Role of Ligand-Bound CO2 in the Hydrogenation of CO2 to Formate with a (PNP)Mn Catalyst
Schlenker, Kevin; Christensen, Elizabeth G.; Zhanserkeev, Asylbek A.; McDonald, Gabriel R.; Yang, Emily L.; Lutz, Kevin T.; Steele, Ryan P.; VanderLinden, Ryan T.; Saouma, Caroline T.; ACS Catalysis 11 (2021) 8358–8369; doi:10.1021/acscatal.1c01709

data_4518859
_publ_section_title
;
 Role of Ligand-Bound CO2 in the Hydrogenation of CO2 to Formate with a
 (PNP)Mn Catalyst
;
_journal_issue                   13
_journal_name_full               'ACS Catalysis'
_journal_page_first              8358
_journal_page_last               8369
_journal_paper_doi               10.1021/acscatal.1c01709
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C25 H43 Mn N O2 P2, B F4'
_chemical_formula_sum            'C25 H43 B F4 Mn N O2 P2'
_chemical_formula_weight         593.29
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3353(11)
_cell_length_b                   14.4426(11)
_cell_length_c                   12.0371(9)
_cell_measurement_reflns_used    5956
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.53
_cell_volume                     2839.8(4)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      103(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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_unetI/netI     0.0678
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24374
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.036
_diffrn_reflns_theta_min         2.531
_diffrn_source                   'Fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_description       RHOMBOHEDRAL
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.238
_exptl_crystal_size_mid          0.235
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Flack x determined using 2573 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         8196
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0307P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0715
_refine_ls_wR_factor_ref         0.0764
_reflns_Friedel_coverage         0.891
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.973
_reflns_number_gt                6847
_reflns_number_total             8196
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c01709_si_002.cif
_cod_data_source_block           20190503CS_P
_cod_database_code               4518859
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.865
_shelx_estimated_absorpt_t_max   0.954
_shelx_res_checksum              33646
_shelx_hkl_checksum              10535