Catalytic Hydrogenation of CO<sub>2</sub> to Methanol Using Multinuclear Iridium Complexes in a Gas-Solid Phase Reaction.
Kanega, Ryoichi; Onishi, Naoya; Tanaka, Shinji; Kishimoto, Haruo; Himeda, Yuichiro; Journal of the American Chemical Society 143 (2021) 1570–1576; doi:10.1021/jacs.0c11927

data_4135612
_publ_section_title
;
 Catalytic Hydrogenation of CO<sub>2</sub> to Methanol Using Multinuclear
 Iridium Complexes in a Gas-Solid Phase Reaction.
;
_journal_issue                   3
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1570
_journal_page_last               1576
_journal_paper_doi               10.1021/jacs.0c11927
_journal_volume                  143
_journal_year                    2021
_chemical_formula_moiety         'C38 H52 Ir2 N4 O14 S2'
_chemical_formula_sum            'C38 H52 Ir2 N4 O14 S2'
_chemical_formula_weight         1237.41
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                64.682(9)
_cell_angle_beta                 89.99(2)
_cell_angle_gamma                89.904(16)
_cell_formula_units_Z            1
_cell_length_a                   10.162(6)
_cell_length_b                   10.528(6)
_cell_length_c                   10.914(5)
_cell_measurement_reflns_used    3127
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.00
_cell_volume                     1055.5(10)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r16'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r16'
_computing_molecular_graphics    'CrystalStructure 4.2'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_structure_refinement  'SHELXL Version 2016/6 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 13.653
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0899
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10580
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.594
_diffrn_reflns_theta_min         3.016
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.485
_exptl_absorpt_correction_T_max  0.273
_exptl_absorpt_correction_T_min  0.175
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.947
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             606.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         2.49
_refine_diff_density_min         -2.34
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     296
_refine_ls_number_reflns         4825
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0060P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0834
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4550
_reflns_number_total             4825
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja0c11927_si_002.cif
_cod_data_source_block           201900805
_cod_database_code               4135612
_shelx_res_checksum              72468
_shelx_hkl_checksum              26437