Rapid nitrite reduction enabled by secondary sphere hydrogen bonds within non-heme iron complexes.
LaDuca, Andrew R.; Gonder, Jared E.; Sarkar, Writhabrata; Gilbertson, John D.; Szymczak, Nathaniel K.; Chemical science 16 (2025) 18364–18371; doi:10.1039/d5sc04153h

data_1575564
_publ_section_title
;
 Rapid nitrite reduction enabled by secondary sphere hydrogen bonds within
 non-heme iron complexes.
;
_journal_issue                   39
_journal_name_full               'Chemical science'
_journal_page_first              18364
_journal_page_last               18371
_journal_paper_doi               10.1039/d5sc04153h
_journal_volume                  16
_journal_year                    2025
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C36 H33 Fe N7 O, C F3 O3 S'
_chemical_formula_sum            'C37 H33 F3 Fe N7 O4 S'
_chemical_formula_weight         784.61
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2024-10-07
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2025-05-05 deposited with the CCDC.	2025-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                102.965(6)
_cell_angle_beta                 93.193(5)
_cell_angle_gamma                103.386(5)
_cell_formula_units_Z            2
_cell_length_a                   10.7613(7)
_cell_length_b                   12.7245(8)
_cell_length_c                   13.5391(10)
_cell_measurement_reflns_used    5575
_cell_measurement_temperature    85
_cell_measurement_theta_max      68.9470
_cell_measurement_theta_min      3.3290
_cell_volume                     1746.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      85
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.949
_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   -110.00  70.00   1.00    5.00    --  -20.00   0.00-180.00  180
  2  \w    -45.00   0.00   1.00    5.00    --  -20.00  72.00   0.00   45
  3  \w    -45.00   0.00   1.00    5.00    --  -20.00  72.00   0.00   45
  4  \w    -25.00  43.00   1.00    5.00    --  -20.00  36.00 120.00   68
  5  \w    -45.00   0.00   1.00    5.00    --  -20.00  72.00-180.00   45
  6  \w   -173.00-128.00   1.00   25.00    --  -92.00 -36.00 120.00   45
  7  \w   -133.00 -88.00   1.00   25.00    --  -92.00 -36.00 -60.00   45
  8  \w   -104.00 -59.00   1.00   25.00    --  -92.00  36.00  60.00   45
  9  \w   -122.00 -77.00   1.00   25.00    --  -92.00 -72.00  60.00   45
 10  \w   -174.00 -78.00   1.00   25.00    --  -92.00 -72.00-120.00   96
 11  \w    -93.00 -35.00   1.00   25.00    --  -92.00  36.00-120.00   58
 12  \w   -176.00 -77.00   1.00   25.00    --  -92.00 -72.00 -60.00   99
 13  \w   -147.00 -75.00   1.00   25.00    --  -92.00 -72.00-180.00   72
 14  \w   -176.00 -77.00   1.00   25.00    --  -92.00 -72.00 120.00   99
 15  \w   -177.00-116.00   1.00   25.00    --  -92.00 -36.00  60.00   61
 16  \w    -87.00  -9.00   1.00   25.00    --  -92.00  36.00 -60.00   78
 17  \w   -102.00 -14.00   1.00   25.00    --  -92.00  36.00   0.00   88
 18  \w   -102.00 -21.00   1.00   25.00    --  -92.00  72.00 120.00   81
 19  \w   -175.00-104.00   1.00   25.00    --  -92.00 -36.00   0.00   71
 20  \w   -104.00 -52.00   1.00   25.00    --  -92.00  72.00  60.00   52
 21  \w   -109.00 -14.00   1.00   25.00    --  -92.00  72.00-120.00   95
 22  \w   -105.00 -24.00   1.00   25.00    --  -92.00  36.00-120.00   81
 23  \w   -105.00  -2.00   1.00   25.00    --  -92.00  36.00-180.00  103
 24  \w   -106.00  -2.00   1.00   25.00    --  -92.00  72.00 -60.00  104
 25  \w   -106.00  -2.00   1.00   25.00    --  -92.00  72.00 -60.00  104
 26  \w   -107.00 -29.00   1.00   25.00    --  -92.00  72.00   0.00   78
 27  \w   -117.00 -72.00   1.00   25.00    --  -92.00  72.00 180.00   45
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0382013000
_diffrn_orient_matrix_UB_12      -0.0567328000
_diffrn_orient_matrix_UB_13      -0.1142430000
_diffrn_orient_matrix_UB_21      0.1426271000
_diffrn_orient_matrix_UB_22      0.0088495000
_diffrn_orient_matrix_UB_23      -0.0148458000
_diffrn_orient_matrix_UB_31      -0.0116517000
_diffrn_orient_matrix_UB_32      -0.1147775000
_diffrn_orient_matrix_UB_33      0.0232282000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23992
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.479
_diffrn_reflns_theta_min         3.371
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    4.609
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85346
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_description       irregular
_exptl_crystal_F_000             810
_exptl_crystal_size_max          0.113
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.054
_refine_diff_density_max         1.588
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         6216
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0972
_refine_ls_R_factor_gt           0.0863
_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^)+(0.1670P)^2^+1.9292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2338
_refine_ls_wR_factor_ref         0.2468
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5237
_reflns_number_total             6216
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc04153h2.cif
_cod_data_source_block           2136no2
_cod_depositor_comments
'Adding full bibliography for 1575564--1575565.cif.'
_cod_database_code               1575564
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C37H34F3FeN7O4S
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C25(H25A,H25B), C13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 N5(H5), N7(H7), N6(H6), C3(H3), C27(H27), C8(H8), C32(H32), C5(H5A), C28(H28),
  C4(H4), C12(H12), C11(H11), C24(H24), C36(H36), C29(H29), C33(H33), C9(H9),
 C17(H17), C15(H15), C34(H34), C23(H23), C10(H10), C35(H35), C16(H16), C20(H20),
  C22(H22), C21(H21)
;
_shelx_res_checksum              92384
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.786
_oxdiff_exptl_absorpt_empirical_full_min 0.648