Identification code | dc150 |
Empirical formula | C34H32O6Ti |
Formula weight | 584.50 |
Temperature/K | 150 |
Crystal system | monoclinic |
Space group | P21/c |
a/Å | 11.2203(12) |
b/Å | 15.8876(16) |
c/Å | 20.1373(19) |
α/° | 90 |
β/° | 121.131(6) |
γ/° | 90 |
Volume/Å3 | 3072.8(6) |
Z | 4 |
ρcalcg/cm3 | 1.2634 |
μ/mm‑1 | 0.321 |
F(000) | 1225.8 |
Crystal size/mm3 | 0.085 × 0.078 × 0.011 |
Radiation | Mo Kα (λ = 0.71073) |
2Θ range for data collection/° | 4.44 to 60.48 |
Index ranges | -15 ≤ h ≤ 15, -22 ≤ k ≤ 22, -28 ≤ l ≤ 24 |
Reflections collected | 37033 |
Independent reflections | 8989 [Rint = 0.0621, Rsigma = 0.0646] |
Data/restraints/parameters | 8989/0/371 |
Goodness-of-fit on F2 | 1.049 |
Final R indexes [I>=2σ (I)] | R1 = 0.0606, wR2 = 0.1616 |
Final R indexes [all data] | R1 = 0.0925, wR2 = 0.1860 |
Largest diff. peak/hole / e Å-3 | 1.21/-0.87 |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
Ti1 | 6966.8(4) | 7776.6(3) | 8486.6(2) | 20.17(12) |
O2 | 5585.9(16) | 7725.2(10) | 7333.7(9) | 23.6(3) |
C10 | 3530(2) | 7635.1(14) | 6069.2(13) | 20.5(4) |
O3 | 5711.1(16) | 6887.3(10) | 8607.1(9) | 24.2(3) |
C26 | 8461(2) | 7550.2(15) | 11612.4(13) | 22.8(4) |
C22 | 5600(2) | 6671.9(13) | 9187.7(13) | 20.0(4) |
C9 | 4273(2) | 7929.0(13) | 6908.1(12) | 19.5(4) |
C25 | 8737(2) | 7669.6(13) | 11006.6(12) | 18.8(4) |
O6 | 8033.9(17) | 8661.4(10) | 8530.4(10) | 27.8(4) |
O4 | 7934.2(16) | 7818.3(10) | 9660.5(9) | 23.0(3) |
O5 | 7964.9(17) | 6904.3(10) | 8413.6(9) | 25.2(3) |
O1 | 5474.1(16) | 8583.8(10) | 8479.6(9) | 23.6(3) |
C27 | 9485(3) | 7743.9(15) | 12386.9(14) | 27.8(5) |
C6 | 3321(2) | 9232.0(13) | 8182.2(13) | 20.6(4) |
C11 | 2169(2) | 7908.6(16) | 5506.9(14) | 26.4(5) |
C23 | 6494(2) | 6980.9(14) | 9958.1(13) | 22.0(4) |
C21 | 4514(2) | 6015.7(14) | 9047.4(13) | 21.7(4) |
C30 | 10061(2) | 7984.9(14) | 11191.6(13) | 22.5(4) |
C28 | 10790(3) | 8057.6(16) | 12559.6(14) | 30.3(5) |
C20 | 3892(2) | 5975.0(14) | 9502.9(14) | 25.3(5) |
C8 | 3538(2) | 8382.0(15) | 7188.1(13) | 26.2(5) |
C24 | 7666(2) | 7494.1(13) | 10165.5(12) | 18.4(4) |
C7 | 4182(2) | 8703.2(13) | 7958.4(13) | 20.3(4) |
C12 | 1485(3) | 7591.9(17) | 4747.6(14) | 30.9(5) |
C29 | 11086(2) | 8172.6(15) | 11967.8(14) | 27.5(5) |
C5 | 1858(2) | 9153.7(14) | 7800.7(14) | 25.2(5) |
C1 | 4006(3) | 9818.3(14) | 8799.0(14) | 25.6(5) |
C15 | 4207(3) | 7045.6(15) | 5849.7(14) | 28.9(5) |
C2 | 3229(3) | 10310.8(15) | 9018.7(15) | 30.0(5) |
