A thiolated copper-hydride nanocluster with chloride bridging as a catalyst for carbonylative C-N coupling of aryl amines under mild conditions: a combined experimental and theoretical study.
Das, Anish Kumar; Biswas, Sourav; Pal, Amit; Manna, Surya Sekhar; Sardar, Avirup; Mondal, Pradip Kumar; Sahoo, Basudev; Pathak, Biswarup; Mandal, Sukhendu; Nanoscale 16 (2024) 3583–3590; doi:10.1039/d3nr05912j

data_1570749
_publ_section_title
;
 A thiolated copper-hydride nanocluster with chloride bridging as a
 catalyst for carbonylative C-N coupling of aryl amines under mild
 conditions: a combined experimental and theoretical study.
;
_journal_issue                   7
_journal_name_full               Nanoscale
_journal_page_first              3583
_journal_page_last               3590
_journal_paper_doi               10.1039/d3nr05912j
_journal_volume                  16
_journal_year                    2024
_chemical_formula_sum            'C121.5 H179.5 B Cl10.5 Cu29 F4 P4 S12'
_chemical_formula_weight         4450.43
_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
;
2023-06-10 deposited with the CCDC.	2024-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                64.888(8)
_cell_angle_beta                 81.085(9)
_cell_angle_gamma                81.878(9)
_cell_formula_units_Z            4
_cell_length_a                   24.596(5)
_cell_length_b                   28.305(6)
_cell_length_c                   29.247(6)
_cell_measurement_reflns_used    193059
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.000
_cell_measurement_theta_min      0.852
_cell_volume                     18149(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SAINT'
_computing_data_reduction        'Bruker APEX2'
_computing_molecular_graphics    'Mercury (Macrae <I>et al. </I>, 2008)'
_computing_publication_material  'WINZX (Farrugia, 2014) and PLATON(Spek, 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.4288
_diffrn_reflns_av_unetI/netI     0.5211
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            193059
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        24.000
_diffrn_reflns_theta_max         24.000
_diffrn_reflns_theta_min         0.852
_exptl_absorpt_coefficient_mu    3.679
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_description       Plate-like
_exptl_crystal_F_000             8884
_exptl_crystal_size_max          0.095
_exptl_crystal_size_mid          0.048
_exptl_crystal_size_min          0.028
_refine_diff_density_max         1.779
_refine_diff_density_min         -1.881
_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.912
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3086
_refine_ls_number_reflns         56494
_refine_ls_number_restraints     5490
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.3605
_refine_ls_R_factor_gt           0.1233
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1874P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2983
_refine_ls_wR_factor_ref         0.4415
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12945
_reflns_number_total             56494
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nr05912j2.cif
_cod_data_source_block           CuTBT_new_a
_cod_depositor_comments
;
          Adding full bibliography for 1570749.cif.

2025-06-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C243 H359 B2 Cl21 Cu58 F8 P8 S24'
_cod_original_formula_weight         8900.87
_cod_original_formula_units_Z            2
_cod_original_cell_volume        18149(6)
_cod_database_code               1570749
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.721
_shelx_estimated_absorpt_t_max   0.904
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              69999
_shelx_hkl_checksum              36277
_shelx_fab_checksum              77575