phw1113

Crystal Submitted by:
Luisa Ciano
Crystal Submitted on:
11/07/2011
Data Collected on:
29/07/2011
Structure Solved by:
Jason Lynam

Table 1: Crystal data and structure refinement for phw1113
Identification code phw1113
Empirical formula C30H33N3O3
Formula weight 483.59
Temperature / K 110.0
Crystal system orthorhombic
Space group Pna21
a / Å, b / Å, c / Å 18.3543(12), 16.464(11), 8.6727(9)
α/°, β/°, γ/° 90.00, 90.00, 90.00
Volume / Å3 2620.8(19)
Z 4
ρcalc / mg mm-3 1.226
μ / mm‑1 0.080
F(000) 1032
Crystal size / mm3 0.1749 × 0.1688 × 0.0631
2Θ range for data collection 5.76 to 57.98°
Index ranges -14 ≤ h ≤ 24, -13 ≤ k ≤ 22, -11 ≤ l ≤ 11
Reflections collected 10192
Independent reflections 5801[R(int) = 0.0197]
Data/restraints/parameters 5801/1/337
Goodness-of-fit on F2 1.061
Final R indexes [I>2σ (I)] R1 = 0.0422, wR2 = 0.0983
Final R indexes [all data] R1 = 0.0511, wR2 = 0.1034
Largest diff. peak/hole / e Å-3 0.171/-0.183

Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for phw1113. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
AtomxyzU(eq)
C1-4683.3(11)-6658.4(12)-266(2)26.0(4)
C2-4561.7(11)-7111.7(12)-1781(2)26.7(4)
C3-4748.1(11)-8018.0(12)-1582(2)26.9(4)
C4-5526.4(10)-8134.1(13)-976(2)27.8(4)
C5-5650.4(11)-7654.7(12)508(2)26.5(4)
C6-5471.3(11)-6757.8(12)259(2)26.9(4)
C7-4082.9(10)-5456.7(12)450(2)24.4(4)
C8-3940.8(10)-4582.3(12)414(2)25.2(4)
C9-4335.8(11)-4072.8(12)-580(2)25.8(4)
C10-4197.8(12)-3237.0(13)-557(2)31.3(5)
C11-3658.6(12)-2925.1(12)391(2)31.2(5)
C12-3248.0(11)-3420.1(13)1367(3)29.8(4)
C13-3406.7(11)-4241.6(12)1371(2)28.1(4)
C14-2652.2(12)-3071.4(14)2360(3)40.9(6)
C15-4174.3(11)-8925.5(12)-3310(2)26.7(4)
C16-4063.5(11)-9320.8(12)-4797(2)26.6(4)
C17-4550.0(11)-9199.8(12)-6023(2)29.8(4)
C18-4410.2(13)-9567.4(12)-7442(3)35.3(5)
C19-3800.5(12)-10043.9(13)-7635(3)35.0(5)
C20-3310.9(12)-10184.7(13)-6438(3)32.8(5)
C21-3451.6(11)-9814.9(13)-5030(2)29.9(5)
C22-2650.7(13)-10726.2(16)-6624(3)44.4(6)
C23-6596.3(11)-8254.0(12)1973(2)28.4(4)
C24-7330.5(11)-8288.4(13)2634(2)29.5(5)
C25-7822.9(12)-7646.3(13)2399(3)34.5(5)
C26-8491.1(13)-7654.6(16)3179(3)42.4(6)
C27-8673.7(12)-8296.3(16)4112(3)42.3(6)
C28-8211.2(12)-8963.6(15)4323(3)38.8(5)
C29-7534.5(11)-8930.0(14)3597(2)32.1(5)
C30-8449.8(14)-9696.3(18)5238(3)53.3(7)
N1-4534.1(9)-5792(1)-469.5(19)25.7(4)
N2-4685.8(9)-8416.7(10)-3084(2)28.6(4)
N3-6414.7(9)-7709.8(10)1006(2)28.2(4)
O1-4847.4(8)-4365.7(9)-1547.2(18)32.6(3)
O2-5145.6(9)-8717.8(10)-5871(2)40.8(4)
O3-7677.9(10)-7018.3(10)1453(2)45.3(4)

