Table 1 |
|
Identification code |
phw1114 |
Empirical formula |
C45H63Cl9N12 |
Formula weight |
1091.12 |
Temperature/K |
109.9 |
|
triclinic |
Space group |
P-1 |
a/Å |
14.3898(12) |
b/Å |
14.5637(14) |
c/Å |
15.0840(10) |
α/° |
88.276(7) |
β/° |
63.722(8) |
γ/° |
71.729(9) |
Volume/Å3 |
2669.5(4) |
Z |
2 |
ρcalcmg/mm3 |
1.357 |
m/mm‑1 |
0.516 |
F(000) |
1140.000 |
|
0.2245 × 0.06 × 0.0362 |
Theta range for data collection |
5.76 to 58.06° |
Index ranges |
-19 ≤ h ≤ 19, -18 ≤ k ≤ 19, -19 ≤ l ≤ 20 |
Reflections collected |
17691 |
Independent reflections |
11923[R(int) = 0.0254] |
Data/restraints/parameters |
11923/0/647 |
Goodness-of-fit on F2 |
1.019 |
Final R indexes [I>2σ (I)] |
R1 = 0.0565, wR2 = 0.1016 |
Final R indexes [all data] |
R1 = 0.0895, wR2 = 0.1161 |
Largest diff. peak/hole / e Å-3 |
0.642/-0.481 |
Table 2 Fractional Atomic Coordinates (×104) and Equivalent Isotropic Displacement Parameters (Å2×103) for phw1114. Ueq is defined as 1/3 of of the trace of the orthogonalised UIJ tensor. |
||||
Atom |
x |
y |
z |
U(eq) |
C1 |
8823.3(19) |
1590.9(18) |
1418.6(17) |
12.9(5) |
C2 |
9797.1(19) |
1343.3(18) |
367.1(17) |
13.7(5) |
C3 |
10903.1(19) |
1214.4(18) |
346.7(17) |
14.8(5) |
C4 |
11104.6(19) |
537.3(19) |
1086.4(17) |
16.7(5) |
C5 |
10147.5(19) |
867.1(18) |
2137.4(17) |
14.4(5) |
C6 |
9096(2) |
886.5(18) |
2111.9(18) |
15.8(5) |
C7 |
7434(2) |
2164.7(19) |
795.9(18) |
16.3(5) |
C8 |
6353(2) |
2137.7(18) |
925.4(18) |
16.1(5) |
C9 |
6124(2) |
1604.0(19) |
363.5(18) |
17.8(5) |
C10 |
4964(2) |
1821(2) |
820.6(19) |
20.5(6) |
C11 |
4528(2) |
2478.9(19) |
1646.0(19) |
20.0(6) |
C12 |
12815(2) |
992(2) |
-927.0(18) |
21.4(6) |
C13 |
13597(2) |
654.0(19) |
-2004.0(18) |
18.2(5) |
C14 |
13850(2) |
1159(2) |
-2814.5(19) |
21.9(6) |
C15 |
14587(2) |
477(2) |
-3674.6(19) |
24.2(6) |
C16 |
14772(2) |
-430(2) |
-3373.2(19) |
24.4(6) |
C17 |
9604(2) |
456.5(19) |
3883.6(18) |
18.3(5) |
C18 |
9404(2) |
1446(2) |
4335.0(17) |
19.0(6) |
C19 |
10009(2) |
1771(2) |
4660.0(18) |
21.7(6) |
C20 |
9443(2) |
2778(2) |
5022.8(19) |
27.9(7) |
C21 |
8507(2) |
3032(2) |
4912(2) |
30.2(7) |
N1 |
7786.4(17) |
1557.0(17) |
1465.4(15) |
14.7(4) |
N2 |
5368.6(17) |
2664.9(17) |
1714.2(16) |
17.3(5) |
N3 |
11775.9(17) |
813.5(16) |
-678.7(15) |
16.6(5) |
N4 |
14170.8(19) |
-312.0(18) |
-2360.5(17) |
22.4(5) |
N5 |
10379.1(18) |
176.0(16) |
2807.0(15) |
16.4(5) |
N6 |
8491(2) |
2226.4(19) |
4489.8(17) |
26.6(6) |
C22 |
4641(2) |
4037.7(19) |
-1068.1(18) |
18.4(5) |
C23 |
4324(2) |
4957.8(19) |
-1522.7(17) |
18.0(5) |
C24 |
5175(2) |
