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_4129490
_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
'C67 H89 Fe2 N4 S, C18 H36 N2 Na O6, 2(C4 H8 O)'
_chemical_formula_sum            'C93 H141 Fe2 N6 Na O8 S'
_chemical_formula_weight         1637.86
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                94.225(7)
_cell_angle_beta                 94.850(7)
_cell_angle_gamma                95.622(7)
_cell_formula_units_Z            2
_cell_length_a                   13.2765(7)
_cell_length_b                   17.6732(10)
_cell_length_c                   19.2600(14)
_cell_measurement_reflns_used    21432
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      67.9
_cell_measurement_theta_min      2.3
_cell_volume                     4466.0(5)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0r15 (Rigaku,2011)'
_computing_data_collection       'CrystalClear-SM Expert 2.0r15 (Rigaku,2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0r15 (Rigaku,2011)'
_computing_molecular_graphics
;
Dolomanov, O.V.; Bourhis, L.J.; Gildea, R.J.; Howard, J.A.K.; Puschmann, H., 
OLEX2: A complete structure solution, refinement and analysis program
(2009). J. Appl. Cryst., 42, 339-341.
;
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 22.2
_diffrn_measured_fraction_theta_full 0.674
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.4633
_diffrn_reflns_av_unetI/netI     0.2739
_diffrn_reflns_Laue_measured_fraction_full 0.674
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            118093
_diffrn_reflns_point_group_measured_fraction_full 0.674
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         54.244
_diffrn_reflns_theta_min         2.310
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    3.315
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_correction_T_min  0.674
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private Communication'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.890
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1021
_refine_ls_number_reflns         10869
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.888
_refine_ls_R_factor_all          0.2229
_refine_ls_R_factor_gt           0.0811
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0251P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1575
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4182
_reflns_number_total             10869
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b06841_si_002.cif
_cod_data_source_block           4
_cod_database_code               4129490
_shelx_estimated_absorpt_t_min   0.636
_shelx_estimated_absorpt_t_max   0.937
_shelxl_version_number           2014-3
_shelx_res_checksum              21990
_shelx_hkl_checksum              21047