Chalcogenide-centered Cu11 clusters heteroleptically passivated by dichalcogenolates and iodo ligands
Brocha Silalahi, Rhone P.; Kuo, Yu-Te; Chiu, Tzu-Hao; Pillay, Michael N.; Liu, C. W.; New Journal of Chemistry 49 (2025) 9965–9972; doi:10.1039/D5NJ01571E

data_7063817
_publ_section_title
;
 Chalcogenide-centered Cu11 clusters heteroleptically passivated by
 dichalcogenolates and iodo ligands
;
_journal_issue                   23
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              9965
_journal_page_last               9972
_journal_paper_doi               10.1039/D5NJ01571E
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         'C54H108Cu11I3N6Se13 + 10(C4H10O)'
_chemical_formula_sum            'C94 H208 Cu11 I3 N6 O10 Se13'
_chemical_formula_weight         3688.78
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2025-05-11 deposited with the CCDC.	2025-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   19.4684(11)
_cell_length_b                   19.4684(11)
_cell_length_c                   42.649(3)
_cell_measurement_reflns_used    9491
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.27
_cell_measurement_theta_min      2.26
_cell_volume                     13999.1(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0350
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            22773
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.415
_diffrn_reflns_theta_min         2.092
_exptl_absorpt_coefficient_mu    8.547
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS applied. PLATON SQUEEZE was also used to remove 431 electrons from six solvent-accessible voids (each approx. 330 A3), corresponding to approximately 10 Et2O molecules, which have been included in the formula.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.626
_exptl_crystal_description       block
_exptl_crystal_F_000             8784
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_refine_diff_density_max         2.403
_refine_diff_density_min         -1.206
_refine_diff_density_rms         0.176
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.40(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         6239
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0564P)^2^+280.6759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1138
_reflns_Friedel_coverage         0.947
_reflns_Friedel_fraction_full    0.963
_reflns_Friedel_fraction_max     0.949
_reflns_number_gt                5414
_reflns_number_total             6239
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj01571e2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7063816--7063818.cif.'
_cod_original_cell_volume        13999.1(18)
_cod_database_code               7063817
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.513
_shelx_estimated_absorpt_t_max   0.628
_shelx_res_checksum              1544
_shelx_fab_checksum              59430
_platon_squeeze_void_probe_radius 1.20