Acid-induced nitrite reduction of nonheme iron(ii)-nitrite: mimicking biological Fe-NiR reactions.
Kulbir, ?; Das, Sandip; Devi, Tarali; Ghosh, Somnath; Chandra Sahoo, Subash; Kumar, Pankaj; Chemical science 14 (2023) 2935–2942; doi:10.1039/d2sc06704h

data_1568527
_publ_section_title
;
 Acid-induced nitrite reduction of nonheme iron(ii)-nitrite: mimicking
 biological Fe-NiR reactions.
;
_journal_issue                   11
_journal_name_full               'Chemical science'
_journal_page_first              2935
_journal_page_last               2942
_journal_paper_doi               10.1039/d2sc06704h
_journal_volume                  14
_journal_year                    2023
_chemical_compound_source        synthesized
_chemical_formula_moiety         'C12 H28 Fe N5 O2, C F3 O3 S'
_chemical_formula_sum            'C13 H28 F3 Fe N5 O5 S'
_chemical_formula_weight         479.31
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-06-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-06-26 deposited with the CCDC.	2023-02-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.654(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.1966(5)
_cell_length_b                   16.5801(5)
_cell_length_c                   16.2444(5)
_cell_measurement_reflns_used    16268
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.2650
_cell_measurement_theta_min      3.2990
_cell_volume                     4287.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.988
_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    -51.00 -26.00   0.50   20.00    --   -9.95 135.00  86.00   50
  2  \w    -60.00 -35.00   0.50   20.00    --   -9.95 135.00 -93.00   50
  3  \w     12.00  37.00   0.50   20.00    --   10.22-135.00-159.00   50
  4  \w     12.00  37.00   0.50   20.00    --   10.22-135.00  20.00   50
  5  \w    -58.00  -9.00   0.50   20.00    --   -9.95 125.00-180.00   98
  6  \w    -19.00  40.00   0.50   20.00    --   10.22 -99.00-180.00  118
  7  \w     -8.00  39.00   0.50   20.00    --   10.22 -99.00  60.00   94
  8  \w    -12.00  70.00   0.50   20.00    --   10.22  77.00   0.00  164
  9  \w    -50.00  22.00   0.50   20.00    --   10.22 -38.00  60.00  144
 10  \w     19.00  44.00   0.50   20.00    --   10.22  38.00-120.00   50
 11  \w    -21.00  24.00   0.50   20.00    --   10.22 -38.00-180.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0095756000
_diffrn_orient_matrix_UB_12      -0.0101809000
_diffrn_orient_matrix_UB_13      -0.0431196000
_diffrn_orient_matrix_UB_21      0.0422713000
_diffrn_orient_matrix_UB_22      0.0076785000
_diffrn_orient_matrix_UB_23      -0.0035727000
_diffrn_orient_matrix_UB_31      0.0103542000
_diffrn_orient_matrix_UB_32      -0.0408479000
_diffrn_orient_matrix_UB_33      0.0100380000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37140
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         3.148
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.859
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56683
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.31d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_description       plate
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.035
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         8656
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.1046
_refine_ls_R_factor_gt           0.0689
_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^)+(0.1321P)^2^+0.0202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2031
_refine_ls_wR_factor_ref         0.2304
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5388
_reflns_number_total             8656
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06704h2.cif
_cod_data_source_block           scs-pakjno2
_cod_depositor_comments
'Adding full bibliography for 1568527--1568528.cif.'
_cod_database_code               1568527
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Co F S O N C H'
_olex2_refinement_description
;
1. Rigid body (RIGU) restrains
 O10A, O10, O9A, O9
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
2. Others
 Fixed Sof: O9(0.5) O3(0.7) O4A(0.5) O4(0.5) O10A(0.5) O10(0.5) O9A(0.5)
 O3A(0.3)
3.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C2(H2A,H2B), C5(H5A,H5B), C1(H1A,H1B),
 C8(H8A,H8B), C18(H18A,H18B), C15(H15A,H15B), C13(H13A,H13B), C17(H17A,H17B),
 C19(H19A,H19B), C7(H7A,H7B), C16(H16A,H16B), C20(H20A,H20B), C14(H14A,H14B)
3.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C22(H22A,H22B,H22C), C9(H9A,H9B,H9C), C12(H12A,H12B,
 H12C), C11(H11A,H11B,H11C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C)
;
_shelx_res_checksum              66154
_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 1.525
_oxdiff_exptl_absorpt_empirical_full_min 0.657