DC133

Table 1 Crystal data and structure refinement for DC133.
Identification code DC133
Empirical formula C11H14O3TiBr
Formula weight 309.07
Temperature/K 150.0
Crystal system orthorhombic
Space group Ccc2
a/Å 11.4688(12)
b/Å 22.418(2)
c/Å 10.6590(12)
α/° 90
β/° 90
γ/° 90
Volume/Å3 2740.5(5)
Z 8
ρcalcmg/mm3 1.4981
m/mm‑1 3.261
F(000) 1239.6
Crystal size/mm3 N/A × N/A × N/A
Radiation Mo Kα (λ = 0.71073)
2Θ range for data collection 3.64 to 67.1°
Index ranges -17 ≤ h ≤ 17, -34 ≤ k ≤ 22, -16 ≤ l ≤ 16
Reflections collected 19850
Independent reflections 5371 [Rint = 0.0238, Rsigma = 0.0410]
Data/restraints/parameters 5371/0/151
Goodness-of-fit on F2 0.964
Final R indexes [I>=2σ (I)] R1 = 0.0281, wR2 = N/A
Final R indexes [all data] R1 = 0.0380, wR2 = 0.0714
Largest diff. peak/hole / e Å-3 1.09/-0.46
Flack parameter0.016(7)

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for DC133. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Br12149.0(2)4970.04(8)9611.39(18)48.27(7)
Ti1250075003142.8(3)20.54(7)
O32380.4(8)6881.5(5)2035.1(12)27.2(2)
O22219.9(9)6912.5(5)4634.8(12)24.76(19)
O1791.5(8)7665.6(5)3392.3(9)25.5(2)
C102664.3(13)6158.1(8)6631.9(16)28.9(3)
C92844.6(15)5722.8(8)7556.0(18)33.5(3)
C81926.8(16)5579.0(7)8374.7(16)35.7(4)
C51572.0(12)6449.8(7)6514.5(14)24.7(3)
C1-1087.3(14)7879.8(10)4222.8(18)44.8(5)
C298.2(11)7582.8(7)4334.8(15)26.2(3)
C3368.7(14)7234.6(8)5397.2(16)30.1(3)
C41404.0(12)6890.4(6)5465.7(13)22.5(3)
C7857.7(18)5869.7(8)8301.0(19)47.5(4)
C6680.5(16)6308.2(8)7374.5(17)40.9(4)
C112540.9(17)6264.1(9)1859(2)44.1(5)
C123800.3(18)6062.3(9)2051(3)56.8(6)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for DC133. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U12U13U23
Br183.92(15)28.98(9)31.91(9)-1.85(8)-8.18(11)7.86(8)
Ti117.09(11)30.30(17)14.23(13)-2.27(12)-00
O325.8(5)32.7(6)23.2(5)-1.5(4)-2.4(4)-4.7(5)
O221.9(4)31.3(5)21.1(5)-0.1(4)2.7(4)3.2(5)
O119.7(4)38.2(5)18.7(5)-1.8(4)-0.5(3)3.1(4)
C1032.1(8)27.6(8)27.1(8)-1.7(5)-1.8(6)1.0(7)
C939.2(8)27.9(8)33.3(9)0.4(6)-8.3(7)0.8(7)
C859.2(10)24.7(7)23.1(8)-4.1(7)-6.0(7)1.8(6)
C529.6(7)25.4(7)19.2(6)-4.0(5)0.1(5)-0.6(6)
C129.7(8)69.6(13)35.0(9)15.2(8)8.1(7)14.4(9)
C220.4(5)34.5(8)23.8(8)-0.1(5)1.8(5)1.1(6)
C327.8(6)41.0(9)21.5(7)4.1(6)6.6(6)5.4(7)
C425.1(6)25.3(7)17.0(6)-2.2(5)-0.2(5)-0.9(5)
C757.6(10)45.2(10)39.6(11)0.4(8)14.9(9)16.8(9)
C639.2(9)44.3(10)39.1(10)3.9(7)12.0(8)15.5(8)
C1141.5(9)33.0(9)58.0(14)-5.8(7)-6.8(9)-3.4(9)
C1245(1)36.2(9)89.1(18)6.9(8)-7.4(12)-5.4(12)

 

