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_1575565
_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_formula_moiety         'C21 H24 Fe N4 O, C2 F6 N O4 S2'
_chemical_formula_sum            'C23 H24 F6 Fe N5 O5 S2'
_chemical_formula_weight         684.44
_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_date             2025-03-01
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-05-05 deposited with the CCDC.	2025-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.1257(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.61513(15)
_cell_length_b                   18.7796(2)
_cell_length_c                   13.19575(19)
_cell_measurement_reflns_used    20802
_cell_measurement_temperature    85
_cell_measurement_theta_max      69.1430
_cell_measurement_theta_min      4.0690
_cell_volume                     2684.91(7)
_computing_cell_refinement       'CrysAlisPro 1.171.43.130a (Rigaku OD, 2024)'
_computing_data_collection
'DTREK_VERSION=d*TREK version 9.9.9.4 W9RSSI -- Aug 22 2012'
_computing_data_reduction        'CrysAlisPro 1.171.43.130a (Rigaku OD, 2024)'
_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      85.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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    1.00    --  -20.00   0.00-180.00  180
  2  \w    -45.00   0.00   1.00    1.00    --  -20.00  72.00   0.00   45
  3  \w    -45.00   0.00   1.00    1.00    --  -20.00  72.00   0.00   45
  4  \w    -25.00  43.00   1.00    1.00    --  -20.00  36.00 120.00   68
  5  \w    -45.00   0.00   1.00    1.00    --  -20.00  72.00-180.00   45
  6  \w   -173.00-128.00   1.00    2.00    --  -92.00 -36.00 120.00   45
  7  \w   -133.00 -88.00   1.00    2.00    --  -92.00 -36.00 -60.00   45
  8  \w   -104.00 -59.00   1.00    2.00    --  -92.00  36.00  60.00   45
  9  \w   -122.00 -77.00   1.00    2.00    --  -92.00 -72.00  60.00   45
 10  \w   -174.00 -78.00   1.00    2.00    --  -92.00 -72.00-120.00   96
 11  \w    -93.00 -35.00   1.00    2.00    --  -92.00  36.00-120.00   58
 12  \w   -176.00 -77.00   1.00    2.00    --  -92.00 -72.00 -60.00   99
 13  \w   -147.00 -75.00   1.00    2.00    --  -92.00 -72.00-180.00   72
 14  \w   -176.00 -77.00   1.00    2.00    --  -92.00 -72.00 120.00   99
 15  \w   -177.00-116.00   1.00    2.00    --  -92.00 -36.00  60.00   61
 16  \w    -87.00  -9.00   1.00    2.00    --  -92.00  36.00 -60.00   78
 17  \w   -102.00 -14.00   1.00    2.00    --  -92.00  36.00   0.00   88
 18  \w   -102.00 -21.00   1.00    2.00    --  -92.00  72.00 120.00   81
 19  \w   -175.00-104.00   1.00    2.00    --  -92.00 -36.00   0.00   71
 20  \w   -104.00 -52.00   1.00    2.00    --  -92.00  72.00  60.00   52
 21  \w   -109.00 -14.00   1.00    2.00    --  -92.00  72.00-120.00   95
 22  \w   -105.00 -24.00   1.00    2.00    --  -92.00  36.00-120.00   81
 23  \w   -105.00  -2.00   1.00    2.00    --  -92.00  36.00-180.00  103
 24  \w   -106.00  -2.00   1.00    2.00    --  -92.00  72.00 -60.00  104
 25  \w   -106.00  -2.00   1.00    2.00    --  -92.00  72.00 -60.00  104
 26  \w   -107.00 -29.00   1.00    2.00    --  -92.00  72.00   0.00   78
 27  \w   -117.00 -72.00   1.00    2.00    --  -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_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0696
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            39953
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.353
_diffrn_reflns_theta_min         4.080
_exptl_absorpt_coefficient_mu    6.763
_exptl_absorpt_correction_T_max  0.31379
_exptl_absorpt_correction_T_min  0.23533
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.130a (Rigaku Oxford Diffraction, 2024)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_description       needle
_exptl_crystal_F_000             1396
_exptl_crystal_size_max          0.151
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.095
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         4997
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0505P)^2^+1.4367P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0957
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4722
_reflns_number_total             4997
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc04153h2.cif
_cod_data_source_block           arl4139
_cod_depositor_comments
'Adding full bibliography for 1575564--1575565.cif.'
_cod_database_code               1575565
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C14(H14A,H14B), C23(H23A,H23B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C16(H16), C17(H17),
 C18(H18)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C13(H13A,H13B,H13C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              5797
_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
;