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.
Atom | x | y | z | U(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]
Atom | U11 | U22 | U33 | U23 | U13 | U12 |
C1 | 31.6(10) | 24(1) | 22.4(10) | 1.5(8) | -3.5(8) | -2.0(8) |
C2 | 29.4(10) | 26.6(10) | 24.1(10) | -0.1(8) | 2.0(8) | -1.5(8) |
C3 | 30.3(10) | 26.9(10) | 23.5(10) | -1.3(9) | -2.1(8) | 1.2(8) |
C4 | 30.3(10) | 26.4(10) | 26.7(10) | -2.4(8) | -0.6(8) | -1.5(8) |
C5 | 28.4(9) | 28.1(10) | 23.1(10) | 0.7(8) | -0.8(8) | -1.3(9) |
C6 | 33.7(10) | 25.4(10) | 21.6(9) | -0.5(8) | 0.3(8) | -0.6(8) |
C7 | 25.6(9) | 26.2(10) | 21.3(9) | 2.1(8) | 0.4(8) | 1.9(8) |
C8 | 27.8(9) | 24.5(9) | 23.1(10) | -0.2(8) | 4.5(8) | 0.3(8) |
C9 | 30.2(10) | 27.7(10) | 19.5(9) | 0.6(8) | 3.8(8) | 2.0(8) |
C10 | 44.2(12) | 25.9(10) | 23.8(10) | 4.2(9) | 3.2(9) | 4.8(9) |
C11 | 43.0(12) | 23.5(10) | 27.1(10) | -0.9(9) | 10.0(9) | -1.0(9) |
C12 | 27.6(9) | 30.5(10) | 31.5(11) | -6.4(9) | 4.8(8) | -0.6(9) |
C13 | 27.8(10) | 30.1(10) | 26.5(10) | 0.3(9) | 0.8(8) | 2.3(9) |
C14 | 34.2(11) | 35.4(12) | 53.1(15) | -12.0(11) | -4.5(11) | -0.7(10) |
C15 | 28.5(9) | 25.9(10) | 25.7(10) | 1.1(8) | -1.2(8) | -3.8(8) |
C16 | 31.3(10) | 22.3(9) | 26.3(10) | -0.3(8) | 2.0(8) | -4.6(8) |
C17 | 37.5(11) | 21.7(9) | 30.2(11) | 0.0(8) | -1.8(9) | -0.9(9) |
C18 | 51.7(13) | 26.2(11) | 28.0(11) | 2.1(9) | -6.8(10) | -6.2(10) |
C19 | 51.7(13) | 27.3(11) | 25.9(11) | -3.6(9) | 8.6(10) | -9.2(10) |
C20 | 37.8(11) | 28.6(11) | 32.1(11) | -2.1(9) | 8.5(9) | -5.9(9) |
C21 | 31.1(10) | 31.2(11) | 27.4(11) | -0.5(9) | 3.1(8) | -5.6(9) |
C22 | 44.5(13) | 49.3(14) | 39.3(13) | -6.3(12) | 14.3(11) | 1.0(12) |
C23 | 33(1) | 26.5(10) | 25.8(10) | -2.0(8) | -2.8(8) | -3.5(9) |
C24 | 32.4(10) | 35.1(11) | 21.1(10) | -6.6(8) | -0.2(8) | -5.5(9) |
C25 | 36.5(12) | 36.4(12) | 30.6(11) | -7.9(10) | 1.5(9) | -1.4(10) |
C26 | 34.4(11) | 49.7(14) | 43.3(14) | -17.7(12) | 2.6(10) | 0.7(11) |
C27 | 33.3(11) | 62.7(16) | 30.8(12) | -15.8(12) | 5.1(10) | -13.6(11) |
C28 | 39.4(12) | 53.0(15) | 24(1) | -6.2(11) | -1.5(9) | -19.1(11) |
C29 | 33.5(10) | 38.9(11) | 23.8(10) | -3.8(9) | -3.6(8) | -8.8(10) |
C30 | 50.8(14) | 73.4(19) | 35.5(13) | 2.7(14) | 2.0(12) | -28.2(14) |
N1 | 31.3(8) | 24.1(8) | 21.8(8) | 1.8(7) | -0.7(7) | -1.6(7) |
N2 | 32.1(9) | 25.9(8) | 27.8(9) | -1.5(7) | 0.6(7) | -1.0(8) |
N3 | 31.6(9) | 28.5(9) | 24.6(8) | -1.9(7) | 2.2(7) | -1.1(8) |
O1 | 39.5(8) | 28.7(8) | 29.7(8) | 4.1(7) | -8.2(7) | 1.1(7) |
O2 | 48.4(9) | 38.4(9) | 35.7(9) | -5.8(8) | -13.1(8) | 10.4(8) |
O3 | 43.1(10) | 40.3(9) | 52.6(11) | 3.3(8) | 9.2(8) | 9.3(8) |
Table 4 Bond Lengths for phw1113.