4861.6(19) |
-2605.5(18) |
17.4(5) |
C25 |
6312(2) |
4661.5(19) |
-2668.2(18) |
18.5(5) |
C26 |
6645(2) |
3740.7(19) |
-2215.8(18) |
17.6(5) |
C27 |
5781(2) |
3828.9(19) |
-1138.1(17) |
17.9(5) |
C28 |
2788(2) |
4083(2) |
147(2) |
28.8(7) |
C29 |
2171(2) |
3895(2) |
1189(2) |
22.6(6) |
C30 |
1828(2) |
3121(2) |
1545(2) |
25.9(6) |
C31 |
1347(2) |
3279(2) |
2593(2) |
27.6(7) |
C32 |
1420(2) |
4131(2) |
2842(2) |
28.5(7) |
C33 |
3912(2) |
5934.8(19) |
-3202.7(18) |
17.9(5) |
C34 |
3872(2) |
6684.8(19) |
-3887.1(18) |
18.0(5) |
C35 |
4188(2) |
6578(2) |
-4896.0(19) |
23.7(6) |
C36 |
4091(2) |
7512(2) |
-5212(2) |
27.6(7) |
C37 |
3714(2) |
8162(2) |
-4394.3(19) |
23.4(6) |
C38 |
8102(2) |
2768(2) |
-1793(2) |
27.6(7) |
C39 |
9284(2) |
2526.5(19) |
-2031.5(19) |
21.2(6) |
C40 |
9833(2) |
3068(2) |
-1880(2) |
27.7(6) |
C41 |
10942(2) |
2464(2) |
-2230(2) |
26.8(6) |
C42 |
11037(2) |
1575(2) |
-2591(2) |
23.8(6) |
N7 |
3853.7(18) |
4125.5(18) |
-16.3(16) |
20.7(5) |
N8 |
1912.9(19) |
4513.4(19) |
1986.8(17) |
24.5(5) |
N9 |
4902.9(18) |
5756.1(16) |
-3054.4(16) |
17.4(5) |
N10 |
3591.0(18) |
7650.8(17) |
-3591.8(17) |
18.9(5) |
N11 |
7741.2(18) |
3598.4(16) |
-2281.4(17) |
18.9(5) |
N12 |
10023.6(18) |
1619.1(17) |
-2470.6(16) |
20.8(5) |
C43 |
7836(2) |
6826(2) |
-5456(2) |
30.6(7) |
Cl1 |
6556.5(6) |
6880.1(8) |
-5345.7(6) |
47.0(2) |
Cl2 |
7653.5(7) |
7556.6(7) |
-4446.5(6) |
46.0(2) |
Cl3 |
8642.0(9) |
5623.8(7) |
-5518.2(8) |
69.4(3) |
C44 |
6461(2) |
10390(2) |
-2725.3(19) |
25.1(6) |
Cl4 |
7478.0(6) |
10802.2(6) |
-3651.5(6) |
40.7(2) |
Cl5 |
5735.3(7) |
11233.8(7) |
-1643.1(6) |
43.6(2) |
Cl6 |
7081.9(6) |
9230.9(6) |
-2478.8(6) |
34.04(18) |
C45 |
9170(3) |
4527(2) |
1725(2) |
36.3(8) |
Cl7 |
8082.5(8) |
5631.5(6) |
1980.3(7) |
52.3(2) |
Cl8 |
9524.6(8) |
3909.2(6) |
570.6(6) |
48.0(2) |
Cl9 |
8776.9(6) |
3810.5(6) |
2692.5(6) |
34.47(18) |
Table 3 Anisotropic Displacement Parameters (Å2×103) for phw1114. The Anisotropic displacement factor exponent takes the form: -2π2[h2a*2U11+...+2hka×b×U12] |
||||||
Atom |
U11 |
U22 |
U33 |
U23 |
U13 |
U12 |
C1 |
13.5(12) |
12.1(12) |
14.5(12) |
2.2(9) |
-8.3(10) |
-3.3(10) |
C2 |
14.8(12) |
15.3(13) |
12.2(12) |
4.6(10) |
-7.8(10) |
-4.5(10) |
C3 |
12.5(12) |
17.3(13) |
11.4(12) |
0.9(10) |
-3.6(10) |
-3.5(10) |
C4 |
10.0(12) |
21.5(14) |
16.6(13) |
1(1) |
-6.3(10) |
-2.2(11) |
C5 |
14.5(12) |
14.7(13) |
14.0(12) |
3.1(10) |
-8.2(10) |
-2.3(10) |
C6 |
14.9(12) |
17.0(13) |
14.8(13) |
4.3(10) |
-7.5(11) |
-3.5(11) |
C7 |
14.0(12) |
19.4(14) |
15.6(13) |
7.9(10) |
-7.9(11) |
