DC104_Mo_250

Table 1 Crystal data and structure refinement for DC104_Mo_250.
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

 

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for DC104_Mo_250. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
Ti16329.2(6)1221.7(2)3632.7(6)50.0(2)
O17040(2)1935.2(8)4102(2)54.0(6)
C17798(4)2753.2(14)3841(4)66(1)
O24844(2)1580.1(7)2314(2)47.3(5)
C26912(3)2310.7(12)3320(3)46.5(7)
O35344(2)1365.1(8)5223(2)53.5(6)
C35971(3)2336.9(11)2069(3)44.9(7)
O47867(2)976.1(8)5140(2)52.2(5)
C44929(3)1984.9(11)1646(3)40.0(7)
O55340(2)654.7(8)3320(2)59.1(6)
C53810(3)2058.1(11)401(3)38.1(6)
O67532(2)1158.8(9)2510(2)66.2(7)
C62856(3)1677.1(12)-37(3)47.8(7)
C71838(3)1726.9(13)-1212(3)54.6(8)
C81721(3)2155.8(13)-1988(3)50.3(8)
C92641(3)2539.1(13)-1525(3)51.4(8)
C103674(3)2495.9(11)-359(3)45.3(7)
C11666(4)2194.7(17)-3319(3)76.9(12)
C124513(4)1326.7(14)7253(4)69.6(10)
C135613(3)1221.2(11)6438(4)49.6(8)
C146850(3)981.2(12)7058(3)52.3(8)
C157941(3)881.1(11)6393(3)44.3(7)
C169293(3)650.6(11)7121(3)43.8(7)
C179637(3)603.1(13)8518(3)58.5(9)
C1810902(4)399.5(13)9133(4)61.6(9)
C1911862(3)228.5(13)8412(4)57.8(9)
C2011503(4)265.6(16)7022(4)73.3(11)
C2110233(3)483.5(14)6375(3)60.5(9)
C2213240(4)5.0(18)9118(4)91.4(14)
C23A3967(10)477(4)2837(9)65(3)
C23B4218(11)371(4)3620(17)101(4)
C24A3194(15)453(5)4000(12)93(4)
C24B2855(13)621(6)3261(18)114(5)
C25A8609(17)1326(9)1850(20)77(6)
C25B8911(12)1048(5)2377(15)87(3)
C25C9032(12)1342(6)2827(14)90(4)
C26A9990(20)1100(10)2480(30)90(7)
C26B9655(19)1499(7)2480(20)135(6)
C26C9568(13)1268(5)1593(13)90(3)

 

