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 parameter | 0.016(7) |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
Br1 | 2149.0(2) | 4970.04(8) | 9611.39(18) | 48.27(7) |
Ti1 | 2500 | 7500 | 3142.8(3) | 20.54(7) |
O3 | 2380.4(8) | 6881.5(5) | 2035.1(12) | 27.2(2) |
O2 | 2219.9(9) | 6912.5(5) | 4634.8(12) | 24.76(19) |
O1 | 791.5(8) | 7665.6(5) | 3392.3(9) | 25.5(2) |
C10 | 2664.3(13) | 6158.1(8) | 6631.9(16) | 28.9(3) |
C9 | 2844.6(15) | 5722.8(8) | 7556.0(18) | 33.5(3) |
C8 | 1926.8(16) | 5579.0(7) | 8374.7(16) | 35.7(4) |
C5 | 1572.0(12) | 6449.8(7) | 6514.5(14) | 24.7(3) |
C1 | -1087.3(14) | 7879.8(10) | 4222.8(18) | 44.8(5) |
C2 | 98.2(11) | 7582.8(7) | 4334.8(15) | 26.2(3) |
C3 | 368.7(14) | 7234.6(8) | 5397.2(16) | 30.1(3) |
C4 | 1404.0(12) | 6890.4(6) | 5465.7(13) | 22.5(3) |
C7 | 857.7(18) | 5869.7(8) | 8301.0(19) | 47.5(4) |
C6 | 680.5(16) | 6308.2(8) | 7374.5(17) | 40.9(4) |
C11 | 2540.9(17) | 6264.1(9) | 1859(2) | 44.1(5) |
C12 | 3800.3(18) | 6062.3(9) | 2051(3) | 56.8(6) |
Atom | U11 | U22 | U33 | U12 | U13 | U23 |
---|---|---|---|---|---|---|
Br1 | 83.92(15) | 28.98(9) | 31.91(9) | -1.85(8) | -8.18(11) | 7.86(8) |
Ti1 | 17.09(11) | 30.30(17) | 14.23(13) | -2.27(12) | -0 | 0 |
O3 | 25.8(5) | 32.7(6) | 23.2(5) | -1.5(4) | -2.4(4) | -4.7(5) |
O2 | 21.9(4) | 31.3(5) | 21.1(5) | -0.1(4) | 2.7(4) | 3.2(5) |
O1 | 19.7(4) | 38.2(5) | 18.7(5) | -1.8(4) | -0.5(3) | 3.1(4) |
C10 | 32.1(8) | 27.6(8) | 27.1(8) | -1.7(5) | -1.8(6) | 1.0(7) |
C9 | 39.2(8) | 27.9(8) | 33.3(9) | 0.4(6) | -8.3(7) | 0.8(7) |
C8 | 59.2(10) | 24.7(7) | 23.1(8) | -4.1(7) | -6.0(7) | 1.8(6) |
C5 | 29.6(7) | 25.4(7) | 19.2(6) | -4.0(5) | 0.1(5) | -0.6(6) |
C1 | 29.7(8) | 69.6(13) | 35.0(9) | 15.2(8) | 8.1(7) | 14.4(9) |
C2 | 20.4(5) | 34.5(8) | 23.8(8) | -0.1(5) | 1.8(5) | 1.1(6) |
C3 | 27.8(6) | 41.0(9) | 21.5(7) | 4.1(6) | 6.6(6) | 5.4(7) |
C4 | 25.1(6) | 25.3(7) | 17.0(6) | -2.2(5) | -0.2(5) | -0.9(5) |
C7 | 57.6(10) | 45.2(10) | 39.6(11) | 0.4(8) | 14.9(9) | 16.8(9) |
C6 | 39.2(9) | 44.3(10) | 39.1(10) | 3.9(7) | 12.0(8) | 15.5(8) |
C11 | 41.5(9) | 33.0(9) | 58.0(14) | -5.8(7) | -6.8(9) | -3.4(9) |
C12 | 45(1) | 36.2(9) | 89.1(18) | 6.9(8) | -7.4(12) | -5.4(12) |
Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
---|---|---|---|---|---|---|
Br1 | C8 | 1.9148(17) | C10 | C5 | 1.419(2) | |
Ti1 | O3 | 1.8264(12) | C9 | C8 | 1.405(3) | |
Ti1 | O31 | 1.8264(12) | C8 | C7 | 1.391(3) | |
