Table
1 Crystal data and structure refinement for phw1202 |
|
Identification
code |
phw1202
|
Empirical
formula |
C24H26.4977Cl2N6Ru
|
Formula
weight |
570.98
|
Temperature/K
|
110.00(10)
|
Crystal
system |
triclinic
|
Space
group |
P-1
|
a/Å
|
10.5125(7)
|
b/Å
|
12.8761(8)
|
c/Å
|
13.0224(9)
|
α/°
|
102.955(6)
|
β/°
|
110.920(6)
|
γ/°
|
107.384(6)
|
Volume/Å3
|
1459.07(16)
|
Z |
2 |
ρcalcmg/mm3 |
1.300
|
m/mm‑1
|
0.741
|
F(000)
|
581.0
|
Crystal
size/mm3 |
0.2465
× 0.1333 × 0.0709 |
2Θ
range for data collection |
5.94
to 64.28° |
Index
ranges |
-9
≤ h ≤ 15, -18 ≤ k ≤ 14, -18 ≤ l ≤ 16 |
Reflections
collected |
15679
|
Independent
reflections |
9142[R(int) = 0.0248] |
Data/restraints/parameters
|
9142/0/308
|
Goodness-of-fit
on F2 |
1.032
|
Final
R indexes [I>=2σ (I)] |
R1
= 0.0491, wR2 = 0.1266 |
Final
R indexes [all data] |
R1
= 0.0592, wR2 = 0.1330 |
Largest
diff. peak/hole / e Å-3 |
1.43/-1.23
|
Table
2 Fractional Atomic Coordinates (×104) and Equivalent
Isotropic Displacement Parameters (Å2×103)
for phw1202. Ueq is defined as 1/3 of of the trace of the orthogonalised
UIJ tensor. |
||||
Atom |
x |
y |
z |
U(eq) |
C1 |
-1783(3) |
8514(2) |
1537(2) |
29.5(5) |
C2 |
-2932(4) |
8677(3) |
769(3) |
34.7(6) |
C3 |
-3976(4) |
7774(3) |
-301(3) |
42.9(7) |
C4 |
-3836(4) |
6721(3) |
-548(3) |
43.0(7) |
C5 |
-2674(3) |
6598(2) |
279(2) |
32.0(6) |
C6 |
-2521(4) |
5504(3) |
163(3) |
37.2(6) |
C7 |
1222(4) |
8469(3) |
896(3) |
35.9(6) |
C8 |
2331(5) |
9057(4) |
644(4) |
54.4(10) |
C9 |
3690(5) |
8971(4) |
1065(4) |
60.5(11) |
C10 |
3896(4) |
8294(3) |
1719(3) |
45.2(8) |
C11 |
2763(3) |
7726(3) |
1971(2) |
33.5(6) |
C12A |
2789(6) |
6844(4) |
2528(4) |
35.1(9) |
C12B |
3080(20) |
7221(14) |
2834(16) |
35.1(9) |
C13 |
2008(4) |
9734(3) |
3883(3) |
41.8(7) |
C14 |
2557(4) |
10726(3) |
4871(3) |
47.7(8) |
C15 |
2218(4) |
10621(3) |
5786(3) |
45.9(8) |
C16 |
1343(4) |
9529(3) |
5676(3) |
42.7(7) |
C17 |
808(3) |
8563(3) |
4661(2) |
33.7(6) |
C18 |
-137(4) |
7360(3) |
4535(3) |
37.4(6) |
C19 |
-1368(4) |
4457(3) |
1176(3) |
40.6(7) |
C20 |
166(5) |
4437(4) |
1633(4) |
50.7(9) |
C21 |
