mo_B0200_0m

Table 1 Crystal data and structure refinement for mo_B0200_0m.
Identification code mo_B0200_0m
Empirical formula C50H52Cl2Fe2N2O2Si2Zn2
Formula weight 1082.45
Temperature/K 100.01
Crystal system triclinic
Space group P-1
a/Å 9.814(4)
b/Å 11.567(4)
c/Å 12.187(4)
α/° 94.998(12)
β/° 110.814(11)
γ/° 111.671(12)
Volume/Å3 1163.1(7)
Z 1
ρcalcg/cm3 1.545
μ/mm‑1 1.839
F(000) 556.0
Crystal size/mm3 0.196 × 0.105 × 0.104
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.792 to 53.998
Index ranges -12 ≤ h ≤ 12, -14 ≤ k ≤ 14, -15 ≤ l ≤ 15
Reflections collected 17366
Independent reflections 5048 [Rint = 0.0557, Rsigma = 0.0591]
Data/restraints/parameters 5048/0/282
Goodness-of-fit on F2 1.041
Final R indexes [I>=2σ (I)] R1 = 0.0396, wR2 = 0.0728
Final R indexes [all data] R1 = 0.0639, wR2 = 0.0799
Largest diff. peak/hole / e Å-3 0.51/-0.54

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for mo_B0200_0m. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Zn13503.1(4)-104.0(4)5014.3(3)14.0(1)
Fe14411.7(5)4020.8(4)7533.7(4)14.97(11)
Cl12157.9(10)-1244.2(8)5942.6(8)23.58(19)
Si16547.3(10)2172.9(8)7182.0(8)13.17(18)
O15840(2)1069(2)5953.8(19)14.1(4)
N12644(3)1091(2)4143(2)14.8(5)
C14777(3)2395(3)7237(3)14.5(6)
C23444(4)2391(3)6209(3)15.2(6)
C32260(4)2449(3)6604(3)18.8(7)
C42843(4)2501(3)7861(3)19.5(7)
C54374(4)2479(3)8241(3)16.0(7)
C66240(4)5589(3)7491(3)24.2(8)
C74720(4)5507(3)6723(3)23.9(8)
C83880(4)5568(3)7440(3)25.9(8)
C94865(5)5674(3)8641(3)30.4(9)
C106323(4)5687(3)8678(3)28.3(8)
C113395(4)2401(3)4975(3)15.6(7)
C123011(4)1243(3)3069(3)20.1(7)
C13867(4)546(3)3730(3)22.7(7)
C148138(3)3697(3)7180(3)14.9(6)
C158138(4)4000(3)6088(3)19.1(7)
C169182(4)5205(3)6093(3)23.2(8)
C1710281(4)6113(3)7175(3)26.5(8)
C1810336(4)5823(3)8264(3)23.9(8)
C199261(4)4630(3)8256(3)19.8(7)
C207398(4)1599(3)8546(3)17.1(7)
C219058(4)1945(3)9164(3)24.7(8)
C229638(5)1412(4)10086(3)33.1(9)
C238576(5)523(4)10425(3)38.4(10)
C246930(5)146(4)9828(3)33.9(9)
C256358(4)686(3)8896(3)23.3(8)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for mo_B0200_0m. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Zn111.98(18)15.2(2)13.6(2)1.65(16)4.92(15)5.52(16)
Fe113.7(2)14.5(3)15.8(3)0.7(2)5.9(2)6.1(2)
Cl124.1(4)24.9(5)28.4(5)10.5(4)17.5(4)10.4(4)
Si111.1(4)14.2(5)11.8(5)0.3(4)3.6(4)4.6(4)
O111.5(10)15.4(12)15.0(12)1.4(10)5.0(9)6.5(10)
N113.1(12)14.2(14)15.1(14)1.7(12)5.7(11)4.5(12)
C114.0(15)12.0(16)14.9(17)0.9(14)5.7(13)3.8(14)
C214.1(15)14.1(17)15.4(17)1.0(14)4.6(13)6.2(14)
C313.0(15)18.9(18)22.5(19)-0.4(15)7.4(14)6.1(14)
C417.7(16)16.8(18)26(2)1.6(15)13.5(15)5.7(15)
C514.6(15)16.1(17)14.6(17)1.4(14)5.7(13)4.7(14)
C621.3(17)13.1(18)38(2)7.2(17)15.2(17)4.9(16)
C728.3(19)15.8(18)26(2)5.0(16)9.7(16)9.1(16)
C826.0(18)18.9(19)36(2)3.4(17)12.3(17)14.7(16)
C942(2)20(2)29(2)-2.6(17)20.3(19)9.7(18)
C1022.2(18)14.4(19)30(2)-0.9(16)-1.7(16)2.0(16)
C1113.8(15)12.6(17)17.3(18)1.4(14)4.1(14)5.1(14)
C1224.1(17)19.2(18)17.4(18)4.0(15)8.8(15)9.6(16)
C1313.5(15)27(2)20.1(19)1.8(16)2.0(14)6.7(15)
C1412.4(14)14.7(17)18.0(18)-0.2(14)6.4(13)7.1(14)
C1515.9(15)21.2(19)19.4(19)0.8(15)6.6(14)8.7(15)
C1624.8(18)26(2)28(2)11.6(17)18.1(17)12.9(17)
C1722.3(18)18.1(19)44(2)8.9(18)20.6(18)7.4(16)
C1819.1(17)19.2(19)27(2)0.4(16)7.8(16)3.8(16)
C1917.4(16)22.3(19)17.6(18)2.2(15)6.7(15)7.5(15)
C2018.7(16)19.2(18)12.6(17)-0.5(14)3.8(14)10.9(15)
C2122.2(17)20.4(19)23(2)-3.0(16)0.7(15)11.1(16)
C2234(2)29(2)25(2)-1.9(18)-4.8(17)18.9(19)
C2361(3)45(3)15(2)9.6(19)7(2)39(2)
C2453(3)40(2)32(2)20(2)28(2)32(2)
C2529.4(18)30(2)21.0(19)9.8(17)14.2(16)19.8(18)

