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_7714678
_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         'C42 H40 N6 O4 Zn2, 2(B F4)'
_chemical_formula_sum            'C42 H40 B2 F8 N6 O4 Zn2'
_chemical_formula_weight         997.16
_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
_audit_creation_date             2022-12-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-12-16 deposited with the CCDC.	2023-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                105.549(12)
_cell_angle_beta                 90.387(11)
_cell_angle_gamma                91.566(12)
_cell_formula_units_Z            1
_cell_length_a                   9.8506(14)
_cell_length_b                   10.1305(15)
_cell_length_c                   10.4984(13)
_cell_measurement_reflns_used    1431
_cell_measurement_temperature    146.7(6)
_cell_measurement_theta_max      22.1350
_cell_measurement_theta_min      2.0430
_cell_volume                     1008.8(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      146.7(6)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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 -84.92  114
  2  \w    -59.55  22.45   1.00   10.00    --  -15.95  83.74  72.05   82
  3  \w   -100.91  13.09   1.00   10.00    --  -15.95 -59.25 173.08  114
  4  \w    -59.55  22.45   1.00   10.00    --  -15.95  83.74 -29.95   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      -0.0169015000
_diffrn_orient_matrix_UB_12      0.0697991000
_diffrn_orient_matrix_UB_13      0.0243042000
_diffrn_orient_matrix_UB_21      -0.0323554000
_diffrn_orient_matrix_UB_22      -0.0025891000
_diffrn_orient_matrix_UB_23      -0.0612222000
_diffrn_orient_matrix_UB_31      -0.0621071000
_diffrn_orient_matrix_UB_32      -0.0201960000
_diffrn_orient_matrix_UB_33      0.0240877000
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0865
_diffrn_reflns_av_unetI/netI     0.1339
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8880
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.866
_diffrn_source_type              Micro-focus
_exptl_absorpt_coefficient_mu    1.279
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61984
_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            colorless
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.887
_refine_diff_density_min         -1.094
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         3498
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.0757
_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^)+(0.0761P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1615
_refine_ls_wR_factor_ref         0.1864
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2289
_reflns_number_total             3498
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03768a2.cif
_cod_data_source_block           sol1_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7714674--7714686.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7714678
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Zn B F S'
_shelx_estimated_absorpt_t_max   0.802
_shelx_estimated_absorpt_t_min   0.766
_reflns_odcompleteness_completeness 98.51
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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:
 C9(H9A,H9B), C10(H10A,H10B), C16(H16A,H16B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C12(H12), C13(H13), C14(H14), C15(H15), C18(H18),
 C19(H19), C20(H20), C21(H21)
2.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C)
;
_shelx_res_checksum              74969
_shelx_hkl_checksum              99192
_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 1.732
_oxdiff_exptl_absorpt_empirical_full_min 0.540