1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
66
67
68
69
70
71
72
73
74
75
76
77
78
79
80
81
82
83
84
85
86
87
88
89
90
91
92
93
94
95
96
97
98
99
100
101
102
103
104
105
106
107
108
109
110
111
112
113
114
115
116
117
118
119
120
121
122
123
124
125
126
127
128
129
130
131
132
133
134
135
136
137
138
139
140
141
142
143
144
145
146
147
148
149
150
151
152
153
154
155
156
157
158
159
160
161
162
163
164
165
166
167
168
169
170
171
172
173
174
175
176
177
178
179
180
181
182
183
184
185
186
187
188
189
190
191
192
193
194
195
196
197
198
199
200
201
202
203
204
205
206
207
208
209
210
211
212
213
214
215
216
217
218
219
220
221
222
223
224
225
226
227
228
229
230
231
232
233
234
235
236
237
238
239
240
241
242
243
244
245
246
247
248
249
250
251
252
253
254
255
256
257
258
259
260
261
262
263
264
265
266
267
268
269
270
271
272
273
274
275
276
277
278
279
280
281
282
283
284
285
286
287
288
289
290
291
292
293
294
295
296
297
298
299
300
301
302
303
304
305
306
307
308
309
310
|
SADABS-2012/1 - Bruker AXS area detector scaling and absorption correction
--------------------------------------------------------------------------
Equivalent reflections defined by point group -1 for scaling
Equivalent reflections defined by point group -1 for error model
Reading file bn_ed_1_0m.raw
Mean and maximum errors in direction cosine check function = 0.000 0.003
The mean error should not exceed 0.005, and is usually caused by matrix
changes during data processing.
Approximate wavelength, cell and maximum 2-theta (from cosines etc.):
0.71073 9.301 12.049 19.888 95.444 98.233 97.284 104.34
==============================================================================
PART 1 - Refinement of parameters to model systematic errors
Thresholds should now be specified for excluding reflections from the
parameter refinement; these reflections may still be corrected and included
in the final output .hkl file
275884 Reflections of which 45285 unique; 26.67 data per frame
Redundancy: 1 2 3 4 5 6 7 8 9+
Number of groups: 10606 10793 4385 2268 2484 2057 1433 902 10357
Mean(I/sigma): -inf 0 1 2 3 5 10 15 20 +inf
Number of groups: 3224 6821 4680 3682 5581 9892 4388 2667 4350
Settings for parameter refinement:
Maximum resolution = 0.1000 A
(Intensity/sigma) threshold = 1.500
Restraint esd for equal adjacent scale factors = 0.0050
Maximum odd and even orders for spherical harmonics = 3 6
199114 Reflections employed for parameter determination
Effective data to parameter ratio = 16.64
wR2(int) = 0.1348 (selected reflections only, before parameter refinement)
Cycle wR2(incid) wR2(diffr) Mean wt.
1 0.1052 0.0857 0.8486
2 0.0735 0.0668 0.8778
3 0.0622 0.0593 0.8895
4 0.0565 0.0548 0.8963
5 0.0529 0.0518 0.9006
6 0.0504 0.0497 0.9033
7 0.0487 0.0482 0.9051
8 0.0475 0.0472 0.9064
9 0.0467 0.0464 0.9072
10 0.0461 0.0459 0.9078
11 0.0456 0.0455 0.9082
12 0.0452 0.0451 0.9085
13 0.0449 0.0449 0.9088
14 0.0447 0.0447 0.9090
15 0.0445 0.0445 0.9092
16 0.0444 0.0444 0.9093
17 0.0443 0.0443 0.9094
18 0.0442 0.0442 0.9095
19 0.0441 0.0441 0.9096
20 0.0440 0.0440 0.9096
21 0.0440 0.0440 0.9097
22 0.0440 0.0440 0.9097
23 0.0439 0.0439 0.9098
24 0.0439 0.0439 0.9098
25 0.0439 0.0439 0.9098
26 0.0439 0.0439 0.9098
27 0.0438 0.0438 0.9099
28 0.0438 0.0438 0.9099
29 0.0438 0.0438 0.9099
30 0.0438 0.0438 0.9099
0 Reflections masked out
==============================================================================
PART 2 - Reject outliers and establish error model
Rejected reflections are ignored in the statistics and Postscript plots
(except the detector diagnostics) and in the output .hkl file
Before applying rejections there are:
275884 total and 45285 unique reflections assuming Friedel's law.
