Supplementary Material (ESI) for Dalton Transactions
This journal is © The Royal Society of Chemistry 2001
Supplementary Material: X-ray powder diffraction reflections
Powder X-ray diffraction patterns (PXD) data were collected using a Philips XPERT -2
diffractometer with Cu-K radiation. Samples were mounted on flat glass plate sample holders. Ca.
40 minute scans were run for each sample to assess phase purity. Typically short scans were run
over the range 5o < 2 < 70o with step size 0.02o 2 and times per step of 0.7 s. Purity was assessed
by using the IDENTIFY routine as part of the Philips PC diffraction software allowing access to the
JCPDS database. The simulated powder pattern was generated using the PC software packages
LAZY PULVERIX and POWDERCELL, taking the single crystal structural data for each
compound as a model.
Compound 2
Angle
[o2]
5.865
11.770
13.505
15.680
16.240
17.225
18.420
20.000
23.665
25.885
28.035
31.220
35.055
38.690
39.605
48.150
53.450
d-value
1 [Å]
15.0569
7.5128
6.5512
5.6471
5.4536
5.1439
4.8128
4.4360
3.7566
3.4393
3.1802
2.8626
2.5577
2.3254
2.2738
1.8883
1.7129
d-value Peak width
2 [Å]
[o2]
15.0939
7.5312
6.5674
5.6610
5.4670
5.1565
4.8246
4.4469
3.7659
3.4477
3.1880
2.8697
2.5640
2.3311
2.2793
1.8929
1.7171
0.160
0.200
0.200
0.240
0.120
0.160
0.100
0.280
0.200
0.240
0.400
0.960
0.640
0.320
0.320
0.640
0.480
Peak int Back. int Rel. int
[counts]
[counts]
[%]
88
56
130
102
156
94
190
92
106
259
42
6
17
18
23
9
9
36
45
49
55
56
59
62
67
71
66
62
64
52
61
66
45
40
34.1
21.7
50.1
39.4
60.3
36.3
73.5
35.6
40.9
100.0
16.3
2.4
6.5
7.1
8.9
3.5
3.5
Signif.
1.42
1.42
2.52
0.78
1.12
1.13
1.32
4.22
2.33
5.60
2.41
1.44
1.11
0.97
0.81
1.76
0.79
Compound 3
Angle d-value d-value Peak width
[o2]
1 [Å]
2 [Å]
[o2]
5.120
8.595
9.550
11.185
13.340
14.085
15.405
16.300
16.540
18.025
18.255
19.645
20.765
21.295
22.485
23.160
25.280
25.560
26.940
17.2459
10.2795
9.2536
7.9044
6.6319
6.2828
5.7472
5.4336
5.3553
4.9173
4.8559
4.5153
4.2743
4.1691
3.9510
3.8374
3.5202
3.4822
3.3069
17.2884
10.3048
9.2764
7.9238
6.6482
6.2982
5.7614
5.4470
5.3685
4.9294
4.8678
4.5264
4.2848
4.1793
3.9607
3.8468
3.5288
3.4908
3.3150
0.200
0.200
0.120
0.160
0.160
0.120
0.160
0.160
0.120
0.160
0.160
0.100
0.160
0.200
0.240
0.200
0.080
0.080
0.100
Peak int Back. int Rel. int Signif.
