Anionic Roussin's Red Esters (RREs) syn-/anti-[Fe(μ-SEt)(NO)2]2-: the Critical Role of Thiolate Ligands in Regulating the Transformation of RREs into Dinitrosyl Iron Complexes and the Anionic RREs
Tsai-Te Lu; Chih-Chin Tsou; Hsiao-Wen Huang; I-Jui Hsu; Jin-Ming Chen; Ting-Shen Kuo; Yu Wang; Wen-Feng Liaw; Inorganic Chemistry 47 (2008) 6040–6050; doi:10.1021/ic800360m

data_4305374
_publ_section_title
;
Anionic Roussin's Red Esters (RREs) syn-/anti-[Fe(\m-SEt)(NO)2]2-: the
Critical Role of Thiolate Ligands in Regulating the Transformation of RREs
into Dinitrosyl Iron Complexes and the Anionic RREs
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6040
_journal_page_last               6050
_journal_paper_doi               10.1021/ic800360m
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C24 H50 Fe2 N4 Na O12 S2'
_chemical_formula_sum            'C24 H50 Fe2 N4 Na O12 S2'
_chemical_formula_weight         785.49
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 103.016(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.7703(6)
_cell_length_b                   12.5442(4)
_cell_length_c                   14.3511(4)
_cell_measurement_reflns_used    10097
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.037
_cell_volume                     3643.06(19)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0821
_diffrn_reflns_av_sigmaI/netI    0.0572
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11435
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    0.981
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.7275
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1652
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.598
_refine_diff_density_min         -1.053
_refine_diff_density_rms         0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         3330
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0703P)^2^+1.3953P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1109
_refine_ls_wR_factor_ref         0.1304
_reflns_number_gt                2729
_reflns_number_total             3330
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800360m-file003_4.cif
_cod_data_source_block           7084
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4305374