dc150

Table 1 Crystal data and structure refinement for dc150.
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

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for dc150. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Ti16966.8(4)7776.6(3)8486.6(2)20.17(12)
O25585.9(16)7725.2(10)7333.7(9)23.6(3)
C103530(2)7635.1(14)6069.2(13)20.5(4)
O35711.1(16)6887.3(10)8607.1(9)24.2(3)
C268461(2)7550.2(15)11612.4(13)22.8(4)
C225600(2)6671.9(13)9187.7(13)20.0(4)
C94273(2)7929.0(13)6908.1(12)19.5(4)
C258737(2)7669.6(13)11006.6(12)18.8(4)
O68033.9(17)8661.4(10)8530.4(10)27.8(4)
O47934.2(16)7818.3(10)9660.5(9)23.0(3)
O57964.9(17)6904.3(10)8413.6(9)25.2(3)
O15474.1(16)8583.8(10)8479.6(9)23.6(3)
C279485(3)7743.9(15)12386.9(14)27.8(5)
C63321(2)9232.0(13)8182.2(13)20.6(4)
C112169(2)7908.6(16)5506.9(14)26.4(5)
C236494(2)6980.9(14)9958.1(13)22.0(4)
C214514(2)6015.7(14)9047.4(13)21.7(4)
C3010061(2)7984.9(14)11191.6(13)22.5(4)
C2810790(3)8057.6(16)12559.6(14)30.3(5)
C203892(2)5975.0(14)9502.9(14)25.3(5)
C83538(2)8382.0(15)7188.1(13)26.2(5)
C247666(2)7494.1(13)10165.5(12)18.4(4)
C74182(2)8703.2(13)7958.4(13)20.3(4)
C121485(3)7591.9(17)4747.6(14)30.9(5)
C2911086(2)8172.6(15)11967.8(14)27.5(5)
C51858(2)9153.7(14)7800.7(14)25.2(5)
C14006(3)9818.3(14)8799.0(14)25.6(5)
C154207(3)7045.6(15)5849.7(14)28.9(5)
C23229(3)10310.8(15)9018.7(15)30.0(5)
C31774(3)10220.1(15)8641.8(15)29.1(5)
C41086(2)9640.3(15)8031.5(15)27.6(5)
C164124(3)5424.8(15)8444.3(14)28.5(5)
C132162(3)7003.1(17)4538.2(15)35.1(6)
C182516(3)4765.8(16)8759.6(16)33.2(6)
C143522(3)6736.7(17)5082.1(15)38.3(6)
C192887(3)5356.5(16)9355.2(15)31.8(5)
C173131(3)4795.1(16)8305.0(15)35.1(6)
C317781(3)6023.2(17)8240.6(17)39.5(6)
C338752(3)9392(2)8978(2)49.4(8)
C347829(4)10054(2)8989(2)61.3(10)
C328554(5)5513(2)8986(2)75.0(13)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for dc150. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U12U13U23