-4.4(11) |
C8 |
15.9(12) |
16.1(13) |
17.4(13) |
6.5(10) |
-9.8(11) |
-3.6(11) |
C9 |
16.6(13) |
19.9(14) |
14.3(13) |
3.4(10) |
-6.7(11) |
-3.5(11) |
C10 |
18.7(13) |
25.7(15) |
23.6(14) |
8.2(11) |
-13.2(12) |
-10.7(12) |
C11 |
14.2(13) |
23.8(15) |
23.4(14) |
9.0(11) |
-10.0(11) |
-6.7(11) |
C12 |
17.4(13) |
27.3(16) |
18.7(14) |
2.7(11) |
-5.9(11) |
-9.9(12) |
C13 |
13.5(12) |
22.3(15) |
20.9(14) |
5.0(11) |
-8.4(11) |
-7.9(11) |
C14 |
16.4(13) |
24.8(15) |
25.9(15) |
7.8(12) |
-10.8(12) |
-7.1(12) |
C15 |
20.4(14) |
37.2(18) |
15.5(14) |
7.6(12) |
-7.4(12) |
-12.0(13) |
C16 |
18.2(14) |
30.1(16) |
19.8(14) |
-4.0(12) |
-4.3(12) |
-7.6(12) |
C17 |
18.4(13) |
23.4(15) |
16.6(13) |
7.4(11) |
-10.7(11) |
-7.8(11) |
C18 |
18.0(13) |
24.2(15) |
9.9(12) |
5.2(10) |
-3.4(11) |
-5.6(12) |
C19 |
20.2(14) |
27.4(16) |
18.7(14) |
4.9(11) |
-8.5(12) |
-10.3(12) |
C20 |
32.7(16) |
31.1(17) |
18.3(14) |
-1.5(12) |
-6.6(13) |
-15.7(14) |
C21 |
31.6(17) |
25.9(17) |
22.0(15) |
-6.4(12) |
-7.9(13) |
-1.0(13) |
N1 |
14.5(11) |
15.7(12) |
15.8(11) |
5.2(9) |
-9.2(9) |
-4.5(9) |
N2 |
14.6(11) |
17.1(12) |
18.1(11) |
0.8(9) |
-7.5(9) |
-2.6(9) |
N3 |
12.9(11) |
22.4(12) |
12.7(11) |
2.6(9) |
-4.9(9) |
-5.0(9) |
N4 |
21.6(12) |
23.3(13) |
18.9(12) |
7.4(10) |
-6.7(10) |
-7.3(11) |
N5 |
12.9(11) |
21.3(12) |
14.9(11) |
3.4(9) |
-8.7(9) |
-2.4(9) |
N6 |
20.9(13) |
30.7(15) |
24.1(13) |
-1.5(10) |
-11.5(11) |
-1.2(11) |
C22 |
19.8(13) |
19.3(14) |
15.7(13) |
5(1) |
-8.1(11) |
-6.4(11) |
C23 |
16.0(13) |
20.6(14) |
16.0(13) |
4.1(10) |
-8.3(11) |
-2.9(11) |
C24 |
19.1(13) |
16.4(14) |
15.5(13) |
3.4(10) |
-9.3(11) |
-2.5(11) |
C25 |
16.8(13) |
19.9(14) |
15.9(13) |
4.8(10) |
-7.1(11) |
-3.2(11) |
C26 |
16.9(13) |
17.2(14) |
16.4(13) |
2.2(10) |
-7.8(11) |
-2.5(11) |
C27 |
19.0(13) |
18.5(14) |
16.4(13) |
4.8(10) |
-10.1(11) |
-3.8(11) |
C28 |
23.1(15) |
44.2(19) |
24.0(15) |
12.6(13) |
-12.8(13) |
-15.1(14) |
C29 |
15.3(13) |
30.1(16) |
23.1(14) |
7.8(12) |
-9.3(12) |
-7.9(12) |
C30 |
19.6(14) |
29.5(17) |
31.6(16) |
5.4(13) |
-13.7(13) |
-9.3(13) |
C31 |
20.3(14) |
34.0(18) |
29.5(16) |
14.1(13) |
-10.0(13) |
-13.3(13) |
C32 |
20.3(14) |
37.1(18) |
20.0(15) |
6.1(13) |
-5.6(12) |
-5.3(13) |
C33 |
15.4(13) |
17.5(14) |
19.8(13) |
3.2(10) |
-9.5(11) |
-1.9(11) |
C34 |
14.1(12) |
21.3(14) |
18.7(13) |
4.1(11) |
-10.0(11) |
-2.3(11) |
C35 |
19.1(14) |
29.6(16) |
21.4(14) |
1.4(12) |
-12.8(12) |
-1.2(12) |
C36 |
20.4(15) |
39.4(19) |
16.9(15) |
10.1(13) |
-9.2(12) |
-1.9(13) |
C37 |
15.0(13) |
27.1(16) |
26.3(15) |
13.6(12) |
-9.9(12) |