1267(5) |
5335(4) |
2886(4) |
51.3(9) |
C22 |
584(5) |
5263(3) |
3739(3) |
48.3(8) |
C23 |
-935(4) |
5296(3) |
3302(3) |
40.0(7) |
C24 |
-1986(4) |
4379(3) |
2064(3) |
42.2(7) |
N1 |
-1631(3) |
7494.9(19) |
1324.2(19) |
25.7(4) |
N2 |
-1340(3) |
5555(2) |
983(2) |
31.6(5) |
N3 |
1434(3) |
7826(2) |
1576(2) |
30.4(5) |
N4A |
1637(4) |
6448(4) |
2724(4) |
38.1(8) |
N4B |
1887(15) |
6797(12) |
3260(13) |
38.1(8) |
N5 |
1140(3) |
8656(2) |
3765(2) |
33.9(5) |
N6 |
-868(3) |
6487(2) |
3313(2) |
32.0(5) |
Ru1 |
84.4(2) |
7102.98(19) |
2283.46(19) |
27.59(7) |
Cl1 |
-4140.1(10) |
6321.0(7) |
2539.3(10) |
56.7(3) |
Cl2 |
-2592(2) |
11555.5(12) |
2095.6(15) |
66.2(5) |
Cl2A |
-1587(8) |
11696(4) |
2280(5) |
66.2(5) |
Table
3 Anisotropic Displacement Parameters (Å2×103)
for phw1202. The Anisotropic displacement factor exponent takes the form:
-2π2[h2a*2U11+...+2hka×b×U12] |
||||||
Atom |
U11 |
U22 |
U33 |
U23 |
U13 |
U12 |
C1 |
34.4(14) |
24.0(12) |
26.4(12) |
6.6(10) |
14.7(11) |
8.5(10) |
C2 |
38.2(15) |
31.6(14) |
37.6(15) |
13.5(12) |
19.0(13) |
16.2(12) |
C3 |
36.1(16) |
39.1(16) |
42.2(17) |
11.4(13) |
6.9(13) |
17.3(14) |
C4 |
35.4(16) |
38.5(16) |
34.0(15) |
3.4(13) |
1.8(12) |
13.4(13) |
C5 |
31.1(13) |
28.2(13) |
26.5(12) |
2(1) |
8.7(10) |
10.9(11) |
C6 |
40.2(16) |
29.5(14) |
27.0(13) |
-1.6(11) |
8.7(12) |
12.5(12) |
C7 |
39.6(16) |
36.4(15) |
31.9(14) |
13.6(12) |
19.8(12) |
10.9(13) |
C8 |
68(3) |
61(2) |
58(2) |
34.1(19) |
44(2) |
27(2) |
C9 |
58(2) |
63(3) |
79(3) |
33(2) |
51(2) |
19(2) |
C10 |
36.9(17) |
54(2) |
44.9(18) |
14.1(15) |
24.6(15) |
15.1(15) |
C11 |
31.5(14) |
37.5(15) |
25.4(12) |
3.8(11) |
14.5(11) |
10.4(12) |
C12A |
33(3) |
33(3) |
33(3) |
3.0(18) |
15(2) |
12(2) |
C12B |
33(3) |
33(3) |
33(3) |
3.0(18) |
15(2) |
12(2) |
C13 |
38.0(16) |
33.3(15) |
33.7(15) |
8.9(12) |
9.4(13) |
0.1(13) |
C14 |
43.6(18) |
31.8(15) |
39.1(17) |
8.3(13) |
5.7(14) |
-0.6(13) |
C15 |
47.9(19) |
34.9(16) |
28.1(14) |
2.2(12) |
1.5(13) |
9.8(14) |
C16 |
50.1(19) |
40.4(17) |
24.7(13) |
8.1(12) |
9.0(13) |
15.2(15) |
C17 |
32.9(14) |
33.8(14) |
23.8(12) |
10.3(11) |
