Complete Series of {FeNO}(8), {FeNO}(7), and {FeNO}(6) Complexes Stabilized by a Tetracarbene Macrocycle.
Kupper, Claudia; Rees, Julian A.; Dechert, Sebastian; DeBeer, Serena; Meyer, Franc; Journal of the American Chemical Society 138 (2016) 7888–7898; doi:10.1021/jacs.6b00584

data_4130130
_publ_section_title
;
 Complete Series of {FeNO}(8), {FeNO}(7), and {FeNO}(6) Complexes
 Stabilized by a Tetracarbene Macrocycle.
;
_journal_issue                   25
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7888
_journal_page_last               7898
_journal_paper_doi               10.1021/jacs.6b00584
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C18 H20 Fe N9 O +, C F3 O3 S -'
_chemical_formula_sum            'C19 H20 F3 Fe N9 O4 S'
_chemical_formula_weight         583.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 113.068(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6972(6)
_cell_length_b                   12.3023(4)
_cell_length_c                   15.4558(8)
_cell_measurement_reflns_used    29419
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      26.799
_cell_measurement_theta_min      1.743
_cell_volume                     2221.23(18)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2012)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29419
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.799
_diffrn_reflns_theta_min         1.743
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.849
_exptl_absorpt_correction_T_max  0.8201
_exptl_absorpt_correction_T_min  0.6665
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2002)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_description       block
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.849
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4713
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0559P)^2^+1.2910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1025
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4083
_reflns_number_total             4713
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b00584_si_002.cif
_cod_data_source_block           2-clk-feno8
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4130130
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.686
_shelx_estimated_absorpt_t_max   0.842
_shelx_res_checksum              13385
_shelx_hkl_checksum              97340