-4.8(12) |
C38 |
23.1(15) |
24.3(16) |
40.9(18) |
16.8(13) |
-19.4(14) |
-8.8(13) |
C39 |
20.0(14) |
18.2(14) |
26.2(15) |
9.7(11) |
-13.2(12) |
-4.1(11) |
C40 |
31.2(16) |
18.9(15) |
38.0(17) |
6.3(12) |
-20.1(14) |
-8.5(13) |
C41 |
26.8(15) |
26.6(16) |
37.2(17) |
16.1(13) |
-21.0(14) |
-13.5(13) |
C42 |
19.0(14) |
23.8(15) |
26.4(15) |
8.7(12) |
-9.8(12) |
-5.8(12) |
N7 |
20.0(12) |
24.8(13) |
19.2(12) |
12(1) |
-10.7(10) |
-8.1(10) |
N8 |
21.5(12) |
21.7(14) |
28.2(13) |
7.5(11) |
-10.2(11) |
-6.6(11) |
N9 |
14.0(11) |
21.2(12) |
15.5(12) |
6.6(9) |
-7.6(10) |
-3.2(10) |
N10 |
18.9(12) |
20.6(13) |
14.0(12) |
3.6(9) |
-7.2(10) |
-3.1(10) |
N11 |
14.5(11) |
19.7(12) |
17.0(12) |
4.9(9) |
-6.2(10) |
-0.6(9) |
N12 |
20.8(12) |
18.9(13) |
26.6(13) |
6(1) |
-14.1(10) |
-7.3(10) |
C43 |
22.3(15) |
37.3(19) |
27.0(16) |
2.4(13) |
-9.3(13) |
-6.3(14) |
Cl1 |
25.9(4) |
81.0(7) |
36.3(5) |
2.0(4) |
-15.4(4) |
-18.3(4) |
Cl2 |
41.0(5) |
44.3(5) |
54.1(5) |
-10.5(4) |
-26.8(4) |
-6.6(4) |
Cl3 |
73.9(7) |
41.0(6) |
90.3(8) |
-21.7(5) |
-57.1(6) |
16.6(5) |
C44 |
20.1(14) |
33.4(17) |
21.2(14) |
0.6(12) |
-10.4(12) |
-6.4(13) |
Cl4 |
31.6(4) |
48.0(5) |
37.5(4) |
23.8(4) |
-14.5(4) |
-10.3(4) |
Cl5 |
43.6(5) |
46.6(5) |
35.3(4) |
-12.6(4) |
-17.0(4) |
-8.5(4) |
Cl6 |
32.7(4) |
31.1(4) |
42.1(4) |
11.8(3) |
-17.6(4) |
-15.3(3) |
C45 |
34.3(18) |
29.4(18) |
46(2) |
0.6(15) |
-17.0(16) |
-14.1(15) |
Cl7 |
66.3(6) |
22.4(4) |
64.3(6) |
-1.9(4) |
-30.1(5) |
-8.7(4) |
Cl8 |
68.6(6) |
28.2(5) |
36.7(5) |
4.2(3) |
-18.3(4) |
-11.3(4) |
Cl9 |
34.7(4) |
37.3(5) |
38.0(4) |
2.7(3) |
-21.7(4) |
-12.6(4) |
Table 4 Bond Lengths for phw1114. |
||||||
Atom |
Atom |
Length/Å |
|
Atom |
Atom |
Length/Å |
C1 |
C2 |
1.536(3) |
|
C24 |
N9 |
1.473(3) |
C1 |
C6 |
1.532(3) |
|
C25 |
C26 |
1.525(3) |
C1 |
N1 |
1.479(3) |
|
C26 |
C27 |
1.525(3) |
C2 |
C3 |
1.529(3) |
|
C26 |
N11 |
1.484(3) |
C3 |
C4 |
1.530(3) |
|
C28 |
C29 |
1.492(4) |
C3 |
N3 |
1.478(3) |
|
C28 |
N7 |
1.463(3) |
C4 |
C5 |
1.529(3) |
|
C29 |
C30 |
1.370(4) |
C5 |
C6 |
1.521(3) |
|
C29 |
N8 |
1.363(4) |
C5 |
N5 |
1.473(3) |
|
C30 |
C31 |
1.409(4) |
C7 |
C8 |
1.492(3) |
|
C31 |
C32 |
1.356(4) |
C7 |
N1 |
1.476(3) |
|
C32 |
N8 |
1.368(3) |
C8 |
C9 |
1.371(3) |
|
C33 |
C34 |
1.486(3) |
C8 |
N2 |
1.376(3) |
|
C33 |
N9 |
1.483(3) |
C9 |
C10 |
1.423(3) |
|
C34 |
C35 |
1.380(3) |
C10 |
C11 |
1.366(4) |
|
C34 |
N10 |
1.365(3) |
C11 |
N2 |
1.365(3) |
|
C35 |
C36 |
1.414(4) |
C12 |
C13 |
1.493(3) |
|
C36 |
C37 |
1.367(4) |
C12 |
N3 |
1.479(3) |
|
C37 |
N10 |
1.375(3) |
C13 |
C14 |
1.374(3) |
|
C38 |