 

Table 4 Bond Lengths for mo_B0200_0m.
AtomAtomLength/Å AtomAtomLength/Å
Zn1Zn112.8711(13) C1C21.453(4)
Zn1Cl12.1903(10) C1C51.420(4)
Zn1O11.994(2) C2C31.427(4)
Zn1O111.974(2) C2C111.489(4)
Zn1N12.057(2) C3C41.418(5)
Fe1C12.066(3) C4C51.417(4)
Fe1C22.030(3) C6C71.413(5)
Fe1C32.038(3) C6C101.411(5)
Fe1C42.044(3) C7C81.411(4)
Fe1C52.041(3) C8C91.403(5)
Fe1C62.047(3) C9C101.409(5)
Fe1C72.036(3) C14C151.405(4)
Fe1C82.042(3) C14C191.395(4)
Fe1C92.042(3) C15C161.391(5)
Fe1C102.044(4) C16C171.385(5)
Si1O11.620(2) C17C181.384(5)
Si1C11.870(3) C18C191.391(5)
Si1C141.875(3) C20C211.406(4)
Si1C201.875(3) C20C251.390(5)
O1Zn111.974(2) C21C221.376(5)
N1C111.497(4) C22C231.380(6)
N1C121.484(4) C23C241.384(5)
N1C131.483(4) C24C251.387(5)

11-X,-Y,1-Z

 

