Dinitrosyl Iron Complexes (DNICs) Bearing O-Bound Nitrito Ligand: Reversible Transformation between the Six-Coordinate {Fe(NO)2}9[(1-MeIm)2(η2-ONO)Fe(NO)2] (g= 2.013) and Four-Coordinate {Fe(NO)2}9[(1-MeIm)(ONO)Fe(NO)2] (g= 2.03)
Fu-Te Tsai; Ting-Shen Kuo; Wen-Feng Liaw; Journal of the American Chemical Society 131 (2009) 3426–3427; doi:10.1021/ja808743g

data_4104011
_publ_section_title
;
 Dinitrosyl Iron Complexes (DNICs) Bearing O-Bound Nitrito Ligand:
 Reversible Transformation between the Six-Coordinate
 {Fe(NO)2}9[(1-MeIm)2(\h2-ONO)Fe(NO)2] (g= 2.013) and Four-Coordinate
 {Fe(NO)2}9[(1-MeIm)(ONO)Fe(NO)2] (g= 2.03)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3426
_journal_page_last               3427
_journal_paper_doi               10.1021/ja808743g
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C20 H36 Fe N7 O10'
_chemical_formula_sum            'C20 H36 Fe N7 O10'
_chemical_formula_weight         590.41
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.9510(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2996(3)
_cell_length_b                   13.4256(3)
_cell_length_c                   15.8455(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     2802.10(10)
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20278
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.600
_exptl_absorpt_correction_T_max  0.9260
_exptl_absorpt_correction_T_min  0.8405
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.027
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         4860
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0598P)^2^+4.5143P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1245
_refine_ls_wR_factor_ref         0.1343
_reflns_number_gt                3990
_reflns_number_total             4860
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja808743g_si_003.cif
_cod_data_source_block           a8606
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4104011