Table 4 Bond Lengths for DC133.
AtomAtomLength/Å AtomAtomLength/Å
Br1C81.9148(17) C10C51.419(2)
Ti1O31.8264(12) C9C81.405(3)
Ti1O311.8264(12) C8C71.391(3)
Ti1O212.0897(12) C5C41.504(2)
Ti1O22.0897(12) C5C61.409(2)
Ti1O12.0119(9) C1C21.519(2)
Ti1O112.0119(9) C2C31.410(2)
O3C111.409(2) C3C41.418(2)
O2C41.2894(18) C7C61.408(2)
O1C21.2946(17) C11C121.527(3)
C10C91.402(3)    

11/2-X,3/2-Y,+Z

 

Table 5 Bond Angles for DC133.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
O31Ti1O399.44(8) C5C10C9120.87(15)
O2Ti1O390.11(5) C8C9C10119.06(16)
O2Ti1O31169.12(5) C9C8Br1119.45(14)
O21Ti1O3169.12(5) C7C8Br1119.36(14)
O21Ti1O3190.11(5) C7C8C9121.19(17)
O21Ti1O280.89(7) C4C5C10118.78(13)
O1Ti1O3191.06(4) C6C5C10118.65(14)
O1Ti1O398.77(4) C6C5C4122.57(13)
O11Ti1O3198.77(4) C1C2O1115.22(14)
O11Ti1O391.06(4) C3C2O1124.58(13)
O1Ti1O282.30(4) C3C2C1120.19(14)
O1Ti1O2186.15(4) C4C3C2121.79(14)
O11Ti1O286.15(4) C5C4O2116.28(12)
O11Ti1O2182.30(4) C3C4O2123.47(14)
O11Ti1O1164.81(6) C3C4C5120.19(13)
C11O3Ti1145.30(14) C6C7C8119.60(16)
C4O2Ti1131.18(9) C7C6C5120.58(16)
C2O1Ti1132.40(9) C12C11O3113.37(16)

11/2-X,3/2-Y,+Z

 

Table 6 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for DC133.
AtomxyzU(eq)
H103281.7(13)6259.1(8)6077.0(16)34.7(4)
H93577.1(15)5527.9(8)7627.6(18)40.2(4)
H1a-986.5(17)8313.3(11)4174(16)67.1(7)
H1b-1480(6)7737(6)3463(9)67.1(7)
H1c-1561(6)7781(6)4959(8)67.1(7)
H3-157.1(14)7230.3(8)6085.8(16)36.1(4)
H7250.6(18)5773.1(8)8872.3(19)57.0(5)
H6-46.3(16)6510.4(8)7328.7(17)49.0(5)
H11a2033.4(17)6045.7(9)2454(2)53.0(6)
H11b2293.0(17)6157.1(9)998(2)53.0(6)
H12a4319(2)6304(5)1525(12)85.2(9)
H12b4016(5)6112(7)2934(4)85.2(9)
H12c3875(4)5641(2)1816(15)85.2(9)

Experimental

Single crystals of C11H14O3TiBr [DC133] were [?]. A suitable crystal was selected and [MiTeGen crystal mount] on a Bruker X8 diffractometer. The crystal was kept at 150.0 K during data collection. Using Olex2 [1], the structure was solved with the Superflip [2] structure solution program using Charge Flipping and refined with the olex2.refine [3] refinement package using Gauss-Newton 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. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst., 40, 786-790; Palatinus, L. & van der Lee, A. (2008). J. Appl. Cryst. 41, 975-984; Palatinus, L., Prathapa, S. J. & van Smaalen, S. (2012). J. Appl. Cryst. 45, 575-580
  3. Bourhis, L.J., Dolomanov, O.V., Gildea, R.J., Howard, J.A.K., Puschmann, H. (2013). in preparation

Crystal structure determination of [DC133]

Crystal Data for C11H14O3TiBr (=309.07): orthorhombic, space group Ccc2 (no. 37), a = 11.4688(12) Å, b = 22.418(2) Å, c = 10.6590(12) Å, = 2740.5(5) Å3, Z = 8, T = 150.0 K, μ(Mo Kα) = 3.261 mm-1, Dcalc = 1.4981 g/mm3, 19850 reflections measured (3.64 ≤ 2Θ ≤ 67.1), 5371 unique (Rint = 0.0238, Rsigma = 0.0410) which were used in all calculations. The final R1 was 0.0281 (I>=2u(I)) and wR2 was 0.0714 (all data).

Refinement model description

Number of restraints - 0, number of constraints - 21.

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:
C10(H10), C9(H9), C3(H3), C7(H7), C6(H6)
2.c Idealised Me refined as rotating group:
C1(H1a,H1b,H1c), C12(H12a,H12b,H12c)

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