Cyclopentadienone‒NHC iron(0) complexes as low valent electrocatalysts for water oxidation
Cingolani, Andrea; Gualandi, Isacco; Scavetta, Erika; Cesari, Cristiana; Zacchini, Stefano; Tonelli, Domenica; Zanotti, Valerio; Franchi, Paola; Lucarini, Marco; Sicilia, Emilia; Mazzone, Gloria; Nanni, Daniele; Mazzoni, Rita; Catalysis Science & Technology 11 (2021) 1407–1418; doi:10.1039/D0CY02329A

data_1559971
_publ_section_title
;
 Cyclopentadienone--NHC iron(0) complexes as low valent electrocatalysts
 for water oxidation
;
_journal_issue                   4
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              1407
_journal_page_last               1418
_journal_paper_doi               10.1039/D0CY02329A
_journal_volume                  11
_journal_year                    2021
_chemical_formula_sum            'C20 H30 Fe N2 O4 Si2'
_chemical_formula_weight         474.49
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-07-24 deposited with the CCDC.	2021-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.570(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4055(6)
_cell_length_b                   18.3319(12)
_cell_length_c                   15.0466(10)
_cell_measurement_reflns_used    9815
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.242
_cell_measurement_theta_min      2.6025
_cell_volume                     2316.2(3)
_computing_cell_refinement       'APEX3 (Bruker AXS, 2015)'
_computing_data_collection       'APEX3 (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT (Bruker AXS, 2015)'
_computing_molecular_graphics    'ORTEPIII (Johnson, 1996)'
_computing_publication_material  'XCIF 2014/2 (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'PHOTON100 area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28207
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.997
_diffrn_reflns_theta_min         1.752
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.782
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6310
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1583 (selected reflections only, before parameter refinement)
 R(int) =  0.0682 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       prism
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.421
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         5504
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.421
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0751
_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^)+7.4456P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1296
_refine_ls_wR_factor_ref         0.1319
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4943
_reflns_number_total             5504
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cy02329a2.cif
_cod_data_source_block           p21n
_cod_depositor_comments          'Adding full bibliography for 1559971.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1559971
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.853
_shelx_estimated_absorpt_t_max   0.892
_shelx_res_checksum              6916