Table 3 Anisotropic Displacement Parameters (Å2×103) for DC104_Mo_250. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+2hka*b*U12+…].
AtomU11U22U33U23U13U12
Ti147.0(3)48.0(4)54.6(4)12.7(3)9.2(3)7.6(3)
O151.3(12)54.8(14)50.3(13)9.8(11)-2.6(10)-1.3(10)
C163(2)62(2)65(2)3.6(18)-5.9(17)-14.5(17)
O244.7(11)41.2(12)53.7(13)10.1(10)4.4(9)-1.7(9)
C240.2(15)48.3(19)50.2(19)4.7(15)6.9(14)-2.4(13)
O348.8(12)53.6(14)60.7(15)13.3(11)17.4(10)14.1(10)
C343.4(16)44.6(18)46.3(18)8.9(14)8.2(13)-1.8(13)
O448.3(12)62.7(14)47.7(13)16.7(11)15.2(9)15.4(10)
C436.6(14)40.7(17)44.4(17)3.9(13)12.3(12)4.5(12)
O563.1(14)45.5(13)69.2(15)10.0(11)15.1(12)2.8(11)
C535.3(13)43.6(17)36.8(15)1.2(13)10.7(11)0.5(12)
O659.3(14)84.0(18)61.7(15)18.3(13)26.9(11)11.5(12)
C647.2(16)48.5(18)47.9(19)6.5(14)10.0(14)-3.0(14)
C746.8(17)61(2)53(2)-2.8(17)2.5(15)-14.5(15)
C838.6(15)72(2)41.0(17)2.3(16)8.6(13)0.1(15)
C951.8(18)58(2)43.8(18)15.2(15)9.5(14)0.7(16)
C1046.0(16)44.7(18)44.6(17)5.7(14)7.6(13)-5.4(13)
C1162(2)113(4)50(2)11(2)-1.9(17)-5(2)
C1263(2)73(3)81(3)0(2)33.8(19)6.7(18)
C1351.9(18)39.4(17)61(2)-5.3(15)20.3(16)-0.8(14)
C1455.1(18)56(2)47.5(19)2.8(15)15.0(15)4.8(15)
C1546.8(16)33.9(16)52.4(19)-0.8(14)10.2(14)-4.6(13)
C1647.5(16)33.5(16)50.2(18)0.6(13)9.8(14)-5.3(13)
C1753.4(19)68(2)54(2)1.7(17)9.5(16)-0.2(16)
C1865(2)65(2)50(2)5.5(17)-0.5(17)-3.0(18)
C1948.6(18)58(2)60(2)-1.9(17)-3.8(16)5.3(15)
C2058(2)95(3)66(3)-8(2)10.1(19)19(2)
C2155.3(19)83(3)41.5(18)1.4(17)5.7(15)6.9(18)
C2266(2)106(4)88(3)0(3)-15(2)30(2)
C23A84(7)59(5)48(5)7(4)5(4)-11(5)
C23B104(9)73(7)125(11)0(8)21(9)-17(6)
C24A68(7)90(10)123(11)-17(7)24(7)-12(6)
C24B73(8)113(11)145(13)19(9)-1(8)-15(7)

 

Table 4 Bond Lengths for DC104_Mo_250.
AtomAtomLength/Å AtomAtomLength/Å
Ti1O12.060(2) C6C71.380(4)
Ti1O21.9939(19) C7C81.382(5)
Ti1O32.057(2) C8C91.381(4)
Ti1O42.006(2) C8C111.510(4)
Ti1O51.795(2) C9C101.380(4)
Ti1O61.790(2) C12C131.500(4)
O1C21.268(3) C13C141.393(4)
C1C21.498(4) C14C151.389(4)
O2C41.289(3) C15C161.500(4)
C2C31.394(4) C16C171.377(4)
O3C131.253(4) C16C211.370(4)
C3C41.387(4) C17C181.371(4)
O4C151.268(3) C18C191.372(5)
C4C51.491(4) C19C201.368(5)
O5C23A1.406(9) C19C221.505(4)
O5C23B1.412(11) C20C211.399(5)
C5C61.391(4) C23AC24A1.512(13)
C5C101.394(4) C23BC24B1.463(13)
O6C25A1.419(15) C25AC26A1.489(17)
O6C25B1.405(11) C25BC26B1.40(2)
O6C25C1.509(12) C25CC26C1.451(18)

 

