Hemilabile Proton Relays and Redox Activity Lead to {FeNO} <sup>x</sup> and Significant Rate Enhancements in NO<sub>2</sub><sup>-</sup> Reduction.
Cheung, Pui Man; Burns, Kyle T.; Kwon, Yubin M.; Deshaye, Megan Y.; Aguayo, Kristopher J.; Oswald, Victoria F.; Seda, Takele; Zakharov, Lev N.; Kowalczyk, Tim; Gilbertson, John D.; Journal of the American Chemical Society 140 (2018) 17040–17050; doi:10.1021/jacs.8b08520

data_4133102
_publ_section_title
;
 Hemilabile Proton Relays and Redox Activity Lead to {FeNO} <sup>x</sup>
 and Significant Rate Enhancements in NO<sub>2</sub><sup>-</sup>
 Reduction.
;
_journal_issue                   49
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17040
_journal_page_last               17050
_journal_paper_doi               10.1021/jacs.8b08520
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C51 H58 B Fe N5 O'
_chemical_formula_weight         823.68
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                81.601(2)
_cell_angle_beta                 85.289(2)
_cell_angle_gamma                71.560(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3063(4)
_cell_length_b                   14.0433(5)
_cell_length_c                   14.6725(5)
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      66.61
_cell_measurement_theta_min      3.05
_cell_volume                     2184.75(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Apex II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26251
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        66.613
_diffrn_reflns_theta_max         66.613
_diffrn_reflns_theta_min         3.047
_diffrn_source                   'Incoatec I\mS'
_exptl_absorpt_coefficient_mu    3.097
_exptl_absorpt_correction_T_max  0.5842
_exptl_absorpt_correction_T_min  0.5079
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            dark-blue
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_description       cut-block
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         7692
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0504P)^2^+0.9061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.0976
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7221
_reflns_number_total             7692
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b08520_si_002.cif
_cod_data_source_block           cu_gilb274_0m_a
_cod_database_code               4133102
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.621
_shelx_estimated_absorpt_t_max   0.727
_shelx_res_checksum              13311
_shelx_hkl_checksum              52362