2.7 Experimental Section
53
2.7.8 Data for Single-Crystal X-ray Structural Analyses
Single-crystal X-ray structural analyses were carried out on a Rigaku R-AXIS RAPID
diffractometer using graphite monochromated Mo-K α radiation. The structure was
solved by direct methods and expanded using Fourier techniques. Non-hydrogen
atoms were refined anisotropically. Hydrogen atoms were refined using the riding
model. All calculations were performed using the CrystalStructure crystallographic
software package except for refinement, which was performed using SHELXL-2013
[24] (Table 2.4; Figs. 2.26, 2.27, 2.28, 2.29, 2.30, 2.31, 2.32, 2.33, 2.34, 2.35 and
2.36).
Table 2.4 Summary of X-ray crystallographic data of 3/solvent
Compound
3/CHCl 3
3/Py
3/CH 2 Cl 2
3/CH 2 Br 2
CCDC
Number
1486479
1486482
1486477
1486476
Empirical
formula
C 27 H 19 Au 2 Cl 3 N 2
C 28.5 H 20.5 Au 2 N 2.5 C 27 H 20 Au 2 Cl 2 N 2
C 27 H 20 Au 2 Br 2 N 2
Formula
weight
871.75
791.93
837.31
926.21
Crystal
system
Orthorhombic
Monoclinic
Monoclinic
Monoclinic
Crystal size
(mm)
0.577 × 0.079 ×
0.037
0.098 × 0.074 ×
0.070
0.103 × 0.097 ×
0.078
0.194 × 0.123 ×
0.086
a (Å)
15.6589(7)
14.0428(11)
14.3824(8)
14.3746(13)
b (Å)
21.6542(10)
22.6970(14)
22.3603(9)
22.3016(17)
c (Å)
15.3795(6)
15.0676(12)
15.4312(7)
15.6172(16)
α (°)
90
90
90
90
β (°)
90
95.697(6)
94.258(3)
94.317(8)
γ (°)
90
90
90
90
V (Å 3 )
5214.9(4)
4778.8(6)
4948.9(4)
4992.3(8)
Space group
Pbcn (#60)
I2/a (#15)
I2/a (#15)
I2/a (#15)
Z value
8
8
8
8
D calc
(g cm −3 )
2.221
2.201
2.242
2.464
Temperature
(K)
123
123
123
123
2θ max (°)
55.0
55.0
55.0
55.0
μ(Mo K α )
(cm −1 )
116.053
123.291
121.191
149.720
(continued)
53
2.7.8 Data for Single-Crystal X-ray Structural Analyses
Single-crystal X-ray structural analyses were carried out on a Rigaku R-AXIS RAPID
diffractometer using graphite monochromated Mo-K α radiation. The structure was
solved by direct methods and expanded using Fourier techniques. Non-hydrogen
atoms were refined anisotropically. Hydrogen atoms were refined using the riding
model. All calculations were performed using the CrystalStructure crystallographic
software package except for refinement, which was performed using SHELXL-2013
[24] (Table 2.4; Figs. 2.26, 2.27, 2.28, 2.29, 2.30, 2.31, 2.32, 2.33, 2.34, 2.35 and
2.36).
Table 2.4 Summary of X-ray crystallographic data of 3/solvent
Compound
3/CHCl 3
3/Py
3/CH 2 Cl 2
3/CH 2 Br 2
CCDC
Number
1486479
1486482
1486477
1486476
Empirical
formula
C 27 H 19 Au 2 Cl 3 N 2
C 28.5 H 20.5 Au 2 N 2.5 C 27 H 20 Au 2 Cl 2 N 2
C 27 H 20 Au 2 Br 2 N 2
Formula
weight
871.75
791.93
837.31
926.21
Crystal
system
Orthorhombic
Monoclinic
Monoclinic
Monoclinic
Crystal size
(mm)
0.577 × 0.079 ×
0.037
0.098 × 0.074 ×
0.070
0.103 × 0.097 ×
0.078
0.194 × 0.123 ×
0.086
a (Å)
15.6589(7)
14.0428(11)
14.3824(8)
14.3746(13)
b (Å)
21.6542(10)
22.6970(14)
22.3603(9)
22.3016(17)
c (Å)
15.3795(6)
15.0676(12)
15.4312(7)
15.6172(16)
α (°)
90
90
90
90
β (°)
90
95.697(6)
94.258(3)
94.317(8)
γ (°)
90
90
90
90
V (Å 3 )
5214.9(4)
4778.8(6)
4948.9(4)
4992.3(8)
Space group
Pbcn (#60)
I2/a (#15)
I2/a (#15)
I2/a (#15)
Z value
8
8
8
8
D calc
(g cm −3 )
2.221
2.201
2.242
2.464
Temperature
(K)
123
123
123
123
2θ max (°)
55.0
55.0
55.0
55.0
μ(Mo K α )
(cm −1 )
116.053
123.291
121.191
149.720
(continued)