Table 5 Bond Angles for mo_B0200_0m.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
Cl1Zn1Zn11128.47(3) Si1O1Zn11142.46(12)
O11Zn1Zn1143.93(6) Si1O1Zn1123.91(11)
O1Zn1Zn1143.38(6) C11N1Zn1110.78(18)
O11Zn1Cl1114.34(7) C12N1Zn1111.43(17)
O1Zn1Cl1119.20(7) C12N1C11107.7(2)
O11Zn1O187.31(9) C13N1Zn1109.55(19)
O1Zn1N1101.60(10) C13N1C11109.0(2)
O11Zn1N1112.95(9) C13N1C12108.4(2)
N1Zn1Zn11114.07(7) Si1C1Fe1131.96(16)
N1Zn1Cl1117.29(7) C2C1Fe167.90(16)
C2Fe1C141.55(12) C2C1Si1125.9(2)
C2Fe1C341.08(11) C5C1Fe168.85(17)
C2Fe1C468.59(13) C5C1Si1127.9(2)
C2Fe1C568.56(13) C5C1C2105.9(2)
C2Fe1C6117.15(13) C1C2Fe170.55(18)
C2Fe1C7106.87(14) C1C2C11124.7(2)
C2Fe1C8127.69(14) C3C2Fe169.77(18)
C2Fe1C9166.14(13) C3C2C1108.6(3)
C2Fe1C10151.24(13) C3C2C11126.6(3)
C3Fe1C169.49(12) C11C2Fe1122.9(2)
C3Fe1C440.67(13) C2C3Fe169.16(18)
C3Fe1C568.57(13) C4C3Fe169.88(19)
C3Fe1C6148.42(14) C4C3C2107.5(3)
C3Fe1C8105.52(14) C3C4Fe169.45(18)
C3Fe1C9127.97(13) C5C4Fe169.61(18)
C3Fe1C10167.60(13) C5C4C3108.3(3)
C4Fe1C168.68(12) C1C5Fe170.71(17)
C4Fe1C6170.64(14) C4C5Fe169.80(18)
C4Fe1C10131.38(15) C4C5C1109.6(3)
C5Fe1C140.44(11) C7C6Fe169.35(19)
C5Fe1C440.59(11) C10C6Fe169.72(19)
C5Fe1C6132.71(12) C10C6C7107.7(3)
C5Fe1C8149.28(13) C6C7Fe170.16(19)
C5Fe1C9118.60(14) C8C7Fe169.97(19)
C5Fe1C10111.47(14) C8C7C6108.0(3)
C6Fe1C1110.17(12) C7C8Fe169.54(18)
C7Fe1C1130.42(12) C9C8Fe169.90(19)
C7Fe1C3114.28(14) C9C8C7108.1(3)
C7Fe1C4147.28(13) C8C9Fe169.9(2)
C7Fe1C5170.04(12) C8C9C10108.2(3)
C7Fe1C640.50(13) C10C9Fe169.9(2)
C7Fe1C840.49(13) C6C10Fe169.9(2)
C7Fe1C967.90(15) C9C10Fe169.7(2)
C7Fe1C1067.96(15) C9C10C6108.1(3)
C8Fe1C1167.91(13) C2C11N1114.1(3)
C8Fe1C4115.21(13) C15C14Si1121.1(2)
C8Fe1C667.95(13) C19C14Si1121.1(2)
C8Fe1C1067.76(14) C19C14C15117.5(3)
C9Fe1C1151.32(14) C16C15C14120.6(3)
C9Fe1C4108.39(14) C17C16C15120.6(3)
C9Fe1C667.87(14) C18C17C16119.8(3)
C9Fe1C840.19(14) C17C18C19119.5(3)
C9Fe1C1040.34(14) C18C19C14122.0(3)
C10Fe1C1119.14(13) C21C20Si1122.7(3)
C10Fe1C640.36(14) C25C20Si1119.6(2)
O1Si1C1106.13(13) C25C20C21117.3(3)
O1Si1C14110.90(13) C22C21C20121.6(3)
O1Si1C20110.10(13) C21C22C23119.6(3)
C1Si1C14112.20(13) C22C23C24120.5(3)
C1Si1C20107.28(13) C23C24C25119.4(4)
C20Si1C14110.11(15) C24C25C20121.6(3)
Zn11O1Zn192.69(9)     

11-X,-Y,1-Z

 