C39 |
1.496(4) |
C13 |
N4 |
1.369(3) |
|
C38 |
N11 |
1.472(3) |
C14 |
C15 |
1.412(4) |
|
C39 |
C40 |
1.364(4) |
C15 |
C16 |
1.368(4) |
|
C39 |
N12 |
1.366(3) |
C16 |
N4 |
1.365(3) |
|
C40 |
C41 |
1.415(4) |
C17 |
C18 |
1.500(4) |
|
C41 |
C42 |
1.362(4) |
C17 |
N5 |
1.483(3) |
|
C42 |
N12 |
1.368(3) |
C18 |
C19 |
1.368(4) |
|
C43 |
Cl1 |
1.750(3) |
C18 |
N6 |
1.371(3) |
|
C43 |
Cl2 |
1.757(3) |
C19 |
C20 |
1.421(4) |
|
C43 |
Cl3 |
1.749(3) |
C20 |
C21 |
1.364(4) |
|
C44 |
Cl4 |
1.773(3) |
C21 |
N6 |
1.364(4) |
|
C44 |
Cl5 |
1.753(3) |
C22 |
C23 |
1.520(3) |
|
C44 |
Cl6 |
1.760(3) |
C22 |
C27 |
1.527(3) |
|
C45 |
Cl7 |
1.763(3) |
C22 |
N7 |
1.465(3) |
|
C45 |
Cl8 |
1.766(3) |
C23 |
C24 |
1.524(3) |
|
C45 |
Cl9 |
1.757(3) |
C24 |
C25 |
1.528(3) |
|
|
|
|
Table 5 Bond Angles for phw1114. |
||||||||
Atom |
Atom |
Atom |
Angle/˚ |
|
Atom |
Atom |
Atom |
Angle/˚ |
C6 |
C1 |
C2 |
110.5(2) |
|
N9 |
C24 |
C23 |
111.3(2) |
N1 |
C1 |
C2 |
114.59(19) |
|
N9 |
C24 |
C25 |
108.7(2) |
N1 |
C1 |
C6 |
107.21(19) |
|
C26 |
C25 |
C24 |
111.4(2) |
C3 |
C2 |
C1 |
114.05(19) |
|
C25 |
C26 |
C27 |
109.9(2) |
C2 |
C3 |
C4 |
112.08(19) |
|
N11 |
C26 |
C25 |
108.8(2) |
N3 |
C3 |
C2 |
107.85(19) |
|
N11 |
C26 |
C27 |
111.4(2) |
N3 |
C3 |
C4 |
110.1(2) |
|
C26 |
C27 |
C22 |
111.2(2) |
C5 |
C4 |
C3 |
111.5(2) |
|
N7 |
C28 |
C29 |
110.0(2) |
C6 |
C5 |
C4 |
109.03(19) |
|
C30 |
C29 |
C28 |
130.8(3) |
N5 |
C5 |
C4 |
108.9(2) |
|
N8 |
C29 |
C28 |
121.3(2) |
N5 |
C5 |
C6 |
110.12(19) |
|
N8 |
C29 |
C30 |
107.8(2) |
C5 |
C6 |
C1 |
112.14(19) |
|
C29 |
C30 |
C31 |
107.5(3) |
N1 |
C7 |
C8 |
111.00(19) |
|
C32 |
C31 |
C30 |
107.2(2) |
C9 |
C8 |
C7 |
129.9(2) |
|
C31 |
C32 |
N8 |
108.6(3) |
C9 |
C8 |
N2 |
107.3(2) |
|
N9 |
C33 |
C34 |
109.8(2) |
N2 |
C8 |
C7 |
122.7(2) |
|
C35 |
C34 |
C33 |
130.0(3) |
C8 |
C9 |
C10 |
107.8(2) |
|
N10 |
C34 |
C33 |
122.2(2) |
C11 |
C10 |
C9 |
106.9(2) |
|
N10 |
C34 |
C35 |
107.4(2) |
N2 |
C11 |
C10 |
108.5(2) |
|
C34 |
C35 |
C36 |
107.6(3) |
N3 |
C12 |
C13 |
110.0(2) |
|
C37 |
C36 |
C35 |
107.4(2) |
C14 |
C13 |
C12 |
131.1(3) |
|
C36 |
C37 |
N10 |
107.9(3) |
N4 |
C13 |
C12 |
122.1(2) |
|
N11 |
C38 |
C39 |
111.8(2) |
N4 |
C13 |
C14 |
106.7(2) |
|
C40 |
C39 |
C38 |
131.6(3) |
C13 |
C14 |
C15 |
107.9(2) |
|
C40 |
C39 |
N12 |
107.7(2) |
C16 |
C15 |
C14 |
107.5(2) |
|
N12 |
C39 |
C38 |
120.8(2) |
N4 |
C16 |
C15 |
107.4(2) |
|
C39 |
C40 |
C41 |
107.5(3) |
N5 |
C17 |
C18 |
117.0(2) |
|
C42 |
C41 |
C40 |
107.5(2) |
C19 |
C18 |
C17 |
131.0(2) |
|
C41 |
C42 |
N12 |
107.7(3) |
C19 |
C18 |
N6 |
107.1(2) |
|
C28 |
N7 |
C22 |
114.2(2) |
