NHC ligand-based half-sandwich iridium complexes: synthesis, structure and catalytic activity in acceptorless dehydrogenation and transfer hydrogenation
Li, Rong-Jian; Wang, Yang; Jin, Yan; Deng, Wei; Liu, Zhen-Jiang; Yao, Zi-Jian; New Journal of Chemistry 45 (2021) 19002–19010; doi:10.1039/D1NJ03824A

data_7060996
_publ_section_title
;
 NHC ligand-based half-sandwich iridium complexes: synthesis, structure
 and catalytic activity in acceptorless dehydrogenation and transfer
 hydrogenation
;
_journal_issue                   40
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              19002
_journal_page_last               19010
_journal_paper_doi               10.1039/D1NJ03824A
_journal_volume                  45
_journal_year                    2021
_chemical_formula_sum            'C21 H23 Br0.3 Cl0.7 Ir N3'
_chemical_formula_weight         558.41
_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   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-06-30 deposited with the CCDC.	2021-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.794(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9625(14)
_cell_length_b                   15.3150(13)
_cell_length_c                   8.0607(7)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      56.86
_cell_measurement_theta_min      3.49
_cell_volume                     1960.5(3)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.0805
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            28794
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         57.033
_diffrn_reflns_theta_min         4.845
_exptl_absorpt_coefficient_mu    9.809
_exptl_absorpt_correction_T_max  0.751
_exptl_absorpt_correction_T_min  0.521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.892
_exptl_crystal_description       needle
_exptl_crystal_F_000             1074
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.955
_refine_diff_density_min         -1.043
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         4007
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0294P)^2^+3.4360P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0801
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3256
_reflns_number_total             4007
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj03824a2.cif
_cod_data_source_block           ga_210507da_a
_cod_depositor_comments
'Adding full bibliography for 7060996--7060997.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C21 H23 Br0.30 Cl0.70 Ir N3'
_cod_database_code               7060996
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.140
_shelx_estimated_absorpt_t_max   0.757
_shelx_res_checksum              65217