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_4129489
_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
'C58 H83 Fe2 N4 S, C18 H36 N2 Na O6, 2(C4 H10 O)'
_chemical_formula_sum            'C84 H139 Fe2 N6 Na O8 S'
_chemical_formula_weight         1527.75
_chemical_name_common            holna06
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                87.134(3)
_cell_angle_beta                 87.195(3)
_cell_angle_gamma                76.886(3)
_cell_formula_units_Z            2
_cell_length_a                   13.876(2)
_cell_length_b                   15.610(3)
_cell_length_c                   20.119(3)
_cell_measurement_reflns_used    3973
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      23.72
_cell_measurement_theta_min      2.39
_cell_volume                     4235.7(12)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2013)'
_computing_publication_material  'SHELXTL (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1337
_diffrn_reflns_av_unetI/netI     0.1179
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            57279
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.030
_diffrn_reflns_theta_max         25.101
_diffrn_reflns_theta_min         1.713
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.428
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6116
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2012)'
_exptl_crystal_colour            'dark red-orange'
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     947
_refine_ls_number_reflns         15036
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1345
_refine_ls_R_factor_gt           0.0690
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0699P)^2^+2.6209P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1471
_refine_ls_wR_factor_ref         0.1730
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8809
_reflns_number_total             15036
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b06841_si_002.cif
_cod_data_source_block           3
_cod_database_code               4129489
_shelx_estimated_absorpt_t_min   0.912
_shelx_estimated_absorpt_t_max   0.943
_shelxl_version_number           2013-2
_shelx_res_checksum              90008
_shelx_hkl_checksum              26816