3099

Table 1 Crystal data and structure refinement for 3099.
Identification code 3099
Empirical formula C38H56Br2Fe2N2O3Si2Zn
Formula weight 981.91
Temperature/K 173
Crystal system monoclinic
Space group C2/c
a/Å 12.5345(7)
b/Å 27.3803(19)
c/Å 12.0501(9)
α/° 90
β/° 100.600(7)
γ/° 90
Volume/Å3 4065.0(5)
Z 4
ρcalcg/cm3 1.604
μ/mm‑1 3.352
F(000) 2008.0
Crystal size/mm3 0.3 × 0.2 × 0.1
Radiation MoKα (λ = 0.71073)
2Θ range for data collection/° 4.548 to 53.998
Index ranges -15 ≤ h ≤ 15, -34 ≤ k ≤ 33, -14 ≤ l ≤ 15
Reflections collected 18217
Independent reflections 4399 [Rint = 0.0609, Rsigma = 0.0630]
Data/restraints/parameters 4399/0/233
Goodness-of-fit on F2 1.045
Final R indexes [I>=2σ (I)] R1 = 0.0406, wR2 = 0.0669
Final R indexes [all data] R1 = 0.0659, wR2 = 0.0745
Largest diff. peak/hole / e Å-3 0.60/-0.39

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for 3099. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Br1927.4(3)2054.1(2)1342.6(3)28.46(11)
Zn102557.1(2)250019.46(14)
Fe13281.9(4)4266.5(2)4758.8(4)20.61(13)
Si1868.9(7)3570.3(4)3569.7(7)16.3(2)
O103788.8(12)250017.4(7)
O21075.1(15)2993.9(8)3406.7(17)18.2(5)
N13071(2)2809.4(11)3182(2)20.6(7)
C12184(2)3896.6(13)3550(3)19.3(8)
C23267(2)3687.0(13)3700(3)21.1(8)
C33992(3)4058.2(14)3452(3)26.3(9)
C43400(3)4490.2(14)3164(3)27.0(9)
C52299(3)4393.7(13)3225(3)22.9(8)
C63829(3)4025.4(16)6380(3)34.6(10)
C74536(3)4383.1(16)6078(3)34.4(10)
C83945(3)4818.7(15)5809(3)34.1(10)
C92859(3)4729.8(15)5935(3)33.7(10)
C102789(3)4240.3(15)6292(3)31.7(9)
