Asymmetrically PNP-chelate diiron ethanedithiolate complexes Fe2(μ-edt)(CO)4{κ-(Ph2P)2NR} as diiron subsite models of [FeFe]-hydrogenases: Structural and electrocatalytic investigation
Li, Jian-Rong; Hu, Meng-Yuan; Zhao, Pei-Hua; Tian, Wen-Jing; Xu, Ting-Ting; Li, Yu-Long; Inorganica Chimica Acta 505 (2020) 119493–; doi:10.1016/j.ica.2020.119493

data_1565208
_publ_section_title
;
 Asymmetrically PNP-chelate diiron ethanedithiolate complexes
 Fe2(\m-edt)(CO)4{\k-(Ph2P)2NR} as diiron subsite models of
 [FeFe]-hydrogenases: Structural and electrocatalytic investigation
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119493
_journal_paper_doi               10.1016/j.ica.2020.119493
_journal_volume                  505
_journal_year                    2020
_chemical_formula_sum            'C35 H35 Fe2 N O4 P2 S2'
_chemical_formula_weight         771.40
_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-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 101.334(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0913(7)
_cell_length_b                   20.9676(14)
_cell_length_c                   16.2187(11)
_cell_measurement_reflns_used    9387
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.93
_cell_measurement_theta_min      2.56
_cell_volume                     3698.2(4)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            71754
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.101
_diffrn_reflns_theta_max         25.101
_diffrn_reflns_theta_min         2.269
_exptl_absorpt_coefficient_mu    1.021
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6237
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.048
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         6570
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0583P)^2^+5.9018P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1239
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5304
_reflns_number_total             6570
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-505-119493.cif
_cod_data_source_block           20180504e_0m
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1565208
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.6237
_shelx_estimated_absorpt_t_max   0.7452