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_7714675
_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         'C27 H25 N3 O2 Se Zn'
_chemical_formula_sum            'C27 H25 N3 O2 Se Zn'
_chemical_formula_weight         567.83
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-09-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-09-22 deposited with the CCDC.	2023-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1361(8)
_cell_length_b                   12.0931(5)
_cell_length_c                   10.4127(4)
_cell_measurement_reflns_used    8839
_cell_measurement_temperature    145(2)
_cell_measurement_theta_max      25.66
_cell_measurement_theta_min      2.71
_cell_volume                     2409.65(17)
_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      145.01
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0579
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            26224
_diffrn_reflns_point_group_measured_fraction_full 0.925
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.722
_diffrn_reflns_theta_min         2.715
_diffrn_source_type              Micro-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.560
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5300
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1177 before and 0.0695 after correction.
The Ratio of minimum to maximum transmission is 0.7111.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.010(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         4240
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0289
_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^)+(0.0210P)^2^+0.2693P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0550
_refine_ls_wR_factor_ref         0.0584
_reflns_Friedel_coverage         0.735
_reflns_Friedel_fraction_full    0.843
_reflns_Friedel_fraction_max     0.827
_reflns_number_gt                3793
_reflns_number_total             4240
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03768a2.cif
_cod_data_source_block           mo_am130922_0ma
_cod_depositor_comments
'Adding full bibliography for 7714674--7714686.cif.'
_cod_original_sg_symbol_H-M      Pca21
_cod_database_code               7714675
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.656
_shelx_estimated_absorpt_t_min   0.603
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.990(13)
 0.010(13)
2. 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
3.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C16(H16A,H16B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C6(H6), C12(H12), C13(H13), C14(H14), C15(H15), C18(H18),
 C19(H19), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27)
3.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_shelx_res_checksum              64963
_shelx_hkl_checksum              34039
_olex2_submission_special_instructions 'No special instructions were received'