Stereoselective amination via vinyl-silver intermediates derived from silver-catalyzed carboxylative cyclization of propargylamine.
Sadamitsu, Yuta; Saito, Kodai; Yamada, Tohru; Chemical communications (Cambridge, England) 56 (2020) 9517–9520; doi:10.1039/d0cc02273j

data_7126942
_publ_section_title
;
 Stereoselective amination via vinyl-silver intermediates derived from
 silver-catalyzed carboxylative cyclization of propargylamine.
;
_journal_issue                   66
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9517
_journal_page_last               9520
_journal_paper_doi               10.1039/d0cc02273j
_journal_volume                  56
_journal_year                    2020
_chemical_formula_sum            'C26 H39 N3 O7'
_chemical_formula_weight         505.60
_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   geom
_audit_update_record
;
2020-03-28 deposited with the CCDC.	2020-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                92.3150(10)
_cell_angle_beta                 106.4430(10)
_cell_angle_gamma                104.2890(10)
_cell_formula_units_Z            2
_cell_length_a                   9.6147(2)
_cell_length_b                   12.4662(3)
_cell_length_c                   12.8127(3)
_cell_measurement_reflns_used    4641
_cell_measurement_temperature    298.(2)
_cell_measurement_theta_max      25.8076
_cell_measurement_theta_min      2.2352
_cell_volume                     1417.26(6)
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298.(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0533
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16382
_diffrn_reflns_theta_full        27.28
_diffrn_reflns_theta_max         27.28
_diffrn_reflns_theta_min         2.46
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            transparent
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.382
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.449
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         6161
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.449
_refine_ls_R_factor_all          0.1190
_refine_ls_R_factor_gt           0.0758
_refine_ls_shift/su_max          0.200
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1085P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2259
_refine_ls_wR_factor_ref         0.2620
_reflns_number_gt                3775
_reflns_number_total             6161
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02273j2.cif
_cod_data_source_block           20190726_DV2
_cod_depositor_comments
'Adding full bibliography for 7126941--7126942.cif.'
_cod_database_code               7126942
_shelx_res_checksum              5182
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