Formation and reactivity of a unique M⋯C-H interaction stabilized by carborane cages.
Liu, Xin-Ran; Cui, Peng-Fei; García-Rodeja, Yago; Solà, Miquel; Jin, Guo-Xin; Chemical science 15 (2024) 9274–9280; doi:10.1039/d4sc01158a

data_1571659
_publ_section_title
;
 Formation and reactivity of a unique M&#x22ef;C-H interaction stabilized
 by carborane cages.
;
_journal_issue                   24
_journal_name_full               'Chemical science'
_journal_page_first              9274
_journal_page_last               9280
_journal_paper_doi               10.1039/d4sc01158a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_sum            'C17.6 H32.8 B16 Ir0.8 N1.6 S1.6'
_chemical_formula_weight         644.87
_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   mixed
_audit_creation_method           SHELXL-2019/2
_audit_update_record
;
2023-10-25 deposited with the CCDC.	2024-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.2970(10)
_cell_angle_gamma                90
_cell_formula_units_Z            5
_cell_length_a                   19.1073(6)
_cell_length_b                   13.3046(4)
_cell_length_c                   13.9712(4)
_cell_measurement_reflns_used    9852
_cell_measurement_temperature    174(2)
_cell_measurement_theta_max      54.79
_cell_measurement_theta_min      3.55
_cell_volume                     3505.03(18)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      174(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           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23569
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        52.187
_diffrn_reflns_theta_max         52.187
_diffrn_reflns_theta_min         3.537
_exptl_absorpt_coefficient_mu    5.715
_exptl_absorpt_correction_T_max  0.750
_exptl_absorpt_correction_T_min  0.421
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_description       block
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.673
_refine_diff_density_min         -1.847
_refine_diff_density_rms         0.177
_refine_ls_extinction_coef       0.00042(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         5958
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0357
_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^)+(0.0899P)^2^+2.6626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1171
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5528
_reflns_number_total             5958
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01158a2.cif
_cod_data_source_block           230804b_0ma_a
_cod_depositor_comments
'Adding full bibliography for 1571656--1571663.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C17.60 H32.80 B16 Ir0.80 N1.60 S1.60'
_cod_database_code               1571659
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_min   0.318
_shelx_estimated_absorpt_t_max   0.394
_shelx_res_checksum              87985