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_4518017
_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         'C26 H28 N2 O4 S2'
_chemical_formula_sum            'C26 H28 N2 O4 S2'
_chemical_formula_weight         496.62
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                73.734(7)
_cell_angle_beta                 83.867(6)
_cell_angle_gamma                67.198(6)
_cell_formula_units_Z            2
_cell_length_a                   9.950(2)
_cell_length_b                   10.420(2)
_cell_length_c                   13.328(3)
_cell_measurement_reflns_used    1591
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.866
_cell_measurement_theta_min      2.196
_cell_volume                     1222.9(4)
_computing_cell_refinement       'APEX3 v2019.1.0'
_computing_data_collection       'APEX3 v2019.1.0'
_computing_data_reduction        'Saint, APEX v2019.1.0.'
_computing_molecular_graphics    'POV-Ray v 3.7'
_computing_publication_material  'APEX3 v2018.7.2'
_computing_structure_refinement  SHELXTL-2018/3
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.869
_diffrn_measurement_device_type  'Bruker AXS D8 Venture '
_diffrn_measurement_method       'profile data from \q/2\q scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.869
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            39075
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.869
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.866
_diffrn_reflns_theta_min         2.196
_exptl_absorpt_coefficient_mu    0.253
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.896
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_description       'prism frag'
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.443
_exptl_crystal_size_mid          0.301
_exptl_crystal_size_min          0.255
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.0055(9)
_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   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         6128
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0364P)^2^+0.6937P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0828
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5665
_reflns_number_total             6128
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c02676_si_002.cif
_cod_data_source_block           msu_032_a
_cod_database_code               4518017
_shelx_estimated_absorpt_t_min   0.896
_shelx_estimated_absorpt_t_max   0.938
_shelx_res_checksum              95497
_shelx_hkl_checksum              78463