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_4133101
_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 N6 O2'
_chemical_formula_weight         853.69
_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                77.913(6)
_cell_angle_beta                 75.424(6)
_cell_angle_gamma                84.359(6)
_cell_formula_units_Z            2
_cell_length_a                   10.4011(12)
_cell_length_b                   14.4990(17)
_cell_length_c                   15.8935(18)
_cell_measurement_reflns_used    9761
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      66.60
_cell_measurement_theta_min      2.93
_cell_volume                     2265.6(5)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0582
_diffrn_reflns_av_unetI/netI     0.0581
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27378
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        66.696
_diffrn_reflns_theta_max         66.696
_diffrn_reflns_theta_min         2.927
_diffrn_source                   'Incoatec I\mS'
_exptl_absorpt_coefficient_mu    3.029
_exptl_absorpt_correction_T_max  0.5842
_exptl_absorpt_correction_T_min  0.4948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_description       cut-b;lock
_exptl_crystal_F_000             906
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         7963
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0595P)^2^+0.4432P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1110
_refine_ls_wR_factor_ref         0.1149
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6915
_reflns_number_total             7963
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b08520_si_002.cif
_cod_data_source_block           cu_gilb271_0m_a
_cod_database_code               4133101
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.643
_shelx_estimated_absorpt_t_max   0.694
_shelx_res_checksum              37918
_shelx_hkl_checksum              20815