phw1101
Crystal Submitted by: |
LC |
Crystal Submitted on: |
31/1/2011 |
Data Collected on: |
|
Structure Solved by: |
NCS |
|
|
Table 1: Crystal data and structure refinement for phw1101
Identification code
|
phw1101
|
Empirical formula
|
C27H27N3O3
|
Formula weight
|
441.52
|
Temperature / K
|
120.0
|
Crystal system
|
monoclinic
|
Space group
|
P21/c
|
a / Å, b / Å, c / Å
|
5.9979(2), 24.6161(8), 15.3079(6)
|
α/°, β/°, γ/°
|
90.00, 91.843(2), 90.00
|
Volume / Å3
|
2258.96(14)
|
Z
|
4
|
ρcalc / mg mm-3
|
1.298
|
μ / mm‑1
|
0.086
|
F(000)
|
936
|
Crystal size / mm3
|
0.32 × 0.05 × 0.04
|
2Θ range for data collection
|
6.28 to 55.14°
|
Index ranges
|
-7 ≤ h ≤ 7, -29 ≤ k ≤ 31, -19 ≤ l ≤ 19
|
Reflections collected
|
18092
|
Independent reflections
|
5165[R(int) = 0.0524]
|
Data/restraints/parameters
|
5165/0/311
|
Goodness-of-fit on F2
|
1.114
|
Final R indexes [I>2σ (I)]
|
R1 = 0.0679, wR2 =
0.1184
|
Final R indexes [all data]
|
R1 = 0.1034, wR2 = 0.1352
|
Largest diff. peak/hole / e Å-3
|
0.265/-0.239
|
Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for phw1101. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor.
Atom | x | y | z | U(eq) |
C1 | 5935(4) | 5439.9(9) | -2045.5(15) | 20.2(5) |
C2 | 4433(3) | 5080.0(9) | -1513.4(15) | 19.5(5) |
C3 | 5719(3) | 4626.7(9) | -1036.1(15) | 19.6(5) |
C4 | 7114(4) | 4300.5(9) | -1669.5(15) | 19.5(5) |
C5 | 8600(3) | 4679.2(9) | -2185.3(15) | 19.7(5) |
C6 | 7242(4) | 5102.7(9) | -2694.7(15) | 20.8(5) |
C7 | 5127(4) | 6343.3(9) | -2490.8(16) | 20.5(5) |
C8 | 3721(4) | 6765.0(9) | -2886.6(15) | 20.3(5) |
C9 | 1608(4) | 6637.4(9) | -3269.9(16) | 22.3(5) |
C10 | 258(4) | 7049.5(10) | -3607.4(17) | 28.4(6) |
C11 | 965(4) | 7584.3(11) | -3561.0(18) | 32.1(6) |
C12 | 3038(4) | 7715(1) | -3182.8(17) | 28.9(6) |
C13 | 4399(4) | 7308.7(9) | -2852.3(16) | 24.3(5) |
C14 | 4365(4) | 3808.1(9) | -383.8(15) | 20.6(5) |
C15 | 2753(4) | 3499.8(9) | 112.3(15) | 20.7(5) |
C16 | 777(4) | 3745.4(9) | 397.9(15) | 21.0(5) |
C17 | -715(4) | 3446.5(10) | 882.1(16) | 24.9(5) |
C18 | -263(4) | 2908.9(10) | 1079.5(17) | 28.2(6) |
C19 | 1658(4) | 2656(1) | 796.4(17) | 28.0(6) |
C20 | 3150(4) | 2952.2(10) | 316.2(16) | 25.0(5) |
C21 | 10698(4) | 4474.4(11) | -3458.1(17) | 29.9(6) |
C22 | 12438(4) | 4178.8(11) | -3903.7(17) | 30.5(6) |
C23 | 13525(4) | 3731.4(10) | -3507.1(17) | 24.9(5) |
C24 | 15328(4) | 3491.7(11) | -3914.2(18) | 31.7(6) |
C25 | 16022(5) | 3683.3(13) | -4702.9(19) | 43.0(8) |
C26 | 14945(6) | 4117.9(16) | -5108(2) | 61.3(11) |
C27 | 13176(5) | 4362.5(15) | -4701(2) | 54.8(10) |
N1 | 4536(3) | 5842.4(7) | -2504.1(13) | 20.6(4) |
N2 | 4069(3) | 4310.7(7) | -554.5(13) | 20.2(4) |
