Highly Enantioselective, Hydrogen-Bond-Donor Catalyzed Additions to Oxetanes.
Strassfeld, Daniel A.; Wickens, Zachary K.; Picazo, Elias; Jacobsen, Eric N.; Journal of the American Chemical Society 142 (2020) 9175–9180; doi:10.1021/jacs.0c03991

data_4134915
_publ_section_title
;
 Highly Enantioselective, Hydrogen-Bond-Donor Catalyzed Additions to
 Oxetanes.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9175
_journal_page_last               9180
_journal_paper_doi               10.1021/jacs.0c03991
_journal_volume                  142
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_sum            'C17 H17 Br Cl N3 O'
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_space_group_name_Hall           'P 2ac 2ab'
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_cell_length_c                   32.5860(8)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.7
_cell_measurement_theta_min      3.31
_cell_volume                     3403.10(15)
_computing_cell_refinement       'SAINT 8.37A (Bruker-AXS, 2015)'
_computing_data_reduction        'SAINT 8.37A (Bruker-AXS, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick, 2015)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 2015)'
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_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
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_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type
;
Bruker D8 goniometer with CCD area detector  
;
_diffrn_measurement_method       'omega and phi scans'
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_diffrn_radiation_type           CuK\a
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_diffrn_reflns_av_unetI/netI     0.0574
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_diffrn_reflns_limit_h_max       8
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_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
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_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            36923
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
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_diffrn_reflns_theta_max         66.824
_diffrn_reflns_theta_min         2.712
_exptl_absorpt_coefficient_mu    4.796
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6084
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_description       needle
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Flack x determined using 1910 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.017(16)
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         5929
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+4.5081P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.0996
_reflns_Friedel_coverage         0.743
_reflns_Friedel_fraction_full    0.978
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                5058
_reflns_number_total             5929
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c03991_si_002.cif
_cod_data_source_block           DAS-V-181-1
_cod_depositor_comments
'Adding full bibliography for 4134915--4134918.cif.'
_cod_database_code               4134915
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.392
_shelx_estimated_absorpt_t_max   0.700
_shelx_res_checksum              73951
_shelx_hkl_checksum              14202