Atom | Atom | Length/Å | | Atom | Atom | Length/Å |
C1 | C2 | 1.527(3) | | C15 | N2 | 1.273(3) |
C1 | C6 | 1.525(3) | | C16 | C17 | 1.403(3) |
C1 | N1 | 1.463(3) | | C16 | C21 | 1.401(3) |
C2 | C3 | 1.540(3) | | C17 | C18 | 1.395(3) |
C3 | C4 | 1.534(3) | | C17 | O2 | 1.357(3) |
C3 | N2 | 1.463(3) | | C18 | C19 | 1.377(3) |
C4 | C5 | 1.527(3) | | C19 | C20 | 1.393(3) |
C5 | C6 | 1.528(3) | | C20 | C21 | 1.388(3) |
C5 | N3 | 1.470(2) | | C20 | C22 | 1.513(3) |
C7 | C8 | 1.463(3) | | C23 | C24 | 1.465(3) |
C7 | N1 | 1.276(2) | | C23 | N3 | 1.272(3) |
C8 | C9 | 1.404(3) | | C24 | C25 | 1.406(3) |
C8 | C13 | 1.402(3) | | C24 | C29 | 1.398(3) |
C9 | C10 | 1.399(3) | | C25 | C26 | 1.401(3) |
C9 | O1 | 1.348(2) | | C25 | O3 | 1.346(3) |
C10 | C11 | 1.385(3) | | C26 | C27 | 1.372(4) |
C11 | C12 | 1.396(3) | | C27 | C28 | 1.400(4) |
C12 | C13 | 1.384(3) | | C28 | C29 | 1.393(3) |
C12 | C14 | 1.506(3) | | C28 | C30 | 1.509(4) |
C15 | C16 | 1.459(3) | | | | |
Table 5 Bond Angles for phw1113.
Atom | Atom | Atom | Angle/˚ | | Atom | Atom | Atom | Angle/˚ |
C6 | C1 | C2 | 110.06(16) | | C21 | C16 | C15 | 119.90(18) |
N1 | C1 | C2 | 110.21(16) | | C21 | C16 | C17 | 118.87(18) |
N1 | C1 | C6 | 108.54(16) | | C18 | C17 | C16 | 119.4(2) |
C1 | C2 | C3 | 110.16(16) | | O2 | C17 | C16 | 121.46(18) |
C4 | C3 | C2 | 111.46(16) | | O2 | C17 | C18 | 119.17(19) |
N2 | C3 | C2 | 108.52(16) | | C19 | C18 | C17 | 120.3(2) |
N2 | C3 | C4 | 108.78(16) | | C18 | C19 | C20 | 121.9(2) |
C5 | C4 | C3 | 111.30(16) | | C19 | C20 | C22 | 122.4(2) |
C4 | C5 | C6 | 110.37(17) | | C21 | C20 | C19 | 117.5(2) |
N3 | C5 | C4 | 110.95(16) | | C21 | C20 | C22 | 120.1(2) |
N3 | C5 | C6 | 107.85(16) | | C20 | C21 | C16 | 122.1(2) |
C1 | C6 | C5 | 110.49(16) | | N3 | C23 | C24 | 121.8(2) |
N1 | C7 | C8 | 121.88(18) | | C25 | C24 | C23 | 120.35(19) |
C9 | C8 | C7 | 120.58(18) | | C29 | C24 | C23 | 120.6(2) |
C13 | C8 | C7 | 120.38(18) | | C29 | C24 | C25 | 118.9(2) |
C13 | C8 | C9 | 119.04(18) | | C26 | C25 | C24 | 119.0(2) |
C10 | C9 | C8 | 119.02(19) | | O3 | C25 | C24 | 122.6(2) |
O1 | C9 | C8 | 121.85(18) | | O3 | C25 | C26 | 118.4(2) |
O1 | C9 | C10 | 119.12(18) | | C27 | C26 | C25 | 120.4(2) |