C3 | 1774(3) | 10220.1(15) | 8641.8(15) | 29.1(5) |
C4 | 1086(2) | 9640.3(15) | 8031.5(15) | 27.6(5) |
C16 | 4124(3) | 5424.8(15) | 8444.3(14) | 28.5(5) |
C13 | 2162(3) | 7003.1(17) | 4538.2(15) | 35.1(6) |
C18 | 2516(3) | 4765.8(16) | 8759.6(16) | 33.2(6) |
C14 | 3522(3) | 6736.7(17) | 5082.1(15) | 38.3(6) |
C19 | 2887(3) | 5356.5(16) | 9355.2(15) | 31.8(5) |
C17 | 3131(3) | 4795.1(16) | 8305.0(15) | 35.1(6) |
C31 | 7781(3) | 6023.2(17) | 8240.6(17) | 39.5(6) |
C33 | 8752(3) | 9392(2) | 8978(2) | 49.4(8) |
C34 | 7829(4) | 10054(2) | 8989(2) | 61.3(10) |
C32 | 8554(5) | 5513(2) | 8986(2) | 75.0(13) |
Atom | U11 | U22 | U33 | U12 | U13 | U23 |
---|---|---|---|---|---|---|
Ti1 | 15.53(19) | 30.8(2) | 12.5(2) | -1.48(14) | 6.05(15) | -0.62(14) |
O2 | 18.4(8) | 37.3(9) | 13.0(8) | 2.0(6) | 6.6(6) | -0.3(6) |
C10 | 19.4(10) | 28.8(11) | 13.4(10) | -2.5(8) | 8.6(9) | -1.0(8) |
O3 | 20.8(8) | 33.8(8) | 15.2(8) | -6.4(6) | 7.4(7) | -2.9(6) |
C26 | 20.8(10) | 29.9(11) | 16.9(11) | -0.3(8) | 9.2(9) | -2.6(8) |
C22 | 15.0(9) | 25.4(10) | 16.8(10) | -0.2(8) | 6.2(8) | 0.1(8) |
C9 | 19.2(10) | 26.5(10) | 12.8(10) | -3.2(8) | 8.2(8) | -0.0(8) |
C25 | 17.4(10) | 23.5(10) | 12.6(10) | 0.8(8) | 5.7(8) | -2.7(7) |
O6 | 25.6(8) | 34.7(9) | 23.9(9) | -5.9(7) | 13.4(7) | -1.6(7) |
O4 | 17.8(8) | 34.7(8) | 13.7(7) | -4.7(6) | 6.3(6) | -1.4(6) |
O5 | 20.9(8) | 32.9(8) | 18.7(8) | 1.3(6) | 8.2(7) | -1.1(6) |
O1 | 19.4(8) | 34.8(8) | 14.0(8) | -0.6(6) | 6.7(6) | -3.4(6) |
C27 | 30.0(13) | 35.7(12) | 14.7(11) | 3.4(10) | 9.6(10) | -1.4(9) |
C6 | 22.4(11) | 24.3(10) | 15.8(10) | -0.3(8) | 10.3(9) | 1.3(8) |
C11 | 21.0(11) | 40.5(13) | 16.4(11) | 1.7(9) | 8.8(9) | -1.8(9) |
C23 | 19.3(10) | 31.0(11) | 14.3(10) | -4.7(8) | 7.7(9) | -1.5(8) |
C21 | 15.6(9) | 26.2(10) | 15.6(10) | -1.1(8) | 2.6(8) | 1.2(8) |
C30 | 17.7(10) | 29.5(11) | 17.7(11) | -2.1(8) | 7.2(9) | -5.5(8) |
C28 | 25.6(12) | 38.4(13) | 15.9(11) | 0.3(10) | 2.9(10) | -6.8(9) |
C20 | 19.7(10) | 28.9(11) | 22.3(12) | -1.3(8) | 7.2(9) | 0.2(9) |
C8 | 18.3(10) | 40.4(13) | 15.5(11) | 2.0(9) | 5.6(9) | -4.6(9) |
C24 | 16.1(10) | 23.2(9) | 13.1(10) | 2.6(7) | 5.6(8) | -0.8(7) |
C7 | 20.8(10) | 25.8(10) | 16(1) | -2.1(8) | 10.6(9) | -0.5(8) |
C12 | 21.7(12) | 46.9(14) | 15.3(11) | -1.6(10) | 3.4(10) | -0.2(10) |
C29 | 17.6(11) | 35.9(12) | 22.3(12) | -3.2(9) | 5.4(9) | -6.1(9) |
C5 | 24.2(11) | 29.1(11) | 21.2(11) | -1.5(9) | 11(1) | -2.0(9) |
C1 | 24.9(11) | 29.3(11) | 22.1(12) | -3.2(9) | 11.8(10) | -3.5(9) |
