) C34Si4C21C22158.4(5)
C17Si2C3Fe1-160.9(4) C35Si4C21Fe2-46.5(5)
C17Si2C3C2100.7(6) C35Si4C21C20-143.6(6)
C17Si2C3C4-74.8(5) C35Si4C21C2239.0(6)
C18Si2C3Fe1-45.5(5) C36Si4C21Fe2-163.7(4)
C18Si2C3C2-144.0(6) C36Si4C21C2099.1(7)
C18Si2C3C440.5(6) C36Si4C21C22-78.3(6)

11-X,-Y,1-Z; 22-X,-1-Y,1-Z

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for mo_B0273_0m_4.
AtomxyzU(eq)
H46855-434101818
H54679-814179317
H618821788179626
H736052881187722
H85458249465925
H948931185-16322
H10270671955126
H11A3481-1484328227
H11B2360-885267327
H11C1914-1004364827
H12A12401070411929
H12B12201176311729
H12C21601732362729
H13A46501918338613
H13B61012148297613
H14A47071983480925
H14B57842652453225
H14C62021855523525
H15A83881110446021
H15B80461994383621
H15C8359954347121
H16A75712682174030
H16B92422474147630
H16C87022241241330
H17A990276243328
H17B10850360164628
H17C9969-446155428
H18A843042411731
H18B935912178831
H18C7656150911131
H2210715-528788722
H238714-5609187019
H246099-3225197637
H257699-2102230339
H269487-2121106633
H279010-3235-832
H286912-390754731
H29A7623-6199339734
H29B6425-5442295834
H29C6285-5632395134
H30A6128-3617442529
H30B5972-3421343829
H30C7151-3037391329
H31A10942-2897290313
H31B9540-3051343313
H32A13112-3227353736
H32B13180-4258319036
H32C13483-4119415036
H33A10017-3057483629
H33B11136-2469444229
H33C11640-3311509029
H34A12058-2318148829
H34B13692-2613114929
H34C13238-2831210529
H35A12008-4433-10839
H35B13226-3838-25739
H35C11607-3313-5039
H36A14407-4962198142
H36B15082-4743107242
H36C14089-5499117242

Experimental

Single crystals of C36H60Br2Fe2N2O2Si4Zn2 [mo_B0273_0m_4] were []. A suitable crystal was selected and [] on a Bruker SMART APEX2 area detector diffractometer. The crystal was kept at 99.99 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_B0273_0m_4]

Crystal Data for C36H60Br2Fe2N2O2Si4Zn2 (=1067.48 g/mol): triclinic, space group P-1 (no. 2), a = 9.606(3) Å, b = 14.581(6) Å, c = 15.922(6) Å, α = 88.661(11)°, β = 86.404(8)°, γ = 77.905(11)°, = 2176.1(13) Å3, Z = 2, T = 99.99 K, μ(MoKα) = 3.722 mm-1, Dcalc = 1.629 g/cm3, 11416 reflections measured (4.344° ≤ 2Θ ≤ 51.996°), 11416 unique (Rint = ?, Rsigma = 0.0452) which were used in all calculations. The final R1 was 0.0482 (I > 2σ(I)) and wR2 was 0.1001 (all data).

Refinement model description

Number of restraints - 0, number of constraints - unknown.

Details:

1. Twinned data refinement
Scales: 0.7583(6) 0.2417(6)
2. 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
3.a Secondary CH2 refined with riding coordinates:
C13(H13A,H13B), C31(H31A,H31B)
3.b Aromatic/amide H refined with riding coordinates:
C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C22(H22), C23(H23),
C24(H24), C25(H25), C26(H26), C27(H27), C28(H28)
3.c Idealised Me refined as rotating group:
C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C29(H29A,
H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C),
C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C)

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