C113581(2)3176.2(13)4052(3)23.7(8)
C123308(3)2903.9(15)2043(3)28.1(9)
C133398(3)2307.3(14)3567(3)29.7(9)
C14241(2)3709.3(13)4824(3)19.0(8)
C15-801(3)3412.9(15)4820(3)29.0(9)
C16-1345(3)3537.8(17)5816(4)44.6(11)
C17-1586(4)4081.4(18)5855(4)53.5(13)
C18-558(3)4382.4(17)5878(3)44.6(11)
C19-21(3)4258.6(14)4879(3)26.9(8)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for 3099. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Br121.43(18)24.8(2)37.6(2)-8.73(17)1.42(15)4.15(15)
Zn114.5(3)15.0(3)27.2(3)0-0.5(2)0
Fe119.8(2)21.8(3)18.6(3)-0.6(2)-1.0(2)-5.5(2)
Si113.0(4)16.9(5)17.9(5)-1.0(4)-0.3(4)-0.8(4)
O113.9(15)18(2)18.9(17)00.6(13)0
O213.7(10)16.7(14)22.5(13)-1.4(10)-1.1(9)0.5(9)
N114.3(14)22.1(18)24.8(16)-1.6(13)2.1(13)2.7(12)
C119.1(16)22(2)15.8(17)-2.2(14)0.0(14)-2.8(14)
C220.4(17)24(2)17.7(18)-3.4(15)0.6(14)-2.5(14)
C318.2(17)39(3)21(2)-1.7(17)3.3(15)-9.0(16)
C431.7(19)26(2)21.9(19)5.6(16)2.1(16)-10.4(17)
C522.7(17)22(2)20.7(18)1.1(16)-3.1(15)-3.2(15)
C644(2)34(3)20(2)2.1(17)-7.7(18)-7.2(19)
C725.8(19)49(3)24(2)-6.7(19)-7.7(16)-7.9(19)
C841(2)33(3)26(2)-8.9(18)-0.2(18)-17.0(19)
C937(2)36(3)25(2)-15.7(18)-3.1(17)0.8(19)
C1031(2)40(3)24(2)-5.4(18)4.2(16)-13.9(18)
C1115.2(16)29(2)25.0(19)-1.2(16)-0.9(14)2.1(15)
C1218.7(17)38(3)27(2)-4.3(18)2.5(15)0.3(16)
C1325.4(19)23(2)39(2)-1.8(18)0.0(17)7.1(16)
C1418.4(16)19(2)18.3(17)-0.7(14)0.8(14)0.8(14)
C1520.7(18)35(3)32(2)2.1(18)6.6(16)-1.9(16)
C1636(2)57(3)46(3)9(2)22(2)-2(2)
C1756(3)65(4)49(3)7(3)37(2)18(2)
C1863(3)39(3)34(2)-5(2)16(2)16(2)
C1928.1(19)27(2)27(2)-2.6(17)6.3(16)4.7(16)