5.4(10) |
9.8(11) |
C18 |
46.2(17) |
32.8(14) |
25.1(13) |
9.3(11) |
14.7(12) |
9.3(13) |
C19 |
53.1(19) |
30.1(14) |
40.9(17) |
11.3(12) |
23.0(15) |
19.8(14) |
C20 |
69(3) |
54(2) |
55(2) |
30.9(18) |
36(2) |
42(2) |
C21 |
53(2) |
55(2) |
61(2) |
34.7(19) |
24.6(18) |
32.9(18) |
C22 |
65(2) |
43.2(18) |
44.0(19) |
25.4(15) |
22.8(17) |
27.2(17) |
C23 |
56(2) |
31.9(14) |
37.6(16) |
18.1(12) |
24.6(15) |
16.5(14) |
C24 |
53(2) |
27.8(14) |
44.6(18) |
13.0(13) |
24.8(15) |
12.6(14) |
N1 |
25.8(10) |
23.9(10) |
23.4(10) |
5.2(8) |
11.5(8) |
7.4(8) |
N2 |
38.4(13) |
31.4(12) |
26.8(11) |
8.2(9) |
16.4(10) |
16.9(10) |
N3 |
29.8(11) |
30.3(11) |
25.1(11) |
7.8(9) |
12.3(9) |
7.3(9) |
N4A |
37.1(19) |
33(2) |
43(2) |
12.5(17) |
17.4(19) |
16.1(17) |
N4B |
37.1(19) |
33(2) |
43(2) |
12.5(17) |
17.4(19) |
16.1(17) |
N5 |
31.4(12) |
31.2(12) |
25.9(11) |
9.4(9) |
6.4(9) |
5.5(10) |
N6 |
38.7(13) |
26.5(11) |
28.4(11) |
10.6(9) |
15.7(10) |
9.7(10) |
Ru1 |
25.68(11) |
28.79(12) |
24.28(11) |
9.90(8) |
10.12(8) |
7.77(8) |
Cl1 |
31.6(4) |
33.2(4) |
76.0(6) |
-6.0(4) |
13.1(4) |
9.8(3) |
Cl2 |
96.2(13) |
43.1(6) |
74.9(9) |
36.2(6) |
42.7(10) |
33.6(8) |
Cl2A |
96.2(13) |
43.1(6) |
74.9(9) |
36.2(6) |
42.7(10) |
33.6(8) |
Table
4 Bond Lengths for phw1202. |
||||||
Atom |
Atom |
Length/Å |
|
Atom |
Atom |
Length/Å |
C1 |
C2 |
1.374(4) |
|
C16 |
C17 |
1.387(4) |
C1 |
N1 |
1.348(3) |
|
C17 |
C18 |
1.504(4) |
C2 |
C3 |
1.385(5) |
|
C17 |
N5 |
1.351(4) |
C3 |
C4 |
1.385(5) |
|
C18 |
N6 |
1.482(4) |
C4 |
C5 |
1.390(4) |
|
C19 |
C20 |
1.518(5) |
C5 |
C6 |
1.446(4) |
|
C19 |
C24 |
1.523(5) |
C5 |
N1 |
1.364(3) |
|
C19 |
N2 |
1.484(4) |
C6 |
N2 |
1.288(4) |
|
C20 |
C21 |
1.531(6) |
C7 |
C8 |
1.377(5) |
|
C21 |
C22 |
1.528(6) |
C7 |
N3 |
1.348(4) |
|
C21 |
N4A |
1.453(5) |
C8 |
C9 |
1.384(6) |
|
C21 |
N4B |
1.684(14) |
C9 |
C10 |
1.359(6) |
|
C22 |
C23 |
1.509(5) |
C10 |
C11 |
1.387(4) |
|
C23 |
C24 |
1.519(5) |
C11 |
C12A |
1.481(6) |
|
C23 |
N6 |
1.511(4) |
C11 |
C12B |
1.41(2) |
|
N1 |
Ru1 |
2.070(2) |
C11 |
N3 |
1.363(4) |
|
N2 |
Ru1 |
1.994(3) |
C12A |
N4A |
1.305(7) |
|
N3 |
Ru1 |
2.063(2) |
