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1
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0028967178
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J. L. Bada Nature 1995 374 594
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(1995)
Nature
, vol.374
, pp. 594
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Bada, J.L.1
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4
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0005859516
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K. Asakura K. Kobayashi Y. Mizusawa T. Ozawa T. Miura A. Tanaka Y. Kushibe S. Osanai Recent Res. Dev. Pure Appl. Chem. 1997 1 123
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(1997)
Recent Res. Dev. Pure Appl. Chem.
, vol.1
, pp. 123
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Asakura, K.1
Kobayashi, K.2
Mizusawa, Y.3
Ozawa, T.4
Miura, T.5
Tanaka, A.6
Kushibe, Y.7
Osanai, S.8
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8
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33646927752
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Nobel Lecture
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A. Werner, "On the constitution and configuration of higher-order compounds", Nobel Lecture, December 11, 1913
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(1913)
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Werner, A.1
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10
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84977584366
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In these experiments, starting materials, solvents and reagents were used both "as supplied" and, in separate experiments, following purification using standard techniques (
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A. Werner A. Vilmos Z. Anorg. Chem. 1899 22 145
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(1899)
Z. Anorg. Chem.
, vol.22
, pp. 145
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Werner, A.1
Vilmos, A.2
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11
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0004055425
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Butterworth, Oxford, ). In order to minimize the risk of problems arising from undetected and unremovable trace impurities generated in different manufacturing processes, commercially available materials were sourced from at least two suppliers (Aldrich Chemical Company, Acros Organics or Fisher Scientific) and the preparation of 1 and the conversion from 1 to 2 were repeated with each combination of materials. The conversion from 1 to 2 was examined repeatedly at the optimum conditions from ref. 5 for spontaneous resolution, and also at the extremes of the conditions found to be successful in that work. In total, considering all different sets of conditions, the preparation of 2 was carried out ca. 30 times. All of the samples were tested for optical activity, but for none of the samples was optical activity observed. Powder XRD data were recorded for 5 samples; in each case, the powder XRD pattern indicated the formation of phase III
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D. D. Perrin and W. L. F. Armarego, Purification of Laboratory Chemicals, Butterworth, Oxford, 1996
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(1996)
Purification of Laboratory Chemicals
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Perrin, D.D.1
Armarego, W.L.F.2
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12
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33646942125
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From a survey of the Cambridge Structural Database (Version 5.26, update August 2005)
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From a survey of the Cambridge Structural Database (Version 5.26, update August 2005)
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13
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0031076502
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H. Nakagawa S. Ohba K. Asakura T. Miura A. Tanaka S. Osanai Acta Crystallogr., Sect. C: Cryst. Struct. Commun. 1997 53 216
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(1997)
Acta Crystallogr., Sect. C: Cryst. Struct. Commun.
, vol.53
, pp. 216
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Nakagawa, H.1
Ohba, S.2
Asakura, K.3
Miura, T.4
Tanaka, A.5
Osanai, S.6
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17
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84921552589
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W. I. F. David, K. Shankland, L. B. McCusker and C. Baerlocher, OUP/IUCr, Oxford
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Structure Determination from Powder Diffraction Data, ed., W. I. F. David,,, K. Shankland,,, L. B. McCusker, and, C. Baerlocher,, OUP/IUCr, Oxford, 2002
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(2002)
Structure Determination from Powder Diffraction Data, Ed.
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19
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33646913802
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L. B. McCusker and C. Baerlocher, 782
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Z. Kristallogr., ed., L. B. McCusker, and, C. Baerlocher,, 2004, 216 ( 12 ), 782
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(2004)
Z. Kristallogr., Ed.
, Issue.12
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20
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33646904189
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note
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For structure determination, the powder XRD pattern was recorded at ambient temperature on Station 2.3 at the Synchrotron Radiation Source, Daresbury Laboratory [capillary, 0.7 mm; λ = 1.3034 Å (the maximum flux at this station is between 1.1 Å and 1.5 Å); 2θ range 10-70°; step size 0.02°; data collection time 7 h]
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22
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0001083481
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((b) H. A. Levy S. W. Peterson J. Am. Chem. Soc. 1953 75 1536), both of which are plausible impurity phases in the material recovered from the reaction
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(1953)
J. Am. Chem. Soc.
, vol.75
, pp. 1536
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Levy, H.A.1
Peterson, S.W.2
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28
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27744535910
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Cardiff University and University of Birmingham
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S. Habershon, G. W. Turner, B. M. Kariuki, E. Y. Cheung, A. J. Hanson, E. Tedesco, D. Albesa-Jové, M.-H. Chao, O. J. Lanning, R. L. Johnston and K. D. M. Harris, EAGER - A Computer Program for Direct-Space Structure Solution from Powder X-ray Diffraction Data, Cardiff University and University of Birmingham
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EAGER - A Computer Program for Direct-Space Structure Solution from Powder X-ray Diffraction Data
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Habershon, S.1
Turner, G.W.2
Kariuki, B.M.3
Cheung, E.Y.4
Hanson, A.J.5
Tedesco, E.6
Albesa-Jové, D.7
Chao, M.-H.8
Lanning, O.J.9
Johnston, R.L.10
Harris, K.D.M.11
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29
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0344545210
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Los Alamos Laboratory Report No. LA-UR-86-748
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A. C. Larson and R. B. Von Dreele, 1987, GSAS, Los Alamos Laboratory Report No. LA-UR-86-748
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(1987)
GSAS
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Larson, A.C.1
Von Dreele, R.B.2
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30
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33646936834
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The GA calculation involved the evolution of 80 generations for a population of 100 trial structures, with 50 mating operations and 30 mutation operations carried out in each generation
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The GA calculation involved the evolution of 80 generations for a population of 100 trial structures, with 50 mating operations and 30 mutation operations carried out in each generation
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31
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33646921126
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- anion, 3 structural variables {x, y, z} are required to define the position in the unit cell
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- anion, 3 structural variables {x, y, z} are required to define the position in the unit cell
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32
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33646948490
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p = 7.40%; 3000 profile points; 110 refined variables
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p = 7.40%; 3000 profile points; 110 refined variables
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33
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33646949645
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3 ligand: 1.976 Å; Co-Br distance 2.408 Å; N-C-C-N torsion angles for en moieties: -48.48° and -49.78°
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3 ligand: 1.976 Å; Co-Br distance 2.408 Å; N-C-C-N torsion angles for en moieties: -48.48° and -49.78°
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34
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33646940667
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note
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3 groups in neighbouring complexes, but the N⋯Br distances are greater than 3.4 Å and in some cases the N-H⋯Br angles are far from linear; these contacts are more appropriately assigned as van der Waals interactions
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35
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33646946710
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note
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In order to further explore the possibility of obtaining a conglomerate crystalline phase from a racemic sample of 2, re-crystallization of the sample of 2 obtained directly from the reaction was carried out using a variety of solvents and under a range of different concentration conditions. The samples obtained were either phase II or phase III or mixtures of phases II and III. We found no evidence for the formation of phase I in these re-crystallization experiments.
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