Nitrogenase-Relevant Reactivity of a Synthetic Iron-Sulfur-Carbon Site.
Speelman, Amy L.; Čorić, Ilija; Van Stappen, Casey; DeBeer, Serena; Mercado, Brandon Q.; Holland, Patrick L.; Journal of the American Chemical Society 141 (2019) 13148–13157; doi:10.1021/jacs.9b05353

data_4127851
_publ_section_title
;
 Nitrogenase-Relevant Reactivity of a Synthetic Iron-Sulfur-Carbon Site.
;
_journal_issue                   33
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13148
_journal_page_last               13157
_journal_paper_doi               10.1021/jacs.9b05353
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C48 H54 F2 Fe S2, 2(C20 H40 K O8)'
_chemical_formula_sum            'C88 H134 F2 Fe K2 O16 S2'
_chemical_formula_weight         1684.11
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
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_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 102.513(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0250(6)
_cell_length_b                   26.0513(8)
_cell_length_c                   32.5801(11)
_cell_measurement_reflns_used    21655
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      25.2890
_cell_measurement_theta_min      2.9630
_cell_volume                     13278.2(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.31a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.31a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.31a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB-2014/2 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 5.8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Dectris Pilatus 3R'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1135
_diffrn_reflns_av_unetI/netI     0.0843
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
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_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            153728
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.849
_diffrn_source                   'microfocus rotating anode'
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_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.39.31a (Rigaku Oxford Diffraction, 2017) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    0.842
_exptl_crystal_description       Block
_exptl_crystal_F_000             3616
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.726
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1058
_refine_ls_number_reflns         30432
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0602
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0870P)^2^+3.1436P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1513
_refine_ls_wR_factor_ref         0.1696
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20054
_reflns_number_total             30432
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           007c-19008
_cod_database_code               4127851
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.951
_shelx_estimated_absorpt_t_max   0.963
_shelx_res_checksum              53712
_shelx_hkl_checksum              74477
_shelx_fab_checksum              32712