 

Table 4 Bond Lengths for 3099.
AtomAtomLength/Å AtomAtomLength/Å
Br1Zn12.4061(5) N1C121.480(4)
Zn1Br112.4061(5) N1C131.484(4)
Zn1O21.974(2) C1C21.455(4)
Zn1O211.975(2) C1C51.431(5)
Fe1C12.075(3) C2C31.431(5)
Fe1C22.034(3) C2C111.493(5)
Fe1C32.028(4) C3C41.406(5)
Fe1C42.048(3) C4C51.420(4)
Fe1C52.054(3) C6C71.413(5)
Fe1C62.057(3) C6C101.416(5)
Fe1C72.045(3) C7C81.410(5)
Fe1C82.047(4) C8C91.418(5)
Fe1C92.043(4) C9C101.415(5)
Fe1C102.055(4) C14C151.538(4)
Si1O11.6398(14) C14C191.543(5)
Si1O21.617(2) C15C161.524(5)
Si1C11.878(3) C16C171.521(6)
Si1C141.867(3) C17C181.526(6)
O1Si111.6398(14) C18C191.522(5)
N1C111.506(4)    

1-X,+Y,1/2-Z

 

Table 5 Bond Angles for 3099.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
Br11Zn1Br1110.17(3) O2Si1C1107.61(14)
O2Zn1Br11112.29(6) O2Si1C14113.45(14)
O21Zn1Br11108.31(6) C14Si1C1114.48(15)
O21Zn1Br1112.29(6) Si11O1Si1137.2(2)
O2Zn1Br1108.31(6) Si1O2Zn1123.40(11)
O2Zn1O21105.43(13) C12N1C11113.4(3)
C2Fe1C141.45(12) C12N1C13111.1(3)
C2Fe1C468.81(14) C13N1C11110.1(3)
C2Fe1C568.45(14) Si1C1Fe1133.92(17)
C2Fe1C6107.97(15) C2C1Fe167.78(17)
C2Fe1C7121.78(15) C2C1Si1127.7(3)
C2Fe1C8156.87(14) C5C1Fe168.94(18)
C2Fe1C9161.06(15) C5C1Si1126.1(2)
C2Fe1C10124.58(15) C5C1C2105.7(3)
C3Fe1C169.34(13) C1C2Fe170.77(19)
C3Fe1C241.25(13) C1C2C11126.6(3)
C3Fe1C440.35(14) C3C2Fe169.1(2)
C3Fe1C567.99(14) C3C2C1108.0(3)
C3Fe1C6121.98(15) C3C2C11125.5(3)
C3Fe1C7105.25(14) C11C2Fe1125.5(2)
C3Fe1C8120.08(15) C2C3Fe169.6(2)
C3Fe1C9156.93(16) C4C3Fe170.6(2)
C3Fe1C10159.38(16) C4C3C2108.8(3)
C4Fe1C168.93(13) C3C4Fe169.1(2)
C4Fe1C540.51(12) C3C4C5107.7(3)
C4Fe1C6156.67(15) C5C4Fe169.97(19)
C4Fe1C10160.05(16) C1C5Fe170.51(18)
C5Fe1C140.55(13) C4C5Fe169.52(18)
C5Fe1C6161.69(14) C4C5C1109.8(3)
C5Fe1C10125.86(14) C7C6Fe169.4(2)
C6Fe1C1124.92(15) C7C6C10107.8(4)
C7Fe1C1159.71(16) C10C6Fe169.8(2)
C7Fe1C4120.33(14) C6C7Fe170.29(19)
C7Fe1C5157.13(15) C8C7Fe169.93(19)
C7Fe1C640.29(14) C8C7C6108.5(3)
C7Fe1C840.30(15) C7C8Fe169.8(2)
C7Fe1C1067.75(14) C7C8C9107.7(4)
C8Fe1C1159.39(15) C9C8Fe169.6(2)
C8Fe1C4105.54(15) C8C9Fe169.9(2)
C8Fe1C5122.64(15) C10C9Fe170.2(2)
C8Fe1C667.87(16) C10C9C8108.0(3)
C8Fe1C1067.97(15) C6C10Fe169.9(2)
C9Fe1C1124.53(14) C9C10Fe169.4(2)
C9Fe1C4122.55(16) C9C10C6108.0(3)
C9Fe1C5109.28(15) C2C11N1111.8(3)
C9Fe1C667.92(16) C15C14Si1112.0(2)
C9Fe1C767.91(15) C15C14C19109.1(3)
C9Fe1C840.57(14) C19C14Si1111.0(2)
C9Fe1C1040.41(15) C16C15C14112.5(3)
C10Fe1C1110.12(14) C17C16C15111.3(3)
C10Fe1C640.30(14) C16C17C18110.9(3)
O1Si1C1105.90(13) C19C18C17111.1(3)
O1Si1C14104.13(11) C18C19C14112.3(3)
O2Si1O1111.01(13)     

1-X,+Y,1/2-Z

 

Table 6 Hydrogen Bonds for 3099.
DHAd(D-H)/Åd(H-A)/Åd(D-A)/ÅD-H-A/°
N1H1O20.90(3)1.73(4)2.615(3)169(4)

 

