Inhibition of [FeFe]-Hydrogenase by Formaldehyde: Proposed Mechanism and Reactivity of FeFe Alkyl Complexes
Zhang, Fanjun; Woods, Toby John; Zhu, Lingyang; Rauchfuss, Thomas; Chemical Science  (2021) –; doi:10.1039/D1SC05803G

data_1565269
_publ_section_title
;
 Inhibition of [FeFe]-Hydrogenase by Formaldehyde: Proposed Mechanism and
 Reactivity of FeFe Alkyl Complexes
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC05803G
_journal_year                    2021
_chemical_formula_moiety         'C27 H21 Fe2 N3 O4 P S2, C8 H20 N'
_chemical_formula_sum            'C35 H41 Fe2 N4 O4 P S2'
_chemical_formula_weight         788.51
_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     'dual space'
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-08-18 deposited with the CCDC.	2021-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.0904(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8201(7)
_cell_length_b                   17.3607(7)
_cell_length_c                   13.5621(6)
_cell_measurement_reflns_used    29494
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.46
_cell_measurement_theta_min      2.58
_cell_volume                     3719.3(3)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2019)'
_computing_data_collection       'APEX3 V2019.11-0 (Bruker, 2019)'
_computing_data_reduction
; 
SAINT V8.40B, XPREP v2014/2, (Bruker, 2019), SADABS V2016/2 
(Krause et al., 2015) 
;
_computing_molecular_graphics
; 
SHELXTL v2014-7 (Bruker, 2019), CrystalMaker v9.2.8 (CrystalMaker, 2016) 
;
_computing_publication_material  'XCIF V2014-2 (Bruker, 2019)'
_computing_structure_refinement  'SHELXL-2018-3 (Sheldrick, 2015a)'
_computing_structure_solution    'SHELXT-2018-2 (Sheldrick, 2015b)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'Bruker D8 Venture/Photon II'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  ed82Ls
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            73436
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.477
_diffrn_reflns_theta_min         1.983
_exptl_absorpt_coefficient_mu    0.978
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2016/2 (Krause et al., 2015)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1640
_exptl_crystal_id                ed82Ls
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Paratone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (1 -4 0) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.468
_exptl_crystal_size_mid          0.305
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         7636
_refine_ls_number_restraints     332
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0600
_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^)+18.8367P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1300
_refine_ls_wR_factor_ref         0.1341
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6670
_reflns_number_total             7636
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05803g2.cif
_cod_data_source_block           ed82Ls
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1565269
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.658
_shelx_estimated_absorpt_t_max   0.949
_shelx_res_checksum              90162
_shelx_hkl_checksum              37583