N6 |
C18 |
C17 |
121.9(2) |
|
C29 |
N8 |
C32 |
108.9(2) |
C18 |
C19 |
C20 |
107.9(3) |
|
C24 |
N9 |
C33 |
113.9(2) |
C21 |
C20 |
C19 |
107.0(3) |
|
C34 |
N10 |
C37 |
109.7(2) |
N6 |
C21 |
C20 |
108.0(3) |
|
C38 |
N11 |
C26 |
113.1(2) |
C7 |
N1 |
C1 |
114.09(19) |
|
C39 |
N12 |
C42 |
109.6(2) |
C11 |
N2 |
C8 |
109.5(2) |
|
Cl1 |
C43 |
Cl2 |
110.00(16) |
C3 |
N3 |
C12 |
114.21(19) |
|
Cl3 |
C43 |
Cl1 |
110.98(17) |
C16 |
N4 |
C13 |
110.5(2) |
|
Cl3 |
C43 |
Cl2 |
110.36(17) |
C5 |
N5 |
C17 |
115.9(2) |
|
Cl5 |
C44 |
Cl4 |
109.19(16) |
C21 |
N6 |
C18 |
110.0(3) |
|
Cl5 |
C44 |
Cl6 |
110.87(15) |
C23 |
C22 |
C27 |
110.8(2) |
|
Cl6 |
C44 |
Cl4 |
109.96(15) |
N7 |
C22 |
C23 |
111.3(2) |
|
Cl7 |
C45 |
Cl8 |
109.13(19) |
N7 |
C22 |
C27 |
108.3(2) |
|
Cl9 |
C45 |
Cl7 |
109.90(17) |
C22 |
C23 |
C24 |
110.3(2) |
|
Cl9 |
C45 |
Cl8 |
111.13(17) |
C23 |
C24 |
C25 |
110.0(2) |
|
|
|
|
|
Table 6 Torsion Angles for phw1114. |
||||
A |
B |
C |
D |
Angle/˚ |
C1 |
C2 |
C3 |
C4 |
48.8(3) |
C1 |
C2 |
C3 |
N3 |
170.20(19) |
C2 |
C1 |
C6 |
C5 |
55.2(3) |
C2 |
C1 |
N1 |
C7 |
-54.2(3) |
C2 |
C3 |
C4 |
C5 |
-53.3(3) |
C2 |
C3 |
N3 |
C12 |
157.8(2) |
C3 |
C4 |
C5 |
C6 |
58.6(3) |
C3 |
C4 |
C5 |
N5 |
178.8(2) |
C4 |
C3 |
N3 |
C12 |
-79.6(3) |
C4 |
C5 |
C6 |
C1 |
-60.2(3) |
C4 |
C5 |
N5 |
C17 |
172.3(2) |
C6 |
C1 |
C2 |
C3 |
-49.1(3) |
C6 |
C1 |
N1 |
C7 |
-177.2(2) |
C6 |
C5 |
N5 |
C17 |
-68.3(3) |
C7 |
C8 |
C9 |
C10 |
178.2(2) |
C7 |
C8 |
N2 |
C11 |
-178.7(2) |
C8 |
C7 |
N1 |
C1 |
-176.8(2) |
C8 |
C9 |
C10 |
C11 |
-0.1(3) |
C9 |
C8 |
N2 |
C11 |
-0.8(3) |
C9 |
C10 |
C11 |
N2 |
-0.4(3) |
C10 |
C11 |
N2 |
C8 |
0.8(3) |
C12 |
C13 |
C14 |
C15 |
-175.8(3) |
C12 |
C13 |
N4 |
C16 |
176.1(2) |
C13 |
C12 |
N3 |
C3 |
-174.1(2) |
C13 |
C14 |
C15 |
C16 |
0.0(3) |
C14 |
C13 |
N4 |
C16 |
-0.4(3) |
C14 |
C15 |
C16 |
N4 |
-0.2(3) |
C15 |
C16 |
N4 |
C13 |
0.3(3) |
C17 |
C18 |
C19 |
C20 |
180.0(2) |
C17 |
C18 |
N6 |
C21 |
179.6(2) |
C18 |
C17 |
N5 |
C5 |
-53.2(3) |
C18 |
C19 |
C20 |
C21 |
0.4(3) |
C19 |
C18 |
N6 |
C21 |
-0.4(3) |
C19 |
C20 |
C21 |
N6 |
-0.6(3) |
C20 |
C21 |
N6 |
C18 |
0.7(3) |
N1 |
C1 |
C2 |
C3 |
-170.4(2) |
N1 |
C1 |
C6 |
C5 |
-179.27(19) |
N1 |
C7 |
C8 |
C9 |
-99.6(3) |
N1 |
C7 |
C8 |
N2 |
77.8(3) |
N2 |
C8 |
C9 |
C10 |
0.5(3) |
N3 |
C3 |
C4 |
C5 |
-173.35(19) |
N3 |
C12 |
C13 |
C14 |
98.9(3) |
N3 |
C12 |
C13 |
N4 |
-76.6(3) |
N4 |
C13 |
C14 |
C15 |
0.2(3) |
N5 |
C5 |
C6 |
C1 |
-179.6(2) |
N5 |
C17 |
C18 |
C19 |
-80.4(3) |
N5 |
C17 |
C18 |
N6 |
99.5(3) |
N6 |
C18 |
C19 |
C20 |
0.0(3) |
C22 |
C23 |
C24 |
C25 |
-57.8(3) |
C22 |
C23 |
C24 |
N9 |
