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_1565267
_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
; 
C31 H39 Fe2 N O4 P3 S2, B F4, 0.93(C4 H10 O), 0.07(C H2 Cl2) 
;
_chemical_formula_sum            'C34.79 H48.44 B Cl0.14 F4 Fe2 N O4.93 P3 S2'
_chemical_formula_weight         920.04
_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                 101.5008(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5415(3)
_cell_length_b                   17.0231(4)
_cell_length_c                   18.4766(4)
_cell_measurement_reflns_used    26830
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.39
_cell_volume                     4173.68(16)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'APEX3 V2018.7-2 (Bruker, 2018)'
_computing_data_reduction
; 
SAINT V8.38A, XPREP v2014/2, (Bruker, 2018), SADABS V2016/2 
(Krause et al., 2015) 
;
_computing_molecular_graphics
; 
SHELXTL v2014-7 (Bruker, 2018), CrystalMaker v9.2.8 (CrystalMaker, 2016) 
;
_computing_publication_material  'XCIF V2014-2 (Bruker, 2018)'
_computing_structure_refinement  'SHELXL-2018-3 (Sheldrick, 2015a)'
_computing_structure_solution    'SHELXT-2014-5 (Sheldrick, 2015b)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  ed15Ls
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            60739
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.089
_exptl_absorpt_coefficient_mu    0.977
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7005
_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    1.464
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1904
_exptl_crystal_id                ed15Ls
_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 1 -2) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.223
_exptl_crystal_size_mid          0.214
_exptl_crystal_size_min          0.079
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         9573
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0168P)^2^+5.8109P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0718
_refine_ls_wR_factor_ref         0.0750
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8432
_reflns_number_total             9573
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05803g2.cif
_cod_data_source_block           ed15Ls
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1565267
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.812
_shelx_estimated_absorpt_t_max   0.927
_shelx_res_checksum              80451
_shelx_hkl_checksum              62528