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_4331176
_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         '(Fe 3+)2 (C4H10N -)2 (Se 2-) (C6H18NSi2 1-)2'
_chemical_formula_sum            'C20 H56 Fe2 N4 Se Si4'
_chemical_formula_weight         655.71
_chemical_name_common            Fe2(mu-NHtBu)(mu-Se)[N(TMS)2]2
_chemical_name_systematic        Fe2(mu-NHtBu)(mu-Se)[N(TMS)2]2
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 101.6310(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.4943(6)
_cell_length_b                   9.0935(3)
_cell_length_c                   23.5967(8)
_cell_measurement_reflns_used    9963
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.78
_cell_measurement_theta_min      2.97
_cell_volume                     3466.6(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0284
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            38823
_diffrn_reflns_theta_full        30.05
_diffrn_reflns_theta_max         30.05
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    2.039
_exptl_absorpt_correction_T_max  0.8221
_exptl_absorpt_correction_T_min  0.5112
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   APEXII
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_description       block
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.061
_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     288
_refine_ls_number_reflns         10145
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0303P)^2^+1.5250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0765
_reflns_number_gt                8091
_reflns_number_total             10145
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301868m_si_002_4.cif
_cod_data_source_block           sl35-wz
_cod_database_code               4331176