The application of design of experiments (DoE) reaction optimisation and solvent selection in the development of new synthetic chemistry.
Murray, Paul M.; Bellany, Fiona; Benhamou, Laure; Bučar, Dejan-Krešimir; Tabor, Alethea B.; Sheppard, Tom D.; Organic & biomolecular chemistry 14 (2016) 2373–2384; doi:10.1039/c5ob01892g

data_7154857
_publ_section_title
;
 The application of design of experiments (DoE) reaction optimisation and
 solvent selection in the development of new synthetic chemistry.
;
_journal_issue                   8
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2373
_journal_page_last               2384
_journal_paper_doi               10.1039/c5ob01892g
_journal_volume                  14
_journal_year                    2016
_chemical_absolute_configuration ad
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_chemical_formula_sum            'C9 H11 N5 S'
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_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-09-10T10:50:37-00:00
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2015-09-10 deposited with the CCDC.
2015-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_measurement_temperature    200.00(10)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
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_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.03
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_diffrn_reflns_limit_k_min       -4
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_diffrn_reflns_point_group_measured_fraction_max 0.99
_diffrn_reflns_theta_full        67.684
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_diffrn_reflns_theta_min         4.209
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
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_exptl_absorpt_correction_T_max  1.00000
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics, implemented in 
SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       prism
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_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.141
_refine_diff_density_min         -0.188
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_refine_ls_abs_structure_details
;
 Flack x determined using 916 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(8)
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_reflns         2040
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+0.1641P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0684
_reflns_Friedel_coverage         0.899
_reflns_Friedel_fraction_full    1
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                1980
_reflns_number_total             2040
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ob01892g3.cif
_cod_data_source_block           13b
_cod_depositor_comments
'Adding full bibliography for 7154857--7154858.cif.'
_cod_database_code               7154857