Identification code | DC104_Mo_250 |
Empirical formula | C26H32O6Ti |
Formula weight | 488.42 |
Temperature/K | 250.00(10) |
Crystal system | monoclinic |
Space group | P21/c |
a/Å | 9.7197(8) |
b/Å | 26.883(3) |
c/Å | 10.0214(9) |
α/° | 90.00 |
β/° | 101.848(9) |
γ/° | 90.00 |
Volume/Å3 | 2562.7(4) |
Z | 4 |
ρcalcg/cm3 | 1.266 |
μ/mm‑1 | 0.371 |
F(000) | 1032.0 |
Crystal size/mm3 | 0.14 × 0.09 × 0.07 |
Radiation | MoKα (λ = 0.71073) |
2Θ range for data collection/° | 6.12 to 56.56 |
Index ranges | -12 ≤ h ≤ 9, -35 ≤ k ≤ 35, -12 ≤ l ≤ 13 |
Reflections collected | 17295 |
Independent reflections | 6352 [Rint = 0.0599, Rsigma = 0.0787] |
Data/restraints/parameters | 6352/8/328 |
Goodness-of-fit on F2 | 1.023 |
Final R indexes [I>=2σ (I)] | R1 = 0.0697, wR2 = 0.1440 |
Final R indexes [all data] | R1 = 0.1348, wR2 = 0.1735 |
Largest diff. peak/hole / e Å-3 | 0.51/-0.34 |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
Ti1 | 6329.2(6) | 1221.7(2) | 3632.7(6) | 50.0(2) |
O1 | 7040(2) | 1935.2(8) | 4102(2) | 54.0(6) |
C1 | 7798(4) | 2753.2(14) | 3841(4) | 66(1) |
O2 | 4844(2) | 1580.1(7) | 2314(2) | 47.3(5) |
C2 | 6912(3) | 2310.7(12) | 3320(3) | 46.5(7) |
O3 | 5344(2) | 1365.1(8) | 5223(2) | 53.5(6) |
C3 | 5971(3) | 2336.9(11) | 2069(3) | 44.9(7) |
O4 | 7867(2) | 976.1(8) | 5140(2) | 52.2(5) |
C4 | 4929(3) | 1984.9(11) | 1646(3) | 40.0(7) |
O5 | 5340(2) | 654.7(8) | 3320(2) | 59.1(6) |
C5 | 3810(3) | 2058.1(11) | 401(3) | 38.1(6) |
O6 | 7532(2) | 1158.8(9) | 2510(2) | 66.2(7) |
C6 | 2856(3) | 1677.1(12) | -37(3) | 47.8(7) |
C7 | 1838(3) | 1726.9(13) | -1212(3) | 54.6(8) |
C8 | 1721(3) | 2155.8(13) | -1988(3) | 50.3(8) |
C9 | 2641(3) | 2539.1(13) | -1525(3) | 51.4(8) |
C10 | 3674(3) | 2495.9(11) | -359(3) | 45.3(7) |
C11 | 666(4) | 2194.7(17) | -3319(3) | 76.9(12) |
C12 | 4513(4) | 1326.7(14) | 7253(4) | 69.6(10) |
C13 | 5613(3) | 1221.2(11) | 6438(4) | 49.6(8) |
C14 | 6850(3) | 981.2(12) | 7058(3) | 52.3(8) |
C15 | 7941(3) | 881.1(11) | 6393(3) | 44.3(7) |
C16 | 9293(3) | 650.6(11) | 7121(3) | 43.8(7) |
C17 | 9637(3) | 603.1(13) | 8518(3) | 58.5(9) |
C18 | 10902(4) | 399.5(13) | 9133(4) | 61.6(9) |
C19 | 11862(3) | 228.5(13) | 8412(4) | 57.8(9) |
C20 | 11503(4) | 265.6(16) | 7022(4) | 73.3(11) |
C21 | 10233(3) | 483.5(14) | 6375(3) | 60.5(9) |
C22 | 13240(4) | 5.0(18) | 9118(4) | 91.4(14) |