C12B |
N4B |
1.55(2) |
|
N4A |
Ru1 |
2.019(4) |
C13 |
C14 |
1.382(5) |
|
N4B |
Ru1 |
2.077(13) |
C13 |
N5 |
1.353(4) |
|
N5 |
Ru1 |
2.090(3) |
C14 |
C15 |
1.383(5) |
|
N6 |
Ru1 |
2.095(2) |
C15 |
C16 |
1.374(5) |
|
|
|
|
Table
5 Bond Angles for phw1202. |
||||||||
Atom |
Atom |
Atom |
Angle/˚ |
|
Atom |
Atom |
Atom |
Angle/˚ |
N1 |
C1 |
C2 |
123.4(3) |
|
C1 |
N1 |
C5 |
117.2(2) |
C1 |
C2 |
C3 |
119.5(3) |
|
C1 |
N1 |
Ru1 |
129.59(19) |
C2 |
C3 |
C4 |
118.3(3) |
|
C5 |
N1 |
Ru1 |
113.00(18) |
C3 |
C4 |
C5 |
119.6(3) |
|
C6 |
N2 |
C19 |
118.0(3) |
C4 |
C5 |
C6 |
123.8(3) |
|
C6 |
N2 |
Ru1 |
118.0(2) |
N1 |
C5 |
C4 |
122.1(3) |
|
C19 |
N2 |
Ru1 |
120.0(2) |
N1 |
C5 |
C6 |
113.9(3) |
|
C7 |
N3 |
C11 |
118.1(3) |
N2 |
C6 |
C5 |
115.8(3) |
|
C7 |
N3 |
Ru1 |
128.0(2) |
N3 |
C7 |
C8 |
121.6(3) |
|
C11 |
N3 |
Ru1 |
113.47(19) |
C7 |
C8 |
C9 |
120.1(4) |
|
C12A |
N4A |
C21 |
118.7(4) |
C10 |
C9 |
C8 |
118.7(3) |
|
C12A |
N4A |
Ru1 |
118.2(3) |
C9 |
C10 |
C11 |
119.8(3) |
|
C21 |
N4A |
Ru1 |
120.3(3) |
C10 |
C11 |
C12A |
123.9(3) |
|
C12B |
N4B |
C21 |
109.0(10) |
C10 |
C11 |
C12B |
119.6(9) |
|
C12B |
N4B |
Ru1 |
106.1(11) |
C12B |
C11 |
C12A |
18.7(6) |
|
C21 |
N4B |
Ru1 |
106.5(7) |
N3 |
C11 |
C10 |
121.7(3) |
|
C13 |
N5 |
Ru1 |
127.5(2) |
N3 |
C11 |
C12A |
113.9(3) |
|
C17 |
N5 |
C13 |
117.6(3) |
N3 |
C11 |
C12B |
117.6(9) |
|
C17 |
N5 |
Ru1 |
114.7(2) |
N4A |
C12A |
C11 |
113.9(4) |
|
C18 |
N6 |
C23 |
111.8(2) |
C11 |
C12B |
N4B |
118.3(15) |
|
C18 |
N6 |
Ru1 |
111.50(18) |
N5 |
C13 |
C14 |
122.9(3) |
|
C23 |
N6 |
Ru1 |
113.83(19) |
C13 |
C14 |
C15 |
119.1(3) |
|
N1 |
Ru1 |
N4B |
176.9(4) |
C16 |
C15 |
C14 |
118.4(3) |
|
N1 |
Ru1 |
N5 |
95.49(9) |
C15 |
C16 |
C17 |
120.2(3) |
|
N1 |
Ru1 |
N6 |
96.68(10) |
C16 |
C17 |
C18 |
120.7(3) |
|
N2 |
Ru1 |
N1 |
78.31(9) |
N5 |
C17 |
C16 |
121.8(3) |
|
N2 |
Ru1 |
N3 |
101.91(10) |
N5 |
C17 |
C18 |
117.5(3) |
|
N2 |
Ru1 |
N4A |
88.70(14) |
N6 |
C18 |
C17 |
113.0(2) |
|
N2 |
Ru1 |
N4B |
104.1(4) |
C20 |
C19 |
C24 |
110.8(3) |
|
N2 |
Ru1 |
N5 |
165.59(10) |
N2 |
C19 |
C20 |
112.8(3) |
|
N2 |
Ru1 |
N6 |
86.35(10) |
N2 |
C19 |
C24 |
