Iron Carbonyl Sulfides, Formaldehyde, and Amines Condense To Give the Proposed Azadithiolate Cofactor of the Fe-Only Hydrogenases
Hongxiang Li; Thomas B. Rauchfuss; Journal of the American Chemical Society 124 (2002) 726–727; doi:10.1021/ja016964n

data_4114599
_publ_section_title
;
 Iron Carbonyl Sulfides, Formaldehyde, and Amines Condense To Give the
 Proposed Azadithiolate Cofactor of the Fe-Only Hydrogenases
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              726
_journal_page_last               727
_journal_paper_doi               10.1021/ja016964n
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C24 H45 Fe2 N5 O4 S2'
_chemical_formula_weight         643.47
_chemical_name_systematic
; 
 ? 
;
_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                   11.9966(6)
_cell_length_b                   14.2977(6)
_cell_length_c                   18.1645(8)
_cell_measurement_temperature    293(2)
_cell_volume                     3115.6(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0447
_diffrn_reflns_av_sigmaI/netI    0.0454
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29223
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    1.101
_exptl_absorpt_correction_T_max  0.7022
_exptl_absorpt_correction_T_min  0.5878
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_description       tabular
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.48
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.557(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         7554
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.677
_refine_ls_shift/su_mean         0.038
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0224P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0641
_reflns_number_gt                6096
_reflns_number_total             7554
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja016964n_s1_2.cif
_cod_data_source_block           p42ne
_cod_database_code               4114599