mo_B0280_0m_4

Table 1 Crystal data and structure refinement for mo_B0280_0m_4.
Identification code mo_B0280_0m_4
Empirical formula C33H50Br2Fe2N2O3Si2Zn2
Formula weight 981.19
Temperature/K 99.98
Crystal system monoclinic
Space group P21
a/Å 15.9023(13)
b/Å 10.8845(9)
c/Å 22.8822(19)
α/° 90
β/° 91.977(3)
γ/° 90
Volume/Å3 3958.3(6)
Z 4
ρcalcg/cm3 1.646
μ/mm‑1 4.029
F(000) 1984.0
Crystal size/mm3 0.136 × 0.053 × 0.051
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.144 to 55.996
Index ranges -21 ≤ h ≤ 20, -14 ≤ k ≤ 14, -30 ≤ l ≤ 30
Reflections collected 24737
Independent reflections 24737 [Rint = ?, Rsigma = 0.0434]
Data/restraints/parameters 24737/1/850
Goodness-of-fit on F2 1.078
Final R indexes [I>=2σ (I)] R1 = 0.0433, wR2 = 0.0998
Final R indexes [all data] R1 = 0.0578, wR2 = 0.1062
Largest diff. peak/hole / e Å-3 0.62/-0.55
Flack parameter-0.003(4)