106.0(2) |
|
N3 |
Ru1 |
N1 |
93.29(9) |
C19 |
C20 |
C21 |
113.5(3) |
|
N3 |
Ru1 |
N4B |
84.3(4) |
C20 |
C21 |
N4B |
124.3(6) |
|
N3 |
Ru1 |
N5 |
91.34(10) |
C22 |
C21 |
C20 |
111.6(3) |
|
N3 |
Ru1 |
N6 |
168.19(10) |
C22 |
C21 |
N4B |
96.0(6) |
|
N4A |
Ru1 |
N1 |
162.70(14) |
N4A |
C21 |
C20 |
103.6(3) |
|
N4A |
Ru1 |
N3 |
78.13(14) |
N4A |
C21 |
C22 |
113.8(3) |
|
N4A |
Ru1 |
N4B |
18.0(3) |
N4A |
C21 |
N4B |
22.2(5) |
|
N4A |
Ru1 |
N5 |
99.66(14) |
C23 |
C22 |
C21 |
114.1(3) |
|
N4A |
Ru1 |
N6 |
93.81(14) |
C22 |
C23 |
C24 |
110.6(3) |
|
N4B |
Ru1 |
N5 |
82.6(4) |
C22 |
C23 |
N6 |
113.0(3) |
|
N4B |
Ru1 |
N6 |
85.5(4) |
N6 |
C23 |
C24 |
109.8(3) |
|
N5 |
Ru1 |
N6 |
81.44(10) |
C23 |
C24 |
C19 |
113.9(3) |
|
|
|
|
|
Table
6 Torsion Angles for phw1202. |
||||
A |
B |
C |
D |
Angle/˚ |
C1 |
C2 |
C3 |
C4 |
1.2(5) |
C1 |
N1 |
Ru1 |
N2 |
177.8(3) |
C1 |
N1 |
Ru1 |
N3 |
-80.7(2) |
C1 |
N1 |
Ru1 |
N4A |
-140.1(4) |
C1 |
N1 |
Ru1 |
N4B |
-41(7) |
C1 |
N1 |
Ru1 |
N5 |
11.0(2) |
C1 |
N1 |
Ru1 |
N6 |
93.0(2) |
C2 |
C1 |
N1 |
C5 |
0.9(4) |
C2 |
C1 |
N1 |
Ru1 |
174.5(2) |
C2 |
C3 |
C4 |
C5 |
0.5(6) |
C3 |
C4 |
C5 |
C6 |
173.2(3) |
C3 |
C4 |
C5 |
N1 |
-1.7(5) |
C4 |
C5 |
C6 |
N2 |
176.9(3) |
C4 |
C5 |
N1 |
C1 |
1.0(4) |
C4 |
C5 |
N1 |
Ru1 |
-173.7(3) |
C5 |
C6 |
N2 |
C19 |
158.0(3) |
C5 |
C6 |
N2 |
Ru1 |
0.5(4) |
C5 |
N1 |
Ru1 |
N2 |
-8.3(2) |
C5 |
N1 |
Ru1 |
N3 |
93.2(2) |
C5 |
N1 |
Ru1 |
N4A |
33.8(5) |
C5 |
N1 |
Ru1 |
N4B |
133(7) |
C5 |
N1 |
Ru1 |
N5 |
-175.1(2) |
C5 |
N1 |
Ru1 |
N6 |
-93.2(2) |
C6 |
C5 |
N1 |
C1 |
-174.4(3) |
C6 |
C5 |
N1 |
Ru1 |
11.0(3) |
C6 |
N2 |
Ru1 |
N1 |
4.2(2) |
C6 |
N2 |
Ru1 |
N3 |
-86.7(3) |
C6 |
N2 |
Ru1 |
N4A |
-164.3(3) |
C6 |
N2 |
Ru1 |
N4B |
-173.8(5) |
C6 |
N2 |
Ru1 |
N5 |
69.8(5) |
C6 |
N2 |
Ru1 |
N6 |
101.8(3) |
C7 |
C8 |
C9 |
C10 |
0.4(7) |
C7 |
N3 |
Ru1 |
N1 |
9.3(3) |
C7 |
N3 |
Ru1 |
N2 |
88.0(3) |
C7 |
N3 |
Ru1 |
N4A |
174.1(3) |
C7 |
N3 |
Ru1 |
N4B |
-168.8(5) |
C7 |
N3 |
Ru1 |
N5 |
-86.3(3) |
C7 |
N3 |
Ru1 |
N6 |
-138.3(4) |
C8 |
C7 |
N3 |
C11 |
-2.9(5) |
C8 |
C7 |
N3 |
Ru1 |
169.2(3) |
C8 |
C9 |
C10 |
C11 |
-1.3(6) |
C9 |
C10 |
C11 |
C12A |