Table 3 Anisotropic Displacement Parameters (Å2×103) for phw1113. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+...+2hka×b×U12]
AtomU11U22U33U23U13U12
C131.6(10)24(1)22.4(10)1.5(8)-3.5(8)-2.0(8)
C229.4(10)26.6(10)24.1(10)-0.1(8)2.0(8)-1.5(8)
C330.3(10)26.9(10)23.5(10)-1.3(9)-2.1(8)1.2(8)
C430.3(10)26.4(10)26.7(10)-2.4(8)-0.6(8)-1.5(8)
C528.4(9)28.1(10)23.1(10)0.7(8)-0.8(8)-1.3(9)
C633.7(10)25.4(10)21.6(9)-0.5(8)0.3(8)-0.6(8)
C725.6(9)26.2(10)21.3(9)2.1(8)0.4(8)1.9(8)
C827.8(9)24.5(9)23.1(10)-0.2(8)4.5(8)0.3(8)
C930.2(10)27.7(10)19.5(9)0.6(8)3.8(8)2.0(8)
C1044.2(12)25.9(10)23.8(10)4.2(9)3.2(9)4.8(9)
C1143.0(12)23.5(10)27.1(10)-0.9(9)10.0(9)-1.0(9)
C1227.6(9)30.5(10)31.5(11)-6.4(9)4.8(8)-0.6(9)
C1327.8(10)30.1(10)26.5(10)0.3(9)0.8(8)2.3(9)
C1434.2(11)35.4(12)53.1(15)-12.0(11)-4.5(11)-0.7(10)
C1528.5(9)25.9(10)25.7(10)1.1(8)-1.2(8)-3.8(8)
C1631.3(10)22.3(9)26.3(10)-0.3(8)2.0(8)-4.6(8)
C1737.5(11)21.7(9)30.2(11)0.0(8)-1.8(9)-0.9(9)
C1851.7(13)26.2(11)28.0(11)2.1(9)-6.8(10)-6.2(10)
C1951.7(13)27.3(11)25.9(11)-3.6(9)8.6(10)-9.2(10)
C2037.8(11)28.6(11)32.1(11)-2.1(9)8.5(9)-5.9(9)
C2131.1(10)31.2(11)27.4(11)-0.5(9)3.1(8)-5.6(9)
C2244.5(13)49.3(14)39.3(13)-6.3(12)14.3(11)1.0(12)
C2333(1)26.5(10)25.8(10)-2.0(8)-2.8(8)-3.5(9)
C2432.4(10)35.1(11)21.1(10)-6.6(8)-0.2(8)-5.5(9)
C2536.5(12)36.4(12)30.6(11)-7.9(10)1.5(9)-1.4(10)
C2634.4(11)49.7(14)43.3(14)-17.7(12)2.6(10)0.7(11)
C2733.3(11)62.7(16)30.8(12)-15.8(12)5.1(10)-13.6(11)
C2839.4(12)53.0(15)24(1)-6.2(11)-1.5(9)-19.1(11)
C2933.5(10)38.9(11)23.8(10)-3.8(9)-3.6(8)-8.8(10)
C3050.8(14)73.4(19)35.5(13)2.7(14)2.0(12)-28.2(14)
N131.3(8)24.1(8)21.8(8)1.8(7)-0.7(7)-1.6(7)
N232.1(9)25.9(8)27.8(9)-1.5(7)0.6(7)-1.0(8)
N331.6(9)28.5(9)24.6(8)-1.9(7)2.2(7)-1.1(8)
O139.5(8)28.7(8)29.7(8)4.1(7)-8.2(7)1.1(7)
O248.4(9)38.4(9)35.7(9)-5.8(8)-13.1(8)10.4(8)
O343.1(10)40.3(9)52.6(11)3.3(8)9.2(8)9.3(8)

Table 4 Bond Lengths for phw1113.
AtomAtomLength/Å AtomAtomLength/Å
C1C21.527(3) C15N21.273(3)
C1C61.525(3) C16C171.403(3)
C1N11.463(3) C16C211.401(3)
C2C31.540(3) C17C181.395(3)
C3C41.534(3) C17O21.357(3)
C3N21.463(3) C18C191.377(3)
C4C51.527(3) C19C201.393(3)
C5C61.528(3) C20C211.388(3)
C5N31.470(2) C20C221.513(3)
C7C81.463(3) C23C241.465(3)
C7N11.276(2) C23N31.272(3)
C8C91.404(3) C24C251.406(3)
C8C131.402(3) C24C291.398(3)
C9C101.399(3) C25C261.401(3)
C9O11.348(2) C25O31.346(3)
C10C111.385(3) C26C271.372(4)
C11C121.396(3) C27C281.400(4)
C12C131.384(3) C28C291.393(3)
C12C141.506(3) C28C301.509(4)
C15C161.459(3)    

Table 5 Bond Angles for phw1113.
AtomAtomAtomAngle/˚ AtomAtomAtomAngle/˚
C6C1C2110.06(16) C21C16C15119.90(18)
N1C1C2110.21(16) C21C16C17118.87(18)
N1C1C6108.54(16) C18C17C16119.4(2)
C1C2C3110.16(16) O2C17C16121.46(18)
C4C3C2111.46(16) O2C17C18119.17(19)
N2C3C2108.52(16) C19C18C17120.3(2)
N2C3C4108.78(16) C18C19C20121.9(2)
C5C4C3111.30(16) C19C20C22122.4(2)
C4C5C6110.37(17) C21C20C19117.5(2)
N3C5C4110.95(16) C21C20C22120.1(2)
N3C5C6107.85(16) C20C21C16122.1(2)
C1C6C5110.49(16) N3C23C24121.8(2)
N1C7C8121.88(18) C25C24C23120.35(19)
C9C8C7120.58(18) C29C24C23120.6(2)
C13C8C7120.38(18) C29C24C25118.9(2)
C13C8C9119.04(18) C26C25C24119.0(2)
C10C9C8119.02(19) O3C25C24122.6(2)
O1C9C8121.85(18) O3C25C26118.4(2)
O1C9C10119.12(18) C27C26C25120.4(2)
C11C10C9120.2(2) C26C27C28122.2(2)
C10C11C12121.94(19) C27C28C30121.3(2)
C11C12C14121.08(19) C29C28C27116.8(2)
C13C12C11117.30(19) C29C28C30121.9(2)
C13C12C14121.6(2) C28C29C24122.6(2)
C12C13C8122.48(19) C7N1C1117.91(17)
N2C15C16122.15(19) C15N2C3119.31(17)
C17C16C15121.21(18) C23N3C5119.15(18)