C23A | 3967(10) | 477(4) | 2837(9) | 65(3) |
C23B | 4218(11) | 371(4) | 3620(17) | 101(4) |
C24A | 3194(15) | 453(5) | 4000(12) | 93(4) |
C24B | 2855(13) | 621(6) | 3261(18) | 114(5) |
C25A | 8609(17) | 1326(9) | 1850(20) | 77(6) |
C25B | 8911(12) | 1048(5) | 2377(15) | 87(3) |
C25C | 9032(12) | 1342(6) | 2827(14) | 90(4) |
C26A | 9990(20) | 1100(10) | 2480(30) | 90(7) |
C26B | 9655(19) | 1499(7) | 2480(20) | 135(6) |
C26C | 9568(13) | 1268(5) | 1593(13) | 90(3) |
Atom | U11 | U22 | U33 | U23 | U13 | U12 |
---|---|---|---|---|---|---|
Ti1 | 47.0(3) | 48.0(4) | 54.6(4) | 12.7(3) | 9.2(3) | 7.6(3) |
O1 | 51.3(12) | 54.8(14) | 50.3(13) | 9.8(11) | -2.6(10) | -1.3(10) |
C1 | 63(2) | 62(2) | 65(2) | 3.6(18) | -5.9(17) | -14.5(17) |
O2 | 44.7(11) | 41.2(12) | 53.7(13) | 10.1(10) | 4.4(9) | -1.7(9) |
C2 | 40.2(15) | 48.3(19) | 50.2(19) | 4.7(15) | 6.9(14) | -2.4(13) |
O3 | 48.8(12) | 53.6(14) | 60.7(15) | 13.3(11) | 17.4(10) | 14.1(10) |
C3 | 43.4(16) | 44.6(18) | 46.3(18) | 8.9(14) | 8.2(13) | -1.8(13) |
O4 | 48.3(12) | 62.7(14) | 47.7(13) | 16.7(11) | 15.2(9) | 15.4(10) |
C4 | 36.6(14) | 40.7(17) | 44.4(17) | 3.9(13) | 12.3(12) | 4.5(12) |
O5 | 63.1(14) | 45.5(13) | 69.2(15) | 10.0(11) | 15.1(12) | 2.8(11) |
C5 | 35.3(13) | 43.6(17) | 36.8(15) | 1.2(13) | 10.7(11) | 0.5(12) |
O6 | 59.3(14) | 84.0(18) | 61.7(15) | 18.3(13) | 26.9(11) | 11.5(12) |
C6 | 47.2(16) | 48.5(18) | 47.9(19) | 6.5(14) | 10.0(14) | -3.0(14) |
C7 | 46.8(17) | 61(2) | 53(2) | -2.8(17) | 2.5(15) | -14.5(15) |
C8 | 38.6(15) | 72(2) | 41.0(17) | 2.3(16) | 8.6(13) | 0.1(15) |
C9 | 51.8(18) | 58(2) | 43.8(18) | 15.2(15) | 9.5(14) | 0.7(16) |
C10 | 46.0(16) | 44.7(18) | 44.6(17) | 5.7(14) | 7.6(13) | -5.4(13) |
C11 | 62(2) | 113(4) | 50(2) | 11(2) | -1.9(17) | -5(2) |
C12 | 63(2) | 73(3) | 81(3) | 0(2) | 33.8(19) | 6.7(18) |
C13 | 51.9(18) | 39.4(17) | 61(2) | -5.3(15) | 20.3(16) | -0.8(14) |
C14 | 55.1(18) | 56(2) | 47.5(19) | 2.8(15) | 15.0(15) | 4.8(15) |
C15 | 46.8(16) | 33.9(16) | 52.4(19) | -0.8(14) | 10.2(14) | -4.6(13) |
C16 | 47.5(16) | 33.5(16) | 50.2(18) | 0.6(13) | 9.8(14) | -5.3(13) |
C17 | 53.4(19) | 68(2) | 54(2) | 1.7(17) | 9.5(16) | -0.2(16) |
C18 | 65(2) | 65(2) | 50(2) | 5.5(17) | -0.5(17) | -3.0(18) |
C19 | 48.6(18) | 58(2) | 60(2) | -1.9(17) | -3.8(16) | 5.3(15) |
C20 | 58(2) | 95(3) | 66(3) | -8(2) | 10.1(19) | 19(2) |