Ti115.53(19)30.8(2)12.5(2)-1.48(14)6.05(15)-0.62(14)
O218.4(8)37.3(9)13.0(8)2.0(6)6.6(6)-0.3(6)
C1019.4(10)28.8(11)13.4(10)-2.5(8)8.6(9)-1.0(8)
O320.8(8)33.8(8)15.2(8)-6.4(6)7.4(7)-2.9(6)
C2620.8(10)29.9(11)16.9(11)-0.3(8)9.2(9)-2.6(8)
C2215.0(9)25.4(10)16.8(10)-0.2(8)6.2(8)0.1(8)
C919.2(10)26.5(10)12.8(10)-3.2(8)8.2(8)-0.0(8)
C2517.4(10)23.5(10)12.6(10)0.8(8)5.7(8)-2.7(7)
O625.6(8)34.7(9)23.9(9)-5.9(7)13.4(7)-1.6(7)
O417.8(8)34.7(8)13.7(7)-4.7(6)6.3(6)-1.4(6)
O520.9(8)32.9(8)18.7(8)1.3(6)8.2(7)-1.1(6)
O119.4(8)34.8(8)14.0(8)-0.6(6)6.7(6)-3.4(6)
C2730.0(13)35.7(12)14.7(11)3.4(10)9.6(10)-1.4(9)
C622.4(11)24.3(10)15.8(10)-0.3(8)10.3(9)1.3(8)
C1121.0(11)40.5(13)16.4(11)1.7(9)8.8(9)-1.8(9)
C2319.3(10)31.0(11)14.3(10)-4.7(8)7.7(9)-1.5(8)
C2115.6(9)26.2(10)15.6(10)-1.1(8)2.6(8)1.2(8)
C3017.7(10)29.5(11)17.7(11)-2.1(8)7.2(9)-5.5(8)
C2825.6(12)38.4(13)15.9(11)0.3(10)2.9(10)-6.8(9)
C2019.7(10)28.9(11)22.3(12)-1.3(8)7.2(9)0.2(9)
C818.3(10)40.4(13)15.5(11)2.0(9)5.6(9)-4.6(9)
C2416.1(10)23.2(9)13.1(10)2.6(7)5.6(8)-0.8(7)
C720.8(10)25.8(10)16(1)-2.1(8)10.6(9)-0.5(8)
C1221.7(12)46.9(14)15.3(11)-1.6(10)3.4(10)-0.2(10)
C2917.6(11)35.9(12)22.3(12)-3.2(9)5.4(9)-6.1(9)
C524.2(11)29.1(11)21.2(11)-1.5(9)11(1)-2.0(9)
C124.9(11)29.3(11)22.1(12)-3.2(9)11.8(10)-3.5(9)
C1528.0(13)35.2(12)17.5(11)6.7(9)7.5(10)-1.7(9)
C233.6(13)30.1(12)26.9(13)-1.7(10)16.1(11)-5.4(10)
C332.2(13)28.5(12)30.8(13)6.1(9)19.3(11)0.9(10)
C421.4(11)34.5(12)26.6(13)3.4(9)12.3(10)0.5(10)
C1625.0(12)34.7(12)19.6(12)-3.6(9)7.2(10)-2.8(9)
C1340.9(15)39.4(13)16.0(12)-4.1(11)8.3(11)-8.1(10)
C1825.5(12)29.7(12)29.7(13)-8.8(9)3.8(11)4.4(10)
C1445.1(16)39.3(14)22.5(13)10.6(12)11.9(12)-5.9(10)
C1924.6(12)37.0(13)29.6(14)-3.6(10)11.0(11)7.3(10)
C1730.9(14)32.8(13)26.3(13)-8.2(10)4.0(11)-5.5(10)
C3143.7(16)38.2(14)41.7(17)-4.6(12)25.6(14)-11.5(12)
C3335.3(16)52.1(17)57(2)-20.8(13)21.5(15)-22.4(15)
C3445.7(19)47.2(18)78(3)-16.7(15)22.9(19)-25.6(18)
C32106(4)34.6(16)72(3)5.3(19)37(3)11.0(17)

