New Members of a Class of Dinitrosyliron Complexes (DNICs): Interconversion and Spectroscopic Discrimination of the Anionic {Fe(NO)2}9[(NO)2Fe(C3H3N2)2]- and [(NO)2Fe(C3H3N2)(SR)]- (C3H3N2= Deprotonated Imidazole; R =tBu, Et, Ph)
Hsiao-Wen Huang; Chih-Chin Tsou; Ting-Shen Kuo; Wen-Feng Liaw; Inorganic Chemistry 47 (2008) 2196–2204; doi:10.1021/ic702000y

data_4304504
_publ_section_title
;
New Members of a Class of Dinitrosyliron Complexes (DNICs): Interconversion
and Spectroscopic Discrimination of the Anionic
{Fe(NO)2}9[(NO)2Fe(C3H3N2)2]- and [(NO)2Fe(C3H3N2)(SR)]- (C3H3N2=
Deprotonated Imidazole; R =tBu, Et, Ph)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2196
_journal_page_last               2204
_journal_paper_doi               10.1021/ic702000y
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C23 H44 Fe N4 Na O9 S'
_chemical_formula_sum            'C23 H44 Fe N4 Na O9 S'
_chemical_formula_weight         631.52
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8695(3)
_cell_length_b                   18.2743(6)
_cell_length_c                   20.1496(7)
_cell_measurement_reflns_used    22081
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.037
_cell_volume                     3265.93(19)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 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_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0617
_diffrn_reflns_av_sigmaI/netI    0.0680
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15795
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    0.588
_exptl_absorpt_correction_T_max  0.9328
_exptl_absorpt_correction_T_min  0.8524
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1340
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.931
_refine_diff_density_min         -0.760
_refine_diff_density_rms         0.216
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(4)
_refine_ls_extinction_coef       0.040(4)
_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   1.077
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         5881
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.1286
_refine_ls_R_factor_gt           0.0905
_refine_ls_shift/su_max          0.184
_refine_ls_shift/su_mean         0.033
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1719P)^2^+0.7943P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2310
_refine_ls_wR_factor_ref         0.2699
_reflns_number_gt                4050
_reflns_number_total             5881
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702000y-file003.cif
_cod_data_source_block           7044
_cod_database_code               4304504