C11 | C10 | C9 | 120.2(2) | | C26 | C27 | C28 | 122.2(2) |
C10 | C11 | C12 | 121.94(19) | | C27 | C28 | C30 | 121.3(2) |
C11 | C12 | C14 | 121.08(19) | | C29 | C28 | C27 | 116.8(2) |
C13 | C12 | C11 | 117.30(19) | | C29 | C28 | C30 | 121.9(2) |
C13 | C12 | C14 | 121.6(2) | | C28 | C29 | C24 | 122.6(2) |
C12 | C13 | C8 | 122.48(19) | | C7 | N1 | C1 | 117.91(17) |
N2 | C15 | C16 | 122.15(19) | | C15 | N2 | C3 | 119.31(17) |
C17 | C16 | C15 | 121.21(18) | | C23 | N3 | C5 | 119.15(18) |
Table 6 Torsion Angles for phw1113.
A | B | C | D | Angle/˚ |
C1 | C2 | C3 | C4 | 55.4(2) |
C1 | C2 | C3 | N2 | 175.18(16) |
C2 | C1 | C6 | C5 | 60.1(2) |
C2 | C1 | N1 | C7 | -126.46(19) |
C2 | C3 | C4 | C5 | -54.3(2) |
C2 | C3 | N2 | C15 | 111.3(2) |
C3 | C4 | C5 | C6 | 55.4(2) |
C3 | C4 | C5 | N3 | 174.90(16) |
C4 | C3 | N2 | C15 | -127.23(19) |
C4 | C5 | C6 | C1 | -58.5(2) |
C4 | C5 | N3 | C23 | 94.0(2) |
C6 | C1 | C2 | C3 | -58.1(2) |
C6 | C1 | N1 | C7 | 112.94(19) |
C6 | C5 | N3 | C23 | -145.01(18) |
C7 | C8 | C9 | C10 | 178.46(18) |
C7 | C8 | C9 | O1 | -1.1(3) |
C7 | C8 | C13 | C12 | 179.35(19) |
C8 | C7 | N1 | C1 | -175.23(17) |
C8 | C9 | C10 | C11 | 2.5(3) |
C9 | C8 | C13 | C12 | -0.5(3) |
C9 | C10 | C11 | C12 | -1.3(3) |
C10 | C11 | C12 | C13 | -0.8(3) |
C10 | C11 | C12 | C14 | 178.5(2) |
C11 | C12 | C13 | C8 | 1.8(3) |
C13 | C8 | C9 | C10 | -1.6(3) |
C13 | C8 | C9 | O1 | 178.83(18) |
C14 | C12 | C13 | C8 | -177.6(2) |
C15 | C16 | C17 | C18 | 177.83(18) |
C15 | C16 | C17 | O2 | -0.7(3) |
C15 | C16 | C21 | C20 | -178.06(19) |
C16 | C15 | N2 | C3 | -177.55(17) |
C16 | C17 | C18 | C19 | 0.0(3) |
C17 | C16 | C21 | C20 | 0.3(3) |
C17 | C18 | C19 | C20 | 0.8(3) |
C18 | C19 | C20 | C21 | -1.0(3) |
C18 | C19 | C20 | C22 | 178.2(2) |
C19 | C20 | C21 | C16 | 0.4(3) |
C21 | C16 | C17 | C18 | -0.5(3) |
C21 | C16 | C17 | O2 | -179.00(18) |
C22 | C20 | C21 | C16 | -178.8(2) |
C23 | C24 | C25 | C26 | -173.2(2) |
C23 | C24 | C25 | O3 | 6.6(3) |
C23 | C24 | C29 | C28 | 176.2(2) |
C24 | C23 | N3 | C5 | 173.62(18) |
C24 | C25 | C26 | C27 | -2.6(3) |
C25 | C24 | C29 | C28 | 0.7(3) |
C25 | C26 | C27 | C28 | -0.2(4) |
C26 | C27 | C28 | C29 | 3.1(3) |
