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_4133105
_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_moiety         'C27 H38 Fe N5 O2, C24 H20 B'
_chemical_formula_sum            'C51 H58 B Fe N5 O2'
_chemical_formula_weight         839.68
_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   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2018-03-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                91.1090(10)
_cell_angle_beta                 97.2010(10)
_cell_angle_gamma                101.1230(10)
_cell_formula_units_Z            2
_cell_length_a                   9.14310(10)
_cell_length_b                   12.8888(2)
_cell_length_c                   19.5058(3)
_cell_measurement_reflns_used    23648
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.2590
_cell_measurement_theta_min      3.3460
_cell_volume                     2235.43(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.4a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.4a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.4a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Pilatus P200K HPC detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -59.00  90.00   0.50    5.00    --    0.00   9.00 108.00  298
  2  \w    -90.00  34.00   0.50    5.00    --    0.00 -82.00 144.00  248
  3  \w    -60.00  17.00   0.50    5.00    --    0.00 -46.00 -36.00  154
  4  \w    -59.00  40.50   0.50    5.00    --    0.00   9.00-144.00  199
;
_diffrn_measurement_device       'ROD XtaLABPRO'
_diffrn_measurement_device_type  'ROD XtaLABPRO with fine-focus sealed tube'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0616038000
_diffrn_orient_matrix_UB_12      -0.0103555000
_diffrn_orient_matrix_UB_13      0.0193124000
_diffrn_orient_matrix_UB_21      0.0239617000
_diffrn_orient_matrix_UB_22      -0.0461527000
_diffrn_orient_matrix_UB_23      0.0124214000
_diffrn_orient_matrix_UB_31      0.0446311000
_diffrn_orient_matrix_UB_32      0.0302428000
_diffrn_orient_matrix_UB_33      0.0286156000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            34528
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.102
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              '3.0 kW Mo X-ray Source'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.383
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83223
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.4a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_description       chunk
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     773
_refine_ls_number_reflns         9128
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0284
_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^)+(0.0381P)^2^+0.9957P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0759
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8300
_reflns_number_total             9128
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b08520_si_002.cif
_cod_data_source_block           Gilb382
_cod_database_code               4133105
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H Fe N O B'
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.167
_oxdiff_exptl_absorpt_empirical_full_min 0.861