[counts]
[counts]
[%]
15
38
128
46
829
256
72
137
137
151
159
159
86
106
106
77
353
272
114
58
53
52
50
50
52
52
52
52
53
53
53
55
55
55
55
56
56
56
1.8
4.6
15.4
5.6
100.0
30.9
8.7
16.5
16.5
18.2
19.1
19.1
10.4
12.8
12.8
9.3
42.6
32.8
13.8
0.93
1.29
2.06
0.87
11.36
2.47
0.90
0.89
1.23
0.76
1.18
0.81
1.02
1.60
2.38
1.31
0.93
0.78
1.05
Supplementary Material (ESI) for Dalton Transactions
This journal is © The Royal Society of Chemistry 2001
28.495
28.960
30.210
31.165
33.245
34.060
35.280
35.850
36.640
39.725
41.705
43.540
45.665
3.1299
3.0807
2.9560
2.8676
2.6927
2.6302
2.5419
2.5028
2.4507
2.2672
2.1640
2.0769
1.9851
3.1376
3.0883
2.9633
2.8746
2.6994
2.6366
2.5482
2.5090
2.4567
2.2727
2.1693
2.0821
1.9900
0.320
0.240
0.240
0.200
0.240
0.400
0.160
0.200
0.400
0.320
0.320
0.480
0.320
114
88
30
31
17
25
48
71
42
48
23
32
23
58
58
58
59
59
61
64
66
66
76
72
69
66
13.8
10.7
3.6
3.8
2.0
3.0
5.7
8.5
5.1
5.7
2.8
3.9
2.8
1.91
1.09
0.99
1.18
1.02
1.29
0.78
1.13
1.06
1.29
0.81
0.77
0.82
Compound 4a
Angle
[o2]
5.155
7.945
9.290
11.670
14.960
15.640
16.780
17.540
20.010
21.415
23.415
24.700
26.130
26.955
27.925
28.280
28.865
30.110
31.145
31.815
33.695
35.080
38.600
40.630
43.050
44.325
44.810
46.985
54.040
d-value d-value Peak width
1 [Å]
2 [Å]
[o2]
17.1289
11.1190
9.5120
7.5769
5.9172
5.6614
5.2793
5.0522
4.4338
4.1460
3.7962
3.6015
3.4076
3.3051
3.1925
3.1532
3.0906
2.9656
2.8694
2.8104
2.6578
2.5560
2.3306
2.2187
2.0994
2.0420
2.0210
1.9324
1.6956
17.1711
11.1464
9.5354
7.5956
5.9317
5.6753
5.2923
5.0646
4.4447
4.1562
3.8055
3.6104
3.4159
3.3132
3.2003
3.1610
3.0982
2.9729
2.8764
2.8174
2.6643
2.5623
2.3363
2.2242
2.1046
2.0470
2.0260
1.9371
1.6997
0.160
0.080
0.320
0.240
0.180
0.160
0.140
0.120
0.120
0.400
0.100
0.060
0.120
0.160
0.100
0.120
0.160
0.240
0.240
0.200
0.160
0.240
0.800
0.800
0.320
0.320
0.240
0.240
0.320
Peak int Back. int Rel. int
[counts]
[counts]
[%]
25
125
27
10
1096
117
246
58
361
92
756
400
117
185
262
164
137
58
59
94
45
31
27
36
36
50
59
22
10
64
64
62
69
110
110
110
110
110
110
110
110
110
110
110
110
110
110
110
110
110
110
98
98
98
98
98
98
76
2.3
11.4
2.5
0.9
100.0
10.6
22.5
5.3
32.9
8.4
69.0
36.5
10.6
16.9
24.0
15.0
12.5
5.3
5.4
8.6
4.1
2.9
2.5
3.3
3.3
4.6
5.4
2.0
0.9
Signif.
1.55
0.93
1.04
0.78
10.08
0.77
2.79
1.32
2.51
0.87
2.63
0.89
1.89
1.30
0.97
1.02
1.03
0.95
1.48
1.37
0.76
0.91
2.09
1.97
0.77
0.87
0.81
0.83
0.88
Mixture of compounds 4a and 4b from reaction in EtOH
Angle
[o2]
7.920
9.265
11.680
13.360
13.800
d-value d-value Peak width
1 [Å]
2 [Å]
[o2]
11.1541
9.5376
7.5705
6.6220
6.4119
11.1815
9.5611
7.5891
6.6383
6.4276
0.100
0.100
0.200
0.160
0.240
Peak int Back. int Rel. int
[counts]
[counts]
[%]
121
196
56
132
219
56
56
58
62
64
8.1
13.2
3.8
8.9
14.7
Signif.
