Enantioconvergent and diastereoselective synthesis of atropisomeric hydrazides bearing a cyclic quaternary stereocenter through ternary catalysis.
Wang, Xia; Wang, Shao-Jie; Xin, Xiaolan; An, Hao; Tu, Zhifeng; Yang, Hui; Wong, Ming Wah; Lu, Shenci; Chemical science 15 (2024) 13240–13249; doi:10.1039/d4sc03190c

data_1572010
_publ_section_title
;
 Enantioconvergent and diastereoselective synthesis of atropisomeric
 hydrazides bearing a cyclic quaternary stereocenter through ternary
 catalysis.
;
_journal_issue                   33
_journal_name_full               'Chemical science'
_journal_page_first              13240
_journal_page_last               13249
_journal_paper_doi               10.1039/d4sc03190c
_journal_volume                  15
_journal_year                    2024
_chemical_formula_sum            'C36 H42 N4 O11'
_chemical_formula_weight         706.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-03-22 deposited with the CCDC.	2024-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.9652(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.78147(11)
_cell_length_b                   14.09396(13)
_cell_length_c                   16.78114(12)
_cell_measurement_temperature    301(2)
_cell_volume                     3686.92(5)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      301(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.951
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            71352
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.415
_diffrn_reflns_theta_min         4.117
_exptl_absorpt_coefficient_mu    0.792
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_F_000             1496
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.036
_refine_ls_extinction_coef       0.0024(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         7355
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0670P)^2^+1.1021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1350
_refine_ls_wR_factor_ref         0.1379
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6676
_reflns_number_total             7355
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03190c2.cif
_cod_data_source_block           zhailele_0320_auto
_cod_depositor_comments
'Adding full bibliography for 1572009--1572010.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1572010
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              29101