Table 7 Torsion Angles for 3099.
ABCDAngle/˚ ABCDAngle/˚
Fe1C1C2C3-59.4(2) C1C2C11N165.3(4)
Fe1C1C2C11120.5(3) C2C1C5Fe1-58.1(2)
Fe1C1C5C458.5(2) C2C1C5C40.4(4)
Fe1C2C3C4-59.9(2) C2C3C4Fe159.3(2)
Fe1C2C11N1156.8(2) C2C3C4C5-0.2(4)
Fe1C3C4C5-59.5(2) C3C2C11N1-114.9(3)
Fe1C4C5C1-59.1(2) C3C4C5Fe158.9(2)
Fe1C6C7C859.7(2) C3C4C5C1-0.2(4)
Fe1C6C10C9-59.1(2) C5C1C2Fe158.8(2)
Fe1C7C8C959.5(2) C5C1C2C3-0.5(4)
Fe1C8C9C1060.1(2) C5C1C2C11179.3(3)
Fe1C9C10C659.5(2) C6C7C8Fe1-59.9(3)
Si1C1C2Fe1-129.2(3) C6C7C8C9-0.5(4)
Si1C1C2C3171.5(2) C7C6C10Fe159.2(3)
Si1C1C2C11-8.7(5) C7C6C10C90.1(4)
Si1C1C5Fe1129.7(3) C7C8C9Fe1-59.6(3)
Si1C1C5C4-171.8(2) C7C8C9C100.5(4)
Si1C14C15C16-177.8(3) C8C9C10Fe1-59.9(2)
Si1C14C19C18178.7(2) C8C9C10C6-0.4(4)
O1Si1O2Zn1-26.39(17) C10C6C7Fe1-59.5(2)
O1Si1C1Fe1129.7(2) C10C6C7C80.2(4)
O1Si1C1C2-135.6(3) C11C2C3Fe1-119.4(3)
O1Si1C1C534.9(3) C11C2C3C4-179.4(3)
O1Si1C14C1567.6(3) C12N1C11C255.1(4)
O1Si1C14C19-54.6(2) C13N1C11C2-179.7(3)
O2Si1O1Si1113.49(9) C14Si1O1Si11-108.94(12)
O2Si1C1Fe1-111.5(2) C14Si1O2Zn190.46(17)
O2Si1C1C2-16.8(3) C14Si1C1Fe115.6(3)
O2Si1C1C5153.6(3) C14Si1C1C2110.3(3)
O2Si1C14C15-53.2(3) C14Si1C1C5-79.2(3)
O2Si1C14C19-175.36(19) C14C15C16C1755.9(4)
C1Si1O1Si11130.00(12) C15C14C19C1854.8(4)
C1Si1O2Zn1-141.84(15) C15C16C17C18-55.5(5)
C1Si1C14C15-177.2(2) C16C17C18C1955.8(5)
C1Si1C14C1960.6(3) C17C18C19C14-56.3(4)
C1C2C3Fe160.4(2) C19C14C15C16-54.5(4)
C1C2C3C40.4(4)      

1-X,+Y,1/2-Z

 

Table 8 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for 3099.
AtomxyzU(eq)
H12370(30)2835(14)3230(30)36(11)
H347504019347932
H436854793296532
H517254625307227
H640173699660241
H752844338606041
H842255118558441
H922804959580340
H1021564084644638
H11A33513106477928
H11B43813144416928
H12A30563232179642
H12B29332661151242
H12C40922881206742
H13A41752264357445
H13B29852070305045
H13C32502257432945
H147753622551923
H15A-13163477410935
H15B-6233060484435
H16A-20303352575354
H16B-8633440652854
H17A-18944154653664
H17B-21314172518464
H18A-7434734585754
H18B-434317658954
H19A6594449493632
H19B-5094356417132

Experimental

Single crystals of C38H56Br2Fe2N2O3Si2Zn [3099] were []. A suitable crystal was selected and [] on a Xcalibur, Sapphire3 diffractometer. The crystal was kept at 173 K during data collection. Using Olex2 [1], the structure was solved with the ShelXS [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. (2008). Acta Cryst. A64, 112-122.
  3. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.

Crystal structure determination of [3099]

Crystal Data for C38H56Br2Fe2N2O3Si2Zn (=981.91 g/mol): monoclinic, space group C2/c (no. 15), a = 12.5345(7) Å, b = 27.3803(19) Å, c = 12.0501(9) Å, β = 100.600(7)°, = 4065.0(5) Å3, Z = 4, T = 173 K, μ(MoKα) = 3.352 mm-1, Dcalc = 1.604 g/cm3, 18217 reflections measured (4.548° ≤ 2Θ ≤ 53.998°), 4399 unique (Rint = 0.0609, Rsigma = 0.0630) which were used in all calculations. The final R1 was 0.0406 (I > 2σ(I)) and wR2 was 0.0745 (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 Ternary CH refined with riding coordinates:
C14(H14)
2.b Secondary CH2 refined with riding coordinates:
C11(H11A,H11B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,
H18B), C19(H19A,H19B)
2.c Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10)
2.d Idealised Me refined as rotating group:
C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)

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