C26 | C27 | C28 | C30 | -174.5(2) |
C27 | C28 | C29 | C24 | -3.4(3) |
C29 | C24 | C25 | C26 | 2.3(3) |
C29 | C24 | C25 | O3 | -177.9(2) |
C30 | C28 | C29 | C24 | 174.2(2) |
N1 | C1 | C2 | C3 | -177.77(16) |
N1 | C1 | C6 | C5 | -179.24(16) |
N1 | C7 | C8 | C9 | 4.1(3) |
N1 | C7 | C8 | C13 | -175.77(18) |
N2 | C3 | C4 | C5 | -173.90(16) |
N2 | C15 | C16 | C17 | -4.5(3) |
N2 | C15 | C16 | C21 | 173.78(19) |
N3 | C5 | C6 | C1 | -179.80(16) |
N3 | C23 | C24 | C25 | -9.9(3) |
N3 | C23 | C24 | C29 | 174.75(19) |
O1 | C9 | C10 | C11 | -177.91(18) |
O2 | C17 | C18 | C19 | 178.50(19) |
O3 | C25 | C26 | C27 | 177.7(2) |
Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for phw1113.
Atom | x | y | z | U(eq) |
H1 | -4350 | -6883 | 540 | 31 |
H2A | -4047 | -7054 | -2103 | 32 |
H2B | -4873 | -6873 | -2596 | 32 |
H3 | -4396 | -8271 | -846 | 32 |
H4A | -5878 | -7952 | -1769 | 33 |
H4B | -5614 | -8718 | -778 | 33 |
H5 | -5329 | -7877 | 1338 | 32 |
H6A | -5802 | -6528 | -530 | 32 |
H6B | -5547 | -6455 | 1232 | 32 |
H7 | -3832 | -5784 | 1180 | 29 |
H10 | -4475 | -2883 | -1192 | 38 |
H11 | -3565 | -2358 | 376 | 37 |
H13 | -3144 | -4588 | 2048 | 34 |
H14A | -2250 | -2888 | 1704 | 61 |
H14B | -2476 | -3489 | 3073 | 61 |
H14C | -2843 | -2610 | 2949 | 61 |
H15 | -3854 | -9052 | -2483 | 32 |
H18 | -4737 | -9489 | -8278 | 42 |
H19 | -3711 | -10284 | -8613 | 42 |
H21 | -3123 | -9900 | -4199 | 36 |
H22A | -2657 | -11148 | -5827 | 67 |
H22B | -2207 | -10400 | -6520 | 67 |
H22C | -2661 | -10981 | -7645 | 67 |
H23 | -6247 | -8649 | 2276 | 34 |
H26 | -8820 | -7213 | 3062 | 51 |
H27 | -9129 | -8288 | 4632 | 51 |
H29 | -7199 | -9360 | 3764 | 38 |
H30A | -8027 | -10041 | 5455 | 80 |
H30B | -8809 | -10006 | 4643 | 80 |
H30C | -8669 | -9518 | 6212 | 80 |
H1A | -4821(13) | -4923(17) | -1410.0(3) | 44(7) |
H2 | -5139 | -8493 | -5002 | 61 |
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,
M =483.59,
orthorhombic,
a = 18.3543(12) Å, b = 16.464(11) Å, c = 8.6727(9) Å,
U = 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).
This report has been created with Olex2, compiled on 2011.02.15 svn.r1672. Please let us know if there are any errors or if you would like to have additional featrues.