Origin of and a Solution for Uneven Efficiency by Cinchona Alkaloid-Derived, Pseudoenantiomeric Catalysts for Asymmetric Reactions.
Hu, Bin; Bezpalko, Mark W.; Fei, Chao; Dickie, Diane A.; Foxman, Bruce M.; Deng, Li; Journal of the American Chemical Society 140 (2018) 13913–13920; doi:10.1021/jacs.8b09010

data_4133214
_publ_section_title
;
 Origin of and a Solution for Uneven Efficiency by Cinchona
 Alkaloid-Derived, Pseudoenantiomeric Catalysts for Asymmetric Reactions.
;
_journal_issue                   42
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13913
_journal_page_last               13920
_journal_paper_doi               10.1021/jacs.8b09010
_journal_volume                  140
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_sum            'C53 H47 Br Cl3 N3 O2'
_chemical_formula_weight         944.19
_chemical_name_common            binh-02-60
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.5144(5)
_cell_length_b                   15.5144(5)
_cell_length_c                   53.2848(17)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    120.(2)
_cell_measurement_theta_max      14.4579
_cell_measurement_theta_min      2.1820
_cell_volume                     12825.5(7)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'Bruker Instrument Service v2012.12.0.3'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT, VERSION 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1016
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            107082
_diffrn_reflns_theta_full        18.91
_diffrn_reflns_theta_max         18.91
_diffrn_reflns_theta_min         1.37
_diffrn_source                   'fine-focus tube'
_exptl_absorpt_coefficient_mu    0.798
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS V2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.978
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3904
_exptl_crystal_size_max          0.717
_exptl_crystal_size_mid          0.254
_exptl_crystal_size_min          0.242
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.243
_refine_ls_abs_structure_details
;

Flack x determined using 1229 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.060(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         5081
_refine_ls_number_restraints     505
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0618
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0982P)^2^+18.1819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1591
_refine_ls_wR_factor_ref         0.1849
_reflns_number_gt                3767
_reflns_number_total             5081
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Q-1.cif
_cod_data_source_block           binh_02_60
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        12825.5(9)
_cod_database_code               4133214
_shelx_res_checksum              37753
_shelx_hkl_checksum              60139
_shelx_fab_checksum              87815