171.1(4) |
C9 |
C10 |
C11 |
C12B |
-167.4(8) |
C9 |
C10 |
C11 |
N3 |
0.1(5) |
C10 |
C11 |
C12A |
N4A |
177.7(4) |
C10 |
C11 |
C12B |
N4B |
169.0(9) |
C10 |
C11 |
N3 |
C7 |
2.0(4) |
C10 |
C11 |
N3 |
Ru1 |
-171.2(2) |
C11 |
C12A |
N4A |
C21 |
159.7(4) |
C11 |
C12A |
N4A |
Ru1 |
-1.2(5) |
C11 |
C12B |
N4B |
C21 |
116.3(12) |
C11 |
C12B |
N4B |
Ru1 |
1.9(14) |
C11 |
N3 |
Ru1 |
N1 |
-178.4(2) |
C11 |
N3 |
Ru1 |
N2 |
-99.6(2) |
C11 |
N3 |
Ru1 |
N4A |
-13.5(2) |
C11 |
N3 |
Ru1 |
N4B |
3.6(4) |
C11 |
N3 |
Ru1 |
N5 |
86.0(2) |
C11 |
N3 |
Ru1 |
N6 |
34.1(6) |
C12A |
C11 |
C12B |
N4B |
-82(3) |
C12A |
C11 |
N3 |
C7 |
-169.9(3) |
C12A |
C11 |
N3 |
Ru1 |
16.9(3) |
C12A |
N4A |
Ru1 |
N1 |
69.4(6) |
C12A |
N4A |
Ru1 |
N2 |
110.4(4) |
C12A |
N4A |
Ru1 |
N3 |
8.0(3) |
C12A |
N4A |
Ru1 |
N4B |
-100.7(15) |
C12A |
N4A |
Ru1 |
N5 |
-81.4(4) |
C12A |
N4A |
Ru1 |
N6 |
-163.3(3) |
C12B |
C11 |
C12A |
N4A |
95(3) |
C12B |
C11 |
N3 |
C7 |
169.7(7) |
C12B |
C11 |
N3 |
Ru1 |
-3.5(8) |
C12B |
N4B |
Ru1 |
N1 |
-43(8) |
C12B |
N4B |
Ru1 |
N2 |
98.1(9) |
C12B |
N4B |
Ru1 |
N3 |
-2.8(8) |
C12B |
N4B |
Ru1 |
N4A |
65.9(14) |
C12B |
N4B |
Ru1 |
N5 |
-94.9(9) |
C12B |
N4B |
Ru1 |
N6 |
-176.8(9) |
C13 |
C14 |
C15 |
C16 |
-0.1(6) |
C13 |
N5 |
Ru1 |
N1 |
-76.5(3) |
C13 |
N5 |
Ru1 |
N2 |
-140.2(4) |
C13 |
N5 |
Ru1 |
N3 |
16.9(3) |
C13 |
N5 |
Ru1 |
N4A |
95.1(3) |
C13 |
N5 |
Ru1 |
N4B |
101.0(5) |
C13 |
N5 |
Ru1 |
N6 |
-172.5(3) |
C14 |
C13 |
N5 |
C17 |
0.0(5) |
C14 |
C13 |
N5 |
Ru1 |
174.6(3) |
C14 |
C15 |
C16 |
C17 |
-0.6(5) |
C15 |
C16 |
C17 |
C18 |
179.3(3) |
C15 |
C16 |
C17 |
N5 |
1.0(5) |
C16 |
C17 |
C18 |
N6 |
167.9(3) |
C16 |
C17 |
N5 |
C13 |
-0.7(5) |
C16 |
C17 |
N5 |
Ru1 |
-176.0(2) |
C17 |
C18 |
N6 |
C23 |
143.4(3) |
C17 |
C18 |
N6 |
Ru1 |
14.7(3) |
C17 |
N5 |
Ru1 |
N1 |
98.1(2) |
C17 |
N5 |
Ru1 |
N2 |
34.5(5) |
C17 |
N5 |
Ru1 |
N3 |
-168.4(2) |
C17 |
N5 |
Ru1 |
N4A |
-90.2(2) |
C17 |
N5 |
Ru1 |
N4B |
-84.3(4) |
C17 |
N5 |
Ru1 |
N6 |
2.2(2) |
C18 |
C17 |
N5 |
C13 |
-179.1(3) |
C18 |
C17 |
N5 |
Ru1 |
5.7(4) |
C18 |
N6 |
Ru1 |
N1 |
-103.9(2) |
C18 |
N6 |
Ru1 |
N2 |
178.3(2) |
C18 |
N6 |
Ru1 |
N3 |