Reflections rejected for which |I-<I>|/su > 4.00
Where: su^2 = sigma(I)^2 + ( 0.04000 <I>)^2 (sigma(I) from SAINT)
275136 total and 45285 unique reflections left after |I-<I>|/su test
g = 0.0357 gave best error model; g set to 0.0357 for statistics and .hkl
file output
Run 2-theta R(int) Incid. factors Diffr. factors K Total I>2sig(I)
1 -15.0 0.0433 0.677 - 1.522 0.988 - 1.020 0.647 8894 6991
2 -15.0 0.0421 0.881 - 1.568 0.978 - 1.019 0.627 3695 2834
3 -20.0 0.0485 0.633 - 1.473 0.978 - 1.016 0.664 9865 7367
4 -35.0 0.0566 0.671 - 1.557 0.978 - 1.019 0.687 14073 9777
5 -30.0 0.0485 0.793 - 1.479 0.984 - 1.019 0.656 12466 9101
6 -7.5 0.0377 0.559 - 1.522 0.981 - 1.019 0.684 5550 4670
7 -35.0 0.0555 0.807 - 1.451 0.988 - 1.019 0.656 12057 8406
8 -32.5 0.0521 0.726 - 1.514 0.988 - 1.019 0.664 6520 4763
9 -15.0 0.0372 0.520 - 0.845 0.984 - 1.017 0.659 8913 7350
10 -17.5 0.0393 0.546 - 1.304 0.979 - 1.019 0.640 9384 7355
11 0.0 0.0345 0.621 - 1.600 0.984 - 1.019 0.658 6933 5953
12 0.0 0.0274 0.618 - 0.880 0.997 - 1.014 0.645 2519 2251
13 -17.5 0.0418 0.601 - 1.200 0.981 - 1.017 0.664 9371 7298
14 -35.0 0.0528 0.653 - 1.442 0.979 - 1.015 0.666 12961 9146
15 -2.5 0.0367 0.739 - 1.485 0.988 - 1.020 0.654 6809 5797
16 -7.5 0.0480 0.580 - 1.342 0.997 - 1.019 0.813 5088 4171
17 -20.0 0.0484 0.707 - 1.549 0.978 - 1.019 0.658 9907 7312
18 -32.5 0.0502 0.715 - 1.503 0.988 - 1.019 0.659 13228 9599
19 -12.5 0.0399 0.639 - 1.568 0.978 - 1.019 0.652 7956 6383
20 -30.0 0.0416 0.563 - 0.784 0.988 - 1.020 0.667 11880 9261
21 -10.0 0.0347 0.518 - 0.721 0.988 - 1.014 0.674 7458 6385
22 -67.9 0.0220 0.595 - 0.936 0.988 - 1.020 0.659 21697 17186
23 -67.3 0.0262 0.538 - 1.377 0.978 - 1.019 0.657 21836 17171
24 -61.6 0.0236 0.768 - 1.573 0.980 - 1.019 0.691 20751 16492
25 14.6 0.0365 0.635 - 1.579 0.979 - 1.019 0.652 8517 6903
26 -69.8 0.0282 0.650 - 1.510 0.978 - 1.019 0.663 16808 12968
su = K * Sqrt[ sigma^2(I) + (g<I>)^2.00 ] where sigma(I) is from SAINT
The above statistics are based on all non-rejected data, ignoring
reflections without equivalents when estimating R(int) and K.
==============================================================================
PART 3 - Output Postscript diagnostics and corrected data
Diagnostic plots written to Postscript file sad.eps
275136 Corrected reflections written to file sad_noface_u.hkl
Estimated minimum and maximum transmission: 0.9593 1.0000
The ratio of these values is more reliable than their absolute values!
