Synthesis, Characterization, and Nitrogenase-Relevant Reactions of an Iron Sulfide Complex with a Bridging Hydride.
Arnet, Nicholas A.; Dugan, Thomas R.; Menges, Fabian S.; Mercado, Brandon Q.; Brennessel, William W.; Bill, Eckhard; Johnson, Mark A.; Holland, Patrick L.; Journal of the American Chemical Society 137 (2015) 13220–13223; doi:10.1021/jacs.5b06841

data_4129488
_publ_section_title
;
 Synthesis, Characterization, and Nitrogenase-Relevant Reactions of an
 Iron Sulfide Complex with a Bridging Hydride.
;
_journal_issue                   41
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13220
_journal_page_last               13223
_journal_paper_doi               10.1021/jacs.5b06841
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C66 H101 Fe2 N4 Na O2 S, C4 H10 O'
_chemical_formula_sum            'C70 H111 Fe2 N4 Na O3 S'
_chemical_formula_weight         1223.38
_chemical_name_common            holtd02
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.646(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   47.214(7)
_cell_length_b                   12.7204(19)
_cell_length_c                   23.732(4)
_cell_measurement_reflns_used    3721
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      32.05
_cell_measurement_theta_min      2.72
_cell_volume                     13907(4)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       'area detector, \w scans per \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_av_sigmaI/netI    0.0497
_diffrn_reflns_limit_h_max       70
_diffrn_reflns_limit_h_min       -70
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            121264
_diffrn_reflns_theta_full        32.03
_diffrn_reflns_theta_max         32.03
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.499
_exptl_absorpt_correction_T_max  0.8729
_exptl_absorpt_correction_T_min  0.8066
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2007)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5296
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.643
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     854
_refine_ls_number_reflns         24119
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0994
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0821P)^2^+13.6459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1477
_refine_ls_wR_factor_ref         0.1695
_reflns_number_gt                15909
_reflns_number_total             24119
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b06841_si_002.cif
_cod_data_source_block           2
_cod_database_code               4129488