The Electronic Structures of an Isostructural Series of Octahedral Nitrosyliron Complexes {Fe-NO}6,7,8 Elucidated by Mössbauer Spectroscopy
Christina Hauser; Thorsten Glaser; Eckhard Bill; Thomas Weyhermüller; Karl Wieghardt; Journal of the American Chemical Society 122 (2000) 4352–4365; doi:10.1021/ja994161i

data_4115997
_publ_section_title
;
 The Electronic Structures of an Isostructural Series of Octahedral
 Nitrosyliron Complexes {Fe-NO}6,7,8 Elucidated by M\"ossbauer
 Spectroscopy
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4352
_journal_page_last               4365
_journal_paper_doi               10.1021/ja994161i
_journal_volume                  122
_journal_year                    2000
_chemical_formula_structural     '[C6 H15 Fe N6 O5]+, (Cl O4)-'
_chemical_formula_sum            'C6 H15 Cl Fe N6 O9'
_chemical_formula_weight         406.54
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 109.43(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.450(2)
_cell_length_b                   8.1261(8)
_cell_length_c                   13.478(2)
_cell_measurement_reflns_used    7852
_cell_measurement_temperature    100(2)
_cell_volume                     1389.2(4)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       '\w, 1 deg./frame, 258 frames a 30 sec.'
_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  0.0537
_diffrn_reflns_av_sigmaI/netI    0.0743
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8915
_diffrn_reflns_theta_max         30.54
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    1.341
_exptl_absorpt_correction_type   'Not measured'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.944
_exptl_crystal_description       'opaque column'
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.804
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.991
_refine_ls_goodness_of_fit_obs   1.132
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         5807
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.045
_refine_ls_restrained_S_obs      1.153
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_obs          0.0462
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1207
_refine_ls_wR_factor_obs         0.1080
_reflns_number_observed          3975
_reflns_number_total             5814
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja994161i_2.cif
_cod_data_source_block           '[LFe(NO)(ONO)(NO2)]ClO4'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1389.2(3)
_cod_database_code               4115997