A. V. Fratini, I. L. Karle, and J. Karle, "The Crystal Structure of Auramine Perchlorate: Correlation of the Results with Specular Reflection Spectroscopy," Appl. Opt. 6, 2091-2096 (1967)
The x-ray analysis of auramine perchlorate has been performed in order to establish the orientation of the cationic chromophoric group in the crystal for comparison with the orientation that was proposed on the basis of specular reflection studies. The compound crystallizes with two molecules per unit cell in space group P
and cell parameters a = 8.86 Å, b = 9.69 Å, c = 11.27 Å, α = 97° 40′, β = 99° 34′, and γ = 106° 16′. The orientation of the chromophore is in good agreement with the crystal model. Other features of the structure are the hydrogen bonding scheme of the perchlorate ion, the highly distorted chromophoric group, and the planar dimethylamine substituents.
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Fractional Coordinates and Anisotropic Thermal Parameters (βij × 104) for Auramine Perchloratea
Atom
x
y
z
β11
β22
β33
β12
β13
β23
C(1)
0.7249
0.9232
0.8585
168
98
46
8
−18
0
C(2)
0.7503
1.0314
0.6685
154
74
75
−27
25
13
C(3)
0.5602
0.7863
0.6579
70
42
45
6
1
9
C(4)
0.4724
0.6777
0.7125
115
68
29
11
3
18
C(5)
0.5187
0.7700
0.5282
61
61
45
0
15
27
C(6)
0.3956
0.6506
0.4597
69
68
42
59
18
25
C(7)
0.3519
0.5589
0.6433
80
68
33
−5
13
19
C(8)
0.3092
0.5427
0.5150
63
63
28
5
7
8
C(9)
0.1731
0.4185
0.4434
65
74
38
19
20
21
C(10)
0.0785
0.4290
0.3284
42
55
39
7
13
5
C(11)
−0.0050
0.2991
0.2417
100
45
47
7
6
14
C(12)
0.0559
0.5595
0.3027
44
55
51
2
−13
1
C(13)
−0.0477
0.5646
0.1981
60
58
54
19
14
19
C(14)
−0.1090
0.3031
0.1356
92
71
45
32
6
0
C(15)
−0.1336
0.4342
0.1137
72
79
35
17
11
16
C(16)
−0.2674
0.5731
−0.0162
127
128
82
57
−21
42
C(17)
−0.3428
0.2996
−0.0690
154
155
60
25
−67
−21
N(1)
0.6838
0.9046
0.7245
91
52
48
−20
−7
8
N(2)
0.1368
0.2959
0.4859
75
48
53
3
21
11
N(3)
−0.2476
0.4377
0.0142
112
100
53
27
−21
12
O(1)
0.3001
0.2287
0.7186
177
67
68
−6
2
34
O(2)
0.1594
0.0692
0.8297
375
169
67
−38
122
9
O(3)
0.3774
0.0248
0.7553
188
189
322
131
−46
5
O(4)
0.1335
−0.0076
0.6189
226
183
33
−114
−38
−11
Cl
0.2436
0.0773
0.7314
65
58
32
−8
−5
14
Standard Deviations
C
0.0010
0.0008
0.0007
13
9
6
9
7
6
N
0.0007
0.0007
0.0006
11
8
6
8
6
5
O
0.0010
0.0007
0.0006
18
12
9
11
10
8
Cl
0.0002
0.0002
0.0002
3
2
1
2
2
1
The thermal parameters are of the form T = exp [− (β11h2 + β22k2 + β33l2 + 2β12hk + 2β13hl + 2β23kl)]. The coordinates are such that they may be substituted directly into the equations of the least-squares planes.
Table III
The Approximate Coordinates of the Hydrogen Atoms as Determined from the Difference Map
Atom
x
y
z
H(1,1)
0.802
0.837
0.877
H(1,2)
0.627
0.943
0.903
H(1,3)
0.817
0.992
0.883
H(2,1)
0.782
1.002
0.600
H(2,2)
0.848
1.098
0.742
H(2,3)
0.683
1.075
0.653
H(4)
0.502
0.692
0.802
H(5)
0.567
0.847
0.498
H(6)
0.366
0.633
0.370
H(7)
0.302
0.487
0.680
H(N,1)
0.200
0.280
0.525
H(N,2)
0.065
0.217
0.460
H(11)
−0.002
0.217
0.265
H(12)
0.115
0.647
0.340
H(13)
−0.065
0.653
0.195
H(14)
−0.160
0.215
0.083
H(16,1)
−0.337
0.530
−0.075
H(16,2)
−0.195
0.642
0.000
H(16,3)
−0.317
0.630
0.058
H(17,1)
−0.428
0.313
−0.112
H(17,3)
−0.415
0.268
−0.023
Table IV
Direction Cosines of the x and y Vectors from the X-ray Analysis and Crystal Model. The Direction Cosines are Referred to the Orthogonal Set of Axes XYZ
Data taken from Ref. 1. The coordinate system in Ref. 1 has been changed to agree with the system used here.
