Reduction of nitrite to nitric oxide and generation of reactive chalcogen species by mononuclear Fe(II) and Zn(II) complexes of thiolate and selenolate.
Atta, Sayan; Mandal, Amit; Saha, Rahul; Majumdar, Amit; Dalton transactions (Cambridge, England : 2003) 53 (2024) 949–965; doi:10.1039/d3dt03768a

data_7714676
_publ_section_title
;
 Reduction of nitrite to nitric oxide and generation of reactive chalcogen
 species by mononuclear Fe(II) and Zn(II) complexes of thiolate and
 selenolate.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              949
_journal_page_last               965
_journal_paper_doi               10.1039/d3dt03768a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C29 H29 Fe N3 O2 S'
_chemical_formula_sum            'C29 H29 Fe N3 O2 S'
_chemical_formula_weight         539.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-12-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-12-17 deposited with the CCDC.	2023-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.715(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3033(5)
_cell_length_b                   14.9444(6)
_cell_length_c                   15.7897(7)
_cell_measurement_reflns_used    12113
_cell_measurement_temperature    160(20)
_cell_measurement_theta_max      25.6900
_cell_measurement_theta_min      1.8990
_cell_volume                     2591.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(20)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.991
_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   -100.91  13.09   1.00   10.00    --  -15.95 -59.25-135.92  114
  2  \w    -59.55  22.45   1.00   10.00    --  -15.95  83.74  21.05   82
  3  \w   -100.91  13.09   1.00   10.00    --  -15.95 -59.25 122.08  114
  4  \w    -59.55  22.45   1.00   10.00    --  -15.95  83.74 -83.95   82
;
_diffrn_measurement_device_type  'Bruker D8VENTURE with PHOTON II Detector'
_diffrn_measurement_method       'phi, omega and kappa scan'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0410512000
_diffrn_orient_matrix_UB_12      -0.0341430000
_diffrn_orient_matrix_UB_13      0.0195570000
_diffrn_orient_matrix_UB_21      0.0383754000
_diffrn_orient_matrix_UB_22      0.0105711000
_diffrn_orient_matrix_UB_23      -0.0281897000
_diffrn_orient_matrix_UB_31      0.0319073000
_diffrn_orient_matrix_UB_32      0.0312254000
_diffrn_orient_matrix_UB_33      0.0309845000
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24063
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         1.902
_diffrn_source_type              Micro-focus
_exptl_absorpt_coefficient_mu    0.694
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75874
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         4868
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0296
_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^)+(0.0340P)^2^+1.5133P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0764
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4476
_reflns_number_total             4868
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03768a2.cif
_cod_data_source_block           sol1
_cod_depositor_comments
'Adding full bibliography for 7714674--7714686.cif.'
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7714676
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O S Fe'
_shelx_estimated_absorpt_t_max   0.885
_shelx_estimated_absorpt_t_min   0.862
_reflns_odcompleteness_completeness 99.10
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.63
_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), C10(H10A,H10B), C16(H16A,H16B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C8(H8), C12(H12), C13(H13), C14(H14), C15(H15), C18(H18),
 C19(H19), C20(H20), C21(H21), C25(H25), C26(H26), C27(H27)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C24(H24A,H24B,H24C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              38058
_shelx_hkl_checksum              42567
_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 1.712
_oxdiff_exptl_absorpt_empirical_full_min 0.810