An Iron Pyridyl-Carbene Electrocatalyst for Low Overpotential CO2 Reduction to CO
Gonell, Sergio; Lloret-Fillol, Julio; Miller, Alexander J. M.; ACS Catalysis  (2020) 615–626; doi:10.1021/acscatal.0c03798

data_4518364
_publ_section_title
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 An Iron Pyridyl-Carbene Electrocatalyst for Low Overpotential CO2
 Reduction to CO
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              615
_journal_page_last               626
_journal_paper_doi               10.1021/acscatal.0c03798
_journal_year                    2020
_chemical_formula_moiety         'C30 H25 Fe N7, C H2 Cl2, F6 P, F6.43 P'
_chemical_formula_sum            'C31 H27 Cl2 F12.43 Fe N7 P2'
_chemical_formula_weight         922.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-09-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 107.9380(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7127(2)
_cell_length_b                   17.4292(3)
_cell_length_c                   16.0993(2)
_cell_measurement_reflns_used    8844
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.231
_cell_measurement_theta_min      3.842
_cell_volume                     3660.72(10)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 1.000
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            44634
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.275
_diffrn_reflns_theta_min         3.713
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.386
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5162
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1150 before and 0.0569 after correction. The Ratio of minimum to maximum transmission is 0.6854. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1855
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         6701
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0661
_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^)+(0.0616P)^2^+11.9072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1543
_refine_ls_wR_factor_ref         0.1662
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5209
_reflns_number_total             6701
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c03798_si_003.cif
_cod_data_source_block           x1809001
_cod_database_code               4518364
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.663
_shelx_estimated_absorpt_t_min   0.328
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
3. Uiso/Uaniso restraints and constraints
Uanis(F16) \\sim Ueq: with sigma of 0 and sigma for terminal atoms of 0
4. Others
 Sof(H31C)=Sof(H31D)=Sof(Cl2)=1-FVAR(1)
 Sof(H31A)=Sof(H31B)=Sof(Cl3)=FVAR(1)
 Sof(F15)=1-FVAR(2)
 Sof(F16)=FVAR(2)
 Sof(F11)=1-FVAR(3)
 Sof(F10)=FVAR(3)
 Sof(F13)=1-FVAR(4)
 Sof(F12)=FVAR(4)
5.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C31(H31C,H31D)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C27(H27), C4(H4), C28(H28), C17(H17), C25(H25), C16(H16), C13(H13),
 C14(H14), C5(H5), C20(H20), C21(H21), C22(H22), C6(H6), C10(H10), C15(H15),
 C12(H12), C11(H11), C26(H26)
5.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C30(H30A,H30B,H30C)
;
_olex2_submission_special_instructions 'No special instructions were received'