mo_B0201_0m

Table 1 Crystal data and structure refinement for mo_B0201_0m.
Identification code mo_B0201_0m
Empirical formula C50H52Br2Fe2N2O2Si2Zn2
Formula weight 1171.37
Temperature/K 100.0
Crystal system triclinic
Space group P-1
a/Å 9.9882(18)
b/Å 11.630(2)
c/Å 12.246(2)
α/° 95.148(7)
β/° 111.187(6)
γ/° 111.106(7)
Volume/Å3 1197.2(4)
Z 1
ρcalcg/cm3 1.625
μ/mm‑1 3.344
F(000) 592.0
Crystal size/mm3 0.198 × 0.105 × 0.099
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 5.316 to 51.998
Index ranges -12 ≤ h ≤ 12, -14 ≤ k ≤ 14, -15 ≤ l ≤ 14
Reflections collected 21139
Independent reflections 4681 [Rint = 0.0439, Rsigma = 0.0335]
Data/restraints/parameters 4681/0/282
Goodness-of-fit on F2 1.076
Final R indexes [I>=2σ (I)] R1 = 0.0513, wR2 = 0.1434
Final R indexes [all data] R1 = 0.0613, wR2 = 0.1508
Largest diff. peak/hole / e Å-3 1.93/-0.72

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for mo_B0201_0m. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Br12217.1(6)-1252.3(5)6058.7(5)30.82(18)
Zn13537.7(6)-91.2(5)5020.5(5)20.91(17)
Fe14415.3(9)4024.7(7)7535.9(7)24.2(2)
Si16530.4(16)2167.5(13)7190.2(12)21.6(3)
O15842(4)1070(3)5960(3)21.5(7)
N12644(5)1098(4)4130(4)21.2(8)
C14772(6)2389(5)7236(5)23.1(10)
C23477(6)2399(5)6218(5)23.9(10)
C32309(6)2463(5)6613(5)26.4(11)
C42892(6)2526(5)7868(5)28.3(11)
C54393(6)2488(5)8246(5)25.2(10)
C66208(7)5580(5)7495(6)34.9(13)
C74708(7)5508(5)6734(6)34.7(13)
C83873(7)5572(5)7433(6)36.2(13)
C94869(8)5679(5)8647(6)39.8(14)
C106303(7)5680(5)8690(6)37.6(14)
C113395(6)2394(5)4968(5)24.6(10)
C122997(6)1230(5)3060(5)26.9(11)
C13934(6)560(6)3744(5)32.4(12)
C148086(6)3677(5)7182(5)24.6(10)
C159184(7)4594(5)8269(5)29.3(11)
C1610261(7)5771(5)8273(6)33.7(12)
C1710227(7)6054(6)7199(6)34.8(13)
C189117(7)5155(6)6103(6)33.4(12)
C198077(6)3975(5)6098(5)27.3(11)
C207414(7)1618(5)8556(5)27.9(11)
C219049(7)1948(5)9145(5)34.1(13)
C229655(8)1429(6)10082(6)44.8(16)
C238650(9)575(7)10459(6)49.1(18)
C247040(9)220(7)9902(6)45.3(16)
C256422(7)731(6)8951(5)32.7(12)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for mo_B0201_0m. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Br131.4(3)31.6(3)36.9(3)12.4(2)21.3(2)13.6(2)
Zn118.9(3)21.4(3)20.6(3)2.8(2)7.7(2)8.0(2)
Fe125.4(4)22.8(4)23.8(4)2.8(3)10.2(3)10.5(3)
Si120.6(6)22.6(7)18.8(7)3.0(5)6.6(5)8.3(5)
O119.3(16)23.7(17)20.6(17)2.3(13)8.5(13)8.9(14)
N122(2)20(2)17(2)0.5(16)6.4(16)6.7(16)
C129(3)18(2)21(2)3.5(19)11(2)8(2)
C223(2)18(2)25(3)-1.7(19)7(2)6.2(19)
C320(2)21(2)30(3)-2(2)8(2)5(2)
C428(3)26(3)34(3)3(2)19(2)10(2)
C529(3)21(2)23(3)2(2)12(2)8(2)
C635(3)21(3)52(4)8(2)23(3)10(2)
C744(3)24(3)38(3)10(2)18(3)15(2)
C834(3)26(3)51(4)6(3)18(3)17(2)
C957(4)25(3)39(3)-1(2)25(3)17(3)
C1039(3)19(3)37(3)0(2)6(3)7(2)
C1124(2)21(2)26(3)5(2)9(2)9(2)
C1229(3)30(3)21(3)6(2)9(2)13(2)
C1324(3)40(3)31(3)9(2)7(2)15(2)
C1417(2)26(3)31(3)5(2)10(2)10(2)
C1533(3)25(3)28(3)3(2)13(2)11(2)
C1629(3)24(3)36(3)-2(2)9(2)6(2)
C1733(3)31(3)47(4)12(3)23(3)14(2)
C1837(3)37(3)35(3)13(2)21(3)17(3)
C1927(3)29(3)29(3)7(2)13(2)14(2)
C2034(3)24(3)21(3)1(2)6(2)14(2)
C2135(3)26(3)30(3)-1(2)5(2)11(2)
C2244(4)40(3)35(3)0(3)-4(3)25(3)
C2369(5)52(4)28(3)11(3)7(3)41(4)
C2467(5)51(4)43(4)25(3)33(3)39(4)
C2539(3)39(3)29(3)11(2)17(2)23(3)