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for mo_B0280_0m_4. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Br16205.8(6)5289.6(9)8167.1(4)30.5(2)
Br27002.9(6)1438.3(10)6763.4(5)36.4(3)
Zn17592.2(6)4750.3(10)7970.1(4)22.4(2)
Zn27998.1(6)2771.4(9)7193.4(5)23.3(2)
Fe18876.6(8)3051.8(12)9925.8(6)24.1(3)
Fe28909.8(8)4684.1(15)5299.7(6)28.8(3)
Si17732.9(16)2178(2)8610.1(11)22.1(5)
Si27600.6(16)5268(3)6522.5(11)25.7(5)
O17942(4)3015(6)8038(3)23.2(13)
O27850(4)4590(6)7139(3)25.1(14)
N18481(5)5736(7)8459(3)25.3(17)
N29207(4)2482(7)6933(3)25.6(17)
C17961(5)3174(8)9262(4)22.9(19)
C28459(6)4285(8)9314(4)24(2)
C38388(5)4768(9)9884(4)24.9(19)
C47851(6)3985(9)10202(4)28(2)
C57594(5)3034(8)9820(4)26(2)
C69773(6)1790(9)9707(5)33(2)
C710160(6)2900(10)9910(5)34(2)
C89899(6)3124(9)10486(5)33(2)
C99356(6)2152(10)10643(5)36(2)
C109279(7)1340(9)10160(5)39(3)
C116596(5)1782(9)8617(4)28(2)
C128368(6)742(8)8592(4)28(2)
C138974(5)4869(8)8851(4)24.2(19)
C148094(6)6715(9)8816(4)29(2)
C159057(6)6329(9)8053(4)31(2)
C168074(6)4299(9)5934(4)27(2)
C178800(6)3521(9)5985(4)30(2)
C188854(6)2848(9)5458(4)31(2)
C198174(6)3200(9)5073(5)33(2)
C207692(6)4083(9)5371(4)29(2)
C219126(6)6535(9)5217(4)32(2)
C229827(6)5954(10)5499(5)36(2)
C2310127(6)5050(11)5114(5)40(3)
C249612(7)5096(11)4596(5)44(3)
C258995(7)6028(10)4670(5)41(3)
C266441(5)5270(11)6378(4)36(2)
C277979(7)6886(9)6548(5)38(2)
C289419(6)3441(10)6493(4)30(2)
C299284(6)1229(9)6670(5)37(3)
C309815(6)2591(10)7434(4)31(2)
Br32046.9(7)1277.5(10)6828.8(5)35.9(3)
Br41228.1(6)5318.2(9)7972.5(5)33.5(2)
Zn33072.9(6)2650.7(10)7189.2(5)23.6(2)
Zn42634.4(6)4738.3(10)7883.6(4)23.2(2)
Fe33898.9(9)3747.2(14)5183.9(6)27.9(3)
Fe43917.0(8)3143.2(12)9885.0(6)24.4(3)
Si32889.7(16)5054(2)6421.5(11)25.1(6)
Si42721.9(16)2230(2)8599.8(11)23.9(5)
O32999(4)4471(5)7078(3)23.5(14)
O42966(4)3015(6)8020(3)23.6(13)
N34290(5)2236(7)6977(3)24.9(17)
N43450(5)5775(7)8404(3)24.1(17)
C313167(6)3782(9)5907(4)24(2)
C323846(5)2920(8)5976(4)25(2)
C333768(6)2039(9)5524(4)31(2)
C343045(6)2330(9)5174(4)32(2)
C352690(6)3390(9)5403(4)31(2)
C364718(7)5194(10)5175(5)41(3)
C375115(7)4096(10)4994(5)41(3)
C384671(7)3665(11)4486(5)43(3)
C394001(7)4482(10)4363(5)42(3)
C404018(7)5426(11)4793(5)43(3)
C411777(6)5501(10)6249(5)38(3)
C423568(6)6441(9)6361(4)36(2)
C434526(6)2947(9)6450(4)28(2)
C444367(6)897(9)6852(5)36(3)
C454883(6)2552(10)7476(4)33(2)
C462979(6)3247(9)9242(4)28(2)
C473469(6)4358(8)9274(4)26(2)
C483416(5)4865(8)9846(4)25(2)
C492896(6)4074(9)10182(4)30(2)
C502632(5)3098(9)9813(4)26(2)
C514800(6)1871(9)9658(5)33(2)
C525201(6)3004(9)9816(5)32(2)
C534987(6)3265(9)10398(5)34(2)
C544461(6)2315(9)10603(5)34(2)
C554341(6)1459(10)10140(5)37(2)
C563309(6)744(8)8603(4)30(2)
C571569(6)1907(9)8611(4)30(2)
C583970(5)4943(8)8807(4)25(2)
C593030(6)6714(9)8747(4)29(2)
C604038(6)6394(9)8008(4)31(2)
O510123(7)4285(8)2148(5)70(3)
C618683(8)3821(11)2066(6)57(4)
C629520(8)3837(10)2376(6)45(3)
C639576(7)3313(11)2973(6)52(3)
O64879(5)4209(7)1946(4)48(2)
C644598(7)3171(10)2820(5)38(3)
C654362(7)3764(9)2247(5)35(2)
C663450(6)3778(10)2084(6)47(3)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for mo_B0280_0m_4. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Br121.8(4)32.1(5)37.8(6)-5.4(5)2.8(4)2.1(4)