C21 | 55.3(19) | 83(3) | 41.5(18) | 1.4(17) | 5.7(15) | 6.9(18) |
C22 | 66(2) | 106(4) | 88(3) | 0(3) | -15(2) | 30(2) |
C23A | 84(7) | 59(5) | 48(5) | 7(4) | 5(4) | -11(5) |
C23B | 104(9) | 73(7) | 125(11) | 0(8) | 21(9) | -17(6) |
C24A | 68(7) | 90(10) | 123(11) | -17(7) | 24(7) | -12(6) |
C24B | 73(8) | 113(11) | 145(13) | 19(9) | -1(8) | -15(7) |
Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
---|---|---|---|---|---|---|
Ti1 | O1 | 2.060(2) | C6 | C7 | 1.380(4) | |
Ti1 | O2 | 1.9939(19) | C7 | C8 | 1.382(5) | |
Ti1 | O3 | 2.057(2) | C8 | C9 | 1.381(4) | |
Ti1 | O4 | 2.006(2) | C8 | C11 | 1.510(4) | |
Ti1 | O5 | 1.795(2) | C9 | C10 | 1.380(4) | |
Ti1 | O6 | 1.790(2) | C12 | C13 | 1.500(4) | |
O1 | C2 | 1.268(3) | C13 | C14 | 1.393(4) | |
C1 | C2 | 1.498(4) | C14 | C15 | 1.389(4) | |
O2 | C4 | 1.289(3) | C15 | C16 | 1.500(4) | |
C2 | C3 | 1.394(4) | C16 | C17 | 1.377(4) | |
O3 | C13 | 1.253(4) | C16 | C21 | 1.370(4) | |
C3 | C4 | 1.387(4) | C17 | C18 | 1.371(4) | |
O4 | C15 | 1.268(3) | C18 | C19 | 1.372(5) | |
C4 | C5 | 1.491(4) | C19 | C20 | 1.368(5) | |
O5 | C23A | 1.406(9) | C19 | C22 | 1.505(4) | |
O5 | C23B | 1.412(11) | C20 | C21 | 1.399(5) | |
C5 | C6 | 1.391(4) | C23A | C24A | 1.512(13) | |
C5 | C10 | 1.394(4) | C23B | C24B | 1.463(13) | |
O6 | C25A | 1.419(15) | C25A | C26A | 1.489(17) | |
O6 | C25B | 1.405(11) | C25B | C26B | 1.40(2) | |
O6 | C25C | 1.509(12) | C25C | C26C | 1.451(18) |
Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
---|---|---|---|---|---|---|---|---|
O2 | Ti1 | O1 | 82.20(8) | C25B | O6 | Ti1 | 147.0(6) | |
O2 | Ti1 | O3 | 91.95(9) | C25B | O6 | C25A | 38.3(8) | |
O2 | Ti1 | O4 | 169.80(9) | C25B | O6 | C25C | 36.0(6) | |
O3 | Ti1 | O1 | 80.57(9) | C25C | O6 | Ti1 | 124.3(6) | |
O4 | Ti1 | O1 | 88.37(9) | C7 | C6 | C5 | 120.8(3) | |
O4 | Ti1 | O3 | 82.62(8) | C6 | C7 | C8 | 121.5(3) | |
O5 | Ti1 | O1 | 166.64(10) | C7 | C8 | C11 | 121.2(3) | |
O5 | Ti1 | O2 | 90.32(9) | C9 | C8 | C7 | 117.4(3) | |
O5 | Ti1 | O3 | 88.67(10) | C9 | C8 | C11 | 121.4(3) | |
O5 | Ti1 | O4 | 98.15(10) | C10 | C9 | C8 | 122.0(3) | |
O6 | Ti1 | O1 | 89.98(10) | C9 | C10 | C5 | 120.3(3) | |
O6 | Ti1 | O2 | 96.12(10) | O3 | C13 | C12 | 116.2(3) | |
O6 | Ti1 | O3 | 166.65(10) | O3 | C13 | C14 | 124.4(3) | |
O6 | Ti1 | O4 | 87.73(9) | C14 | C13 | C12 | 119.4(3) | |
