6.3 Single Crystal X-ray Diffraction and Thermal Analyses of 1 and 2
163
Table 6.2 (continued)
Compound
2 at 123 K
2 at 193 K
2 at 213 K
2 at 233 K
D calc (g cm −3 )
1.875
1.864
1.853
1.825
Temperature (K) 123
193
213
233
2θ max (°)
55.0
55.0
55.0
55.0
μ(Mo K α )
(cm −1 )
70.186
69.772
69.352
68.307
No. of
reflections
Total: 61,543
Total: 39,622
Total: 63,130
Total: 40,716
Unique: 9759
Unique: 9849
Unique: 9890
Unique: 9941
R int = 0.1205
R int = 0.0892
R int = 0.1152
R int = 0.0866
R 1
a
0.0610
0.0583
0.0627
0.0606
wR 2
b
0.1822
0.1796
0.1890
0.1809
GOF c
1.023
1.017
1.074
1.048
Max./mini. peak
I d (Å 3 )
2.28 e − /−2.38
e −
2.12 e − /−2.57
e −
1.80 e − /−1.95
e −
2.14 e − /−1.78
e −
Compound
2 at 253 K
2 at 273 K
2 at 298 K
CCDC number
1568262
1568263
1568264
Empirical formula
C 50 H 36 Au 2 F 6 P 2
C 50 H 36 Au 2 F 6 P 2
C 50 H 36 Au 2 F 6 P 2
Formula weight
1206.71
1206.71
1206.71
Crystal system
Monoclinic
Monoclinic
Monoclinic
Crystal size (mm)
0.184 × 0.172 ×
0.067
0.203 × 0.201 ×
0.071
0.206 × 0.195 ×
0.070
a (Å)
31.287(2)
31.368(3)
31.414(3)
b (Å)
14.5786(10)
14.5952(10)
14.5653(13)
c (Å)
19.1847(13)
19.2014(14)
19.2042(17)
α (°)
90
90
90
β (°)
97.1376(18)
97.0338(18)
96.824(2)
γ (°)
90
90
90
V (Å 3 )
8682.7(10)
8724.6(11)
8724.8(14)
Space group
C2/c(#15)
C2/c(#15)
C2/c(#15)
Z value
8
8
8
D calc (g cm −3 )
1.846
1.837
1.837
Temperature (K)
253
273
298
2θ max (°)
55.0
55.0
55.0
μ(Mo K α ) (cm −1 )
69.088
68.756
68.754
No. of reflections
Total: 66,125
Total: 65,971
Total: 66,790
Unique: 9926
Unique: 9905
Unique: 9979
R int = 0.1330
R int = 0.1258
R int = 0.1332
R 1
a
0.0621
0.0648
0.0646
(continued)
163
Table 6.2 (continued)
Compound
2 at 123 K
2 at 193 K
2 at 213 K
2 at 233 K
D calc (g cm −3 )
1.875
1.864
1.853
1.825
Temperature (K) 123
193
213
233
2θ max (°)
55.0
55.0
55.0
55.0
μ(Mo K α )
(cm −1 )
70.186
69.772
69.352
68.307
No. of
reflections
Total: 61,543
Total: 39,622
Total: 63,130
Total: 40,716
Unique: 9759
Unique: 9849
Unique: 9890
Unique: 9941
R int = 0.1205
R int = 0.0892
R int = 0.1152
R int = 0.0866
R 1
a
0.0610
0.0583
0.0627
0.0606
wR 2
b
0.1822
0.1796
0.1890
0.1809
GOF c
1.023
1.017
1.074
1.048
Max./mini. peak
I d (Å 3 )
2.28 e − /−2.38
e −
2.12 e − /−2.57
e −
1.80 e − /−1.95
e −
2.14 e − /−1.78
e −
Compound
2 at 253 K
2 at 273 K
2 at 298 K
CCDC number
1568262
1568263
1568264
Empirical formula
C 50 H 36 Au 2 F 6 P 2
C 50 H 36 Au 2 F 6 P 2
C 50 H 36 Au 2 F 6 P 2
Formula weight
1206.71
1206.71
1206.71
Crystal system
Monoclinic
Monoclinic
Monoclinic
Crystal size (mm)
0.184 × 0.172 ×
0.067
0.203 × 0.201 ×
0.071
0.206 × 0.195 ×
0.070
a (Å)
31.287(2)
31.368(3)
31.414(3)
b (Å)
14.5786(10)
14.5952(10)
14.5653(13)
c (Å)
19.1847(13)
19.2014(14)
19.2042(17)
α (°)
90
90
90
β (°)
97.1376(18)
97.0338(18)
96.824(2)
γ (°)
90
90
90
V (Å 3 )
8682.7(10)
8724.6(11)
8724.8(14)
Space group
C2/c(#15)
C2/c(#15)
C2/c(#15)
Z value
8
8
8
D calc (g cm −3 )
1.846
1.837
1.837
Temperature (K)
253
273
298
2θ max (°)
55.0
55.0
55.0
μ(Mo K α ) (cm −1 )
69.088
68.756
68.754
No. of reflections
Total: 66,125
Total: 65,971
Total: 66,790
Unique: 9926
Unique: 9905
Unique: 9979
R int = 0.1330
R int = 0.1258
R int = 0.1332
R 1
a
0.0621
0.0648
0.0646
(continued)