Table 5 Bond Angles for DC104_Mo_250.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
O2Ti1O182.20(8) C25BO6Ti1147.0(6)
O2Ti1O391.95(9) C25BO6C25A38.3(8)
O2Ti1O4169.80(9) C25BO6C25C36.0(6)
O3Ti1O180.57(9) C25CO6Ti1124.3(6)
O4Ti1O188.37(9) C7C6C5120.8(3)
O4Ti1O382.62(8) C6C7C8121.5(3)
O5Ti1O1166.64(10) C7C8C11121.2(3)
O5Ti1O290.32(9) C9C8C7117.4(3)
O5Ti1O388.67(10) C9C8C11121.4(3)
O5Ti1O498.15(10) C10C9C8122.0(3)
O6Ti1O189.98(10) C9C10C5120.3(3)
O6Ti1O296.12(10) O3C13C12116.2(3)
O6Ti1O3166.65(10) O3C13C14124.4(3)
O6Ti1O487.73(9) C14C13C12119.4(3)
O6Ti1O5101.87(11) C15C14C13123.4(3)
C2O1Ti1127.93(19) O4C15C14122.8(3)
C4O2Ti1129.55(17) O4C15C16115.5(3)
O1C2C1116.1(3) C14C15C16121.7(3)
O1C2C3123.9(3) C17C16C15122.6(3)
C3C2C1119.9(3) C21C16C15119.1(3)
C13O3Ti1131.13(19) C21C16C17118.3(3)
C4C3C2122.9(3) C18C17C16120.2(3)
C15O4Ti1133.90(19) C17C18C19122.8(3)
O2C4C3122.5(3) C18C19C22121.5(3)
O2C4C5115.6(2) C20C19C18116.9(3)
C3C4C5121.8(3) C20C19C22121.6(3)
C23AO5Ti1141.7(5) C19C20C21121.3(3)
C23AO5C23B34.0(5) C16C21C20120.5(3)
C23BO5Ti1146.1(6) O5C23AC24A109.6(8)
C6C5C4119.5(3) O5C23BC24B113.6(11)
C6C5C10117.8(3) O6C25AC26A111.3(17)
C10C5C4122.7(2) C26BC25BO6107.3(13)
C25AO6Ti1154.3(10) C26CC25CO6106.0(10)
C25AO6C25C38.9(9)     

 

Table 6 Torsion Angles for DC104_Mo_250.
ABCDAngle/˚ ABCDAngle/˚
Ti1O1C2C1-166.9(2) O4Ti1O6C25A-87.7(19)
Ti1O1C2C316.0(4) O4Ti1O6C25B-5.0(10)
Ti1O2C4C3-22.8(4) O4Ti1O6C25C-46.6(7)
Ti1O2C4C5158.78(18) O4C15C16C17168.6(3)
Ti1O3C13C12-169.4(2) O4C15C16C21-10.8(4)
Ti1O3C13C1411.5(5) C4C5C6C7-177.7(3)
Ti1O4C15C14-6.0(5) C4C5C10C9178.2(3)
Ti1O4C15C16173.91(19) O5Ti1O1C2-86.6(5)
Ti1O5C23AC24A-87.2(11) O5Ti1O2C4-157.4(3)
Ti1O5C23BC24B60(2) O5Ti1O3C1383.9(3)
Ti1O6C25AC26A104(2) O5Ti1O4C15-75.7(3)
Ti1O6C25BC26B-91.6(14) O5Ti1O6C25A174.5(19)
Ti1O6C25CC26C-173.6(7) O5Ti1O6C25B-102.8(10)
O1Ti1O2C433.7(2) O5Ti1O6C25C-144.5(7)
O1Ti1O3C13-104.1(3) C5C6C7C8-0.4(5)
O1Ti1O4C1592.6(3) O6Ti1O1C266.1(3)
O1Ti1O5C23A33.9(8) O6Ti1O2C4-55.4(3)
O1Ti1O5C23B-25.1(12) O6Ti1O3C13-58.5(6)
O1Ti1O6C25A0.7(19) O6Ti1O4C15-177.3(3)
O1Ti1O6C25B83.4(10) O6Ti1O5C23A-118.2(6)
O1Ti1O6C25C41.8(7) O6Ti1O5C23B-177.2(11)
O1C2C3C410.1(5) C6C5C10C9-1.5(4)
C1C2C3C4-166.9(3) C6C7C8C9-1.6(5)
O2Ti1O1C2-30.1(2) C6C7C8C11176.0(3)
O2Ti1O3C13174.2(3) C7C8C9C102.1(5)
O2Ti1O4C1570.2(6) C8C9C10C5-0.6(5)
O2Ti1O5C23A-21.9(6) C10C5C6C72.0(4)
O2Ti1O5C23B-80.8(11) C11C8C9C10-175.5(3)
O2Ti1O6C25A82.8(19) C12C13C14C15-178.1(3)
O2Ti1O6C25B165.6(10) C13C14C15O4-4.0(5)
O2Ti1O6C25C123.9(7) C13C14C15C16176.1(3)
O2C4C5C6-6.6(4) C14C15C16C17-11.5(4)
O2C4C5C10173.7(3) C14C15C16C21169.1(3)
C2C3C4O2-7.3(5) C15C16C17C18-178.5(3)
C2C3C4C5171.0(3) C15C16C21C20-179.9(3)
O3Ti1O1C2-123.4(3) C16C17C18C19-1.1(6)
O3Ti1O2C4113.9(3) C17C16C21C200.6(5)
O3Ti1O4C1511.9(3) C17C18C19C20-0.4(6)
O3Ti1O5C23A70.1(6) C17C18C19C22-179.8(4)
O3Ti1O5C23B11.1(11) C18C19C20C212.1(6)
O3Ti1O6C25A-44.0(19) C19C20C21C16-2.2(6)
O3Ti1O6C25B38.7(12) C21C16C17C181.0(5)
O3Ti1O6C25C-3.0(9) C22C19C20C21-178.6(4)
O3C13C14C151.0(5) C23AO5C23BC24B-47.7(13)
C3C4C5C6175.0(3) C23BO5C23AC24A34.0(11)
C3C4C5C10-4.7(4) C25AO6C25BC26B44.4(19)
O4Ti1O1C2153.8(3) C25AO6C25CC26C-20.6(15)
O4Ti1O2C456.4(6) C25BO6C25AC26A-15.3(15)
O4Ti1O3C13-14.5(3) C25BO6C25CC26C44.5(12)
O4Ti1O5C23A152.4(6) C25CO6C25AC26A44.0(17)
O4Ti1O5C23B93.5(11) C25CO6C25BC26B-22.5(13)