-178.3(2) |
C23 |
C22 |
C27 |
C26 |
-57.0(3) |
C23 |
C22 |
N7 |
C28 |
72.5(3) |
C23 |
C24 |
C25 |
C26 |
58.0(3) |
C23 |
C24 |
N9 |
C33 |
-69.0(3) |
C24 |
C25 |
C26 |
C27 |
-56.8(3) |
C24 |
C25 |
C26 |
N11 |
-178.9(2) |
C25 |
C24 |
N9 |
C33 |
169.7(2) |
C25 |
C26 |
C27 |
C22 |
56.0(3) |
C25 |
C26 |
N11 |
C38 |
175.5(2) |
C27 |
C22 |
C23 |
C24 |
57.6(3) |
C27 |
C22 |
N7 |
C28 |
-165.5(2) |
C27 |
C26 |
N11 |
C38 |
54.3(3) |
C28 |
C29 |
C30 |
C31 |
176.0(3) |
C28 |
C29 |
N8 |
C32 |
-175.8(2) |
C29 |
C28 |
N7 |
C22 |
164.0(2) |
C29 |
C30 |
C31 |
C32 |
-0.6(3) |
C30 |
C29 |
N8 |
C32 |
0.6(3) |
C30 |
C31 |
C32 |
N8 |
1.0(3) |
C31 |
C32 |
N8 |
C29 |
-1.0(3) |
C33 |
C34 |
C35 |
C36 |
-173.8(3) |
C33 |
C34 |
N10 |
C37 |
174.8(2) |
C34 |
C33 |
N9 |
C24 |
-165.2(2) |
C34 |
C35 |
C36 |
C37 |
-0.3(3) |
C35 |
C34 |
N10 |
C37 |
0.5(3) |
C35 |
C36 |
C37 |
N10 |
0.6(3) |
C36 |
C37 |
N10 |
C34 |
-0.7(3) |
C38 |
C39 |
C40 |
C41 |
178.5(3) |
C38 |
C39 |
N12 |
C42 |
-178.7(2) |
C39 |
C38 |
N11 |
C26 |
169.3(2) |
C39 |
C40 |
C41 |
C42 |
0.5(3) |
C40 |
C39 |
N12 |
C42 |
0.6(3) |
C40 |
C41 |
C42 |
N12 |
-0.1(3) |
C41 |
C42 |
N12 |
C39 |
-0.3(3) |
N7 |
C22 |
C23 |
C24 |
178.1(2) |
N7 |
C22 |
C27 |
C26 |
-179.3(2) |
N7 |
C28 |
C29 |
C30 |
-116.4(3) |
N7 |
C28 |
C29 |
N8 |
59.1(4) |
N8 |
C29 |
C30 |
C31 |
0.0(3) |
N9 |
C24 |
C25 |
C26 |
-179.9(2) |
N9 |
C33 |
C34 |
C35 |
98.4(3) |
N9 |
C33 |
C34 |
N10 |
-74.5(3) |
N10 |
C34 |
C35 |
C36 |
-0.1(3) |
N11 |
C26 |
C27 |
C22 |
176.5(2) |
N11 |
C38 |
C39 |
C40 |
58.8(4) |
N11 |
C38 |
C39 |
N12 |
-122.1(3) |
N12 |
C39 |
C40 |
C41 |
-0.6(3) |
Table 7 Hydrogen Atom Coordinates (Å×104) and Isotropic Displacement Parameters (Å2×103) for phw1114. |
||||
Atom |
x |
y |
z |
U(eq) |
H1 |
8689 |
2265 |
1687 |
15 |
H2A |
9849 |
734 |
46 |
16 |
H2B |
9650 |
1870 |
-33 |
16 |
H3 |
10916 |
1867 |
518 |
18 |
H4A |
11203 |
-134 |
864 |
20 |
H4B |
11790 |
528 |
1098 |
20 |
H5 |
10066 |
1534 |
2377 |
17 |
H6A |
8479 |
1084 |
2795 |
19 |
H6B |
9179 |
222 |
1884 |
19 |
H7A |
7995 |
1925 |
95 |
20 |
H7B |
7371 |
2846 |
941 |
20 |
H9A |
6647 |
1167 |
-226 |
21 |
H10A |
4568 |
1559 |
595 |
25 |
H11A |
3769 |
2760 |
2097 |
24 |
H12A |
13148 |
639 |
-511 |
26 |
H12B |
12663 |
1697 |
-783 |
26 |
H14 |
13576 |
1846 |
-2799 |
26 |
H15 |
14899 |
621 |
-4341 |
29 |
H16 |
15233 |
-1031 |
-3791 |
29 |
H17A |
9882 |
-34 |
4255 |
22 |
H17B |
8887 |
419 |
3990 |
22 |
H19 |
10687 |
1390 |
4646 |
26 |
H20 |
9673 |
3195 |
5292 |
34 |
H21 |
7963 |
3661 |
5097 |
36 |
H22 |
4651 |
3476 |
-1442 |
22 |
H23A |
4276 |
5525 |
-1139 |
22 |