Br230.9(5)40.5(6)37.7(6)-12.0(5)1.1(4)-7.7(5)
Zn121.6(5)23.8(5)21.7(5)-1.0(5)0.8(4)-0.2(5)
Zn224.2(5)24.6(6)21.3(6)-1.2(4)2.7(4)-0.1(4)
Fe123.8(7)25.0(7)23.5(7)1.5(6)-1.2(5)2.7(5)
Fe227.0(7)37.1(8)22.6(7)4.3(6)3.1(6)-0.2(7)
Si124.6(13)21.2(12)20.5(13)0(1)2.1(11)-2(1)
Si226.7(13)28.3(13)22.1(13)1.1(11)-0.4(11)1.8(12)
O126(3)24(3)20(3)2(3)2(2)1(3)
O229(3)28(3)19(3)1(3)3(3)3(3)
N129(4)25(4)22(4)0(3)-1(3)0(3)
N217(4)35(4)26(4)4(3)5(3)5(3)
C120(4)25(5)24(5)3(4)3(4)6(4)
C219(5)27(5)26(5)5(4)1(4)5(4)
C327(5)23(4)25(5)0(4)-5(4)5(4)
C431(5)32(5)21(5)3(4)2(4)12(4)
C521(5)26(5)30(5)3(4)1(4)1(4)
C635(6)30(5)34(6)-3(4)-4(5)9(4)
C727(5)34(6)40(6)8(5)-3(5)4(4)
C827(5)35(6)35(6)-1(5)-16(4)5(4)
C928(5)49(7)31(6)8(5)-4(4)12(5)
C1039(6)25(5)52(7)6(5)-13(5)1(5)
C1120(5)30(5)35(6)-3(4)-3(4)-5(4)
C1226(5)30(5)28(5)-1(4)8(4)0(4)
C1322(4)21(4)30(5)5(4)-2(4)-3(4)
C1429(5)31(5)26(5)-4(4)-3(4)4(4)
C1529(5)34(5)29(5)5(4)-7(4)-3(4)
C1624(5)31(5)27(5)2(4)1(4)-3(4)
C1728(5)31(5)31(6)6(4)6(4)1(4)
C1835(5)30(5)29(5)0(4)7(4)5(4)
C1935(6)38(6)25(5)-3(4)3(4)-3(5)
C2023(5)39(6)24(5)0(4)2(4)-3(4)
C2127(5)35(6)33(6)14(5)1(4)-2(4)
C2233(6)37(6)39(6)8(5)5(5)-3(5)
C2329(6)52(7)40(7)9(5)10(5)-2(5)
C2447(7)56(8)29(6)2(5)16(5)-17(6)
C2537(6)48(7)37(6)17(5)-2(5)-5(5)
C2625(5)52(6)31(6)0(5)0(4)6(5)
C2751(7)36(6)28(6)1(4)-1(5)2(5)
C2827(5)39(6)24(5)5(4)6(4)3(4)
C2933(6)37(6)41(6)3(5)14(5)11(5)
C3023(5)42(6)28(5)9(5)3(4)0(4)
Br333.2(6)42.7(6)31.9(6)-6.2(5)1.6(4)-11.3(5)
Br421.7(4)34.1(5)44.8(6)-7.7(5)1.6(4)2.3(4)
Zn323.0(5)26.0(6)22.0(6)-0.5(4)1.6(4)0.7(5)
Zn422.2(5)24.7(5)22.6(5)-1.4(5)0.8(4)0.8(5)
Fe328.7(7)33.1(8)22.1(7)2.4(6)2.5(6)0.4(6)
Fe424.3(7)25.7(7)22.9(7)0.4(6)-0.3(5)1.9(5)
Si327.3(13)24.5(14)23.4(14)-0.2(10)0.3(10)2(1)
Si424.4(13)24.5(13)22.8(13)0(1)1.9(11)-2.7(11)
O326(3)24(3)20(3)-1(3)2(3)1(3)
O424(3)26(3)21(3)-2(3)1(2)-1(3)
N326(4)26(4)23(4)4(3)5(3)4(3)
N425(4)19(4)28(4)-1(3)-2(3)6(3)
C3124(5)28(5)20(5)-1(4)4(4)-3(4)
C3223(5)22(5)30(5)2(4)2(4)-2(4)
C3334(6)28(5)31(6)4(4)9(4)3(4)
C3438(6)33(6)26(5)-8(4)5(4)-10(5)
C3531(5)33(6)30(6)3(4)2(4)-3(4)
C3645(6)43(6)37(6)-1(5)14(5)-19(5)
C3731(6)51(7)40(7)15(5)8(5)1(5)
C3853(7)44(7)31(6)11(5)16(5)6(6)
C3951(7)53(7)23(5)12(5)2(5)1(6)
C4043(6)45(7)42(7)16(6)17(5)10(5)
C4136(6)46(7)33(6)1(5)-3(4)12(5)
C4253(7)33(6)23(5)-1(4)5(5)-5(5)
C4328(5)27(5)30(5)5(4)4(4)1(4)
C4432(6)35(6)43(7)6(5)11(5)15(4)
C4524(5)52(7)24(5)5(5)0(4)0(5)
C4629(5)29(5)24(5)-3(4)-1(4)3(4)
C4718(5)27(5)32(5)3(4)1(4)8(4)
C4827(5)21(5)28(5)-1(4)-3(4)5(4)
C4930(5)33(5)27(5)1(4)1(4)6(4)
C5022(5)33(5)23(5)3(4)1(4)2(4)
C5130(5)29(5)40(6)-5(4)-3(5)10(4)
C5223(5)33(5)41(6)-1(5)0(4)9(4)
C5330(5)29(5)43(7)-3(5)-14(5)8(4)
C5431(6)40(6)31(6)5(5)0(4)13(5)
C5535(6)30(6)45(7)10(5)-4(5)6(5)
C5634(5)27(5)28(5)0(4)2(4)-2(4)
C5729(5)36(6)25(5)-3(4)-1(4)-6(4)
C5820(4)27(5)27(5)5(4)-2(4)2(4)
C5927(5)26(5)33(6)-1(4)-6(4)5(4)
C6037(6)29(5)27(5)10(4)-4(4)-6(4)
O581(8)58(6)73(7)-6(5)33(6)-20(5)
C6167(9)39(7)64(9)-5(6)-23(7)7(6)
C6250(7)24(5)61(8)-13(5)10(6)-5(5)
C6348(7)49(8)57(9)-2(6)-9(6)-8(6)
O654(5)45(5)44(5)6(4)10(4)-4(4)
C6446(6)31(6)37(6)-4(5)-3(5)-1(5)
C6538(6)25(5)40(6)-7(5)-1(5)5(5)
C6635(6)32(6)72(9)9(6)-18(6)-1(5)

