Acid-Assisted Hydrogenation of CO2 to Methanol in a Homogeneous Catalytic Cascade System
Chu, Wan-Yi; Culakova, Zuzana; Wang, Bernie T.; Goldberg, Karen I.; ACS Catalysis 9 (2019) 9317–; doi:10.1021/acscatal.9b02280

data_4514626
_publ_section_title
;
 Acid-Assisted Hydrogenation of CO2 to Methanol in a Homogeneous Catalytic
 Cascade System
;
_journal_issue                   10
_journal_name_full               'ACS Catalysis'
_journal_page_first              9317
_journal_paper_doi               10.1021/acscatal.9b02280
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C26 H44 F3 Ir O4 P2 S, C H2 Cl2'
_chemical_formula_sum            'C27 H46 Cl2 F3 Ir O4 P2 S'
_chemical_formula_weight         848.74
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   direct
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2017-12-21T12:35:22-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 116.5530(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5246(5)
_cell_length_b                   12.6284(4)
_cell_length_c                   17.5400(5)
_cell_measurement_reflns_used    9851
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.36
_cell_measurement_theta_min      2.82
_cell_measurement_wavelength     0.71073
_cell_volume                     3274.16(17)
_computing_cell_refinement       'SAINT V8.34A integration software'
_computing_data_collection       'Bruker APEX2 software'
_computing_data_reduction        'SORTAV (Blessing, 1995)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_orient_matrix_UB_11      0.012526
_diffrn_orient_matrix_UB_12      -0.077686
_diffrn_orient_matrix_UB_13      0.002023
_diffrn_orient_matrix_UB_21      0.066448
_diffrn_orient_matrix_UB_22      0.014484
_diffrn_orient_matrix_UB_23      0.030401
_diffrn_orient_matrix_UB_31      -0.002107
_diffrn_orient_matrix_UB_32      -0.005058
_diffrn_orient_matrix_UB_33      0.055981
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15829
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         28.375
_diffrn_reflns_theta_min         1.408
_diffrn_source                   'sealed x-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.451
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.702
_refine_diff_density_min         -0.67
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     376
_refine_ls_number_reflns         8154
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0195
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0125P)^2^+0.6740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0411
_refine_ls_wR_factor_ref         0.0422
_reflns_Friedel_coverage         0
_reflns_number_gt                7345
_reflns_number_total             8154
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs9b02280_si_004.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4514626
_shelx_estimated_absorpt_t_min   0.428
_shelx_estimated_absorpt_t_max   0.518
_shelx_res_checksum              5537
_shelx_hkl_checksum              72155