mo_B0287_0m

Table 1 Crystal data and structure refinement for mo_B0287_0m.
Identification code mo_B0287_0m
Empirical formula C36H60Cl2Fe2N2O2Si4Zn2
Formula weight 978.56
Temperature/K 99.99
Crystal system monoclinic
Space group P21/n
a/Å 7.5997(14)
b/Å 18.201(2)
c/Å 16.394(2)
α/° 90
β/° 99.971(7)
γ/° 90
Volume/Å3 2233.4(6)
Z 2
ρcalcg/cm3 1.455
μ/mm‑1 1.957
F(000) 1016.0
Crystal size/mm3 0.272 × 0.108 × 0.081
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 5.046 to 55.982
Index ranges -10 ≤ h ≤ 8, -23 ≤ k ≤ 24, -21 ≤ l ≤ 21
Reflections collected 33184
Independent reflections 5365 [Rint = 0.0346, Rsigma = 0.0244]
Data/restraints/parameters 5365/0/233
Goodness-of-fit on F2 1.045
Final R indexes [I>=2σ (I)] R1 = 0.0241, wR2 = 0.0499
Final R indexes [all data] R1 = 0.0319, wR2 = 0.0521
Largest diff. peak/hole / e Å-3 0.42/-0.34

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for mo_B0287_0m. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Zn14475.1(2)4242.7(2)5082.8(2)13.08(5)
Fe16586.2(3)2640.5(2)2987.4(2)14.65(6)
Cl11907.8(5)3662.3(2)4940.0(2)21.28(9)
Si15847.2(6)4514.0(2)3398.0(3)14.17(9)
Si25430.0(7)1354.3(3)4411.8(3)22.52(11)
O15205.9(15)4868.2(6)4212.5(6)15.5(2)
N16603.0(17)3549.0(7)5515.3(8)13.4(3)
C15341(2)3509.6(9)3448.1(9)13.6(3)
C26034(2)2990.0(9)4094.0(9)13.1(3)
C35237(2)2276.4(9)3899.2(10)15.6(3)
C44032(2)2369.9(9)3125.9(10)16.7(3)
C54089(2)3108.0(9)2859.3(10)16.4(3)
C68303(3)3067.5(11)2266.6(12)28.2(4)
C79280(2)2752.1(11)2997.6(12)28.7(4)
C88811(2)1999.1(11)3011.9(11)26.6(4)
C97534(2)1848.6(10)2287.1(11)24.3(4)
C107222(2)2509.1(11)1828.9(11)25.0(4)
