Mapping the structural boundaries of quasiracemate fractional crystallization using 2-substituted diarylamides.
Tinsley, Ian C.; Spaniol, Jacqueline M.; Wheeler, Kraig A.; Chemical communications (Cambridge, England) 53 (2017) 4601–4604; doi:10.1039/c7cc01638g

data_7119932
_publ_section_title
;
 Mapping the structural boundaries of quasiracemate fractional
 crystallization using 2-substituted diarylamides.
;
_journal_issue                   33
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4601
_journal_page_last               4604
_journal_paper_doi               10.1039/c7cc01638g
_journal_volume                  53
_journal_year                    2017
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C16 H14 F3 N O, C15 H14 N2 O3'
_chemical_formula_sum            'C31 H28 F3 N3 O4'
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_symmetry_space_group_name_Hall  'P 2yb'
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;
2017-02-23 deposited with the CCDC.
2017-03-31 downloaded from the CCDC.
;
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_cell_measurement_theta_max      67.96
_cell_measurement_theta_min      2.60
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_computing_cell_refinement       APEX2
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_computing_data_reduction
;
SADABS (Bruker, 2013) and XPREP (Bruker, 2013)
;
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
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_diffrn_measurement_device_type  'Bruker APEXII CCD'
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_diffrn_reflns_av_unetI/netI     0.0795
_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_reflns_limit_h_max       9
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_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
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_diffrn_reflns_point_group_measured_fraction_full 0.984
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_diffrn_reflns_theta_full        67.679
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_diffrn_source                   'fine-focus sealed tube'
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_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: 1:1 hexanes:dichloromethane '
_exptl_crystal_size_max          0.264
_exptl_crystal_size_mid          0.097
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_refine_ls_abs_structure_details
;
 Flack x determined using 1329 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.23(15)
_refine_ls_extinction_method     none
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_refine_ls_R_factor_all          0.0787
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_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0891P)^2^] where P=(Fo^2^+2Fc^2^)/3'
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_refine_ls_wR_factor_ref         0.1708
_reflns_Friedel_coverage         0.847
_reflns_Friedel_fraction_full    0.967
_reflns_Friedel_fraction_max     0.959
_reflns_number_gt                3797
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_reflns_threshold_expression     'I > 2\s(I)'
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_cod_depositor_comments
'Adding full bibliography for 7119927--7119932.cif.'
_cod_original_cell_volume        1368.0(4)
_cod_database_code               7119932
_shelx_estimated_absorpt_t_min   0.800
_shelx_estimated_absorpt_t_max   0.972
_shelx_res_checksum              71878