 

Table 4 Bond Lengths for mo_B0280_0m_4.
AtomAtomLength/Å AtomAtomLength/Å
Br1Zn12.3402(14) Zn3O32.000(6)
Br2Zn22.3389(14) Zn3O41.955(6)
Zn1Zn22.8799(15) Zn3N32.062(7)
Zn1O11.973(6) Zn4O31.973(6)
Zn1O21.968(6) Zn4O41.971(6)
Zn1N12.072(8) Zn4N42.067(8)
Zn2O11.957(6) Fe3C312.056(9)
Zn2O21.997(6) Fe3C322.029(9)
Zn2N22.057(7) Fe3C332.029(10)
Fe1C12.073(9) Fe3C342.055(9)
Fe1C22.034(9) Fe3C352.041(10)
Fe1C32.024(9) Fe3C362.045(10)
Fe1C42.040(9) Fe3C372.033(11)
Fe1C52.046(9) Fe3C382.050(11)
Fe1C62.054(10) Fe3C392.053(10)
Fe1C72.049(10) Fe3C402.046(11)
Fe1C82.036(9) Fe4C462.061(9)
Fe1C92.037(10) Fe4C472.035(9)
Fe1C102.036(10) Fe4C482.038(9)
Fe2C162.045(10) Fe4C492.050(10)
Fe2C172.028(10) Fe4C502.045(9)
Fe2C182.033(10) Fe4C512.052(9)
Fe2C192.051(10) Fe4C522.059(9)
Fe2C202.055(9) Fe4C532.037(10)
Fe2C212.054(10) Fe4C542.040(10)
Fe2C222.050(10) Fe4C552.032(10)
Fe2C232.035(10) Si3O31.634(7)
Fe2C242.041(10) Si3C311.879(10)
Fe2C252.061(10) Si3C411.864(9)
Si1O11.638(6) Si3C421.864(10)
Si1C11.869(9) Si4O41.636(7)
Si1C111.859(9) Si4C461.874(10)
Si1C121.862(9) Si4C561.867(9)
Si2O21.628(6) Si4C571.867(9)
Si2C161.887(10) N3C431.492(12)
Si2C261.863(9) N3C441.491(12)
Si2C271.862(10) N3C451.494(12)
N1C131.504(11) N4C581.516(11)
N1C141.488(11) N4C591.464(11)
N1C151.475(12) N4C601.487(12)
N2C281.497(12) C31C321.436(13)
N2C291.497(13) C31C351.423(13)
N2C301.479(12) C32C331.413(13)
C1C21.448(13) C32C431.504(12)
C1C51.430(13) C33C341.414(13)
C2C31.416(13) C34C351.395(13)
C2C131.501(12) C36C371.420(15)
C3C41.422(13) C36C401.415(15)
C4C51.407(13) C37C381.420(16)
C6C71.426(14) C38C391.409(15)
C6C101.410(15) C39C401.422(16)
C7C81.415(15) C46C471.439(13)
C8C91.419(15) C46C501.443(13)
C9C101.417(14) C47C481.426(13)
C16C171.433(13) C47C581.497(13)
C16C201.425(13) C48C491.435(13)
C17C181.415(14) C49C501.413(13)
C17C281.499(13) C51C521.429(14)
C18C191.424(13) C51C551.416(15)
C19C201.418(13) C52C531.413(15)
C21C221.418(13) C53C541.419(15)
C21C251.378(15) C54C551.419(14)
C22C231.415(15) O5C621.209(14)
C23C241.417(15) C61C621.487(15)
C24C251.425(15) C62C631.480(17)
Br3Zn32.3417(14) O6C651.193(13)
Br4Zn42.3393(15) C64C651.497(15)
Zn3Zn42.8724(15) C65C661.486(13)