C114518(3)4885.4(10)2422.2(10)24.6(4)
C128250(2)4742(1)3417.2(11)20.4(4)
C137400(2)3204.4(9)4829.7(9)13.6(3)
C148032(2)3971.3(10)6048.4(10)21.0(4)
C155936(2)2969.5(10)6018.7(10)20.2(4)
C163394(3)1227.1(12)4902.4(14)38.1(5)
C177510(3)1217.4(11)5190.8(12)36.0(5)
C185406(3)630.8(10)3600.5(12)32.7(5)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for mo_B0287_0m. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Zn113.45(9)12.01(9)14.01(9)-0.64(7)3.02(7)-0.40(7)
Fe115.54(12)15.55(12)13.53(11)-3.44(9)4.40(8)0.02(9)
Cl114.32(19)25.2(2)24.1(2)-0.17(17)2.71(15)-4.47(17)
Si117.7(2)12.8(2)12.46(19)-0.05(16)3.94(16)-0.37(18)
Si232.7(3)14.1(2)19.9(2)0.63(18)2.0(2)-1.9(2)
O119.6(6)13.1(6)14.5(5)-1.5(4)4.9(4)-0.4(5)
N113.2(7)15.0(7)12.2(6)-1.7(5)2.5(5)-0.1(5)
C114.4(8)14.1(8)13.6(7)-1.7(6)5.7(6)0.8(6)
C214.1(8)12.8(8)13.1(7)-1.0(6)4.6(6)0.7(6)
C315.9(8)15.8(8)15.8(7)-2.3(6)4.8(6)-1.1(6)
C415.8(8)17.1(8)17.3(7)-4.5(6)3.2(6)-3.9(7)
C515.5(8)18.6(8)15.0(7)-1.2(6)2.5(6)1.2(7)
C631.7(11)29.1(10)29.9(10)-5.2(8)22.1(8)-3.9(8)
C716.5(9)41.4(12)30.5(10)-16.7(9)10.4(7)-4.1(8)
C822.0(9)33.9(11)24.6(9)-5.4(8)5.9(7)9.8(8)
C922.8(9)25.9(10)25.8(9)-11.1(7)8.8(7)1.8(8)
C1025.2(10)33.9(11)18.1(8)-6.4(7)9.9(7)3.0(8)
C1133.2(10)21.0(9)18.4(8)2.8(7)1.1(7)3.2(8)
C1222.7(9)17.2(8)22.7(8)0.2(7)7.9(7)-4.5(7)
C1313.3(8)14.1(8)14.1(7)-1.1(6)4.1(6)1.0(6)
C1417.0(8)24.6(9)19.5(8)-7.5(7)-2.3(6)1.0(7)
C1523.2(9)20.8(9)17.7(8)5.4(7)6.6(7)2.5(7)
C1650.1(14)27.3(11)40.5(12)5.9(9)17.8(10)-11.4(10)
C1750.1(13)21.3(10)31.1(10)1.1(8)-8.7(9)7.5(9)
C1850.1(13)16.2(9)29.5(10)-4.1(8)0.4(9)-1.9(9)

