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_4331173
_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_compound_source        'Chemical synthesis, S.C. Lee lab'
_chemical_formula_moiety
;
(C8H20N +)2 (Fe 3+)2 (C4H9N 2-) (S 2-) (Cl -)4
;
_chemical_formula_structural     (NC8H20)2(Fe2(NC4H9)SCl4)
_chemical_formula_sum            'C20 H49 Cl4 Fe2 N3 S'
_chemical_formula_weight         617.18
_chemical_name_common            (NEt4)2[Fe2(mu-NtBu)(mu-S)Cl2]
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 95.827(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3855(3)
_cell_length_b                   15.6669(8)
_cell_length_c                   20.7398(11)
_cell_measurement_reflns_used    18845
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      1.63
_cell_volume                     3033.9(2)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'NONIUS COLLECT'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'CIFTAB, Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Nonius KappaCCD'
_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  0.060
_diffrn_reflns_av_sigmaI/netI    0.0685
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18845
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.63
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.390
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange-black
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.865
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.031
_refine_ls_goodness_of_fit_obs   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         5954
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_restrained_S_obs      1.082
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_obs          0.0534
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0871P)^2^+1.2100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1618
_refine_ls_wR_factor_obs         0.1331
_reflns_number_observed          3742
_reflns_number_total             5955
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            ic301868m_si_002_1.cif
_cod_data_source_block           global
_cod_database_code               4331173