Table V
Equations of the Least-Squares Planes for Auramine Perchlorate. The Equations are Referred to the Triclinic Axes and the Value on the Right-Hand Side is the Origin-to-Plane Distance in Å
A: 8.045x − 6.125y − 2.412z = −1.867
C(1), C(2), C(3), N(1)
B: 7.657x − 6.938y − 1.597z = −2.217
C(3), C(4), C(5), C(6), C(7), C(8)
C: 7.420x − 4.419y − 6.481z = −3.441
C(8), C(9), C(10), N(2)
D: 7.451x − 0.004y − 7.354z = −1.819
C(10), O(11), C(12), C(13), C(14), C(15)
E: 7.212x − 0.458y − 7.915z = −2.072
C(15), C(16), C(17), N(3)
Tables (5)
Table I
Reflections Used for Implementing the ∑2 Relation
h
k
l
|E|
sign
3
1
7
2.88
+
2
2.89
+
2
7
4.00
+
0
5
3.99
a
2
7
3.32
b
2
9
3.35
c
0
5
3.04
d
2
6
2.66
e
4
5
2.56
f
Table II
Fractional Coordinates and Anisotropic Thermal Parameters (βij × 104) for Auramine Perchloratea
Atom
x
y
z
β11
β22
β33
β12
β13
β23
C(1)
0.7249
0.9232
0.8585
168
98
46
8
−18
0
C(2)
0.7503
1.0314
0.6685
154
74
75
−27
25
13
C(3)
0.5602
0.7863
0.6579
70
42
45
6
1
9
C(4)
0.4724
0.6777
0.7125
115
68
29
11
3
18
C(5)
0.5187
0.7700
0.5282
61
61
45
0
15
27
C(6)
0.3956
0.6506
0.4597
69
68
42
59
18
25
C(7)
0.3519
0.5589
0.6433
80
68
33
−5
13
19
C(8)
0.3092
0.5427
0.5150
63
63
28
5
7
8
C(9)
0.1731
0.4185
0.4434
65
74
38
19
20
21
C(10)
0.0785
0.4290
0.3284
42
55
39
7
13
5
C(11)
−0.0050
0.2991
0.2417
100
45
47
7
6
14
C(12)
0.0559
0.5595
0.3027
44
55
51
2
−13
1
C(13)
−0.0477
0.5646
0.1981
60
58
54
19
14
19
C(14)
−0.1090
0.3031
0.1356
92
71
45
32
6
0
C(15)
−0.1336
0.4342
0.1137
72
79
35
17
11
16
C(16)
−0.2674
0.5731
−0.0162
127
128
82
57
−21
42
C(17)
−0.3428
0.2996
−0.0690
154
155
60
25
−67
−21
N(1)
0.6838
0.9046
0.7245
91
52
48
−20
−7
8
N(2)
0.1368
0.2959
0.4859
75
48
53
3
21
11
N(3)
−0.2476
0.4377
0.0142
112
100
53
27
−21
12
O(1)
0.3001
0.2287
0.7186
177
67
68
−6
2
34
O(2)
0.1594
0.0692
0.8297
375
169
67
−38
122
9
O(3)
0.3774
0.0248
0.7553
188
189
322
131
−46
5
O(4)
0.1335
−0.0076
0.6189
226
183
33
−114
−38
−11
Cl
0.2436
0.0773
0.7314
65
58
32
−8
−5
14
Standard Deviations
C
0.0010
0.0008
0.0007
13
9
6
9
7
6
N
0.0007
0.0007
0.0006
11
8
6
8
6
5
O
0.0010
0.0007
0.0006
18
12
9
11
10
8
Cl
0.0002
0.0002
0.0002
3
2
1
2
2
1
The thermal parameters are of the form T = exp [− (β11h2 + β22k2 + β33l2 + 2β12hk + 2β13hl + 2β23kl)]. The coordinates are such that they may be substituted directly into the equations of the least-squares planes.
Table III
The Approximate Coordinates of the Hydrogen Atoms as Determined from the Difference Map
Atom
x
y
z
H(1,1)
0.802
0.837
0.877
H(1,2)
0.627
0.943
0.903
H(1,3)
0.817
0.992
0.883
H(2,1)
0.782
1.002
0.600
H(2,2)
0.848
1.098
0.742
H(2,3)
0.683
1.075
0.653
H(4)
0.502
0.692
0.802
H(5)
0.567
0.847
0.498
H(6)
0.366
0.633
0.370
H(7)
0.302
0.487
0.680
H(N,1)
0.200
0.280
0.525
H(N,2)
0.065
0.217
0.460
H(11)
−0.002
0.217
0.265
H(12)
0.115
0.647
0.340
H(13)
−0.065
0.653
0.195
H(14)
−0.160
0.215
0.083
H(16,1)
−0.337
0.530
−0.075
H(16,2)
−0.195
0.642
0.000
H(16,3)
−0.317
0.630
0.058
H(17,1)
−0.428
0.313
−0.112
H(17,3)
−0.415
0.268
−0.023
Table IV
Direction Cosines of the x and y Vectors from the X-ray Analysis and Crystal Model. The Direction Cosines are Referred to the Orthogonal Set of Axes XYZ
Data taken from Ref. 1. The coordinate system in Ref. 1 has been changed to agree with the system used here.
Table V
Equations of the Least-Squares Planes for Auramine Perchlorate. The Equations are Referred to the Triclinic Axes and the Value on the Right-Hand Side is the Origin-to-Plane Distance in Å
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