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_4303204
_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         'C38 H35 Fe2 N5 O4 P2 S2'
_chemical_formula_sum            'C38 H35 Fe2 N5 O4 P2 S2'
_chemical_formula_weight         863.47
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.4860(10)
_cell_angle_beta                 103.0430(10)
_cell_angle_gamma                92.5760(10)
_cell_formula_units_Z            2
_cell_length_a                   9.3297(2)
_cell_length_b                   13.5754(3)
_cell_length_c                   16.2608(4)
_cell_measurement_reflns_used    37954
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.037
_cell_volume                     1940.67(8)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'HKL Denzo and Scalepack'
_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_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.0786
_diffrn_reflns_av_sigmaI/netI    0.0615
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28887
_diffrn_reflns_theta_full        25.37
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    0.984
_exptl_absorpt_correction_T_max  0.7126
_exptl_absorpt_correction_T_min  0.6259
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.735
_refine_diff_density_min         -1.081
_refine_diff_density_rms         0.251
_refine_ls_extinction_coef       0.033(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         7069
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.0952
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1081P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1516
_refine_ls_wR_factor_ref         0.1882
_reflns_number_gt                5212
_reflns_number_total             7069
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9012679_si_002.cif
_cod_data_source_block           8252
_cod_database_code               4303204