 

Table 4 Bond Lengths for mo_B0287_0m.
AtomAtomLength/Å AtomAtomLength/Å
Zn1Zn112.8956(5) Si2C31.8713(17)
Zn1Cl12.1952(5) Si2C161.878(2)
Zn1O11.9786(11) Si2C171.869(2)
Zn1O111.9787(11) Si2C181.8694(19)
Zn1N12.0773(13) O1Zn111.9787(11)
Fe1C12.0532(16) N1C131.5034(19)
Fe1C22.0337(15) N1C141.485(2)
Fe1C32.0631(16) N1C151.482(2)
Fe1C42.0532(17) C1C21.449(2)
Fe1C52.0569(17) C1C51.433(2)
Fe1C62.0585(18) C2C31.445(2)
Fe1C72.0541(18) C2C131.501(2)
Fe1C82.0492(18) C3C41.440(2)
Fe1C92.0495(17) C4C51.416(2)
Fe1C102.0533(17) C6C71.417(3)
Si1O11.6314(11) C6C101.421(3)
Si1C11.8728(17) C7C81.417(3)
Si1C111.8649(17) C8C91.425(3)
Si1C121.8678(18) C9C101.416(3)

11-X,1-Y,1-Z

 

Table 5 Bond Angles for mo_B0287_0m.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
Cl1Zn1Zn11134.617(16) C11Si1C1107.86(8)
O1Zn1Zn1142.97(3) C11Si1C12108.48(8)
O11Zn1Zn1142.97(3) C12Si1C1115.07(8)
O1Zn1Cl1123.73(3) C3Si2C16107.25(9)
O11Zn1Cl1118.20(4) C17Si2C3114.69(9)
O1Zn1O1185.94(5) C17Si2C16110.69(11)
O11Zn1N1106.76(5) C17Si2C18107.16(10)
O1Zn1N1107.26(5) C18Si2C3108.78(8)
N1Zn1Zn11113.57(4) C18Si2C16108.09(10)
N1Zn1Cl1111.65(4) Zn1O1Zn1194.06(5)
C1Fe1C370.27(6) Si1O1Zn11141.02(7)
C1Fe1C468.86(6) Si1O1Zn1121.58(6)
C1Fe1C540.81(6) C13N1Zn1112.90(9)
C1Fe1C6107.37(7) C14N1Zn1109.46(10)
C1Fe1C7116.28(7) C14N1C13107.90(12)
C1Fe1C10128.85(7) C15N1Zn1107.57(10)
C2Fe1C141.53(6) C15N1C13109.90(12)
C2Fe1C341.31(6) C15N1C14109.05(13)
C2Fe1C468.36(6) Si1C1Fe1128.67(8)
C2Fe1C568.43(6) C2C1Fe168.51(8)
C2Fe1C6130.03(7) C2C1Si1128.16(11)
C2Fe1C7108.73(7) C5C1Fe169.73(9)
C2Fe1C8117.24(7) C5C1Si1125.86(12)
C2Fe1C9150.06(7) C5C1C2105.91(13)
C2Fe1C10168.40(7) C1C2Fe169.96(8)
C4Fe1C340.95(6) C1C2C13122.06(14)
C4Fe1C540.30(7) C3C2Fe170.43(9)
C4Fe1C6149.27(7) C3C2C1109.87(13)
C4Fe1C7169.35(8) C3C2C13128.06(14)
C4Fe1C10116.94(7) C13C2Fe1125.26(11)
C5Fe1C368.99(6) Si2C3Fe1127.10(9)
C5Fe1C6116.77(8) C2C3Fe168.25(9)
C6Fe1C3168.90(7) C2C3Si2135.20(12)
C7Fe1C3130.20(7) C4C3Fe169.16(9)
C7Fe1C5149.34(8) C4C3Si2119.34(12)
C7Fe1C640.31(8) C4C3C2105.46(14)
C8Fe1C1149.64(7) C3C4Fe169.89(9)
C8Fe1C3108.34(7) C5C4Fe169.99(9)
C8Fe1C4130.83(8) C5C4C3109.58(14)
C8Fe1C5168.84(7) C1C5Fe169.46(9)
C8Fe1C667.88(8) C4C5Fe169.71(9)
C8Fe1C740.42(8) C4C5C1109.18(14)
C8Fe1C940.68(7) C7C6Fe169.68(11)
C8Fe1C1068.05(7) C7C6C10108.04(18)
C9Fe1C1167.67(7) C10C6Fe169.59(10)
C9Fe1C3116.55(7) C6C7Fe170.01(11)
C9Fe1C4108.90(7) C6C7C8108.02(17)
C9Fe1C5129.88(7) C8C7Fe169.61(10)
C9Fe1C667.96(8) C7C8Fe169.98(11)
C9Fe1C768.15(7) C7C8C9108.00(17)
C9Fe1C1040.37(8) C9C8Fe169.67(10)
C10Fe1C3149.21(7) C8C9Fe169.65(10)
C10Fe1C5108.33(7) C10C9Fe169.96(10)
C10Fe1C640.42(8) C10C9C8107.84(17)
C10Fe1C767.99(7) C6C10Fe169.98(10)
O1Si1C1104.90(6) C9C10Fe169.67(10)
O1Si1C11111.38(7) C9C10C6108.10(16)
O1Si1C12109.16(7) C2C13N1113.38(12)

11-X,1-Y,1-Z

 

