A Sulfido-Bridged Diiron(II) Compound and Its Reactions with Nitrogenase-Relevant Substrates
Javier Vela; Sebastian Stoian; Christine J. Flaschenriem; Eckard Münck; Patrick L. Holland; Journal of the American Chemical Society 126 (2004) 4522–4523; doi:10.1021/ja049417l

data_4112427
_publ_section_title
;
 A Sulfido-Bridged Diiron(II) Compound and Its Reactions with
 Nitrogenase-Relevant Substrates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4522
_journal_page_last               4523
_journal_paper_doi               10.1021/ja049417l
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C60 H94 Fe2 N8 S'
_chemical_formula_weight         1071.19
_chemical_name_common            1(H2NNHMe)2
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.7025(13)
_cell_length_b                   16.3018(14)
_cell_length_c                   25.560(2)
_cell_measurement_reflns_used    9044
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      24.7
_cell_measurement_theta_min      2.5
_cell_volume                     6126.1(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0712
_diffrn_reflns_av_sigmaI/netI    0.0477
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            43715
_diffrn_reflns_theta_full        21.50
_diffrn_reflns_theta_max         21.50
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.550
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_description       Block
_exptl_crystal_F_000             2312
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.55(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         7047
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0289P)^2^+8.4733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.0994
_reflns_number_gt                6073
_reflns_number_total             7047
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja049417lsi20040202_112433_3.cif
_cod_data_source_block           1.(H2NNHMe)2
_cod_original_cell_volume        6126.2(9)
_cod_database_code               4112427