[FeFe]-hydrogenase active site mimics containing pyridyl-functionalized phosphine ligands: Synthesis, characterization and electrochemical investigation
Hu, Shu-Peng; Zhang, Li; Wu, Yu; Feng, Jian-Shen; Wu, Sheng; Xie, Bin; Zou, Li-Ke; Inorganica Chimica Acta 504 (2020) 119435–; doi:10.1016/j.ica.2020.119435

data_1565242
_publ_section_title
;
 [FeFe]-hydrogenase active site mimics containing pyridyl-functionalized
 phosphine ligands: Synthesis, characterization and electrochemical
 investigation
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119435
_journal_paper_doi               10.1016/j.ica.2020.119435
_journal_volume                  504
_journal_year                    2020
_chemical_formula_moiety         'C26 H22 Fe2 N O5 P S2'
_chemical_formula_sum            'C26 H22 Fe2 N O5 P S2'
_chemical_formula_weight         635.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 115.7170(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6214(10)
_cell_length_b                   9.9836(6)
_cell_length_c                   17.6204(11)
_cell_measurement_reflns_used    6648
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5207
_cell_measurement_theta_min      2.4099
_cell_volume                     2634.3(3)
_computing_data_collection       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0215
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            13053
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.007
_diffrn_reflns_theta_max         25.007
_diffrn_reflns_theta_min         2.479
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.359
_exptl_absorpt_correction_T_max  0.8119
_exptl_absorpt_correction_T_min  0.7823
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4628
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0222
_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^)+(0.0248P)^2^+1.3663P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0522
_refine_ls_wR_factor_ref         0.0546
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4118
_reflns_number_total             4628
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            complex3-revision.cif
_cod_data_source_block           ww
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1565242
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.782
_shelx_estimated_absorpt_t_max   0.812
_shelx_res_checksum              83415
_shelx_hkl_checksum              60498