 

Table 4 Bond Lengths for dc150.
AtomAtomLength/Å AtomAtomLength/Å
Ti1O22.0194(16) C6C71.514(3)
Ti1O32.0960(16) C6C51.413(3)
Ti1O61.8189(16) C6C11.419(3)
Ti1O42.0293(16) C11C121.402(3)
Ti1O51.8349(17) C23C241.414(3)
Ti1O12.1036(16) C21C201.412(3)
O2C91.305(3) C21C161.414(3)
C10C91.520(3) C30C291.413(3)
C10C111.420(3) C28C291.404(4)
C10C151.413(3) C20C191.407(3)
O3C221.284(3) C8C71.425(3)
C26C251.417(3) C12C131.400(4)
C26C271.412(3) C5C41.407(3)
C22C231.430(3) C1C21.402(3)
C22C211.516(3) C15C141.412(3)
C9C81.413(3) C2C31.408(3)
C25C301.423(3) C3C41.405(3)
C25C241.512(3) C16C171.413(3)
O6C331.435(3) C13C141.407(4)
O4C241.306(3) C18C191.406(4)
O5C311.431(3) C18C171.403(4)
O1C71.290(3) C31C321.521(5)
C27C281.410(4) C33C341.485(5)

 

Table 5 Bond Angles for dc150.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
O3Ti1O286.77(6) C5C6C7122.01(19)
O6Ti1O2100.46(7) C1C6C7119.00(19)
O6Ti1O3168.62(7) C1C6C5119.0(2)
O4Ti1O2166.17(7) C12C11C10121.1(2)
O4Ti1O382.75(6) C24C23C22122.8(2)
O4Ti1O688.63(7) C20C21C22122.0(2)
O5Ti1O290.84(7) C16C21C22118.6(2)
O5Ti1O388.55(7) C16C21C20119.4(2)
O5Ti1O6100.01(8) C29C30C25120.4(2)
O5Ti1O497.87(7) C29C28C27120.5(2)
O1Ti1O283.22(6) C19C20C21120.4(2)
O1Ti1O380.28(7) C7C8C9123.0(2)
O1Ti1O691.78(7) O4C24C25115.47(18)
O1Ti1O486.12(6) C23C24C25121.07(19)
O1Ti1O5167.61(7) C23C24O4123.4(2)
C9O2Ti1132.81(14) C6C7O1117.44(18)
C11C10C9122.5(2) C8C7O1123.9(2)
C15C10C9118.5(2) C8C7C6118.69(19)
C15C10C11118.9(2) C13C12C11119.5(2)
C22O3Ti1132.23(14) C28C29C30119.8(2)
C27C26C25120.4(2) C4C5C6120.8(2)
C23C22O3123.52(19) C2C1C6119.9(2)
C21C22O3117.43(19) C14C15C10119.8(2)
C21C22C23118.94(19) C3C2C1120.6(2)
C10C9O2115.96(18) C4C3C2119.9(2)
C8C9O2123.9(2) C3C4C5119.7(2)
C8C9C10120.1(2) C17C16C21120.2(2)
C30C25C26119.0(2) C14C13C12120.4(2)
C24C25C26122.62(19) C17C18C19120.4(2)
C24C25C30118.39(19) C13C14C15120.4(2)
C33O6Ti1142.92(18) C18C19C20119.9(2)
C24O4Ti1133.97(14) C18C17C16119.8(2)
C31O5Ti1137.82(16) C32C31O5110.1(2)
C7O1Ti1130.59(14) C34C33O6114.4(2)
C28C27C26119.9(2)     

 

Table 6 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for dc150.
AtomxyzU(eq)
H267582(2)7338.4(15)11496.6(13)27.3(5)
H279295(3)7663.0(15)12790.6(14)33.3(6)
H111714(2)8312.9(16)5647.3(14)31.7(6)
H236293(2)6835.1(14)10347.3(13)26.4(5)
H3010257(2)8069.6(14)10790.5(13)27.1(5)
H2811475(3)8192.4(16)13080.3(14)36.4(6)
H204154(2)6367.6(14)9911.6(14)30.4(6)
H82570(2)8476.7(15)6847.1(13)31.4(6)
H12570(3)7775.4(17)4378.4(14)37.1(6)
H2911973(2)8375.9(15)12089.0(14)33.0(6)
H51390(2)8767.7(14)7383.1(14)30.2(6)
H14989(3)9877.0(14)9062.8(14)30.8(6)
H155120(3)6857.7(15)6217.4(14)34.6(6)
H23690(3)10709.5(15)9425.9(15)35.9(6)
H31258(3)10550.2(15)8799.8(15)34.9(6)
H4105(2)9577.1(15)7775.6(15)33.1(6)
H164530(3)5451.1(15)8131.8(14)34.2(6)
H131700(3)6782.4(17)4026.1(15)42.2(7)
H181845(3)4344.3(16)8664.3(16)39.9(7)
H143982(3)6346.8(17)4931.9(15)46.0(8)
H192460(3)5338.0(16)9657.4(15)38.1(7)
H172881(3)4392.9(16)7904.8(15)42.1(7)
H31a6777(3)5882.6(17)7965.0(17)47.5(8)
H31b8139(3)5879.5(17)7897.0(17)47.5(8)
H33a9418(3)9215(2)9518(2)59.3(10)
H33b9298(3)9638(2)8766(2)59.3(10)
H34a7100(18)10191(13)8456(2)91.9(15)
H34b7400(20)9849(7)9276(14)91.9(15)
H34c8377(7)10560(6)9243(15)91.9(15)
H32a9549(7)5649(15)9254(10)112.5(19)
H32b8190(20)5651(15)9322(8)112.5(19)
H32c8420(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.

  1. Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341.

Crystal structure determination of [dc150]

Crystal Data for C34H32O6Ti (=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)°, = 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)

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