Table 6 Torsion Angles for mo_B0200_0m.
ABCDAngle/˚ ABCDAngle/˚
Zn1N1C11C2-45.3(3) C3C4C5C1-0.8(4)
Fe1C1C2C3-59.6(2) C5C1C2Fe158.6(2)
Fe1C1C2C11117.2(3) C5C1C2C3-1.0(4)
Fe1C1C5C459.1(2) C5C1C2C11175.8(3)
Fe1C2C3C4-59.6(2) C6C7C8Fe1-60.1(2)
Fe1C2C11N1179.36(18) C6C7C8C9-0.6(4)
Fe1C3C4C5-59.0(2) C7C6C10Fe159.2(2)
Fe1C4C5C1-59.7(2) C7C6C10C9-0.4(4)
Fe1C6C7C860.0(2) C7C8C9Fe1-59.3(2)
Fe1C6C10C9-59.5(2) C7C8C9C100.4(4)
Fe1C7C8C959.5(2) C8C9C10Fe1-59.7(3)
Fe1C8C9C1059.7(2) C8C9C10C60.0(4)
Fe1C9C10C659.6(2) C10C6C7Fe1-59.4(2)
Si1C1C2Fe1-126.7(2) C10C6C7C80.6(4)
Si1C1C2C3173.7(2) C11C2C3Fe1-116.6(3)
Si1C1C2C11-9.5(5) C11C2C3C4-176.2(3)
Si1C1C5Fe1127.4(3) C12N1C11C2-167.4(2)
Si1C1C5C4-173.5(2) C13N1C11C275.3(3)
Si1C14C15C16171.1(2) C14Si1O1Zn1-137.63(14)
Si1C14C19C18-172.9(2) C14Si1O1Zn1157.0(2)
Si1C20C21C22-173.4(3) C14Si1C1Fe1-9.9(3)
Si1C20C25C24173.9(3) C14Si1C1C281.6(3)
O1Si1C1Fe1-131.2(2) C14Si1C1C5-104.8(3)
O1Si1C1C2-39.6(3) C14Si1C20C21-23.3(3)
O1Si1C1C5133.9(3) C14Si1C20C25163.9(2)
O1Si1C14C1527.0(3) C14C15C16C172.4(4)
O1Si1C14C19-159.7(2) C15C14C19C180.7(4)
O1Si1C20C2199.3(3) C15C16C17C18-0.4(4)
O1Si1C20C25-73.6(3) C16C17C18C19-1.3(5)
C1Si1O1Zn1-15.53(18) C17C18C19C141.1(4)
C1Si1O1Zn11179.13(19) C19C14C15C16-2.5(4)
C1Si1C14C15-91.5(2) C20Si1O1Zn11-65.1(2)
C1Si1C14C1981.8(3) C20Si1O1Zn1100.26(15)
C1Si1C20C21-145.7(3) C20Si1C1Fe1111.2(2)
C1Si1C20C2541.5(3) C20Si1C1C2-157.3(3)
C1C2C3Fe160.1(2) C20Si1C1C516.3(3)
C1C2C3C40.5(4) C20Si1C14C15149.1(2)
C1C2C11N191.3(4) C20Si1C14C19-37.6(3)
C2C1C5Fe1-58.0(2) C20C21C22C23-0.5(5)
C2C1C5C41.1(4) C21C20C25C240.7(5)
C2C3C4Fe159.1(2) C21C22C23C241.3(6)
C2C3C4C50.2(4) C22C23C24C25-1.0(6)
C3C2C11N1-92.5(4) C23C24C25C200.0(5)
C3C4C5Fe158.9(2) C25C20C21C22-0.4(5)

11-X,-Y,1-Z

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for mo_B0200_0m.
AtomxyzU(eq)
H312622453611423
H423012544836123
H550302515904619
H670585580725229
H743325425587329
H828315542715831
H945965727931437
H1072065751937934
H11A45112863505219
H11B27822885460319
H12A2450410247330
H12B41781559332030
H12C26491858270530
H13A606504443534
H13B368-320320134
H13C4531095328034
H1574183375534123
H1691415408534628
H17109956932717132
H18111026435901029
H1992934443900624
H2197972563894030
H221076516551048840
H2389761661107246
H246200-4771005441
H255229425848828

Experimental

Single crystals of C50H52Cl2Fe2N2O2Si2Zn2 [mo_B0200_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_B0200_0m]

Crystal Data for C50H52Cl2Fe2N2O2Si2Zn2 (=1082.45 g/mol): triclinic, space group P-1 (no. 2), a = 9.814(4) Å, b = 11.567(4) Å, c = 12.187(4) Å, α = 94.998(12)°, β = 110.814(11)°, γ = 111.671(12)°, = 1163.1(7) Å3, Z = 1, T = 100.01 K, μ(MoKα) = 1.839 mm-1, Dcalc = 1.545 g/cm3, 17366 reflections measured (4.792° ≤ 2Θ ≤ 53.998°), 5048 unique (Rint = 0.0557, Rsigma = 0.0591) which were used in all calculations. The final R1 was 0.0396 (I > 2σ(I)) and wR2 was 0.0799 (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)

This report has been created with Olex2, compiled on 2017.01.04 svn.r3372 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.