O6 | Ti1 | O5 | 101.87(11) | C15 | C14 | C13 | 123.4(3) | |
C2 | O1 | Ti1 | 127.93(19) | O4 | C15 | C14 | 122.8(3) | |
C4 | O2 | Ti1 | 129.55(17) | O4 | C15 | C16 | 115.5(3) | |
O1 | C2 | C1 | 116.1(3) | C14 | C15 | C16 | 121.7(3) | |
O1 | C2 | C3 | 123.9(3) | C17 | C16 | C15 | 122.6(3) | |
C3 | C2 | C1 | 119.9(3) | C21 | C16 | C15 | 119.1(3) | |
C13 | O3 | Ti1 | 131.13(19) | C21 | C16 | C17 | 118.3(3) | |
C4 | C3 | C2 | 122.9(3) | C18 | C17 | C16 | 120.2(3) | |
C15 | O4 | Ti1 | 133.90(19) | C17 | C18 | C19 | 122.8(3) | |
O2 | C4 | C3 | 122.5(3) | C18 | C19 | C22 | 121.5(3) | |
O2 | C4 | C5 | 115.6(2) | C20 | C19 | C18 | 116.9(3) | |
C3 | C4 | C5 | 121.8(3) | C20 | C19 | C22 | 121.6(3) | |
C23A | O5 | Ti1 | 141.7(5) | C19 | C20 | C21 | 121.3(3) | |
C23A | O5 | C23B | 34.0(5) | C16 | C21 | C20 | 120.5(3) | |
C23B | O5 | Ti1 | 146.1(6) | O5 | C23A | C24A | 109.6(8) | |
C6 | C5 | C4 | 119.5(3) | O5 | C23B | C24B | 113.6(11) | |
C6 | C5 | C10 | 117.8(3) | O6 | C25A | C26A | 111.3(17) | |
C10 | C5 | C4 | 122.7(2) | C26B | C25B | O6 | 107.3(13) | |
C25A | O6 | Ti1 | 154.3(10) | C26C | C25C | O6 | 106.0(10) | |
C25A | O6 | C25C | 38.9(9) |
A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
---|---|---|---|---|---|---|---|---|---|---|
Ti1 | O1 | C2 | C1 | -166.9(2) | O4 | Ti1 | O6 | C25A | -87.7(19) | |
Ti1 | O1 | C2 | C3 | 16.0(4) | O4 | Ti1 | O6 | C25B | -5.0(10) | |
Ti1 | O2 | C4 | C3 | -22.8(4) | O4 | Ti1 | O6 | C25C | -46.6(7) | |
Ti1 | O2 | C4 | C5 | 158.78(18) | O4 | C15 | C16 | C17 | 168.6(3) | |
Ti1 | O3 | C13 | C12 | -169.4(2) | O4 | C15 | C16 | C21 | -10.8(4) | |
Ti1 | O3 | C13 | C14 | 11.5(5) | C4 | C5 | C6 | C7 | -177.7(3) | |
Ti1 | O4 | C15 | C14 | -6.0(5) | C4 | C5 | C10 | C9 | 178.2(3) | |
Ti1 | O4 | C15 | C16 | 173.91(19) | O5 | Ti1 | O1 | C2 | -86.6(5) | |
Ti1 | O5 | C23A | C24A | -87.2(11) | O5 | Ti1 | O2 | C4 | -157.4(3) | |
Ti1 | O5 | C23B | C24B | 60(2) | O5 | Ti1 | O3 | C13 | 83.9(3) | |
Ti1 | O6 | C25A | C26A | 104(2) | O5 | Ti1 | O4 | C15 | -75.7(3) | |
Ti1 | O6 | C25B | C26B | -91.6(14) | O5 | Ti1 | O6 | C25A | 174.5(19) | |
Ti1 | O6 | C25C | C26C | -173.6(7) | O5 | Ti1 | O6 | C25B | -102.8(10) | |
O1 | Ti1 | O2 | C4 | 33.7(2) | O5 | Ti1 | O6 | C25C | -144.5(7) | |
O1 | Ti1 | O3 | C13 | -104.1(3) | C5 | C6 | C7 | C8 | -0.4(5) | |
O1 | Ti1 | O4 | C15 | 92.6(3) | O6 | Ti1 | O1 | C2 | 66.1(3) | |