43.5(6) |
C18 |
N6 |
Ru1 |
N4A |
89.9(2) |
C18 |
N6 |
Ru1 |
N4B |
73.8(4) |
C18 |
N6 |
Ru1 |
N5 |
-9.4(2) |
C19 |
C20 |
C21 |
C22 |
50.2(4) |
C19 |
C20 |
C21 |
N4A |
-72.6(4) |
C19 |
C20 |
C21 |
N4B |
-63.8(7) |
C19 |
N2 |
Ru1 |
N1 |
-152.8(2) |
C19 |
N2 |
Ru1 |
N3 |
116.3(2) |
C19 |
N2 |
Ru1 |
N4A |
38.7(3) |
C19 |
N2 |
Ru1 |
N4B |
29.2(5) |
C19 |
N2 |
Ru1 |
N5 |
-87.2(4) |
C19 |
N2 |
Ru1 |
N6 |
-55.2(2) |
C20 |
C19 |
C24 |
C23 |
53.6(4) |
C20 |
C19 |
N2 |
C6 |
150.0(3) |
C20 |
C19 |
N2 |
Ru1 |
-53.0(3) |
C20 |
C21 |
C22 |
C23 |
-50.8(4) |
C20 |
C21 |
N4A |
C12A |
-91.1(5) |
C20 |
C21 |
N4A |
Ru1 |
69.3(4) |
C20 |
C21 |
N4B |
C12B |
-76.3(12) |
C20 |
C21 |
N4B |
Ru1 |
37.8(9) |
C21 |
C22 |
C23 |
C24 |
52.1(4) |
C21 |
C22 |
C23 |
N6 |
-71.4(4) |
C21 |
N4A |
Ru1 |
N1 |
-91.2(5) |
C21 |
N4A |
Ru1 |
N2 |
-50.1(3) |
C21 |
N4A |
Ru1 |
N3 |
-152.6(4) |
C21 |
N4A |
Ru1 |
N4B |
98.8(15) |
C21 |
N4A |
Ru1 |
N5 |
118.1(3) |
C21 |
N4A |
Ru1 |
N6 |
36.1(3) |
C21 |
N4B |
Ru1 |
N1 |
-159(7) |
C21 |
N4B |
Ru1 |
N2 |
-18.0(7) |
C21 |
N4B |
Ru1 |
N3 |
-118.9(7) |
C21 |
N4B |
Ru1 |
N4A |
-50.2(11) |
C21 |
N4B |
Ru1 |
N5 |
149.0(7) |
C21 |
N4B |
Ru1 |
N6 |
67.1(6) |
C22 |
C21 |
N4A |
C12A |
147.5(4) |
C22 |
C21 |
N4A |
Ru1 |
-52.0(5) |
C22 |
C21 |
N4B |
C12B |
162.4(10) |
C22 |
C21 |
N4B |
Ru1 |
-83.5(6) |
C22 |
C23 |
C24 |
C19 |
-53.7(4) |
C22 |
C23 |
N6 |
C18 |
-68.8(3) |
C22 |
C23 |
N6 |
Ru1 |
58.7(3) |
C23 |
N6 |
Ru1 |
N1 |
128.4(2) |
C23 |
N6 |
Ru1 |
N2 |
50.7(2) |
C23 |
N6 |
Ru1 |
N3 |
-84.2(5) |
C23 |
N6 |
Ru1 |
N4A |
-37.8(2) |
C23 |
N6 |
Ru1 |
N4B |
-53.8(4) |
C23 |
N6 |
Ru1 |
N5 |
-137.0(2) |
C24 |
C19 |
C20 |
C21 |
-51.4(4) |
C24 |
C19 |
N2 |
C6 |
-88.6(3) |
C24 |
C19 |
N2 |
Ru1 |
68.4(3) |
C24 |
C23 |
N6 |
C18 |
167.3(3) |
C24 |
C23 |
N6 |
Ru1 |
-65.2(3) |
N1 |
C1 |
C2 |
C3 |
-2.0(5) |
N1 |
C5 |
C6 |
N2 |
-7.8(4) |
N2 |
C19 |
C20 |
C21 |
67.2(4) |
N2 |
C19 |
C24 |
C23 |
-69.1(4) |
N3 |
C7 |
C8 |
C9 |
1.8(6) |
N3 |
C11 |
C12A |
N4A |
-10.6(5) |
N3 |
C11 |
C12B |
N4B |
1.0(14) |
N4A |
C21 |
C22 |
C23 |
66.0(5) |
N4A |
C21 |
N4B |
C12B |
-53.0(14) |
N4A |
C21 |
N4B |
Ru1 |
61.1(12) |