C15 | 28.0(13) | 35.2(12) | 17.5(11) | 6.7(9) | 7.5(10) | -1.7(9) |
C2 | 33.6(13) | 30.1(12) | 26.9(13) | -1.7(10) | 16.1(11) | -5.4(10) |
C3 | 32.2(13) | 28.5(12) | 30.8(13) | 6.1(9) | 19.3(11) | 0.9(10) |
C4 | 21.4(11) | 34.5(12) | 26.6(13) | 3.4(9) | 12.3(10) | 0.5(10) |
C16 | 25.0(12) | 34.7(12) | 19.6(12) | -3.6(9) | 7.2(10) | -2.8(9) |
C13 | 40.9(15) | 39.4(13) | 16.0(12) | -4.1(11) | 8.3(11) | -8.1(10) |
C18 | 25.5(12) | 29.7(12) | 29.7(13) | -8.8(9) | 3.8(11) | 4.4(10) |
C14 | 45.1(16) | 39.3(14) | 22.5(13) | 10.6(12) | 11.9(12) | -5.9(10) |
C19 | 24.6(12) | 37.0(13) | 29.6(14) | -3.6(10) | 11.0(11) | 7.3(10) |
C17 | 30.9(14) | 32.8(13) | 26.3(13) | -8.2(10) | 4.0(11) | -5.5(10) |
C31 | 43.7(16) | 38.2(14) | 41.7(17) | -4.6(12) | 25.6(14) | -11.5(12) |
C33 | 35.3(16) | 52.1(17) | 57(2) | -20.8(13) | 21.5(15) | -22.4(15) |
C34 | 45.7(19) | 47.2(18) | 78(3) | -16.7(15) | 22.9(19) | -25.6(18) |
C32 | 106(4) | 34.6(16) | 72(3) | 5.3(19) | 37(3) | 11.0(17) |
Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
---|---|---|---|---|---|---|
Ti1 | O2 | 2.0194(16) | C6 | C7 | 1.514(3) | |
Ti1 | O3 | 2.0960(16) | C6 | C5 | 1.413(3) | |
Ti1 | O6 | 1.8189(16) | C6 | C1 | 1.419(3) | |
Ti1 | O4 | 2.0293(16) | C11 | C12 | 1.402(3) | |
Ti1 | O5 | 1.8349(17) | C23 | C24 | 1.414(3) | |
Ti1 | O1 | 2.1036(16) | C21 | C20 | 1.412(3) | |
O2 | C9 | 1.305(3) | C21 | C16 | 1.414(3) | |
C10 | C9 | 1.520(3) | C30 | C29 | 1.413(3) | |
C10 | C11 | 1.420(3) | C28 | C29 | 1.404(4) | |
C10 | C15 | 1.413(3) | C20 | C19 | 1.407(3) | |
O3 | C22 | 1.284(3) | C8 | C7 | 1.425(3) | |
C26 | C25 | 1.417(3) | C12 | C13 | 1.400(4) | |
C26 | C27 | 1.412(3) | C5 | C4 | 1.407(3) | |
C22 | C23 | 1.430(3) | C1 | C2 | 1.402(3) | |
C22 | C21 | 1.516(3) | C15 | C14 | 1.412(3) | |
C9 | C8 | 1.413(3) | C2 | C3 | 1.408(3) | |
C25 | C30 | 1.423(3) | C3 | C4 | 1.405(3) | |
C25 | C24 | 1.512(3) | C16 | C17 | 1.413(3) | |
O6 | C33 | 1.435(3) | C13 | C14 | 1.407(4) | |
O4 | C24 | 1.306(3) | C18 | C19 | 1.406(4) | |
O5 | C31 | 1.431(3) | C18 | C17 | 1.403(4) | |
O1 | C7 | 1.290(3) | C31 | C32 | 1.521(5) | |
C27 | C28 | 1.410(4) | C33 | C34 | 1.485(5) |
Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
---|---|---|---|---|---|---|---|---|
O3 | Ti1 | O2 | 86.77(6) | C5 | C6 | C7 | 122.01(19) | |
O6 | Ti1 | O2 | 100.46(7) | C1 | C6 | C7 | 119.00(19) | |
O6 | Ti1 | O3 | 168.62(7) | C1 | C6 | C5 | 119.0(2) | |
O4 | Ti1 | O2 | 166.17(7) | C12 | C11 | C10 | 121.1(2) | |