 

Table 5 Bond Angles for mo_B0280_0m_4.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
Br1Zn1Zn2122.62(5) O3Zn3N3103.8(3)
O1Zn1Br1119.30(18) O4Zn3Br3112.88(18)
O1Zn1Zn242.66(18) O4Zn3Zn443.19(18)
O1Zn1N1105.5(3) O4Zn3O385.2(3)
O2Zn1Br1115.94(18) O4Zn3N3112.8(3)
O2Zn1Zn243.81(18) N3Zn3Br3115.2(2)
O2Zn1O185.6(3) N3Zn3Zn4123.4(2)
O2Zn1N1114.0(3) Br4Zn4Zn3120.84(5)
N1Zn1Br1113.3(2) O3Zn4Br4115.67(18)
N1Zn1Zn2123.9(2) O3Zn4Zn344.08(17)
Br2Zn2Zn1124.11(5) O3Zn4N4114.9(3)
O1Zn2Br2116.51(18) O4Zn4Br4119.63(18)
O1Zn2Zn143.10(18) O4Zn4Zn342.77(18)
O1Zn2O285.3(3) O4Zn4O385.5(2)
O1Zn2N2112.5(3) O4Zn4N4105.6(3)
O2Zn2Br2120.80(19) N4Zn4Br4112.7(2)
O2Zn2Zn143.01(17) N4Zn4Zn3126.3(2)
O2Zn2N2104.1(3) C32Fe3C3141.2(4)
N2Zn2Br2114.1(2) C32Fe3C3340.8(4)
N2Zn2Zn1121.7(2) C32Fe3C3468.2(4)
C2Fe1C141.3(4) C32Fe3C3568.1(4)
C2Fe1C468.9(4) C32Fe3C36113.3(4)
C2Fe1C567.9(4) C32Fe3C37110.0(4)
C2Fe1C6119.1(4) C32Fe3C38136.1(4)
C2Fe1C7110.1(4) C32Fe3C39176.0(4)
C2Fe1C8130.0(4) C32Fe3C40142.6(4)
C2Fe1C9167.5(4) C33Fe3C3168.9(4)
C2Fe1C10151.3(4) C33Fe3C3440.5(4)
C3Fe1C169.3(4) C33Fe3C3567.7(4)
C3Fe1C240.8(3) C33Fe3C36141.6(4)
C3Fe1C441.0(4) C33Fe3C37111.3(4)
C3Fe1C567.9(4) C33Fe3C38109.3(4)
C3Fe1C6151.0(4) C33Fe3C39136.1(4)
C3Fe1C7117.1(4) C33Fe3C40176.6(5)
C3Fe1C8106.9(4) C34Fe3C3168.3(4)
C3Fe1C9127.9(4) C35Fe3C3140.6(4)
C3Fe1C10166.8(4) C35Fe3C3439.8(4)
C4Fe1C169.2(4) C35Fe3C36139.0(4)
C4Fe1C540.3(4) C35Fe3C38141.1(4)
C4Fe1C6167.8(4) C35Fe3C39113.9(4)
C4Fe1C7148.5(4) C35Fe3C40112.3(4)
C5Fe1C140.6(3) C36Fe3C31111.9(4)
C5Fe1C6131.5(4) C36Fe3C34177.9(5)
C5Fe1C7170.7(4) C36Fe3C3868.1(5)
C6Fe1C1109.9(4) C36Fe3C3967.7(5)
C7Fe1C1131.9(4) C36Fe3C4040.5(4)
C7Fe1C640.7(4) C37Fe3C31137.5(4)
C8Fe1C1169.9(4) C37Fe3C34140.5(4)
C8Fe1C4114.6(4) C37Fe3C35178.0(5)
C8Fe1C5147.8(4) C37Fe3C3640.8(4)
C8Fe1C668.5(4) C37Fe3C3840.7(5)
C8Fe1C740.5(4) C37Fe3C3968.0(5)
C8Fe1C940.8(4) C37Fe3C4068.7(4)
C9Fe1C1148.9(4) C38Fe3C31177.2(4)
C9Fe1C4105.7(4) C38Fe3C34111.9(4)
C9Fe1C5115.8(4) C38Fe3C3940.2(4)
C9Fe1C668.3(4) C39Fe3C31142.5(4)
C9Fe1C768.3(4) C39Fe3C34110.9(4)
C10Fe1C1117.3(4) C40Fe3C31113.5(4)
C10Fe1C4128.4(4) C40Fe3C34137.5(4)
C10Fe1C5109.0(4) C40Fe3C3868.4(5)
C10Fe1C640.3(4) C40Fe3C3940.6(4)
C10Fe1C768.1(4) C47Fe4C4641.1(4)
C10Fe1C868.4(4) C47Fe4C4841.0(4)
C10Fe1C940.7(4) C47Fe4C4969.1(4)
C16Fe2C1968.8(4) C47Fe4C5068.6(4)
C16Fe2C2040.7(4) C47Fe4C51119.4(4)
C16Fe2C21112.4(4) C47Fe4C52108.7(4)
C16Fe2C22117.0(4) C47Fe4C53128.3(4)
C16Fe2C25134.6(4) C47Fe4C54165.7(4)
C17Fe2C1641.2(4) C48Fe4C4669.3(4)
C17Fe2C1840.8(4) C48Fe4C4941.1(4)
C17Fe2C1968.9(4) C48Fe4C5068.3(4)
C17Fe2C2068.5(4) C48Fe4C51151.7(4)
C17Fe2C21134.6(4) C48Fe4C52116.9(4)
C17Fe2C22109.2(4) C48Fe4C54126.6(4)
C17Fe2C23113.1(4) C49Fe4C4669.4(4)
C17Fe2C24144.3(4) C49Fe4C51167.0(4)
C17Fe2C25173.4(5) C49Fe4C52149.4(4)
C18Fe2C1668.8(4) C50Fe4C4641.2(4)
C18Fe2C1940.8(4) C50Fe4C4940.4(4)
C18Fe2C2068.0(4) C50Fe4C51130.9(4)
C18Fe2C21171.5(4) C50Fe4C52169.4(4)
C18Fe2C22131.1(4) C51Fe4C46110.0(4)
C18Fe2C23106.1(4) C51Fe4C5240.7(4)
C18Fe2C24112.7(4) C52Fe4C46130.2(4)
C18Fe2C25145.8(4) C53Fe4C46167.6(4)
C19Fe2C2040.4(4) C53Fe4C48106.4(4)
C19Fe2C21147.7(4) C53Fe4C49115.6(4)
C19Fe2C25115.7(4) C53Fe4C50149.4(4)
C20Fe2C25111.5(4) C53Fe4C5167.9(4)
C21Fe2C20118.7(4) C53Fe4C5240.4(4)
C21Fe2C2539.1(4) C53Fe4C5440.7(4)
C22Fe2C19169.4(4) C54Fe4C46151.1(4)
C22Fe2C20149.6(4) C54Fe4C49105.7(4)
C22Fe2C2140.4(4) C54Fe4C50116.7(4)
C22Fe2C2567.3(4) C54Fe4C5168.3(4)
C23Fe2C16146.6(4) C54Fe4C5268.6(4)
C23Fe2C19129.8(4) C55Fe4C46118.6(4)
C23Fe2C20169.7(4) C55Fe4C47152.7(4)
C23Fe2C2168.0(4) C55Fe4C48165.4(4)
C23Fe2C2240.5(4) C55Fe4C49127.6(4)
C23Fe2C2440.7(4) C55Fe4C50108.8(4)
C23Fe2C2568.2(4) C55Fe4C5140.6(4)
C24Fe2C16172.7(4) C55Fe4C5268.6(4)
C24Fe2C19107.3(4) C55Fe4C5368.4(4)
C24Fe2C20132.5(4) C55Fe4C5440.8(4)
