Identification code | phw1115 |
Empirical formula | C27H30Cl3N3O3 |
Formula weight | 550.89 |
Temperature/K | 110.00(10) |
Crystal system | trigonal |
Space group | P31c |
a/Å | 13.8281(3) |
b/Å | 13.8281(3) |
c/Å | 8.2311(2) |
α/° | 90.00 |
β/° | 90.00 |
γ/° | 120.00 |
Volume/Å3 | 1363.07(6) |
Z | 2 |
ρcalcmg/mm3 | 1.342 |
m/mm‑1 | 0.370 |
F(000) | 576 |
Crystal size/mm3 | 0.3051 × 0.1453 × 0.116 |
2Θ range for data collection | 5.9 to 64.54° |
Index ranges | -19 ≤ h ≤ 20, -20 ≤ k ≤ 20, -12 ≤ l ≤ 12 |
Reflections collected | 8234 |
Independent reflections | 2940[R(int) = 0.0270] |
Data/restraints/parameters | 2940/1/117 |
Goodness-of-fit on F2 | 1.111 |
Final R indexes [I>=2σ (I)] | R1 = 0.0404, wR2 = 0.1014 |
Final R indexes [all data] | R1 = 0.0463, wR2 = 0.1057 |
Largest diff. peak/hole / e Å-3 | 0.324/-0.241 |
Flack Parameter | 0.02(7) |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
C1 | 4301.7(14) | 13113.2(14) | 2162.2(19) | 24.1(3) |
C2 | 4678.6(16) | 12364.0(15) | 2439(2) | 30.9(4) |
C3 | 4004.2(17) | 11366.8(15) | 3264(2) | 33.7(4) |
C4 | 2961.3(17) | 11131.0(14) | 3769(2) | 31.7(4) |
C5 | 2559.5(15) | 11859.4(14) | 3480(2) | 28.4(3) |
C6 | 3232.8(14) | 12863.0(13) | 2677.9(19) | 23.7(3) |
C7 | 2830.1(13) | 13675.3(14) | 2348(2) | 25.7(3) |
C8 | 3501.1(12) | 15700.4(12) | 2060.6(17) | 20.7(3) |
C9 | 2375.2(12) | 15541.4(12) | 2612(2) | 22.6(3) |
Cl1 | 2137.5(5) | 9920.5(4) | 4896.4(8) | 47.85(16) |
N1 | 3729.3(11) | 14832.8(11) | 2668.1(18) | 22.2(3) |
O1 | 4981.7(10) | 14094.3(11) | 1378.3(16) | 28.4(2) |
Atom | U11 | U22 | U33 | U23 | U13 | U12 |
---|---|---|---|---|---|---|
C1 | 25.3(7) | 23.4(7) | 25.3(7) | -5.6(6) | -4.3(6) | 13.3(6) |
C2 | 30.7(8) | 29.3(8) | 39.2(9) | -11.4(7) | -7.5(7) | 19.9(7) |
C3 | 47.9(10) | 29.3(8) | 32.9(9) | -9.2(7) | -10.2(8) | 26.0(8) |
C4 | 43.8(10) | 19.4(7) | 29.6(8) | -3.4(6) | -6.1(7) | 13.9(7) |
C5 | 30.4(8) | 23.2(7) | 29.5(7) | -4.5(6) | -2.4(7) | 11.9(6) |
C6 | 24.2(7) | 20.2(7) | 26.6(7) | -4.9(5) | -4.8(6) | 11.0(6) |
C7 | 20.1(7) | 19.9(7) | 36.5(8) | -2.1(6) | -5.1(6) | 9.5(6) |
C8 | 20.5(6) | 19.4(6) | 22.7(7) | -0.7(5) | -0.8(5) | 10.4(6) |
C9 | 19.8(6) | 20.6(7) | 27.5(7) | 0.4(6) | -0.6(5) | 10.2(6) |
Cl1 | 68.0(4) | 24.6(2) | 44.5(3) | 5.3(2) | 0.6(3) | 18.3(2) |
N1 | 22.3(6) | 20.0(6) | 25.0(6) | -1.7(5) | -2.9(5) | 11.1(5) |
O1 | 24.9(6) | 27.9(6) | 34.0(6) | -1.8(5) | 1.9(5) | 14.3(5) |
Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
---|---|---|---|---|---|---|
C1 | C2 | 1.392(2) | C5 | C6 | 1.392(2) | |
C1 | C6 | 1.405(2) | C6 | C7 | 1.507(2) | |
C1 | O1 | 1.366(2) | C7 | N1 | 1.479(2) | |
C2 | C3 | 1.395(3) | C8 | C9 | 1.528(2) | |
C3 | C4 | 1.374(3) | C8 | C91 | 1.530(2) | |
C4 | C5 | 1.393(2) | C8 | N1 | 1.4723(19) | |
C4 | Cl1 | 1.7477(18) | C9 | C82 | 1.530(2) |
Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
---|---|---|---|---|---|---|---|---|
C2 | C1 | C6 | 120.45(16) | C1 | C6 | C7 | 119.83(15) | |
O1 | C1 | C2 | 119.26(16) | C5 | C6 | C1 | 119.07(15) | |
O1 | C1 | C6 | 120.29(14) | C5 | C6 | C7 | 121.10(16) | |
C1 | C2 | C3 | 120.10(18) | N1 | C7 | C6 | 110.52(13) | |
C4 | C3 | C2 | 119.03(16) | C9 | C8 | C91 | 110.91(14) | |
C3 | C4 | C5 | 121.85(17) | N1 | C8 | C9 | 113.57(12) | |
C3 | C4 | Cl1 | 119.47(14) | N1 | C8 | C91 | 107.80(12) | |
C5 | C4 | Cl1 | 118.60(15) | C8 | C9 | C82 | 112.26(14) | |
C6 | C5 | C4 | 119.50(17) | C8 | N1 | C7 | 114.49(13) |
D | H | A | d(D-H)/Å | d(H-A)/Å | d(D-A)/Å | D-H-A/° |
---|---|---|---|---|---|---|
O1 | H1A | N1 | 0.78(3) | 1.91(3) | 2.6340(19) | 154(3) |
A | B | C | D | Angle/˚ |
---|---|---|---|---|
C1 | C2 | C3 | C4 | 1.1(2) |
C1 | C6 | C7 | N1 | -42.5(2) |
C2 | C1 | C6 | C5 | 0.5(2) |
C2 | C1 | C6 | C7 | -179.13(15) |
C2 | C3 | C4 | C5 | 0.0(3) |
C2 | C3 | C4 | Cl1 | -176.62(14) |
C3 | C4 | C5 | C6 | -0.9(3) |
C4 | C5 | C6 | C1 | 0.6(2) |
C4 | C5 | C6 | C7 | -179.78(15) |
C5 | C6 | C7 | N1 | 137.89(16) |
C6 | C1 | C2 | C3 | -1.3(2) |
C6 | C7 | N1 | C8 | 167.77(13) |
C91 | C8 | C9 | C82 | 54.4(2) |
C91 | C8 | N1 | C7 | 175.32(13) |
C9 | C8 | N1 | C7 | 52.02(17) |
Cl1 | C4 | C5 | C6 | 175.78(13) |
N1 | C8 | C9 | C82 | 175.99(11) |
O1 | C1 | C2 | C3 | 178.85(15) |
O1 | C1 | C6 | C5 | -179.73(14) |
O1 | C1 | C6 | C7 | 0.7(2) |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
H2 | 5396 | 12532 | 2067 | 37 |
H3 | 4262 | 10858 | 3473 | 40 |
H5 | 1831 | 11673 | 3828 | 34 |
H7A | 2588 | 13607 | 1201 | 31 |
H7B | 2180 | 13495 | 3050 | 31 |
H8 | 3504 | 15680 | 846 | 25 |
H9A | 2331 | 15489 | 3812 | 27 |
H9B | 1769 | 14830 | 2166 | 27 |
H1 | 3862(16) | 14918(15) | 3590(20) | 11(4) |
H1A | 4760(20) | 14490(20) | 1630(30) | 32(6) |
[RSC Journal Format]
Experimental
Single crystals of C27H30Cl3N3O3 [phw1115] were []. A suitable crystal was selected and on a SuperNova, Single source at offset), Eos diffractometer. The crystal was kept at 110.00(10) K during data collection. Using Olex2 [1], the structure was solved with the XS [2] structure solution program using Direct Methods and refined with the XL [3] refinement package using Least Squares minimisation.
Crystal structure determination of [phw1115]
Crystal Data. C27H30Cl3N3O3, M =550.89, trigonal, a = 13.8281(3) Å, c = 8.2311(2) Å, U = 1363.07(6) Å3, T = 110.00(10), space group P31c (no. 159), Z = 2, μ(Mo Kα) = 0.370, 8234 reflections measured, 2940 unique (Rint = 0.0270) which were used in all calculations. The final wR(F2) was 0.1057 (all data).
This report has been created with Olex2, compiled on 2011.09.07 svn.r1971. Please let us know if there are any errors or if you would like to have additional featrues.