N4B |
C21 |
C22 |
C23 |
79.9(6) |
N4B |
C21 |
N4A |
C12A |
108.5(15) |
N4B |
C21 |
N4A |
Ru1 |
-91.0(14) |
N5 |
C13 |
C14 |
C15 |
0.4(6) |
N5 |
C17 |
C18 |
N6 |
-13.8(4) |
N6 |
C23 |
C24 |
C19 |
71.7(4) |
Table
7 Hydrogen Atom Coordinates (Å×104) and Isotropic
Displacement Parameters (Å2×103) for
phw1202. |
||||
Atom |
x |
y |
z |
U(eq) |
H1 |
-1059 |
9151 |
2256 |
35 |
H2 |
-3009 |
9404 |
970 |
42 |
H3 |
-4767 |
7874 |
-852 |
52 |
H4 |
-4531 |
6088 |
-1278 |
52 |
H6 |
-3246 |
4792 |
-477 |
45 |
H7 |
285 |
8517 |
583 |
43 |
H8 |
2162 |
9522 |
181 |
65 |
H9 |
4463 |
9378 |
900 |
73 |
H10 |
4812 |
8210 |
2004 |
54 |
H12A |
3574 |
6589 |
2725 |
42 |
H12B |
4016 |
7803 |
3537 |
42 |
H12C |
3271 |
6543 |
2519 |
42 |
H13 |
2250 |
9813 |
3260 |
50 |
H14 |
3158 |
11470 |
4920 |
57 |
H15 |
2582 |
11289 |
6475 |
55 |
H16 |
1104 |
9434 |
6297 |
51 |
H18A |
501 |
7092 |
5079 |
45 |
H18B |
-919 |
7406 |
4775 |
45 |
H19 |
-2067 |
3775 |
413 |
49 |
H20A |
592 |
4590 |
1088 |
61 |
H20B |
51 |
3643 |
1627 |
61 |
H21 |
2191 |
5189 |
3179 |
62 |
H22A |
494 |
4528 |
3884 |
58 |
H22B |
1275 |
5925 |
4505 |
58 |
H23 |
-1363 |
5096 |
3841 |
48 |
H24A |
-2942 |
4465 |
1773 |
51 |
H24B |
-2206 |
3591 |
2107 |
51 |
H4B |
2262 |
7185 |
4069 |
46 |
H6A |
-1854 |
6400 |
2974 |
38 |
[RSC Journal
Format]
Experimental
Single
crystals of C24H26.4977Cl2N6Ru [phw1202] were [MeOH/Et2O diffusion]. A suitable crystal was
selected and [oil on loop] on a Oxford
Diffraction Super Nova 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 [phw1202]
Crystal
Data. C24H26.4977Cl2N6Ru,
M =570.98, triclinic, a =
10.5125(7) Å, b = 12.8761(8) Å, c =
13.0224(9) Å, α = 102.955(6)°, β =
110.920(6)°, γ = 107.384(6)°, V =
1459.07(16) Å3, T = 110.00(10), space group
P-1 (no. 2), Z = 2, μ(Mo Kα) = 0.741, 15679
reflections measured, 9142 unique (Rint =
0.0248) which were used in all calculations. The final wR2
was 0.1330 (all data) and R1 was 0.0491 (>2sigma(I)).
This report has been
created with Olex2, compiled on 2011.11.01 svn.r2039. Please let us know if
there are any errors or if you would like to have additional featrues.