C24Fe2C2167.3(4) O3Si3C31105.7(4)
C24Fe2C2267.9(4) O3Si3C41111.5(4)
C24Fe2C2540.7(4) O3Si3C42109.8(4)
O1Si1C1106.0(4) C41Si3C31107.5(4)
O1Si1C11111.1(4) C41Si3C42108.7(5)
O1Si1C12108.9(4) C42Si3C31113.7(4)
C11Si1C1106.8(4) O4Si4C46106.0(4)
C11Si1C12109.5(4) O4Si4C56108.8(4)
C12Si1C1114.5(4) O4Si4C57111.7(4)
O2Si2C16105.9(4) C56Si4C46114.4(4)
O2Si2C26111.4(4) C57Si4C46106.8(4)
O2Si2C27109.4(4) C57Si4C56109.2(4)
C26Si2C16106.9(5) Zn4O3Zn392.6(3)
C27Si2C16114.5(5) Si3O3Zn3120.4(3)
C27Si2C26108.7(5) Si3O3Zn4140.9(4)
Zn2O1Zn194.2(3) Zn3O4Zn494.0(3)
Si1O1Zn1122.1(3) Si4O4Zn3135.5(4)
Si1O1Zn2137.0(4) Si4O4Zn4123.8(4)
Zn1O2Zn293.2(3) C43N3Zn3109.9(5)
Si2O2Zn1138.1(4) C43N3C45109.2(7)
Si2O2Zn2121.9(4) C44N3Zn3110.0(6)
C13N1Zn1109.2(5) C44N3C43109.1(8)
C14N1Zn1112.3(6) C44N3C45108.5(8)
C14N1C13109.8(7) C45N3Zn3110.0(6)
C15N1Zn1108.2(6) C58N4Zn4110.0(5)
C15N1C13109.2(7) C59N4Zn4113.6(6)
C15N1C14108.0(7) C59N4C58109.9(7)
C28N2Zn2108.8(5) C59N4C60108.6(7)
C28N2C29109.9(8) C60N4Zn4106.9(6)
C29N2Zn2110.3(6) C60N4C58107.5(7)
C30N2Zn2110.8(6) Si3C31Fe3132.0(5)
C30N2C28108.0(7) C32C31Fe368.4(5)
C30N2C29109.0(8) C32C31Si3127.1(7)
Si1C1Fe1131.2(5) C35C31Fe369.1(5)
C2C1Fe167.9(5) C35C31Si3126.8(7)
C2C1Si1129.8(7) C35C31C32105.8(8)
C5C1Fe168.7(5) C31C32Fe370.4(5)
C5C1Si1125.2(7) C31C32C43125.9(9)
C5C1C2104.8(8) C33C32Fe369.6(6)
C1C2Fe170.8(5) C33C32C31108.4(8)
C1C2C13127.3(9) C33C32C43125.7(8)
C3C2Fe169.2(5) C43C32Fe3125.8(6)
C3C2C1108.9(8) C32C33Fe369.6(5)
C3C2C13123.8(8) C32C33C34108.2(8)
C13C2Fe1126.3(6) C34C33Fe370.7(6)
C2C3Fe170.0(5) C33C34Fe368.8(6)
C2C3C4108.5(8) C35C34Fe369.6(6)
C4C3Fe170.1(5) C35C34C33107.7(9)
C3C4Fe168.9(5) C31C35Fe370.2(5)
C5C4Fe170.1(5) C34C35Fe370.6(6)
C5C4C3106.9(8) C34C35C31109.9(9)
C1C5Fe170.7(5) C37C36Fe369.2(6)
C4C5Fe169.6(5) C40C36Fe369.8(6)
C4C5C1110.9(8) C40C36C37108.6(10)
C7C6Fe169.5(5) C36C37Fe370.1(6)
C10C6Fe169.1(6) C38C37Fe370.3(6)
C10C6C7107.4(10) C38C37C36107.7(10)
C6C7Fe169.9(5) C37C38Fe369.0(6)
C8C7Fe169.3(5) C39C38Fe370.1(6)
C8C7C6108.2(9) C39C38C37107.8(10)
C7C8Fe170.2(6) C38C39Fe369.8(6)
C7C8C9108.0(9) C38C39C40108.8(10)
C9C8Fe169.7(5) C40C39Fe369.4(6)
C8C9Fe169.6(6) C36C40Fe369.7(6)
C10C9Fe169.6(6) C36C40C39107.1(10)
C10C9C8107.7(10) C39C40Fe370.0(6)
C6C10Fe170.5(6) N3C43C32112.3(7)
C6C10C9108.7(9) Si4C46Fe4131.3(5)
C9C10Fe169.7(6) C47C46Fe468.5(5)
C2C13N1113.7(7) C47C46Si4129.7(7)
Si2C16Fe2132.6(5) C47C46C50105.8(8)
C17C16Fe268.8(5) C50C46Fe468.8(5)
C17C16Si2127.8(7) C50C46Si4124.3(7)
C20C16Fe270.1(6) C46C47Fe470.4(5)
C20C16Si2124.7(7) C46C47C58128.4(9)
C20C16C17107.0(9) C48C47Fe469.6(5)
C16C17Fe270.0(6) C48C47C46108.8(8)
C16C17C28127.1(9) C48C47C58122.7(9)
C18C17Fe269.8(6) C58C47Fe4125.7(6)
C18C17C16108.0(9) C47C48Fe469.4(5)
C18C17C28124.9(9) C47C48C49108.2(8)
C28C17Fe2124.3(7) C49C48Fe469.9(5)
C17C18Fe269.4(6) C48C49Fe469.0(5)
C17C18C19108.7(9) C50C49Fe469.6(5)
C19C18Fe270.3(6) C50C49C48107.2(9)
C18C19Fe268.9(6) C46C50Fe470.0(5)
C20C19Fe270.0(6) C49C50Fe470.0(5)
C20C19C18107.2(9) C49C50C46110.0(8)
C16C20Fe269.2(5) C52C51Fe469.9(5)
C19C20Fe269.6(6) C55C51Fe469.0(6)
C19C20C16109.0(9) C55C51C52108.3(10)
C22C21Fe269.6(6) C51C52Fe469.4(5)
C25C21Fe270.7(6) C53C52Fe469.0(5)
C25C21C22109.0(10) C53C52C51107.0(10)
C21C22Fe269.9(6) C52C53Fe470.6(6)
C23C22Fe269.2(6) C52C53C54109.2(9)
C23C22C21107.6(10) C54C53Fe469.7(6)
C22C23Fe270.3(6) C53C54Fe469.5(6)
C22C23C24107.4(10) C55C54Fe469.3(6)
C24C23Fe269.9(6) C55C54C53107.3(10)
C23C24Fe269.4(6) C51C55Fe470.5(6)
C23C24C25107.8(10) C51C55C54108.2(9)
C25C24Fe270.4(6) C54C55Fe469.9(6)
C21C25Fe270.1(6) C47C58N4113.3(7)
C21C25C24108.1(9) O5C62C61120.6(14)
C24C25Fe268.9(6) O5C62C63122.0(13)
N2C28C17113.9(8) C63C62C61117.4(11)
Br3Zn3Zn4121.35(5) O6C65C64121.6(11)
O3Zn3Br3123.35(19) O6C65C66122.5(11)
O3Zn3Zn443.34(18) C66C65C64116.0(10)