N3 | 10136(3) | 4344.7(8) | -2688.9(13) | 21.8(4) |
O1 | 864(3) | 6117.4(7) | -3309.0(12) | 28.1(4) |
O2 | 294(3) | 4274.1(7) | 211.9(11) | 24.2(4) |
O3 | 12879(3) | 3533.2(7) | -2734.4(13) | 32.4(4) |
Table 3 Anisotropic Displacement Parameters (Å2×103) for phw1101. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+...+2hka×b×U12]
Atom | U11 | U22 | U33 | U23 | U13 | U12 |
C1 | 18.9(10) | 19.7(11) | 21.8(13) | -0.1(9) | -1.8(9) | -0.8(9) |
C2 | 16.7(10) | 21.9(11) | 20.0(12) | -1.8(9) | 1.4(8) | 1.6(9) |
C3 | 17.6(10) | 19.4(11) | 21.7(12) | -1.7(9) | 0.5(9) | -0.4(9) |
C4 | 19.5(10) | 19.3(11) | 19.6(12) | -0.4(9) | 1.2(9) | 1.1(9) |
C5 | 17.7(10) | 20.8(11) | 20.5(12) | -3.3(9) | 2.0(9) | 3.0(9) |
C6 | 19.8(10) | 20.0(11) | 22.8(12) | 0.7(9) | 3.4(9) | -1.6(9) |
C7 | 20(1) | 21.9(11) | 19.8(12) | 0.4(9) | 3.8(9) | -0.2(9) |
C8 | 21.2(11) | 23.3(12) | 16.6(12) | 2.6(9) | 3.0(9) | 2.2(9) |
C9 | 24.1(11) | 22.9(12) | 20.2(12) | 0.1(10) | 5.4(9) | 0.8(9) |
C10 | 25.8(12) | 32.2(14) | 27.0(14) | 3.4(11) | -0.5(10) | 5.2(10) |
C11 | 36.5(14) | 31.1(14) | 28.6(15) | 7.2(11) | -0.9(11) | 11.7(11) |
C12 | 39.1(14) | 19.5(12) | 28.2(15) | 4.1(10) | 4.1(11) | 1.2(10) |
C13 | 28.2(12) | 22.7(12) | 22.0(13) | 0.9(10) | 1(1) | -2.9(10) |
C14 | 20.0(11) | 23.3(12) | 18.6(12) | -3.0(9) | 2.5(9) | 1.9(9) |
C15 | 21.1(11) | 22.5(11) | 18.4(12) | -0.5(9) | 0.5(9) | -2.0(9) |
C16 | 22.1(11) | 22.8(12) | 18.0(12) | 0.4(9) | -1.8(9) | -0.3(9) |
C17 | 20.1(11) | 29.9(13) | 25.0(14) | -0.7(10) | 3.4(9) | -1.2(10) |
C18 | 28.2(12) | 30.5(13) | 25.9(14) | 1.4(11) | 3.5(10) | -8.7(10) |
C19 | 31.6(13) | 23.1(12) | 29.3(14) | 2.6(11) | -0.4(11) | -1.7(10) |
C20 | 27.7(12) | 22.8(12) | 24.3(13) | -0.4(10) | 0.8(10) | 3.2(10) |
C21 | 26.7(12) | 40.4(15) | 22.6(14) | 0.6(11) | -0.1(10) | 10.6(11) |
C22 | 28.8(12) | 42.4(15) | 20.3(13) | -2.4(11) | 0.9(10) | 8.5(11) |
C23 | 21.8(11) | 27.8(12) | 25.1(13) | -7.1(10) | 2.1(9) | -2.5(10) |
C24 | 26.4(12) | 36.4(14) | 32.4(15) | -4.9(12) | 1.0(11) | 7.7(11) |
C25 | 37.2(15) | 64(2) | 28.7(16) | -7.0(14) | 7.5(12) | 19.4(14) |
C26 | 68(2) | 93(3) | 24.3(17) | 11.1(17) | 17.4(15) | 40(2) |
C27 | 60(2) | 77(2) | 28.0(17) | 14.3(16) | 10.0(14) | 38.9(18) |
N1 | 20.1(9) | 19.9(10) | 22.0(11) | 1.3(8) | 3.8(8) | 1.3(7) |
N2 | 19.7(9) | 20.5(10) | 20.4(10) | 0.4(8) | 2.0(7) | -2.0(8) |
N3 | 17.3(9) | 22.5(10) | 25.8(11) | -3.5(8) | 0.8(8) | 0.1(8) |
O1 | 24.1(8) | 24.3(9) | 35.6(11) | 3.2(8) | -5.0(7) | -3.6(7) |
O2 | 22.2(8) | 22.8(9) | 27.7(10) | 2.4(7) | 3.1(7) | 4.2(7) |
O3 | 32.2(10) | 27.2(9) | 38.7(12) | 5.4(8) | 13.2(8) | 5.6(8) |
Table 4 Bond Lengths for phw1101.