 

Table 4 Bond Lengths for mo_B0201_0m.
AtomAtomLength/Å AtomAtomLength/Å
Br1Zn12.3275(8) C1C21.440(7)
Zn1Zn112.8709(12) C1C51.424(7)
Zn1O12.003(3) C2C31.437(7)
Zn1O111.980(3) C2C111.502(7)
Zn1N12.087(4) C3C41.417(8)
Fe1C12.082(5) C4C51.420(7)
Fe1C22.035(5) C6C71.417(9)
Fe1C32.040(5) C6C101.423(9)
Fe1C42.045(5) C7C81.408(9)
Fe1C52.053(5) C8C91.423(9)
Fe1C62.057(6) C9C101.414(9)
Fe1C72.043(6) C14C151.400(7)
Fe1C82.060(6) C14C191.400(8)
Fe1C92.053(6) C15C161.402(8)
Fe1C102.057(6) C16C171.375(9)
Si1O11.627(4) C17C181.401(9)
Si1C11.884(5) C18C191.389(8)
Si1C141.883(5) C20C211.408(8)
Si1C201.875(6) C20C251.407(8)
O1Zn111.980(3) C21C221.389(9)
N1C111.496(6) C22C231.381(11)
N1C121.483(7) C23C241.379(10)
N1C131.458(6) C24C251.399(9)

11-X,-Y,1-Z

 

