Fe(III)-Based Tandem Catalysis for Amidomethylative Multiple Substitution Reactions of α-Substituted Styrene Derivatives
Qian, Xiaolin; Zhou, Hui; Chaminda Lakmal, Hetti Handi; Lucore, James; Wang, Xuesong; Valle, Henry U.; Donnadieu, Bruno; Xu, Xue; Cui, Xin; ACS Catalysis  (2020) 10627–; doi:10.1021/acscatal.0c02676

data_4518016
_publ_section_title
;
 Fe(III)-Based Tandem Catalysis for Amidomethylative Multiple Substitution
 Reactions of \a-Substituted Styrene Derivatives
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              10627
_journal_paper_doi               10.1021/acscatal.0c02676
_journal_year                    2020
_chemical_formula_moiety         'C32 H32 N2 O4 S2'
_chemical_formula_sum            'C32 H32 N2 O4 S2'
_chemical_formula_weight         572.71
_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   geom
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 94.8570(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9602(4)
_cell_length_b                   14.7542(6)
_cell_length_c                   18.1626(7)
_cell_measurement_reflns_used    8454
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.518
_cell_measurement_theta_min      3.865
_cell_volume                     2926.5(2)
_computing_cell_refinement
'SHELXTL, Acta Cryst., Sect. A 2008, 64, 112-122.'
_computing_data_collection       'APEX3 v2018.1.0'
_computing_data_reduction        'Saint, APEX v2018.1.0.'
_computing_molecular_graphics    Ortep3
_computing_publication_material  'APEX3 v2018.1.0'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT, Acta Cryst., Sect. A 2015, A71, 3-8.'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker AXS D8 Venture '
_diffrn_measurement_method       'profile data from \q/2\q scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            50601
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.518
_diffrn_reflns_theta_min         3.865
_exptl_absorpt_coefficient_mu    1.968
_exptl_absorpt_correction_T_max  0.722
_exptl_absorpt_correction_T_min  0.491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       'prism frag'
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.421
_exptl_crystal_size_mid          0.272
_exptl_crystal_size_min          0.177
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       0.00075(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         5791
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0531P)^2^+1.4839P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0933
_refine_ls_wR_factor_ref         0.0998
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5623
_reflns_number_total             5791
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c02676_si_003.cif
_cod_data_source_block           i-2791
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4518016
_shelx_estimated_absorpt_t_min   0.491
_shelx_estimated_absorpt_t_max   0.722
_shelx_res_checksum              12367
_shelx_hkl_checksum              2055