Table 6 Torsion Angles for phw1113.
ABCDAngle/˚
C1C2C3C455.4(2)
C1C2C3N2175.18(16)
C2C1C6C560.1(2)
C2C1N1C7-126.46(19)
C2C3C4C5-54.3(2)
C2C3N2C15111.3(2)
C3C4C5C655.4(2)
C3C4C5N3174.90(16)
C4C3N2C15-127.23(19)
C4C5C6C1-58.5(2)
C4C5N3C2394.0(2)
C6C1C2C3-58.1(2)
C6C1N1C7112.94(19)
C6C5N3C23-145.01(18)
C7C8C9C10178.46(18)
C7C8C9O1-1.1(3)
C7C8C13C12179.35(19)
C8C7N1C1-175.23(17)
C8C9C10C112.5(3)
C9C8C13C12-0.5(3)
C9C10C11C12-1.3(3)
C10C11C12C13-0.8(3)
C10C11C12C14178.5(2)
C11C12C13C81.8(3)
C13C8C9C10-1.6(3)
C13C8C9O1178.83(18)
C14C12C13C8-177.6(2)
C15C16C17C18177.83(18)
C15C16C17O2-0.7(3)
C15C16C21C20-178.06(19)
C16C15N2C3-177.55(17)
C16C17C18C190.0(3)
C17C16C21C200.3(3)
C17C18C19C200.8(3)
C18C19C20C21-1.0(3)
C18C19C20C22178.2(2)
C19C20C21C160.4(3)
C21C16C17C18-0.5(3)
C21C16C17O2-179.00(18)
C22C20C21C16-178.8(2)
C23C24C25C26-173.2(2)
C23C24C25O36.6(3)
C23C24C29C28176.2(2)
C24C23N3C5173.62(18)
C24C25C26C27-2.6(3)
C25C24C29C280.7(3)
C25C26C27C28-0.2(4)
C26C27C28C293.1(3)
C26C27C28C30-174.5(2)
C27C28C29C24-3.4(3)
C29C24C25C262.3(3)
C29C24C25O3-177.9(2)
C30C28C29C24174.2(2)
N1C1C2C3-177.77(16)
N1C1C6C5-179.24(16)
N1C7C8C94.1(3)
N1C7C8C13-175.77(18)
N2C3C4C5-173.90(16)
N2C15C16C17-4.5(3)
N2C15C16C21173.78(19)
N3C5C6C1-179.80(16)
N3C23C24C25-9.9(3)
N3C23C24C29174.75(19)
O1C9C10C11-177.91(18)
O2C17C18C19178.50(19)
O3C25C26C27177.7(2)

Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for phw1113.
AtomxyzU(eq)
H1-4350-688354031
H2A-4047-7054-210332
H2B-4873-6873-259632
H3-4396-8271-84632
H4A-5878-7952-176933
H4B-5614-8718-77833
H5-5329-7877133832
H6A-5802-6528-53032
H6B-5547-6455123232
H7-3832-5784118029
H10-4475-2883-119238
H11-3565-235837637
H13-3144-4588204834
H14A-2250-2888170461
H14B-2476-3489307361
H14C-2843-2610294961
H15-3854-9052-248332
H18-4737-9489-827842
H19-3711-10284-861342
H21-3123-9900-419936
H22A-2657-11148-582767
H22B-2207-10400-652067
H22C-2661-10981-764567
H23-6247-8649227634
H26-8820-7213306251
H27-9129-8288463251
H29-7199-9360376438
H30A-8027-10041545580
H30B-8809-10006464380
H30C-8669-9518621280
H1A-4821(13)-4923(17)-1410.0(3)44(7)
H2-5139-8493-500261
H3A-7249(16)-7099(17) 1130.0(4)57(9)

[RSC Journal Format]

Experimental

Single crystals of C30H33N3O3 [phw1113] were recrystallised from [solvents] mounted in inert oil and transferred to the cold gas stream of the diffractometer.

Crystal structure determination of [phw1113]

Crystal Data. C30H33N3O3, =483.59, orthorhombic, a = 18.3543(12) Å, b = 16.464(11) Å, c = 8.6727(9) Å, = 2620.8(19) Å3, T = 110.0, space group Pna21 (no. 33), Z = 4, μ(Mo Kα) = 0.080, 10192 reflections measured, 5801 unique (Rint = 0.0197) which were used in all calculations. The final wR(F2) was 0.1034 (all data).

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