 

Table 6 Torsion Angles for mo_B0280_0m_4.
ABCDAngle/˚ ABCDAngle/˚
Zn1N1C13C2-66.2(8) Zn3N3C43C32-45.3(9)
Zn2N2C28C17-53.9(9) Zn4N4C58C47-70.0(8)
Fe1C1C2C3-58.9(6) Fe3C31C32C33-59.5(7)
Fe1C1C2C13121.5(9) Fe3C31C32C43120.6(9)
Fe1C1C5C458.1(6) Fe3C31C35C3459.6(7)
Fe1C2C3C4-59.7(6) Fe3C32C33C34-60.5(7)
Fe1C2C13N1179.4(6) Fe3C32C43N3-179.5(6)
Fe1C3C4C5-60.1(6) Fe3C33C34C35-58.9(7)
Fe1C4C5C1-58.7(6) Fe3C34C35C31-59.4(7)
Fe1C6C7C858.9(7) Fe3C36C37C3860.5(7)
Fe1C6C10C9-59.4(7) Fe3C36C40C39-60.3(7)
Fe1C7C8C959.7(6) Fe3C37C38C3959.5(8)
Fe1C8C9C1059.4(7) Fe3C38C39C4058.6(8)
Fe1C9C10C659.9(7) Fe3C39C40C3660.1(7)
Fe2C16C17C18-59.7(7) Fe4C46C47C48-59.2(6)
Fe2C16C17C28118.5(10) Fe4C46C47C58120.6(9)
Fe2C16C20C1958.4(7) Fe4C46C50C4958.7(7)
Fe2C17C18C19-59.4(7) Fe4C47C48C49-59.4(6)
Fe2C17C28N2-178.3(6) Fe4C47C58N4178.0(6)
Fe2C18C19C20-59.8(7) Fe4C48C49C50-59.4(6)
Fe2C19C20C16-58.1(7) Fe4C49C50C46-58.7(6)
Fe2C21C22C2359.1(7) Fe4C51C52C5359.0(6)
Fe2C21C25C24-58.7(7) Fe4C51C55C54-60.0(7)
Fe2C22C23C2460.3(7) Fe4C52C53C5459.3(7)
Fe2C23C24C2560.2(7) Fe4C53C54C5559.2(7)
Fe2C24C25C2159.4(7) Fe4C54C55C5160.3(7)
Si1C1C2Fe1-126.0(7) Si3C31C32Fe3-127.1(8)
Si1C1C2C3175.1(7) Si3C31C32C33173.4(7)
Si1C1C2C13-4.5(14) Si3C31C32C43-6.5(14)
Si1C1C5Fe1126.2(7) Si3C31C35Fe3127.6(8)
Si1C1C5C4-175.7(6) Si3C31C35C34-172.8(7)
Si2C16C17Fe2-128.2(8) Si4C46C47Fe4-126.5(8)
Si2C16C17C18172.1(7) Si4C46C47C48174.3(7)
Si2C16C17C28-9.7(15) Si4C46C47C58-5.9(14)
Si2C16C20Fe2128.7(7) Si4C46C50Fe4126.4(7)
Si2C16C20C19-172.9(7) Si4C46C50C49-174.9(7)
O1Si1C1Fe1-113.1(6) O3Si3C31Fe3-135.1(6)
O1Si1C1C2-18.4(9) O3Si3C31C32-41.6(9)
O1Si1C1C5155.4(7) O3Si3C31C35130.6(8)
O2Si2C16Fe2-122.3(6) O4Si4C46Fe4-109.3(7)
O2Si2C16C17-27.1(10) O4Si4C46C47-13.8(9)
O2Si2C16C20143.5(8) O4Si4C46C50159.7(7)
C1Si1O1Zn1-43.3(5) C31Si3O3Zn3-15.6(5)
C1Si1O1Zn2173.5(5) C31Si3O3Zn4-159.1(6)
C1C2C3Fe159.8(6) C31C32C33Fe360.0(7)
C1C2C3C40.1(10) C31C32C33C34-0.5(11)
C1C2C13N186.8(11) C31C32C43N389.8(11)
C2C1C5Fe1-58.7(6) C32C31C35Fe3-58.9(6)
C2C1C5C4-0.6(10) C32C31C35C340.7(11)
C2C3C4Fe159.7(6) C32C33C34Fe359.8(7)
C2C3C4C5-0.4(10) C32C33C34C350.9(11)
C3C2C13N1-92.8(10) C33C32C43N3-90.1(11)
C3C4C5Fe159.4(6) C33C34C35Fe358.4(7)
C3C4C5C10.7(10) C33C34C35C31-1.0(12)
C5C1C2Fe159.2(6) C35C31C32Fe359.4(6)
C5C1C2C30.3(10) C35C31C32C33-0.1(11)
C5C1C2C13-179.3(8) C35C31C32C43180.0(9)
C6C7C8Fe1-59.2(7) C36C37C38Fe3-60.4(7)
C6C7C8C90.4(11) C36C37C38C39-0.9(12)
C7C6C10Fe159.1(7) C37C36C40Fe358.4(7)
C7C6C10C9-0.3(11) C37C36C40C39-1.9(12)
C7C8C9Fe1-60.0(7) C37C38C39Fe3-58.9(8)
C7C8C9C10-0.6(11) C37C38C39C40-0.3(12)
C8C9C10Fe1-59.4(7) C38C39C40Fe3-58.8(8)
C8C9C10C60.6(11) C38C39C40C361.3(12)
C10C6C7Fe1-58.9(7) C40C36C37Fe3-58.8(7)
C10C6C7C8-0.1(11) C40C36C37C381.7(12)
C11Si1O1Zn172.3(5) C41Si3O3Zn3100.9(5)
C11Si1O1Zn2-70.9(6) C41Si3O3Zn4-42.6(7)
C11Si1C1Fe1128.4(6) C41Si3C31Fe3105.8(7)
C11Si1C1C2-137.0(8) C41Si3C31C32-160.7(8)
C11Si1C1C536.9(9) C41Si3C31C3511.5(10)
C12Si1O1Zn1-167.0(4) C42Si3O3Zn3-138.6(5)
C12Si1O1Zn249.8(6) C42Si3O3Zn477.9(7)
C12Si1C1Fe17.0(8) C42Si3C31Fe3-14.6(8)
C12Si1C1C2101.6(8) C42Si3C31C3279.0(9)
C12Si1C1C5-84.5(8) C42Si3C31C35-108.8(9)
C13C2C3Fe1-120.5(8) C43C32C33Fe3-120.1(9)
C13C2C3C4179.7(8) C43C32C33C34179.4(9)
C14N1C13C257.3(10) C44N3C43C3275.5(9)
C15N1C13C2175.6(8) C45N3C43C32-166.1(8)
C16Si2O2Zn1-173.0(5) C46Si4O4Zn3169.3(5)
C16Si2O2Zn2-30.7(5) C46Si4O4Zn4-47.3(5)
C16C17C18Fe259.9(7) C46C47C48Fe459.7(6)
C16C17C18C190.4(12) C46C47C48C490.3(10)
C16C17C28N291.9(12) C46C47C58N485.5(11)
C17C16C20Fe2-59.1(7) C47C46C50Fe4-58.8(6)
C17C16C20C19-0.7(11) C47C46C50C490.0(10)
C17C18C19Fe258.9(7) C47C48C49Fe459.0(6)
C17C18C19C20-0.9(11) C47C48C49C50-0.3(10)
C18C17C28N2-90.2(11) C48C47C58N4-94.8(10)
C18C19C20Fe259.1(7) C48C49C50Fe459.0(6)
C18C19C20C161.0(11) C48C49C50C460.2(11)
C20C16C17Fe259.9(7) C50C46C47Fe459.0(6)
C20C16C17C180.2(11) C50C46C47C48-0.2(10)
C20C16C17C28178.4(9) C50C46C47C58179.6(8)
C21C22C23Fe2-59.6(7) C51C52C53Fe4-59.2(6)
C21C22C23C240.7(12) C51C52C53C540.0(11)
C22C21C25Fe259.3(7) C52C51C55Fe459.0(7)
C22C21C25C240.6(12) C52C51C55C54-0.9(11)
C22C23C24Fe2-60.5(7) C52C53C54Fe4-59.8(7)
C22C23C24C25-0.3(12) C52C53C54C55-0.6(11)
C23C24C25Fe2-59.6(7) C53C54C55Fe4-59.4(7)
C23C24C25C21-0.2(12) C53C54C55C510.9(11)
C25C21C22Fe2-59.9(7) C55C51C52Fe4-58.4(7)
C25C21C22C23-0.8(12) C55C51C52C530.6(11)
C26Si2O2Zn1-57.1(7) C56Si4O4Zn345.8(6)
C26Si2O2Zn285.2(5) C56Si4O4Zn4-170.8(4)
C26Si2C16Fe2118.9(7) C56Si4C46Fe410.6(9)
C26Si2C16C17-145.9(9) C56Si4C46C47106.1(9)
C26Si2C16C2024.7(10) C56Si4C46C50-80.3(9)
C27Si2O2Zn163.2(7) C57Si4O4Zn3-74.8(6)
C27Si2O2Zn2-154.5(4) C57Si4O4Zn468.6(5)
C27Si2C16Fe2-1.6(9) C57Si4C46Fe4131.5(7)
C27Si2C16C1793.6(9) C57Si4C46C47-133.0(9)
C27Si2C16C20-95.8(9) C57Si4C46C5040.5(9)
C28C17C18Fe2-118.4(10) C58C47C48Fe4-120.1(8)
C28C17C18C19-177.9(9) C58C47C48C49-179.5(8)
C29N2C28C1767.0(10) C59N4C58C4755.8(10)
C30N2C28C17-174.2(8) C60N4C58C47173.9(8)