Additional spherical absorption correction applied with mu*r = 0.0000
45285 Corrected reflections written to file sad_noface_m.hkl
Estimated minimum and maximum transmission: 0.9593 1.0000
The ratio of these values is more reliable than their absolute values!
Additional spherical absorption correction applied with mu*r = 0.0000
42035 Corrected reflections written to file xd.hkl
Estimated minimum and maximum transmission: 0.9593 1.0000
The ratio of these values is more reliable than their absolute values!
Additional spherical absorption correction applied with mu*r = 0.0000
==============================================================================
==============================================================================
PART 1 - Refinement of parameters to model systematic errors
Thresholds should now be specified for excluding reflections from the
parameter refinement; these reflections may still be corrected and included
in the final output .hkl file
275884 Reflections of which 45285 unique; 26.67 data per frame
Redundancy: 1 2 3 4 5 6 7 8 9+
Number of groups: 10606 10793 4385 2268 2484 2057 1433 902 10357
Mean(I/sigma): -inf 0 1 2 3 5 10 15 20 +inf
Number of groups: 3224 6821 4680 3682 5581 9892 4388 2667 4350
Reading crystal faces from file: face.p4p
Crystal faces:
H K L d(mm)
0.000 0.000 1.000 0.01700
0.000 0.000 -1.000 0.03900
-2.000 1.000 1.000 0.20600
2.000 -1.000 -1.000 0.16800
0.000 -2.000 1.000 0.12500
0.000 2.000 -1.000 0.14200
-1.000 0.000 1.000 0.18300
1.000 0.000 -1.000 0.17800
8 Faces + 12 Corners = 18 Edges + 2
Linear absorption coefficient set to 0.16 mm-1, giving Rint = 0.1772
Minimum and maximum transmission coefficients = 0.94862 and 0.99129
Minimum and maximum t-bar = 0.0547 and 0.3292 mm
All Rint values calculated using 199114 selected reflections only
Settings for parameter refinement:
Maximum resolution = 0.1000 A
(Intensity/sigma) threshold = 1.500
Restraint esd for equal adjacent scale factors = 0.0050
Maximum odd and even orders for spherical harmonics = 3 6
199114 Reflections employed for parameter determination
Effective data to parameter ratio = 16.64
wR2(int) = 0.1355 (selected reflections only, before parameter refinement)
Cycle wR2(incid) wR2(diffr) Mean wt.
1 0.1063 0.0872 0.8453
2 0.0747 0.0676 0.8764
3 0.0628 0.0598 0.8887
4 0.0570 0.0552 0.8958
5 0.0533 0.0521 0.9002
6 0.0508 0.0500 0.9030
7 0.0490 0.0485 0.9048
8 0.0478 0.0475 0.9060
9 0.0470 0.0468 0.9068
10 0.0464 0.0462 0.9074
11 0.0459 0.0458 0.9079
12 0.0455 0.0454 0.9082
13 0.0452 0.0451 0.9085
14 0.0450 0.0449 0.9087
15 0.0448 0.0447 0.9089
16 0.0446 0.0446 0.9091
17 0.0445 0.0445 0.9092
18 0.0444 0.0444 0.9093
19 0.0443 0.0443 0.9094
20 0.0442 0.0442 0.9094
21 0.0442 0.0442 0.9095
22 0.0441 0.0441 0.9095
23 0.0441 0.0441 0.9096
24 0.0440 0.0441 0.9096
25 0.0440 0.0440 0.9097
26 0.0440 0.0440 0.9097
27 0.0440 0.0440 0.9097
28 0.0440 0.0440 0.9097
29 0.0440 0.0440 0.9098
30 0.0440 0.0440 0.9098
wR2(int) = 0.0440 (selected reflections only, after parameter refinement)
==============================================================================
PART 2 - Reject outliers and establish error model
Rejected reflections are ignored in the statistics and Postscript plots
(except the detector diagnostics) and in the output .hkl file
Before applying rejections there are:
275884 total and 45285 unique reflections assuming Friedel's law.