Table 5 Bond Angles for mo_B0201_0m.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
Br1Zn1Zn11127.62(4) Si1O1Zn1123.42(19)
O1Zn1Br1117.58(10) Si1O1Zn11143.4(2)
O11Zn1Br1114.62(10) C11N1Zn1109.7(3)
O11Zn1Zn1144.20(10) C12N1Zn1110.7(3)
O1Zn1Zn1143.58(10) C12N1C11108.2(4)
O11Zn1O187.77(14) C13N1Zn1109.2(3)
O1Zn1N1102.26(15) C13N1C11109.5(4)
O11Zn1N1112.75(15) C13N1C12109.5(4)
N1Zn1Br1117.62(12) Si1C1Fe1131.4(3)
N1Zn1Zn11114.51(12) C2C1Fe167.8(3)
C2Fe1C140.9(2) C2C1Si1126.0(4)
C2Fe1C341.3(2) C5C1Fe168.7(3)
C2Fe1C468.8(2) C5C1Si1127.5(4)
C2Fe1C568.2(2) C5C1C2106.3(5)
C2Fe1C6117.1(2) C1C2Fe171.3(3)
C2Fe1C7107.5(2) C1C2C11125.6(5)
C2Fe1C8127.9(2) C3C2Fe169.5(3)
C2Fe1C9166.7(2) C3C2C1108.4(5)
C2Fe1C10150.9(2) C3C2C11125.9(5)
C3Fe1C169.0(2) C11C2Fe1123.2(4)
C3Fe1C440.6(2) C2C3Fe169.2(3)
C3Fe1C568.2(2) C4C3Fe169.9(3)
C3Fe1C6148.7(2) C4C3C2107.7(5)
C3Fe1C7114.9(2) C3C4Fe169.5(3)
C3Fe1C8105.6(2) C3C4C5108.0(5)
C3Fe1C9128.3(2) C5C4Fe170.0(3)
C3Fe1C10167.6(2) C1C5Fe171.0(3)
C4Fe1C168.5(2) C4C5Fe169.5(3)
C4Fe1C540.5(2) C4C5C1109.5(5)
C4Fe1C6170.4(3) C7C6Fe169.3(3)
C4Fe1C8115.2(2) C7C6C10107.4(5)
C4Fe1C9108.4(2) C10C6Fe169.8(3)
C4Fe1C10131.0(2) C6C7Fe170.3(3)
C5Fe1C140.3(2) C8C7Fe170.5(3)
C5Fe1C6132.6(2) C8C7C6109.2(6)
C5Fe1C8149.4(2) C7C8Fe169.3(3)
C5Fe1C9118.7(2) C7C8C9106.9(5)
C5Fe1C10111.2(2) C9C8Fe169.5(3)
C6Fe1C1110.4(2) C8C9Fe170.0(3)
C6Fe1C868.0(2) C10C9Fe170.0(3)
C6Fe1C1040.5(3) C10C9C8108.8(5)
C7Fe1C1130.9(2) C6C10Fe169.8(3)
C7Fe1C4147.4(2) C9C10Fe169.7(3)
C7Fe1C5170.2(2) C9C10C6107.6(5)
C7Fe1C640.4(2) N1C11C2114.8(4)
C7Fe1C840.1(2) C15C14Si1120.1(4)
C7Fe1C967.5(3) C19C14Si1121.4(4)
C7Fe1C1067.9(3) C19C14C15118.2(5)
C8Fe1C1167.6(2) C14C15C16120.9(5)
C9Fe1C1151.4(2) C17C16C15120.2(5)
C9Fe1C667.7(3) C16C17C18119.5(5)
C9Fe1C840.5(3) C19C18C17120.4(5)
C9Fe1C1040.2(3) C18C19C14120.7(5)
C10Fe1C1119.2(2) C21C20Si1122.6(4)
C10Fe1C868.2(2) C25C20Si1120.0(4)
O1Si1C1106.1(2) C25C20C21117.0(5)
O1Si1C14110.4(2) C22C21C20121.4(6)
O1Si1C20110.4(2) C23C22C21120.1(6)
C14Si1C1112.5(2) C24C23C22120.3(6)
C20Si1C1108.1(2) C23C24C25119.8(6)
C20Si1C14109.3(2) C24C25C20121.3(6)
Zn11O1Zn192.23(14)     

11-X,-Y,1-Z

 

