Anionic Mixed Thiolate-Sulfide-Bridged Roussin's Red Esters [(NO)2Fe(μ-SR)(μ-S)Fe(NO)2]- (R = Et, Me, Ph): A Key Intermediate for Transformation of Dinitrosyl Iron Complexes (DNICs) to [2Fe-2S] Clusters
Tsai-Te Lu; Hsiao-Wen Huang; Wen-Feng Liaw; Inorganic Chemistry 48 (2009) 9027–9035; doi:10.1021/ic9012679

data_4303205
_publ_section_title
;
Anionic Mixed Thiolate-Sulfide-Bridged Roussin's Red Esters
[(NO)2Fe(\m-SR)(\m-S)Fe(NO)2]- (R = Et, Me, Ph): A Key Intermediate for
Transformation of Dinitrosyl Iron Complexes (DNICs) to [2Fe-2S] Clusters
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9027
_journal_page_last               9035
_journal_paper_doi               10.1021/ic9012679
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C37 H33 Fe2 N5 O4 P2 S2'
_chemical_formula_sum            'C37 H33 Fe2 N5 O4 P2 S2'
_chemical_formula_weight         849.44
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 103.465(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.9174(6)
_cell_length_b                   12.6596(6)
_cell_length_c                   16.2783(8)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     2187.98(19)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0751
_diffrn_reflns_av_sigmaI/netI    0.1115
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6841
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.872
_exptl_absorpt_correction_T_max  0.9828
_exptl_absorpt_correction_T_min  0.7109
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.344
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.92(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.935
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         6841
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.1106
_refine_ls_R_factor_gt           0.0592
_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^)+(0.0683P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1395
_reflns_number_gt                4103
_reflns_number_total             6841
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9012679_si_003.cif
_cod_data_source_block           a8875
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4303205