Hydrogenation of CO2, Hydrogenocarbonate, and Carbonate to Formate in Water using Phosphine Free Bifunctional Iron Complexes
Coufourier, Sébastien; Gaignard Gaillard, Quentin; Lohier, Jean-François; Poater, Albert; Gaillard, Sylvain; Renaud, Jean-Luc; ACS Catalysis  (2020) 2108–2116; doi:10.1021/acscatal.9b04340

data_4517323
_publ_section_title
;
 Hydrogenation of CO2, Hydrogenocarbonate, and Carbonate to Formate in
 Water using Phosphine Free Bifunctional Iron Complexes
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              2108
_journal_page_last               2116
_journal_paper_doi               10.1021/acscatal.9b04340
_journal_year                    2020
_chemical_formula_moiety         'C34 H38.50 Fe N4 O6.25'
_chemical_formula_sum            'C34 H38.5 Fe N4 O6.25'
_chemical_formula_weight         659.04
_chemical_name_systematic
;
1,4-bis(morpholinoethyl)-5,7-diphenyl-1,2,3,4-tetrahyro-6H-cyclopenta[b]
pyrazin-6-one iron tricarbonyl
;
_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   mixed
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.3781(8)
_cell_length_b                   16.2241(10)
_cell_length_c                   31.858(2)
_cell_measurement_reflns_used    8331
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.43
_cell_volume                     6397.8(7)
_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-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.991
_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  0.0357
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            22848
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.017
_diffrn_reflns_theta_min         2.822
_exptl_absorpt_coefficient_mu    0.523
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs 2015/1'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       block
_exptl_crystal_F_000             2772
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_transmission_factor_max   0.7454
_exptl_transmission_factor_min   0.6277
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         6243
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0406P)^2^+3.8509P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.0944
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4970
_reflns_number_total             6243
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            '[Fe]bis(CH2)2-morpholine(Fe3c).cif'
_cod_data_source_block           coufourier23_0m_a
_cod_depositor_comments
'Adding full bibliography for 4517322--4517323.cif.'
_cod_original_formula_sum        'C34 H38.50 Fe N4 O6.25'
_cod_database_code               4517323
_shelx_shelxl_version_number     2017/1
_shelx_res_checksum              55968
_shelx_hkl_checksum              92772