Sequential one-pot <i>N</i>-alkylation and aminocarbonylation of primary amines catalyzed by heterobimetallic Ir/Pd complexes.
Abdolrahimi, Amin; Woite, Philipp; Kretschmar, Konrad; Roemelt, Michael; Braun, Thomas; He, Ouchan; Chemical science 16 (2025) 19414–19422; doi:10.1039/d5sc03892h

data_1575740
_publ_section_title
;
 Sequential one-pot <i>N</i>-alkylation and aminocarbonylation of primary
 amines catalyzed by heterobimetallic Ir/Pd complexes.
;
_journal_issue                   41
_journal_name_full               'Chemical science'
_journal_page_first              19414
_journal_page_last               19422
_journal_paper_doi               10.1039/d5sc03892h
_journal_volume                  16
_journal_year                    2025
_chemical_formula_sum            'C23 H46 Cl3 Ir N4 O3 P2 Pd S2'
_chemical_formula_weight         957.65
_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
_audit_update_record
;
2025-03-10 deposited with the CCDC.	2025-09-15 downloaded from the CCDC.
;
_cell_angle_alpha                104.039(3)
_cell_angle_beta                 92.766(3)
_cell_angle_gamma                92.412(3)
_cell_formula_units_Z            2
_cell_length_a                   8.7278(8)
_cell_length_b                   10.1403(8)
_cell_length_c                   20.1959(17)
_cell_measurement_reflns_used    9644
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.34
_cell_volume                     1729.3(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX4'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            91184
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.341
_diffrn_reflns_theta_min         2.340
_exptl_absorpt_coefficient_mu    4.840
_exptl_absorpt_correction_T_max  0.4920
_exptl_absorpt_correction_T_min  0.2116
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.839
_exptl_crystal_description       prism
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.407
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.052
_refine_diff_density_max         0.793
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         8621
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0172
_refine_ls_R_factor_gt           0.0165
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0187P)^2^+1.4814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0408
_refine_ls_wR_factor_ref         0.0412
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8412
_reflns_number_total             8621
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc03892h2.cif
_cod_data_source_block           mo_o22_HI_007_0m_a
_cod_depositor_comments
'Adding full bibliography for 1575739--1575741.cif.'
_cod_database_code               1575740
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.243
_shelx_estimated_absorpt_t_max   0.787
_shelx_res_checksum              69574