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for mo_B0280_0m_4.
AtomxyzU(eq)
H3865354931003130
H4769640861059633
H572262385991931
H698371421933539
H7105283402969641
H81005938041072439
H9909320621100744
H1089496131014446
H11A62662534866342
H11B64961226894442
H11C64281379824942
H12A8147208827842
H12B8334315896842
H12C8955947852142
H13A92174214860929
H13B94465323904329
H14A78307330855643
H14B85317109906443
H14C76686351906243
H15A93215700781446
H15B94936781827746
H15C87396900779846
H1892752260537637
H1980642899468839
H2071954468521934
H2187997172538038
H22100556138587943
H23105884512518848
H2496694595426052
H2585686259439149
H26A62414423633054
H26B63085735602054
H26C61635654670754
H27A77177319687057
H27B78277295617857
H27C85926896660957
H28A99823261634336
H28B94494250669036
H29A9155606696255
H29B98591108654055
H29C88871152633455
H30A97263373763546
H30B103892563729346
H30C97321910770646
H3341371368546537
H3428381883484339
H3522023790524738
H3648945690549849
H3755923718518049
H3848022952426851
H3936044414404551
H4036316087481951
H41A14124782628758
H41B17295814584858
H41C16066142652158
H42A33787076663154
H42B35296755596054
H42C41536223646254
H43A50492600629634
H43B46403810656434
H44A4241427720454
H44B4941715673754
H44C3969671653454
H45A48253424757350
H45B54622386736550
H45C47512052781750
H4836795600998231
H49275541861057936
H5022782440992332
H5148361464929340
H5255463490957739
H53516639651061741
H54423222631098041
H5540097341015144
H56A3030170833044
H56B3320394899844
H56C3887889848444
H57A12622681865045
H57B14531371894245
H57C13881501824645
H58A42274289857130
H58B44325428899430
H59A27437299848343
H59B34487151899443
H59C26176322899543
H60A43245776777547
H60B44566863824047
H60C37216953774647
H61A83034389225986
H61B84492988207686
H61C87444076165986
H63A94232442295877
H63B91903754322477
H63C101533398313377
H64A44872287279557
H64B42653531312957
H64C51983308291157
H66A31654388232270
H66B32102964215270
H66C33733992166970

Experimental

Single crystals of C33H50Br2Fe2N2O3Si2Zn2 [mo_B0280_0m_4] were []. A suitable crystal was selected and [] on a Bruker SMART APEX2 area detector diffractometer. The crystal was kept at 99.98 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_B0280_0m_4]

Crystal Data for C33H50Br2Fe2N2O3Si2Zn2 (=981.19 g/mol): monoclinic, space group P21 (no. 4), a = 15.9023(13) Å, b = 10.8845(9) Å, c = 22.8822(19) Å, β = 91.977(3)°, = 3958.3(6) Å3, Z = 4, T = 99.98 K, μ(MoKα) = 4.029 mm-1, Dcalc = 1.646 g/cm3, 24737 reflections measured (4.144° ≤ 2Θ ≤ 55.996°), 24737 unique (Rint = ?, Rsigma = 0.0434) which were used in all calculations. The final R1 was 0.0433 (I > 2σ(I)) and wR2 was 0.1062 (all data).

Refinement model description

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

Details:

1. Twinned data refinement
Scales: 0.7753(6) 0.2247(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), C28(H28A,H28B), C43(H43A,H43B), C58(H58A,H58B)
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), C63(H63A,H63B,H63C), C64(H64A,
H64B,H64C), C66(H66A,H66B,H66C)

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.