Iron-Amide-Sulfide and Iron-Imide-Sulfide Clusters: Heteroligated Core Environments Relevant to the Nitrogenase FeMo Cofactor
Xu-Dong Chen; Wei Zhang; Jeremiah S. Duncan; Sonny C. Lee; Inorganic Chemistry 51 (2012) 12891–12904; doi:10.1021/ic301868m

data_4331178
_publ_contact_author_address
;                                                                               
 Department of Chemistry
 University of Waterloo
 200 University Avenue West
 Waterloo, Ontario  N2L 3G1
 CANADA  
;
_publ_contact_author_email       sclee@uwaterloo.ca
_publ_contact_author_fax         519-746-0435
_publ_contact_author_name        'Sonny C. Lee'
_publ_contact_author_phone       '519-885-1211 x37501'
_publ_section_title
;
 Iron-Amide-Sulfide and Iron-Imide-Sulfide Clusters: Heteroligated Core
 Environments Relevant to the Nitrogenase FeMo Cofactor
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12891
_journal_page_last               12904
_journal_paper_doi               10.1021/ic301868m
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety
;
(Et4N +)2 [ (Fe 3+)2 (Fe 2+)2 (NtBu 2-)2 (S 2-)2 (Cl -)4 ]
;
_chemical_formula_sum            'C24 H58 Cl4 Fe4 N4 S2'
_chemical_formula_weight         832.06
_chemical_name_common
; 
 (Et4N)2[Fe4(mu3-NtBu)2(mu3-S)2Cl4] 
;
_chemical_name_systematic
; 
 (Et4N)2[Fe4(mu3-NtBu)2(mu3-S)2Cl4] 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 108.7950(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.8185(12)
_cell_length_b                   11.3121(7)
_cell_length_c                   22.1301(14)
_cell_measurement_reflns_used    3715
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      22.83
_cell_measurement_theta_min      2.92
_cell_volume                     4222.8(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'APEX CCD'
_diffrn_measurement_method       '\w 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  0.0707
_diffrn_reflns_av_sigmaI/netI    0.0828
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            34783
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    1.717
_exptl_absorpt_correction_T_max  0.9665
_exptl_absorpt_correction_T_min  0.7362
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'APEX II'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       plate
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         10178
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0421P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1188
_reflns_number_gt                6330
_reflns_number_total             10178
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301868m_si_002_6.cif
_cod_data_source_block           sl16
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4331178