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_4128892
_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            'C130 H141 B Fe4 N3 O2 P3 S4'
_chemical_formula_weight         2232.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 95.023(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.597(4)
_cell_length_b                   30.822(8)
_cell_length_c                   22.933(6)
_cell_measurement_reflns_used    9827
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.05
_cell_measurement_theta_min      2.35
_cell_volume                     11686(5)
_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 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1103
_diffrn_reflns_av_unetI/netI     0.0605
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            388477
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.650
_diffrn_reflns_theta_min         1.456
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Herbst-Irmer et al., 2015)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4704
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.035
_exptl_transmission_factor_max   0.7461
_exptl_transmission_factor_min   0.6591
_refine_diff_density_max         1.788
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1715
_refine_ls_number_reflns         35911
_refine_ls_number_restraints     2369
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+13.7778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1079
_refine_ls_wR_factor_ref         0.1268
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24228
_reflns_number_total             35911
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b06975_si_003.cif
_cod_data_source_block           LNP3Fe4S4EtBPh4
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4128892
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.804
_shelx_estimated_absorpt_t_max   0.978
_shelx_res_checksum              94205
_shelx_hkl_checksum              90900