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_4104012
_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         'C22 H21 Fe N4 O2 P'
_chemical_formula_sum            'C22 H21 Fe N4 O2 P'
_chemical_formula_weight         460.25
_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                 92.5210(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5191(2)
_cell_length_b                   19.0746(4)
_cell_length_c                   13.2434(3)
_cell_measurement_reflns_used    14287
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.037
_cell_volume                     2402.32(9)
_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  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0440
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14989
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.24
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    0.718
_exptl_absorpt_correction_T_max  0.9129
_exptl_absorpt_correction_T_min  0.7774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.151
_refine_ls_extinction_coef       0.030(2)
_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   1.130
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4306
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0508
_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^)+(0.0846P)^2^+0.4354P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1418
_refine_ls_wR_factor_ref         0.1474
_reflns_number_gt                3496
_reflns_number_total             4306
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja808743g_si_004.cif
_cod_data_source_block           8315
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4104012