Table 6 Torsion Angles for mo_B0201_0m.
ABCDAngle/˚ ABCDAngle/˚
Zn1N1C11C2-45.5(5) C3C4C5C1-0.5(6)
Fe1C1C2C3-59.9(3) C5C1C2Fe158.1(3)
Fe1C1C2C11117.9(5) C5C1C2C3-1.8(5)
Fe1C1C5C458.9(4) C5C1C2C11176.0(5)
Fe1C2C3C4-59.5(4) C6C7C8Fe1-59.9(4)
Fe1C2C11N1-179.3(3) C6C7C8C9-0.3(6)
Fe1C3C4C5-59.6(4) C7C6C10Fe159.3(4)
Fe1C4C5C1-59.9(4) C7C6C10C9-0.5(6)
Fe1C6C7C860.0(4) C7C8C9Fe1-59.5(4)
Fe1C6C10C9-59.7(4) C7C8C9C100.0(6)
Fe1C7C8C959.6(4) C8C9C10Fe1-59.4(4)
Fe1C8C9C1059.4(4) C8C9C10C60.3(6)
Fe1C9C10C659.7(4) C10C6C7Fe1-59.6(4)
Si1C1C2Fe1-125.9(4) C10C6C7C80.5(6)
Si1C1C2C3174.2(4) C11C2C3Fe1-116.8(5)
Si1C1C2C11-8.0(7) C11C2C3C4-176.3(5)
Si1C1C5Fe1126.6(4) C12N1C11C2-166.4(4)
Si1C1C5C4-174.5(4) C13N1C11C274.4(5)
Si1C14C15C16-174.4(4) C14Si1O1Zn1-137.7(2)
Si1C14C19C18172.5(4) C14Si1O1Zn1157.2(4)
Si1C20C21C22-173.7(5) C14Si1C1Fe1-10.5(4)
Si1C20C25C24174.4(5) C14Si1C1C280.5(5)
O1Si1C1Fe1-131.3(3) C14Si1C1C5-104.4(5)
O1Si1C1C2-40.3(5) C14Si1C20C21-24.6(5)
O1Si1C1C5134.8(4) C14Si1C20C25162.6(4)
O1Si1C14C15-159.5(4) C14C15C16C171.6(8)
O1Si1C14C1927.2(5) C15C14C19C18-0.8(8)
O1Si1C20C2197.0(5) C15C16C17C18-0.5(9)
O1Si1C20C25-75.8(5) C16C17C18C19-1.2(8)
C1Si1O1Zn1-15.5(3) C17C18C19C141.9(8)
C1Si1O1Zn11179.3(3) C19C14C15C16-0.9(8)
C1Si1C14C1582.1(5) C20Si1O1Zn11-63.8(4)
C1Si1C14C19-91.1(4) C20Si1O1Zn1101.4(3)
C1Si1C20C21-147.4(4) C20Si1C1Fe1110.3(4)
C1Si1C20C2539.8(5) C20Si1C1C2-158.7(4)
C1C2C3Fe161.0(3) C20Si1C1C516.4(5)
C1C2C3C41.5(6) C20Si1C14C15-38.0(5)
C1C2C11N190.8(6) C20Si1C14C19148.8(4)
C2C1C5Fe1-57.5(3) C20C21C22C23-0.3(9)
C2C1C5C41.4(6) C21C20C25C241.2(8)
C2C3C4Fe159.1(3) C21C22C23C240.7(10)
C2C3C4C5-0.6(6) C22C23C24C25-0.1(10)
C3C2C11N1-91.8(6) C23C24C25C20-0.8(10)
C3C4C5Fe159.3(4) C25C20C21C22-0.7(8)

11-X,-Y,1-Z

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for mo_B0201_0m.
AtomxyzU(eq)
H313242464612132
H423692584836934
H550452524904930
H670055563725242
H743265429588642
H828415549714843
H946125740931948
H1071725737938945
H11A27912881460530
H11B44832843503630
H12A2466397247940
H12B41441558331540
H12C26151824267840
H13A696405444149
H13B432-245312749
H13C5241160340449
H1591994417901535
H16110176374901940
H17109506854720142
H1890755353535940
H1973513363535033
H2197542537889641
H221076216631046454
H2390712301110659
H246352-3691016254
H255310474856439

Experimental

Single crystals of C50H52Br2Fe2N2O2Si2Zn2 [mo_B0201_0m] were []. A suitable crystal was selected and [] on a Bruker APEX-II CCD diffractometer. The crystal was kept at 100.0 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_B0201_0m]

Crystal Data for C50H52Br2Fe2N2O2Si2Zn2 (=1171.37 g/mol): triclinic, space group P-1 (no. 2), a = 9.9882(18) Å, b = 11.630(2) Å, c = 12.246(2) Å, α = 95.148(7)°, β = 111.187(6)°, γ = 111.106(7)°, = 1197.2(4) Å3, Z = 1, T = 100.0 K, μ(MoKα) = 3.344 mm-1, Dcalc = 1.625 g/cm3, 21139 reflections measured (5.316° ≤ 2Θ ≤ 51.998°), 4681 unique (Rint = 0.0439, Rsigma = 0.0335) which were used in all calculations. The final R1 was 0.0513 (I > 2σ(I)) and wR2 was 0.1508 (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:
C11(H11A,H11B)
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), C15(H15),
C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24),
C25(H25)
2.c Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)

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