1.39
1.89
1.00
0.77
3.18
Supplementary Material (ESI) for Dalton Transactions
This journal is © The Royal Society of Chemistry 2001
14.560
14.815
14.935
15.655
16.765
18.635
19.560
19.995
22.350
23.350
24.520
25.905
26.945
27.475
27.825
28.745
30.075
31.005
31.840
33.740
34.970
35.895
36.800
38.170
38.830
40.410
42.810
44.785
52.365
57.790
6.0788
5.9748
5.9270
5.6560
5.2840
4.7577
4.5348
4.4371
3.9746
3.8066
3.6275
3.4366
3.3063
3.2437
3.2037
3.1032
2.9690
2.8820
2.8083
2.6544
2.5638
2.4998
2.4404
2.3559
2.3173
2.2303
2.1107
2.0221
1.7458
1.5941
6.0938
5.9895
5.9416
5.6699
5.2970
4.7694
4.5459
4.4480
3.9844
3.8159
3.6365
3.4451
3.3144
3.2517
3.2116
3.1109
2.9763
2.8891
2.8152
2.6609
2.5701
2.5059
2.4464
2.3617
2.3230
2.2358
2.1158
2.0270
1.7501
1.5981
0.160
0.080
0.080
0.280
0.280
0.200
0.200
0.100
0.400
0.200
0.320
0.320
0.200
0.120
0.240
0.200
0.320
0.400
0.320
0.400
0.240
0.640
0.320
0.640
0.480
0.240
0.480
0.120
0.400
0.240
829
1467
1490
400
331
125
392
630
161
900
853
135
231
369
412
182
79
94
135
53
69
45
32
55
46
67
71
92
12
18
64
66
66
67
71
74
76
77
83
85
86
90
92
94
94
96
100
102
104
106
110
112
114
117
119
123
128
132
104
90
55.7
98.5
100.0
26.8
22.2
8.4
26.3
42.3
10.8
60.4
57.2
9.0
15.5
24.7
27.7
12.2
5.3
6.3
9.0
3.6
4.6
3.0
2.2
3.7
3.1
4.5
4.7
6.2
0.8
1.2
0.76
0.76
1.17
4.38
7.34
1.43
1.27
1.07
1.83
8.19
13.63
3.88
1.85
0.76
2.65
1.55
0.77
1.68
2.65
0.92
1.43
2.27
1.65
1.91
1.03
0.94
1.00
0.84
0.76
0.78
Mixture of compounds 4a and 4b from reaction in iPrOH
Angle
[o2]
7.905
9.210
11.655
13.790
14.900
15.665
16.780
18.685
19.595
20.040
22.465
23.370
23.480
24.600
26.145
26.935
27.850
28.730
31.100
31.845
32.540
33.640
34.960
35.850
38.545
d-value d-value Peak width
1 [Å]
2 [Å]
[o2]
11.1752
9.5945
7.5866
6.4165
5.9409
5.6524
5.2793
4.7451
4.5267
4.4272
3.9545
3.8034
3.7858
3.6159
3.4056
3.3075
3.2009
3.1048
2.8734
2.8079
2.7495
2.6620
2.5645
2.5028
2.3338
11.2027
9.6181
7.6053
6.4323
5.9555
5.6663
5.2923
4.7568
4.5379
4.4381
3.9642
3.8127
3.7951
3.6248
3.4140
3.3157
3.2088
3.1125
2.8805
2.8148
2.7562
2.6686
2.5708
2.5090
2.3395
0.080
0.240
0.240
0.160
0.100
0.160
0.140
0.160
0.160
0.100
0.400
0.080
0.060
0.120
0.160
0.160
0.120
0.240
0.240
0.160
0.200
0.320
0.200
0.480
0.960
Peak int Back. int Rel. int
[counts]
[counts]
[%]
94
69
40
110
1197
240
259
83
272
396
114
784
666
620
85
180
346
139
72
110
66
50
50
38
37
36
36
36
40
41
42
45
48
49
49
53
55
55
58
59
61
62
64
67
69
71
72
74
76
81
7.9
5.8
3.3
9.2
100.0
20.1
21.7
6.9
22.7
33.1
9.6
65.5
55.6
51.8
7.1
15.0
28.9
11.6
6.0
9.2
5.5
4.2
4.2
3.2
3.1
Signif.
0.81
2.70
0.78
0.76
1.77
1.28
2.49
1.19
1.03
0.86
1.67
0.83
0.76
1.59
0.93
1.51
1.32
2.33
1.97
0.84
0.96
1.10
0.86
1.35
2.72
Supplementary Material (ESI) for Dalton Transactions
This journal is © The Royal Society of Chemistry 2001
40.590
42.665
44.785
48.270
2.2208
2.1175
2.0221
1.8839
2.2263
2.1227
2.0270
1.8885
0.800
0.640
0.240
0.960
37
36
53
11
83
86
90
83
3.1
3.0
4.5
0.9
2.28
6.53
1.11
0.78