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_7714685
_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 Fe2 N8 O9'
_chemical_formula_sum            'C42 H40 Fe2 N8 O9'
_chemical_formula_weight         912.52
_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             2023-08-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-08-15 deposited with the CCDC.	2023-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.532(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.613(4)
_cell_length_b                   15.673(6)
_cell_length_c                   14.617(6)
_cell_measurement_reflns_used    9451
_cell_measurement_temperature    125.32
_cell_measurement_theta_max      25.67
_cell_measurement_theta_min      2.34
_cell_volume                     2390.4(16)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      125.32
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker D8VENTURE with PHOTON II Detector'
_diffrn_measurement_method       'phi, omega and kappa scan'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22154
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.841
_diffrn_reflns_theta_min         2.549
_diffrn_source_type              Micro-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.664
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5331
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1446 before and 0.0843 after correction.
The Ratio of minimum to maximum transmission is 0.7153.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            dark-brown
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         4562
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0545
_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^)+(0.0722P)^2^+1.2992P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1467
_refine_ls_wR_factor_ref         0.1604
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3390
_reflns_number_total             4562
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03768a2.cif
_cod_data_source_block           mo_am110823a_0m
_cod_depositor_comments
'Adding full bibliography for 7714674--7714686.cif.'
_cod_original_cell_volume        2390.5(16)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7714685
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.890
_shelx_estimated_absorpt_t_min   0.868
_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. Restrained distances
 O2A-C3 \\sim O2B-C3
 with sigma of 0.02
 Fe1-O4A \\sim Fe1-O4B
 with sigma of 0.02
 O5B-N4B \\sim O5A-N4A
 with sigma of 0.02
 O4B-N4B \\sim O4A-N4A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C3) = Uanis(O2B) = Uanis(O2A)
Uanis(O5B) = Uanis(O5A) = Uanis(N4B) = Uanis(N4A) = Uanis(O4B) = Uanis(O4A)
4. Others
 Sof(O2B)=Sof(O4B)=Sof(N4B)=Sof(O5B)=Sof(H3B)=1-FVAR(1)
 Sof(O2A)=Sof(O4A)=Sof(N4A)=Sof(O5A)=Sof(H3A)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C16(H16A,H16B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3A), C3(H3B), C4(H4), C7(H7), C12(H12), C13(H13), C14(H14), C15(H15),
 C18(H18), C19(H19), C20(H20), C21(H21)
5.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              16684
_shelx_hkl_checksum              81353
_shelx_fab_checksum              14516
_olex2_submission_special_instructions 'No special instructions were received'