O4 | Ti1 | O3 | 82.75(6) | C24 | C23 | C22 | 122.8(2) | |
O4 | Ti1 | O6 | 88.63(7) | C20 | C21 | C22 | 122.0(2) | |
O5 | Ti1 | O2 | 90.84(7) | C16 | C21 | C22 | 118.6(2) | |
O5 | Ti1 | O3 | 88.55(7) | C16 | C21 | C20 | 119.4(2) | |
O5 | Ti1 | O6 | 100.01(8) | C29 | C30 | C25 | 120.4(2) | |
O5 | Ti1 | O4 | 97.87(7) | C29 | C28 | C27 | 120.5(2) | |
O1 | Ti1 | O2 | 83.22(6) | C19 | C20 | C21 | 120.4(2) | |
O1 | Ti1 | O3 | 80.28(7) | C7 | C8 | C9 | 123.0(2) | |
O1 | Ti1 | O6 | 91.78(7) | O4 | C24 | C25 | 115.47(18) | |
O1 | Ti1 | O4 | 86.12(6) | C23 | C24 | C25 | 121.07(19) | |
O1 | Ti1 | O5 | 167.61(7) | C23 | C24 | O4 | 123.4(2) | |
C9 | O2 | Ti1 | 132.81(14) | C6 | C7 | O1 | 117.44(18) | |
C11 | C10 | C9 | 122.5(2) | C8 | C7 | O1 | 123.9(2) | |
C15 | C10 | C9 | 118.5(2) | C8 | C7 | C6 | 118.69(19) | |
C15 | C10 | C11 | 118.9(2) | C13 | C12 | C11 | 119.5(2) | |
C22 | O3 | Ti1 | 132.23(14) | C28 | C29 | C30 | 119.8(2) | |
C27 | C26 | C25 | 120.4(2) | C4 | C5 | C6 | 120.8(2) | |
C23 | C22 | O3 | 123.52(19) | C2 | C1 | C6 | 119.9(2) | |
C21 | C22 | O3 | 117.43(19) | C14 | C15 | C10 | 119.8(2) | |
C21 | C22 | C23 | 118.94(19) | C3 | C2 | C1 | 120.6(2) | |
C10 | C9 | O2 | 115.96(18) | C4 | C3 | C2 | 119.9(2) | |
C8 | C9 | O2 | 123.9(2) | C3 | C4 | C5 | 119.7(2) | |
C8 | C9 | C10 | 120.1(2) | C17 | C16 | C21 | 120.2(2) | |
C30 | C25 | C26 | 119.0(2) | C14 | C13 | C12 | 120.4(2) | |
C24 | C25 | C26 | 122.62(19) | C17 | C18 | C19 | 120.4(2) | |
C24 | C25 | C30 | 118.39(19) | C13 | C14 | C15 | 120.4(2) | |
C33 | O6 | Ti1 | 142.92(18) | C18 | C19 | C20 | 119.9(2) | |
C24 | O4 | Ti1 | 133.97(14) | C18 | C17 | C16 | 119.8(2) | |
C31 | O5 | Ti1 | 137.82(16) | C32 | C31 | O5 | 110.1(2) | |
C7 | O1 | Ti1 | 130.59(14) | C34 | C33 | O6 | 114.4(2) | |
C28 | C27 | C26 | 119.9(2) |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
H26 | 7582(2) | 7338.4(15) | 11496.6(13) | 27.3(5) |
H27 | 9295(3) | 7663.0(15) | 12790.6(14) | 33.3(6) |
H11 | 1714(2) | 8312.9(16) | 5647.3(14) | 31.7(6) |
H23 | 6293(2) | 6835.1(14) | 10347.3(13) | 26.4(5) |
H30 | 10257(2) | 8069.6(14) | 10790.5(13) | 27.1(5) |
H28 | 11475(3) | 8192.4(16) | 13080.3(14) | 36.4(6) |
H20 | 4154(2) | 6367.6(14) | 9911.6(14) | 30.4(6) |
H8 | 2570(2) | 8476.7(15) | 6847.1(13) | 31.4(6) |
H12 | 570(3) | 7775.4(17) | 4378.4(14) | 37.1(6) |
H29 | 11973(2) | 8375.9(15) | 12089.0(14) | 33.0(6) |
H5 | 1390(2) | 8767.7(14) | 7383.1(14) | 30.2(6) |
H1 | 4989(3) | 9877.0(14) | 9062.8(14) | 30.8(6) |
