Catalytic aminomethylative etherification of <i>N</i>-allenamides with <i>N</i>,<i>O</i>-acetals enabled by Lewis/Brønsted acid catalysis.
Zhang, Tao; Ji, Danqing; Sun, Jiangtao; Organic & biomolecular chemistry 21 (2023) 3340–3344; doi:10.1039/d3ob00363a

data_7159269
_publ_section_title
;
 Catalytic aminomethylative etherification of <i>N</i>-allenamides with
 <i>N</i>,<i>O</i>-acetals enabled by Lewis/Br&#xf8;nsted acid catalysis.
;
_journal_issue                   16
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              3340
_journal_page_last               3344
_journal_paper_doi               10.1039/d3ob00363a
_journal_volume                  21
_journal_year                    2023
_chemical_formula_sum            'C32 H34 N2 O3 S'
_chemical_formula_weight         526.67
_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_block_doi                 10.5517/ccdc.csd.cc23qy71
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-10-10 deposited with the CCDC.	2023-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.516(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_c                   16.6079(10)
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_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.46
_cell_volume                     2821.1(3)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
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_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
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_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19950
_diffrn_reflns_point_group_measured_fraction_full 0.999
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_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.352
_exptl_absorpt_coefficient_mu    0.150
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_description       block
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
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_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0498
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_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^)+(0.0396P)^2^+1.2719P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0944
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4115
_reflns_number_total             4979
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ob00363a2.cif
_cod_data_source_block           20181024cz_0m_a
_cod_depositor_comments
'Adding full bibliography for 7159269--7159270.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7159269
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.972
_shelx_estimated_absorpt_t_max   0.978
_shelx_res_checksum              88524