Ti1 | O21 | 2.0897(12) | C5 | C4 | 1.504(2) | |
Ti1 | O2 | 2.0897(12) | C5 | C6 | 1.409(2) | |
Ti1 | O1 | 2.0119(9) | C1 | C2 | 1.519(2) | |
Ti1 | O11 | 2.0119(9) | C2 | C3 | 1.410(2) | |
O3 | C11 | 1.409(2) | C3 | C4 | 1.418(2) | |
O2 | C4 | 1.2894(18) | C7 | C6 | 1.408(2) | |
O1 | C2 | 1.2946(17) | C11 | C12 | 1.527(3) | |
C10 | C9 | 1.402(3) |
Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
---|---|---|---|---|---|---|---|---|
O31 | Ti1 | O3 | 99.44(8) | C5 | C10 | C9 | 120.87(15) | |
O2 | Ti1 | O3 | 90.11(5) | C8 | C9 | C10 | 119.06(16) | |
O2 | Ti1 | O31 | 169.12(5) | C9 | C8 | Br1 | 119.45(14) | |
O21 | Ti1 | O3 | 169.12(5) | C7 | C8 | Br1 | 119.36(14) | |
O21 | Ti1 | O31 | 90.11(5) | C7 | C8 | C9 | 121.19(17) | |
O21 | Ti1 | O2 | 80.89(7) | C4 | C5 | C10 | 118.78(13) | |
O1 | Ti1 | O31 | 91.06(4) | C6 | C5 | C10 | 118.65(14) | |
O1 | Ti1 | O3 | 98.77(4) | C6 | C5 | C4 | 122.57(13) | |
O11 | Ti1 | O31 | 98.77(4) | C1 | C2 | O1 | 115.22(14) | |
O11 | Ti1 | O3 | 91.06(4) | C3 | C2 | O1 | 124.58(13) | |
O1 | Ti1 | O2 | 82.30(4) | C3 | C2 | C1 | 120.19(14) | |
O1 | Ti1 | O21 | 86.15(4) | C4 | C3 | C2 | 121.79(14) | |
O11 | Ti1 | O2 | 86.15(4) | C5 | C4 | O2 | 116.28(12) | |
O11 | Ti1 | O21 | 82.30(4) | C3 | C4 | O2 | 123.47(14) | |
O11 | Ti1 | O1 | 164.81(6) | C3 | C4 | C5 | 120.19(13) | |
C11 | O3 | Ti1 | 145.30(14) | C6 | C7 | C8 | 119.60(16) | |
C4 | O2 | Ti1 | 131.18(9) | C7 | C6 | C5 | 120.58(16) | |
C2 | O1 | Ti1 | 132.40(9) | C12 | C11 | O3 | 113.37(16) |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
H10 | 3281.7(13) | 6259.1(8) | 6077.0(16) | 34.7(4) |
H9 | 3577.1(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) |
H7 | 250.6(18) | 5773.1(8) | 8872.3(19) | 57.0(5) |
H6 | -46.3(16) | 6510.4(8) | 7328.7(17) | 49.0(5) |
H11a | 2033.4(17) | 6045.7(9) | 2454(2) | 53.0(6) |
H11b | 2293.0(17) | 6157.1(9) | 998(2) | 53.0(6) |
H12a | 4319(2) | 6304(5) | 1525(12) | 85.2(9) |
H12b | 4016(5) | 6112(7) | 2934(4) | 85.2(9) |
H12c | 3875(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.
Crystal structure determination of [DC133]
Crystal Data for C11H14O3TiBr (M =309.07): orthorhombic, space group Ccc2 (no. 37), a = 11.4688(12) Å, b = 22.418(2) Å, c = 10.6590(12) Å, V = 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)
This report has been created with Olex2, compiled on 2013.12.10 svn.r2850 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.