H15 | 5120(3) | 6857.7(15) | 6217.4(14) | 34.6(6) |
H2 | 3690(3) | 10709.5(15) | 9425.9(15) | 35.9(6) |
H3 | 1258(3) | 10550.2(15) | 8799.8(15) | 34.9(6) |
H4 | 105(2) | 9577.1(15) | 7775.6(15) | 33.1(6) |
H16 | 4530(3) | 5451.1(15) | 8131.8(14) | 34.2(6) |
H13 | 1700(3) | 6782.4(17) | 4026.1(15) | 42.2(7) |
H18 | 1845(3) | 4344.3(16) | 8664.3(16) | 39.9(7) |
H14 | 3982(3) | 6346.8(17) | 4931.9(15) | 46.0(8) |
H19 | 2460(3) | 5338.0(16) | 9657.4(15) | 38.1(7) |
H17 | 2881(3) | 4392.9(16) | 7904.8(15) | 42.1(7) |
H31a | 6777(3) | 5882.6(17) | 7965.0(17) | 47.5(8) |
H31b | 8139(3) | 5879.5(17) | 7897.0(17) | 47.5(8) |
H33a | 9418(3) | 9215(2) | 9518(2) | 59.3(10) |
H33b | 9298(3) | 9638(2) | 8766(2) | 59.3(10) |
H34a | 7100(18) | 10191(13) | 8456(2) | 91.9(15) |
H34b | 7400(20) | 9849(7) | 9276(14) | 91.9(15) |
H34c | 8377(7) | 10560(6) | 9243(15) | 91.9(15) |
H32a | 9549(7) | 5649(15) | 9254(10) | 112.5(19) |
H32b | 8190(20) | 5651(15) | 9322(8) | 112.5(19) |
H32c | 8420(30) | 4912(2) | 8861(3) | 112.5(19) |
Experimental
Single crystals of C34H32O6Ti [dc150] were [Sample recrystallised from ethanol]. A suitable crystal was selected and [] on a 'Bruker APEX-II CCD' diffractometer. The crystal was kept at 150 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 olex2.refine [3] refinement package using Gauss-Newton minimisation.
Crystal structure determination of [dc150]
Crystal Data for C34H32O6Ti (M =584.50 g/mol): monoclinic, space group P21/c (no. 14), a = 11.2203(12) Å, b = 15.8876(16) Å, c = 20.1373(19) Å, β = 121.131(6)°, V = 3072.8(6) Å3, Z = 4, T = 150 K, μ(Mo Kα) = 0.321 mm-1, Dcalc = 1.2634 g/cm3, 37033 reflections measured (4.44° ≤ 2Θ ≤ 60.48°), 8989 unique (Rint = 0.0621, Rsigma = 0.0646) which were used in all calculations. The final R1 was 0.0606 (I>=2u(I)) and wR2 was 0.1860 (all data).
Refinement model description
Number of restraints - 0, number of constraints - 58.
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:
C31(H31a,H31b), C33(H33a,H33b)
2.b Aromatic/amide H refined with riding coordinates:
C26(H26), C27(H27), C11(H11), C23(H23), C30(H30), C28(H28), C20(H20), C8(H8),
C12(H12), C29(H29), C5(H5), C1(H1), C15(H15), C2(H2), C3(H3), C4(H4), C16(H16),
C13(H13), C18(H18), C14(H14), C19(H19), C17(H17)
2.c Idealised Me refined as rotating group:
C34(H34a,H34b,H34c), C32(H32a,H32b,H32c)
This report has been created with Olex2, compiled on 2015.01.26 svn.r3150 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.