Structural and functional biomimetics of [Fe]-hydrogenase featuring a mono-, di- or tetrasubstituted pyridine ligand with a <i>fac</i>-C, N, and S ligation.
Song, Li-Cheng; Zhang, Zhen-Qing; Liu, Bei-Bei; Dalton transactions (Cambridge, England : 2003) 52 (2023) 9215–9228; doi:10.1039/d3dt01285a

data_7713427
_publ_section_title
;
 Structural and functional biomimetics of [Fe]-hydrogenase featuring a
 mono-, di- or tetrasubstituted pyridine ligand with a <i>fac</i>-C, N,
 and S ligation.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9215
_journal_page_last               9228
_journal_paper_doi               10.1039/d3dt01285a
_journal_volume                  52
_journal_year                    2023
_chemical_formula_sum            'C19.25 H18.5 Cl0.5 Fe I N O4 S'
_chemical_formula_weight         560.38
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-06-02 deposited with the CCDC.	2023-06-23 downloaded from the CCDC.
;
_cell_angle_alpha                68.5670(10)
_cell_angle_beta                 83.0930(10)
_cell_angle_gamma                85.975(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4758(4)
_cell_length_b                   9.5929(4)
_cell_length_c                   12.9156(5)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.17
_cell_volume                     1084.47(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0381
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24743
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.393
_diffrn_reflns_theta_min         2.282
_exptl_absorpt_coefficient_mu    2.300
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0831 before and 0.0517 after correction.
The Ratio of minimum to maximum transmission is 0.3406.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_description       block
_exptl_crystal_F_000             553
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.778
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4430
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0581P)^2^+0.6458P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0885
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3795
_reflns_number_total             4430
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01285a2.cif
_cod_data_source_block           Complex5
_cod_original_formula_sum        'C19.25 H18.50 Cl0.50 Fe I N O4 S'
_cod_database_code               7713427
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.656
_shelx_estimated_absorpt_t_max   0.803
_shelx_res_checksum              60276