O1 | Ti1 | O5 | C23A | 33.9(8) | O6 | Ti1 | O2 | C4 | -55.4(3) | |
O1 | Ti1 | O5 | C23B | -25.1(12) | O6 | Ti1 | O3 | C13 | -58.5(6) | |
O1 | Ti1 | O6 | C25A | 0.7(19) | O6 | Ti1 | O4 | C15 | -177.3(3) | |
O1 | Ti1 | O6 | C25B | 83.4(10) | O6 | Ti1 | O5 | C23A | -118.2(6) | |
O1 | Ti1 | O6 | C25C | 41.8(7) | O6 | Ti1 | O5 | C23B | -177.2(11) | |
O1 | C2 | C3 | C4 | 10.1(5) | C6 | C5 | C10 | C9 | -1.5(4) | |
C1 | C2 | C3 | C4 | -166.9(3) | C6 | C7 | C8 | C9 | -1.6(5) | |
O2 | Ti1 | O1 | C2 | -30.1(2) | C6 | C7 | C8 | C11 | 176.0(3) | |
O2 | Ti1 | O3 | C13 | 174.2(3) | C7 | C8 | C9 | C10 | 2.1(5) | |
O2 | Ti1 | O4 | C15 | 70.2(6) | C8 | C9 | C10 | C5 | -0.6(5) | |
O2 | Ti1 | O5 | C23A | -21.9(6) | C10 | C5 | C6 | C7 | 2.0(4) | |
O2 | Ti1 | O5 | C23B | -80.8(11) | C11 | C8 | C9 | C10 | -175.5(3) | |
O2 | Ti1 | O6 | C25A | 82.8(19) | C12 | C13 | C14 | C15 | -178.1(3) | |
O2 | Ti1 | O6 | C25B | 165.6(10) | C13 | C14 | C15 | O4 | -4.0(5) | |
O2 | Ti1 | O6 | C25C | 123.9(7) | C13 | C14 | C15 | C16 | 176.1(3) | |
O2 | C4 | C5 | C6 | -6.6(4) | C14 | C15 | C16 | C17 | -11.5(4) | |
O2 | C4 | C5 | C10 | 173.7(3) | C14 | C15 | C16 | C21 | 169.1(3) | |
C2 | C3 | C4 | O2 | -7.3(5) | C15 | C16 | C17 | C18 | -178.5(3) | |
C2 | C3 | C4 | C5 | 171.0(3) | C15 | C16 | C21 | C20 | -179.9(3) | |
O3 | Ti1 | O1 | C2 | -123.4(3) | C16 | C17 | C18 | C19 | -1.1(6) | |
O3 | Ti1 | O2 | C4 | 113.9(3) | C17 | C16 | C21 | C20 | 0.6(5) | |
O3 | Ti1 | O4 | C15 | 11.9(3) | C17 | C18 | C19 | C20 | -0.4(6) | |
O3 | Ti1 | O5 | C23A | 70.1(6) | C17 | C18 | C19 | C22 | -179.8(4) | |
O3 | Ti1 | O5 | C23B | 11.1(11) | C18 | C19 | C20 | C21 | 2.1(6) | |
O3 | Ti1 | O6 | C25A | -44.0(19) | C19 | C20 | C21 | C16 | -2.2(6) | |
O3 | Ti1 | O6 | C25B | 38.7(12) | C21 | C16 | C17 | C18 | 1.0(5) | |
O3 | Ti1 | O6 | C25C | -3.0(9) | C22 | C19 | C20 | C21 | -178.6(4) | |
O3 | C13 | C14 | C15 | 1.0(5) | C23A | O5 | C23B | C24B | -47.7(13) | |
C3 | C4 | C5 | C6 | 175.0(3) | C23B | O5 | C23A | C24A | 34.0(11) | |
C3 | C4 | C5 | C10 | -4.7(4) | C25A | O6 | C25B | C26B | 44.4(19) | |
O4 | Ti1 | O1 | C2 | 153.8(3) | C25A | O6 | C25C | C26C | -20.6(15) | |
O4 | Ti1 | O2 | C4 | 56.4(6) | C25B | O6 | C25A | C26A | -15.3(15) | |
O4 | Ti1 | O3 | C13 | -14.5(3) | C25B | O6 | C25C | C26C | 44.5(12) | |