Table 6 Torsion Angles for mo_B0287_0m.
ABCDAngle/˚ ABCDAngle/˚
Zn1N1C13C2-38.65(15) C5C1C2Fe160.05(10)
Fe1C1C2C3-59.28(11) C5C1C2C30.77(17)
Fe1C1C2C13119.77(14) C5C1C2C13179.82(14)
Fe1C1C5C458.51(11) C6C7C8Fe1-59.70(12)
Fe1C2C3Si2121.33(16) C6C7C8C9-0.2(2)
Fe1C2C3C4-59.49(11) C7C6C10Fe159.28(12)
Fe1C2C13N1171.16(10) C7C6C10C9-0.2(2)
Fe1C3C4C5-58.87(12) C7C8C9Fe1-59.72(12)
Fe1C4C5C1-58.36(11) C7C8C9C100.1(2)
Fe1C6C7C859.45(12) C8C9C10Fe1-59.58(12)
Fe1C6C10C9-59.47(12) C8C9C10C60.1(2)
Fe1C7C8C959.53(12) C10C6C7Fe1-59.22(12)
Fe1C8C9C1059.78(12) C10C6C7C80.2(2)
Fe1C9C10C659.66(12) C11Si1O1Zn11-81.61(12)
Si1C1C2Fe1-123.00(13) C11Si1O1Zn1125.29(9)
Si1C1C2C3177.72(12) C11Si1C1Fe189.07(12)
Si1C1C2C13-3.2(2) C11Si1C1C2-179.09(14)
Si1C1C5Fe1123.70(12) C11Si1C1C5-2.71(16)
Si1C1C5C4-177.79(12) C12Si1O1Zn1138.15(13)
Si2C3C4Fe1-121.77(11) C12Si1O1Zn1-114.96(8)
Si2C3C4C5179.36(11) C12Si1C1Fe1-32.15(13)
O1Si1C1Fe1-152.11(9) C12Si1C1C259.69(16)
O1Si1C1C2-60.27(15) C12Si1C1C5-123.92(14)
O1Si1C1C5116.11(14) C13C2C3Fe1-119.99(16)
C1Si1O1Zn18.86(9) C13C2C3Si21.3(3)
C1Si1O1Zn11161.97(10) C13C2C3C4-179.48(15)
C1C2C3Fe158.99(11) C14N1C13C2-159.75(13)
C1C2C3Si2-179.67(13) C15N1C13C281.44(16)
C1C2C3C4-0.49(17) C16Si2C3Fe1-161.18(11)
C1C2C13N184.17(18) C16Si2C3C2102.95(18)
C2C1C5Fe1-59.25(10) C16Si2C3C4-76.15(15)
C2C1C5C4-0.74(18) C17Si2C3Fe175.47(13)
C2C3C4Fe158.89(10) C17Si2C3C2-20.4(2)
C2C3C4C50.02(18) C17Si2C3C4160.50(13)
C3C2C13N1-96.96(18) C18Si2C3Fe1-44.49(13)
C3C4C5Fe158.81(11) C18Si2C3C2-140.37(17)
C3C4C5C10.46(19) C18Si2C3C440.54(16)

11-X,1-Y,1-Z

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for mo_B0287_0m.
AtomxyzU(eq)
H433081994283920
H534073306236820
H683613565209934
H7101043002340634
H892681655343132
H969881387213829
H1064292569131830
H11A32484782241037
H11B49084652194537
H11C46985418239937
H12A84735253359631
H12B85384679286131
H12C90014414380531
H13A82513555464916
H13B80822762504716
H14A84354372572632
H14B90403645624932
H14C75654176652132
H15A53933198645630
H15B69342656626930
H15C50412671566430
H16A33811601533257
H16B3419737515257
H16C23191277447957
H17A85501361494854
H17B7616699535354
H17C74561520568054
H18A4477745312549
H18B5157152382949
H18C6572616342349

Experimental

Single crystals of C36H60Cl2Fe2N2O2Si4Zn2 [mo_B0287_0m] were []. A suitable crystal was selected and [] on a Bruker APEX-II CCD 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 Intrinsic Phasing 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_B0287_0m]

Crystal Data for C36H60Cl2Fe2N2O2Si4Zn2 (=978.56 g/mol): monoclinic, space group P21/n (no. 14), a = 7.5997(14) Å, b = 18.201(2) Å, c = 16.394(2) Å, β = 99.971(7)°, = 2233.4(6) Å3, Z = 2, T = 99.99 K, μ(MoKα) = 1.957 mm-1, Dcalc = 1.455 g/cm3, 33184 reflections measured (5.046° ≤ 2Θ ≤ 55.982°), 5365 unique (Rint = 0.0346, Rsigma = 0.0244) which were used in all calculations. The final R1 was 0.0241 (I > 2σ(I)) and wR2 was 0.0521 (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)
2.b Aromatic/amide H refined with riding coordinates:
C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10)
2.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)

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.