H23B |
3593 |
5070 |
-1488 |
22 |
H24 |
5195 |
4303 |
-2992 |
21 |
H25A |
6860 |
4588 |
-3375 |
22 |
H25B |
6306 |
5224 |
-2310 |
22 |
H26 |
6694 |
3170 |
-2607 |
21 |
H27A |
5767 |
4362 |
-735 |
21 |
H27B |
5981 |
3215 |
-861 |
21 |
H28A |
2901 |
3557 |
-328 |
35 |
H28B |
2357 |
4708 |
28 |
35 |
H30 |
1902 |
2578 |
1156 |
31 |
H31 |
1030 |
2866 |
3042 |
33 |
H32 |
1171 |
4416 |
3501 |
34 |
H33A |
3243 |
6160 |
-2553 |
22 |
H33B |
3933 |
5321 |
-3488 |
22 |
H35 |
4429 |
5984 |
-5304 |
28 |
H37 |
3564 |
8846 |
-4383 |
28 |
H38A |
7996 |
2191 |
-2013 |
33 |
H38B |
7641 |
2926 |
-1062 |
33 |
H40 |
9527 |
3730 |
-1592 |
33 |
H41 |
11516 |
2645 |
-2217 |
32 |
H42 |
11690 |
1024 |
-2876 |
29 |
H43 |
8227 |
7086 |
-6085 |
37 |
H44 |
5937 |
10342 |
-2975 |
30 |
H45 |
9821 |
4676 |
1678 |
44 |
H1A |
7840(20) |
1000(20) |
1330(20) |
30(9) |
H2 |
5300(20) |
3080(20) |
2130(20) |
32(9) |
H3A |
11540(20) |
1096(19) |
-1080(19) |
14(7) |
H4 |
14170(20) |
-750(20) |
-2010(20) |
20(8) |
H5A |
11040(20) |
112(19) |
2744(18) |
17(7) |
H6 |
7990(20) |
2190(20) |
4430(20) |
29(9) |
H7 |
4090(20) |
3670(20) |
235(19) |
18(8) |
H8 |
2070(30) |
5010(20) |
1980(20) |
37(10) |
H9 |
5420(20) |
5740(20) |
-3580(20) |
34(9) |
H10 |
3300(20) |
7900(20) |
-3010(20) |
23(8) |
H11 |
8200(30) |
3470(20) |
-2880(20) |
40(10) |
H12 |
9840(20) |
1140(20) |
-2600(20) |
25(8) |
H36 |
4260(20) |
7650(20) |
-5840(20) |
30(8) |
[RSC
Journal Format]
Experimental
Single
crystals of C45H63Cl9N12 [phw1114] were [].
A suitable crystal was selected and mounted on a Oxford
Diffraction SuperNova diffractometer. The crystal was kept at 109.9 K.
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.
[1] O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H.
Puschmann, OLEX2: a complete structure solution, refinement and analysis
program. J. Appl. Cryst. (2009). 42, 339-341.
[2] XS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122
[3] XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122
Crystal
structure determination of [phw1114]
Crystal
Data. C45H63Cl9N12,
M =1091.12, triclinic, a =
14.3898(12) Å, b = 14.5637(14) Å, c =
15.0840(10) Å, α = 88.276(7)°, β =
63.722(8)°, γ = 71.729(9)°, U =
2669.5(4) Å3, T = 109.9, space group P-1 (no.
2), Z = 2, μ(Mo Kα) = 0.516, 17691 reflections
measured, 11923 unique (Rint = 0.0254) which were used
in all calculations. The final wR(F2) was 0.1161 (all
data).
This report has been
created with Olex2, compiled on 2011.08.18 svn.r1932. Please let us know if
there are any errors or if you would like to have additional featrues.