6.3 Single Crystal X-ray Diffraction and Thermal Analyses of 1 and 2
161
Table 6.2 Summary of X-ray crystallographic data of the crystal 1 and 2
Compound
1 at 123 K
1 at 193 K
1 at 213 K
CCDC number
1568271
1568265
1568266
Empirical formula
C 46 H 28 Au 2 F 6 P 2
C 46 H 28 Au 2 F 6 P 2
C 46 H 28 Au 2 F 6 P 2
Formula weight
1150.60
1150.60
1150.60
Crystal system
Triclinic
Triclinic
Triclinic
Crystal size (mm)
0.138 × 0.076 ×
0.051
0.141 × 0.081 ×
0.056
0.088 × 0.143 ×
0.067
a (Å)
11.9234(11)
11.9564(13)
11.9603(16)
b (Å)
14.1307(12)
14.1676(17)
14.179(2)
c (Å)
14.1890(11)
14.2228(15)
14.2356(19)
α (°)
68.637(2)
69.048(3)
68.990(3)
β (°)
67.907(2)
67.782(3)
67.695(4)
γ (°)
65.678(2)
65.550(4)
65.533(4)
V (Å)
1955.5(3)
1971.7(4)
1974.0(5)
Space group
P-1(#2)
P-1(#2)
P-1(#2)
Z value
2
2
2
D calc (g cm −3 )
1.954
1.938
1.936
Temperature (K)
123
193
213
2θ max (°)
55.0
55.0
55.0
μ(Mo K α ) (cm −1 )
76.639
76.007
75.919
No. of reflections
Total: 19,295
Total: 19,553
Total: 19,475
Unique: 8875
Unique: 8990
Unique: 8982
R int = 0.0897
R int = 0.0918
R int = 0.0965
R 1
a
0.0883
0.0929
0.1027
wR 2
b
0.3233
0.3064
0.3774
GOF c
0.869
1.079
1.086
Max./mini. peak I d
(Å 3 )
2.58 e – /−4.00 e −
2.52 e − /−3.91 e −
2.58 e − /−4.00 e −
Compound
1 at 233 K
1 at 253 K
1 at 273 K
1 at 298 K
CCDC number
1568267
1568268
1568269
1568270
Empirical
formula
C 46 H 28 Au 2 F 6 P 2 C 46 H 28 Au 2 F 6 P 2 C 46 H 28 Au 2 F 6 P 2 C 46 H 28 Au 2 F 6 P 2
Formula weight
1150.60
1150.60
1150.60
1150.60
Crystal system
Triclinic
Triclinic
Triclinic
Triclinic
Crystal size
(mm)
0.145 × 0.090
× 0.069
0.146 × 0.092
× 0.070
0.148 × 0.095
× 0.072
0.151 × 0.098
× 0.076
a (Å)
11.9857(16)
12.001(2)
12.061(3)
12.0427(18)
b (Å)
14.187(2)
14.205(2)
14.190(4)
14.236(2)
(continued)
161
Table 6.2 Summary of X-ray crystallographic data of the crystal 1 and 2
Compound
1 at 123 K
1 at 193 K
1 at 213 K
CCDC number
1568271
1568265
1568266
Empirical formula
C 46 H 28 Au 2 F 6 P 2
C 46 H 28 Au 2 F 6 P 2
C 46 H 28 Au 2 F 6 P 2
Formula weight
1150.60
1150.60
1150.60
Crystal system
Triclinic
Triclinic
Triclinic
Crystal size (mm)
0.138 × 0.076 ×
0.051
0.141 × 0.081 ×
0.056
0.088 × 0.143 ×
0.067
a (Å)
11.9234(11)
11.9564(13)
11.9603(16)
b (Å)
14.1307(12)
14.1676(17)
14.179(2)
c (Å)
14.1890(11)
14.2228(15)
14.2356(19)
α (°)
68.637(2)
69.048(3)
68.990(3)
β (°)
67.907(2)
67.782(3)
67.695(4)
γ (°)
65.678(2)
65.550(4)
65.533(4)
V (Å)
1955.5(3)
1971.7(4)
1974.0(5)
Space group
P-1(#2)
P-1(#2)
P-1(#2)
Z value
2
2
2
D calc (g cm −3 )
1.954
1.938
1.936
Temperature (K)
123
193
213
2θ max (°)
55.0
55.0
55.0
μ(Mo K α ) (cm −1 )
76.639
76.007
75.919
No. of reflections
Total: 19,295
Total: 19,553
Total: 19,475
Unique: 8875
Unique: 8990
Unique: 8982
R int = 0.0897
R int = 0.0918
R int = 0.0965
R 1
a
0.0883
0.0929
0.1027
wR 2
b
0.3233
0.3064
0.3774
GOF c
0.869
1.079
1.086
Max./mini. peak I d
(Å 3 )
2.58 e – /−4.00 e −
2.52 e − /−3.91 e −
2.58 e − /−4.00 e −
Compound
1 at 233 K
1 at 253 K
1 at 273 K
1 at 298 K
CCDC number
1568267
1568268
1568269
1568270
Empirical
formula
C 46 H 28 Au 2 F 6 P 2 C 46 H 28 Au 2 F 6 P 2 C 46 H 28 Au 2 F 6 P 2 C 46 H 28 Au 2 F 6 P 2
Formula weight
1150.60
1150.60
1150.60
1150.60
Crystal system
Triclinic
Triclinic
Triclinic
Triclinic
Crystal size
(mm)
0.145 × 0.090
× 0.069
0.146 × 0.092
× 0.070
0.148 × 0.095
× 0.072
0.151 × 0.098
× 0.076
a (Å)
11.9857(16)
12.001(2)
12.061(3)
12.0427(18)
b (Å)
14.187(2)
14.205(2)
14.190(4)
14.236(2)
(continued)