Reflections rejected for which |I-<I>|/su > 4.00
Where: su^2 = sigma(I)^2 + ( 0.04000 <I>)^2 (sigma(I) from SAINT)
275137 total and 45285 unique reflections left after |I-<I>|/su test
g = 0.0364 gave best error model; g set to 0.0364 for statistics and .hkl
file output
Run 2-theta R(int) Incid. factors Diffr. factors K Total I>2sig(I)
1 -15.0 0.0433 0.670 - 1.527 0.984 - 1.025 0.646 8894 6996
2 -15.0 0.0423 0.883 - 1.576 0.982 - 1.025 0.627 3695 2834
3 -20.0 0.0486 0.626 - 1.479 0.982 - 1.023 0.663 9865 7369
4 -35.0 0.0566 0.663 - 1.564 0.982 - 1.025 0.686 14073 9779
5 -30.0 0.0491 0.787 - 1.483 0.982 - 1.025 0.657 12467 9098
6 -7.5 0.0388 0.554 - 1.518 0.984 - 1.025 0.694 5550 4663
7 -35.0 0.0555 0.805 - 1.455 0.982 - 1.025 0.655 12057 8411
8 -32.5 0.0522 0.719 - 1.517 0.984 - 1.025 0.664 6520 4764
9 -15.0 0.0374 0.512 - 0.843 0.982 - 1.023 0.657 8913 7352
10 -17.5 0.0395 0.538 - 1.306 0.982 - 1.025 0.639 9384 7355
11 0.0 0.0347 0.614 - 1.606 0.987 - 1.025 0.657 6933 5953
12 0.0 0.0275 0.615 - 0.880 0.991 - 1.010 0.643 2519 2251
13 -17.5 0.0419 0.592 - 1.200 0.982 - 1.013 0.663 9371 7298
14 -35.0 0.0528 0.644 - 1.444 0.982 - 1.022 0.665 12961 9149
15 -2.5 0.0368 0.732 - 1.491 0.982 - 1.025 0.652 6809 5797
16 -7.5 0.0507 0.576 - 1.331 0.996 - 1.025 0.842 5088 4158
17 -20.0 0.0485 0.699 - 1.553 0.982 - 1.025 0.657 9907 7314
18 -32.5 0.0503 0.709 - 1.506 0.982 - 1.025 0.658 13228 9601
19 -12.5 0.0400 0.630 - 1.575 0.982 - 1.025 0.650 7956 6384
20 -30.0 0.0415 0.559 - 0.781 0.982 - 1.013 0.665 11880 9268
21 -10.0 0.0347 0.513 - 0.712 0.982 - 1.014 0.671 7458 6387
22 -67.9 0.0220 0.591 - 0.935 0.982 - 1.013 0.656 21697 17189
23 -67.3 0.0263 0.530 - 1.379 0.982 - 1.025 0.655 21836 17175
24 -61.6 0.0236 0.759 - 1.577 0.982 - 1.025 0.690 20751 16496
25 14.6 0.0367 0.628 - 1.584 0.982 - 1.025 0.651 8517 6903
26 -69.8 0.0283 0.643 - 1.513 0.982 - 1.025 0.661 16808 12971
su = K * Sqrt[ sigma^2(I) + (g<I>)^2.00 ] where sigma(I) is from SAINT
The above statistics are based on all non-rejected data, ignoring
reflections without equivalents when estimating R(int) and K.
==============================================================================
PART 3 - Output Postscript diagnostics and corrected data
Diagnostic plots written to Postscript file sad_face.eps
275137 Corrected reflections written to file sad_face_u.hkl
Estimated minimum and maximum transmission: 0.9385 1.0000
The ratio of these values is more reliable than their absolute values!
Additional spherical absorption correction applied with mu*r = 0.0000
45285 Corrected reflections written to file sad_face_m.hkl
Estimated minimum and maximum transmission: 0.9385 1.0000
The ratio of these values is more reliable than their absolute values!
Additional spherical absorption correction applied with mu*r = 0.0000
42039 Corrected reflections written to file xd_face.hkl
Estimated minimum and maximum transmission: 0.9385 1.0000
The ratio of these values is more reliable than their absolute values!
Additional spherical absorption correction applied with mu*r = 0.0000
|