Atom | Atom | Length/Å | | Atom | Atom | Length/Å |
C1 | C2 | 1.519(3) | | C14 | C15 | 1.461(3) |
C1 | C6 | 1.530(3) | | C14 | N2 | 1.276(3) |
C1 | N1 | 1.463(3) | | C15 | C16 | 1.412(3) |
C2 | C3 | 1.529(3) | | C15 | C20 | 1.402(3) |
C3 | C4 | 1.529(3) | | C16 | C17 | 1.390(3) |
C3 | N2 | 1.475(3) | | C16 | O2 | 1.361(3) |
C4 | C5 | 1.527(3) | | C17 | C18 | 1.382(3) |
C5 | C6 | 1.522(3) | | C18 | C19 | 1.391(3) |
C5 | N3 | 1.472(3) | | C19 | C20 | 1.384(3) |
C7 | C8 | 1.457(3) | | C21 | C22 | 1.460(3) |
C7 | N1 | 1.283(3) | | C21 | N3 | 1.276(3) |
C8 | C9 | 1.414(3) | | C22 | C23 | 1.407(4) |
C8 | C13 | 1.399(3) | | C22 | C27 | 1.387(4) |
C9 | C10 | 1.388(3) | | C23 | C24 | 1.396(3) |
C9 | O1 | 1.357(3) | | C23 | O3 | 1.348(3) |
C10 | C11 | 1.384(4) | | C24 | C25 | 1.373(4) |
C11 | C12 | 1.392(4) | | C25 | C26 | 1.386(4) |
C12 | C13 | 1.377(3) | | C26 | C27 | 1.386(4) |
Table 5 Bond Angles for phw1101.
Atom | Atom | Atom | Angle/˚ | | Atom | Atom | Atom | Angle/˚ |
C2 | C1 | C6 | 110.91(18) | | C16 | C15 | C14 | 121.0(2) |
N1 | C1 | C2 | 108.17(17) | | C20 | C15 | C14 | 120.3(2) |
N1 | C1 | C6 | 110.70(19) | | C20 | C15 | C16 | 118.8(2) |
C1 | C2 | C3 | 112.55(17) | | C17 | C16 | C15 | 120.0(2) |
C2 | C3 | C4 | 110.99(19) | | O2 | C16 | C15 | 121.3(2) |
N2 | C3 | C2 | 106.73(17) | | O2 | C16 | C17 | 118.8(2) |
N2 | C3 | C4 | 115.45(18) | | C18 | C17 | C16 | 119.9(2) |
C5 | C4 | C3 | 110.35(18) | | C17 | C18 | C19 | 121.2(2) |
C6 | C5 | C4 | 111.79(18) | | C20 | C19 | C18 | 119.1(2) |
N3 | C5 | C4 | 108.35(18) | | C19 | C20 | C15 | 121.1(2) |
N3 | C5 | C6 | 116.64(19) | | N3 | C21 | C22 | 121.4(2) |
C5 | C6 | C1 | 108.40(19) | | C23 | C22 | C21 | 121.1(2) |
N1 | C7 | C8 | 121.5(2) | | C27 | C22 | C21 | 120.1(2) |
C9 | C8 | C7 | 120.9(2) | | C27 | C22 | C23 | 118.6(2) |
C13 | C8 | C7 | 120.2(2) | | C24 | C23 | C22 | 119.5(2) |
C13 | C8 | C9 | 118.9(2) | | O3 | C23 | C22 | 121.3(2) |
C10 | C9 | C8 | 119.8(2) | | O3 | C23 | C24 | 119.2(2) |
O1 | C9 | C8 | 121.1(2) | | C25 | C24 | C23 | 120.6(3) |
O1 | C9 | C10 | 119.1(2) | | C24 | C25 | C26 | 120.5(3) |