O4 | Ti1 | O5 | C23A | 152.4(6) | C25C | O6 | C25A | C26A | 44.0(17) | |
O4 | Ti1 | O5 | C23B | 93.5(11) | C25C | O6 | C25B | C26B | -22.5(13) |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
H1A | 7478 | 2894 | 4604 | 99 |
H1B | 7723 | 2997 | 3131 | 99 |
H1C | 8762 | 2652 | 4123 | 99 |
H3 | 6044 | 2602 | 1493 | 54 |
H6 | 2905 | 1385 | 468 | 57 |
H7 | 1217 | 1466 | -1488 | 66 |
H9 | 2562 | 2836 | -2013 | 62 |
H10 | 4282 | 2760 | -80 | 54 |
H11A | 1146 | 2272 | -4041 | 115 |
H11B | 3 | 2454 | -3252 | 115 |
H11C | 179 | 1884 | -3509 | 115 |
H12A | 4554 | 1671 | 7511 | 104 |
H12B | 4679 | 1123 | 8058 | 104 |
H12C | 3600 | 1253 | 6713 | 104 |
H14 | 6951 | 883 | 7962 | 63 |
H17 | 9010 | 709 | 9046 | 70 |
H18 | 11118 | 376 | 10079 | 74 |
H20 | 12114 | 144 | 6497 | 88 |
H21 | 10026 | 515 | 5431 | 73 |
H22A | 14000 | 210 | 8959 | 137 |
H22B | 13331 | -323 | 8766 | 137 |
H22C | 13269 | -15 | 10080 | 137 |
H23A | 4003 | 149 | 2445 | 78 |
H23B | 3472 | 697 | 2130 | 78 |
H23C | 4414 | 296 | 4587 | 121 |
H23D | 4165 | 58 | 3130 | 121 |
H24D | 3700 | 242 | 4706 | 140 |
H24E | 2269 | 321 | 3675 | 140 |
H24F | 3123 | 782 | 4357 | 140 |
H24A | 2910 | 939 | 3706 | 171 |
H24B | 2152 | 421 | 3550 | 171 |
H24C | 2608 | 668 | 2291 | 171 |
H25E | 8680 | 1685 | 1922 | 92 |
H25F | 8367 | 1239 | 894 | 92 |
H25A | 9349 | 821 | 3090 | 105 |
H25B | 8904 | 894 | 1501 | 105 |
H25C | 9066 | 1692 | 3072 | 108 |
H25D | 9584 | 1155 | 3577 | 108 |
H26G | 10230 | 1185 | 3426 | 135 |
H26H | 10700 | 1224 | 2024 | 135 |
H26I | 9930 | 745 | 2380 | 135 |
H26A | 9221 | 1719 | 1766 | 202 |
H26B | 10610 | 1436 | 2412 | 202 |
H26C | 9645 | 1650 | 3351 | 202 |
H26D | 8989 | 1444 | 853 | 134 |
H26E | 9556 | 919 | 1381 | 134 |
H26F | 10515 | 1390 | 1729 | 134 |
Atom | Occupancy | Atom | Occupancy | Atom | Occupancy | ||
---|---|---|---|---|---|---|---|
C23A | 0.50 | H23A | 0.50 | H23B | 0.50 | ||
C23B | 0.50 | H23C | 0.50 | H23D | 0.50 | ||
C24A | 0.50 | H24D | 0.50 | H24E | 0.50 | ||
H24F | 0.50 | C24B | 0.50 | H24A | 0.50 | ||
H24B | 0.50 | H24C | 0.50 | C25A | 0.20 | ||
H25E | 0.20 | H25F | 0.20 | C25B | 0.40 | ||
H25A | 0.40 | H25B | 0.40 | C25C | 0.40 | ||
H25C | 0.40 | H25D | 0.40 | C26A | 0.20 | ||
H26G | 0.20 | H26H | 0.20 | H26I | 0.20 | ||
C26B | 0.40 | H26A | 0.40 | H26B | 0.40 | ||
H26C | 0.40 | C26C | 0.40 | H26D | 0.40 | ||
H26E | 0.40 | H26F | 0.40 |