A Synthetic Model of Enzymatic [Fe<sub>4</sub>S<sub>4</sub>]-Alkyl Intermediates.
Ye, Mengshan; Thompson, Niklas B.; Brown, Alexandra C.; Suess, Daniel L. M.; Journal of the American Chemical Society 141 (2019) 13330–13335; doi:10.1021/jacs.9b06975

data_4128891
_publ_section_title
;
 A Synthetic Model of Enzymatic [Fe<sub>4</sub>S<sub>4</sub>]-Alkyl
 Intermediates.
;
_journal_issue                   34
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13330
_journal_page_last               13335
_journal_paper_doi               10.1021/jacs.9b06975
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C125.82 H130.19 B Cl2.45 Fe4 N3 O1.27 P3 S4'
_chemical_formula_weight         2247.06
_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-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 106.247(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.6783(10)
_cell_length_b                   19.0664(8)
_cell_length_c                   27.5418(11)
_cell_measurement_reflns_used    9473
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.99
_cell_measurement_theta_min      2.37
_cell_volume                     11433.3(8)
_computing_cell_refinement       'SAINT 8.38A (Bruker-AXS, 2017)'
_computing_data_collection       'APEX3 v2017.3.0 (Bruker-AXS, 2017)'
_computing_data_reduction        'SAINT 8.38A (Bruker-AXS, 2017)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.4
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Photon2 CPAD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1111
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            488735
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.302
_diffrn_reflns_theta_min         2.271
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Herbst-Irmer et al., 2015)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4704
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.005
_exptl_transmission_factor_max   0.7458
_exptl_transmission_factor_min   0.6558
_refine_diff_density_max         1.510
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1751
_refine_ls_number_reflns         31006
_refine_ls_number_restraints     2847
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0940
_refine_ls_R_factor_gt           0.0527
_refine_ls_shift/su_max          0.062
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0715P)^2^+11.8410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1277
_refine_ls_wR_factor_ref         0.1530
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20733
_reflns_number_total             31006
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b06975_si_002.cif
_cod_data_source_block           LNP3Fe4S4ClBPh4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4128891
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.813
_shelx_estimated_absorpt_t_max   0.996
_shelx_res_checksum              71055
_shelx_hkl_checksum              47995