C11 | C10 | C9 | 120.1(2) | | C27 | C26 | C25 | 119.1(3) |
C10 | C11 | C12 | 120.6(2) | | C26 | C27 | C22 | 121.6(3) |
C13 | C12 | C11 | 119.7(2) | | C7 | N1 | C1 | 119.31(19) |
C12 | C13 | C8 | 120.9(2) | | C14 | N2 | C3 | 121.54(19) |
N2 | C14 | C15 | 121.4(2) | | C21 | N3 | C5 | 122.1(2) |
Table 6 Hydrogen Bonds for phw1101.
D | H | A | d(D-H)/Å | d(H-A)/Å | d(D-A)/Å | D-H-A/° |
O1 | H1A | N1 | 1.01(4) | 1.67(4) | 2.580(3) | 147(3) |
O2 | H2 | N2 | 0.96(3) | 1.72(3) | 2.585(2) | 149(3) |
O3 | H3A | N3 | 1.02(4) | 1.69(4) | 2.591(3) | 145(3) |
Table 7 Torsion Angles for phw1101.
A | B | C | D | Angle/˚ |
C1 | C2 | C3 | C4 | -53.1(2) |
C1 | C2 | C3 | N2 | -179.72(18) |
C2 | C1 | C6 | C5 | -58.0(2) |
C2 | C1 | N1 | C7 | 133.3(2) |
C2 | C3 | C4 | C5 | 53.3(2) |
C2 | C3 | N2 | C14 | 151.9(2) |
C3 | C4 | C5 | C6 | -58.2(2) |
C3 | C4 | C5 | N3 | 171.90(18) |
C4 | C3 | N2 | C14 | 28.0(3) |
C4 | C5 | C6 | C1 | 59.9(2) |
C4 | C5 | N3 | C21 | 142.6(2) |
C6 | C1 | C2 | C3 | 55.9(3) |
C6 | C1 | N1 | C7 | -105.0(2) |
C6 | C5 | N3 | C21 | 15.4(3) |
C7 | C8 | C9 | C10 | 177.1(2) |
C7 | C8 | C9 | O1 | -2.4(3) |
C7 | C8 | C13 | C12 | -176.6(2) |
C8 | C7 | N1 | C1 | -175.8(2) |
C8 | C9 | C10 | C11 | -0.7(4) |
C9 | C8 | C13 | C12 | 0.2(4) |
C9 | C10 | C11 | C12 | 0.5(4) |
C10 | C11 | C12 | C13 | 0.1(4) |
C11 | C12 | C13 | C8 | -0.4(4) |
C13 | C8 | C9 | C10 | 0.4(3) |
C13 | C8 | C9 | O1 | -179.2(2) |
C14 | C15 | C16 | C17 | -178.9(2) |
C14 | C15 | C16 | O2 | 0.8(3) |
C14 | C15 | C20 | C19 | 179.0(2) |
C15 | C14 | N2 | C3 | 178.5(2) |
C15 | C16 | C17 | C18 | -0.3(4) |
C16 | C15 | C20 | C19 | -0.7(4) |
C16 | C17 | C18 | C19 | -0.5(4) |
C17 | C18 | C19 | C20 | 0.7(4) |
C18 | C19 | C20 | C15 | -0.1(4) |
C20 | C15 | C16 | C17 | 0.9(3) |
C20 | C15 | C16 | O2 | -179.4(2) |
C21 | C22 | C23 | C24 | -173.7(2) |
C21 | C22 | C23 | O3 | 5.4(4) |
C21 | C22 | C27 | C26 | 174.7(3) |
C22 | C21 | N3 | C5 | 171.9(2) |
C22 | C23 | C24 | C25 | -1.1(4) |
C23 | C22 | C27 | C26 | -0.2(5) |
C23 | C24 | C25 | C26 | 0.0(5) |
C24 | C25 | C26 | C27 | 0.9(6) |
C25 | C26 | C27 | C22 | -0.9(6) |
C27 | C22 | C23 | C24 | 1.1(4) |
C27 | C22 | C23 | O3 | -179.8(3) |