 

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for DC104_Mo_250.
AtomxyzU(eq)
H1A74782894460499
H1B77232997313199
H1C87622652412399
H360442602149354
H62905138546857
H712171466-148866
H925622836-201362
H1042822760-8054
H11A11462272-4041115
H11B32454-3252115
H11C1791884-3509115
H12A455416717511104
H12B467911238058104
H12C360012536713104
H146951883796263
H179010709904670
H18111183761007974
H2012114144649788
H2110026515543173
H22A140002108959137
H22B13331-3238766137
H22C13269-1510080137
H23A4003149244578
H23B3472697213078
H23C44142964587121
H23D4165583130121
H24D37002424706140
H24E22693213675140
H24F31237824357140
H24A29109393706171
H24B21524213550171
H24C26086682291171
H25E86801685192292
H25F8367123989492
H25A93498213090105
H25B89048941501105
H25C906616923072108
H25D958411553577108
H26G1023011853426135
H26H1070012242024135
H26I99307452380135
H26A922117191766202
H26B1061014362412202
H26C964516503351202
H26D89891444853134
H26E95569191381134
H26F1051513901729134

 

Table 8 Atomic Occupancy for DC104_Mo_250.
AtomOccupancy AtomOccupancy AtomOccupancy
C23A0.50 H23A0.50 H23B0.50
C23B0.50 H23C0.50 H23D0.50
C24A0.50 H24D0.50 H24E0.50
H24F0.50 C24B0.50 H24A0.50
H24B0.50 H24C0.50 C25A0.20
H25E0.20 H25F0.20 C25B0.40
H25A0.40 H25B0.40 C25C0.40
H25C0.40 H25D0.40 C26A0.20
H26G0.20 H26H0.20 H26I0.20
C26B0.40 H26A0.40 H26B0.40
H26C0.40 C26C0.40 H26D0.40
H26E0.40 H26F0.40