Light-driven CO2 reduction with substituted imidazole-pyridine Re catalysts favoring formic acid production
Chafin, Ryan; Sujan, Majharul Islam; Parkin, Sean; Jurss, Jonah W.; Huckaba, Aron J.; RSC Advances 15 (2025) 12547–12556; doi:10.1039/D5RA01561H

data_7250298
_publ_section_title
;
 Light-driven CO2 reduction with substituted imidazole-pyridine Re
 catalysts favoring formic acid production
;
_journal_issue                   16
_journal_name_full               'RSC Advances'
_journal_page_first              12547
_journal_page_last               12556
_journal_paper_doi               10.1039/D5RA01561H
_journal_volume                  15
_journal_year                    2025
_chemical_formula_moiety         'C21 H19 Br N3 O3 Re'
_chemical_formula_sum            'C21 H19 Br N3 O3 Re'
_chemical_formula_weight         627.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-2019/2 and CIFFIX'
_audit_update_record
;
2025-03-05 deposited with the CCDC.	2025-04-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.4135(6)
_cell_length_b                   13.9657(5)
_cell_length_c                   19.9434(9)
_cell_measurement_reflns_used    9766
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      3.34
_cell_volume                     4014.5(3)
_computing_cell_refinement       '<i>APEX3</i> (Bruker-AXS, 2016)'
_computing_data_collection       '<i>APEX3</i> (Bruker-AXS, 2016)'
_computing_data_reduction        '<i>APEX3</i> (Bruker-AXS, 2016)'
_computing_molecular_graphics    '<i>XP in SHELXTL</i> (Sheldrick, 2008)'
_computing_publication_material
'<i>SHELX</i> (Sheldrick, 2008) and <i>CIFFIX</i> (Parkin, 2013)'
_computing_structure_refinement  '<i>SHELXL-2019/2</i> (Sheldrick, 2015b)'
_computing_structure_solution    '<i>SHELXT</i> (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture dual source'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            43216
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.507
_diffrn_reflns_theta_min         2.042
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    8.073
_exptl_absorpt_correction_T_max  0.801
_exptl_absorpt_correction_T_min  0.476
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '<i>SADABS</i> (Krause et al., 2015)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    2.076
_exptl_crystal_description       plate
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.652
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       0.00056(5)
_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   1.163
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4593
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0195
_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^)+6.8148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0434
_refine_ls_wR_factor_ref         0.0440
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4349
_reflns_number_total             4593
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra01561h2.cif
_cod_data_source_block           m23269
_cod_database_code               7250298
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_min   0.282
_shelx_estimated_absorpt_t_max   0.794
_exptl_absorpt_special_details
; 
In addition to absorption, multi-scan techniques also correct other slowly 
varying changes in scale factor over reciprocal space, such as those caused 
by X-ray beam inhomogeneity, goniometer imperfection, crystal decomposition, 
crystal longer than the X-ray beam cross section, absorption by the crystal 
mount, scan truncation etc. These account, by and large, for the difference 
between SHELX estimates of Tmin and Tmax and the _exptl_absorpt_correction_ 
values. 
;
_shelx_res_checksum              2108