N1 | C1 | C2 | C3 | 177.50(18) |
N1 | C1 | C6 | C5 | -178.06(17) |
N1 | C7 | C8 | C9 | 2.5(3) |
N1 | C7 | C8 | C13 | 179.2(2) |
N2 | C3 | C4 | C5 | 174.87(18) |
N2 | C14 | C15 | C16 | 1.9(3) |
N2 | C14 | C15 | C20 | -177.9(2) |
N3 | C5 | C6 | C1 | -174.64(18) |
N3 | C21 | C22 | C23 | 1.4(4) |
N3 | C21 | C22 | C27 | -173.3(3) |
O1 | C9 | C10 | C11 | 178.9(2) |
O2 | C16 | C17 | C18 | 180.0(2) |
O3 | C23 | C24 | C25 | 179.8(3) |
Table 8 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for phw1101.
Atom | x | y | z | U(eq) |
H1 | 7011 | 5632 | -1640 | 24 |
H2A | 3276 | 4916 | -1907 | 23 |
H2B | 3669 | 5306 | -1080 | 23 |
H3 | 6765 | 4800 | -597 | 23 |
H4A | 8052 | 4036 | -1339 | 23 |
H4B | 6115 | 4096 | -2078 | 23 |
H5 | 9542 | 4883 | -1745 | 24 |
H6A | 6200 | 4922 | -3117 | 25 |
H6B | 8245 | 5341 | -3024 | 25 |
H7 | 6513 | 6442 | -2217 | 25 |
H10 | -1155 | 6965 | -3871 | 34 |
H11 | 28 | 7865 | -3789 | 39 |
H12 | 3512 | 8083 | -3153 | 35 |
H13 | 5816 | 7399 | -2598 | 29 |
H14 | 5659 | 3631 | -583 | 25 |
H17 | -2041 | 3612 | 1077 | 30 |
H18 | -1285 | 2708 | 1415 | 34 |
H19 | 1942 | 2285 | 931 | 34 |
H20 | 4466 | 2782 | 122 | 30 |
H21 | 9968 | 4770 | -3747 | 36 |
H24 | 16081 | 3194 | -3643 | 38 |
H25 | 17251 | 3516 | -4973 | 52 |
H26 | 15414 | 4246 | -5658 | 74 |
H27 | 12450 | 4664 | -4974 | 66 |
H1A | 2030.0(6) | 5881(14) | -3000.0(2) | 67(11) |
H2 | 1530.0(5) | 4416(13) | -100.0(2) | 55(10) |
H3A | 11610.0(6) | 3767(15) | -2520.0(3) | 83(13) |
[RSC Journal Format]
Experimental
Single crystals of C27H27N3O3
[phw1101]
were recrystallised from
[solvents]
mounted in inert oil and transferred to the cold gas stream of the diffractometer.
Crystal structure determination of
[phw1101]
Crystal Data.
C27H27N3O3,
M =441.52,
monoclinic,
a = 5.9979(2) Å, b = 24.6161(8) Å, c = 15.3079(6) Å, β = 91.843(2)°,
U = 2258.96(14) Å3,
T = 120.0,
space group P21/c (no. 14),
Z = 4,
μ(MO Kα) = 0.086,
18092 reflections measured,
5165 unique (Rint = 0.0524) which were used in all calculations.
The final wR(F2) was 0.1352 (all data).
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