Biomimetic catalysis of nitrite reductase enzyme using copper complexes in chemical and electrochemical reduction of nitrite
P. Ferreira, Millena; Bezerra Castro, Caio; de Araújo Neto, João Honorato; he, sheng; Gonçalves Guimarães Júnior, Walber; Esmieu, Charlene; Castellano, Eduardo; de Moura, André Farias; Truzzi, Daniela Ramos; Nascimento, Otaciro; Simonneau, Antoine; Netto, Caterina Gruenwaldt Cunha Marques; Dalton Transactions  (2023) –; doi:10.1039/D3DT01091K

data_7713559
_publ_section_title
;
 Biomimetic catalysis of nitrite reductase enzyme using copper complexes
 in chemical and electrochemical reduction of nitrite
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01091K
_journal_year                    2023
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C29 H33 N5'
_chemical_formula_sum            'C29 H33 N5'
_chemical_formula_weight         451.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-04
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_audit_update_record
;
2021-10-04 deposited with the CCDC.	2023-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.845(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.8878(7)
_cell_length_b                   8.4324(7)
_cell_length_c                   15.4023(12)
_cell_measurement_reflns_used    10885
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.2390
_cell_measurement_theta_min      2.8280
_cell_volume                     1268.94(17)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -69.00 118.00   1.00   35.00    --   27.63  54.00 -90.00  187
  2  \w    -69.00 118.00   1.00   35.00    --   27.63  54.00  30.00  187
  3  \w    -69.00 118.00   1.00   35.00    --   27.63  54.00 120.00  187
  4  \w    -69.00 118.00   1.00   35.00    --   27.63  54.00 -30.00  187
  5  \w    -69.00 118.00   1.00   35.00    --   27.63  54.00-180.00  187
  6  \w    -69.00 -34.00   1.00   35.00    --   27.63  54.00  60.00   35
  7  \w    -69.00 118.00   1.00   35.00    --   27.63  54.00-150.00  187
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0075821000
_diffrn_orient_matrix_UB_12      0.0001687000
_diffrn_orient_matrix_UB_13      0.0465646000
_diffrn_orient_matrix_UB_21      0.0307160000
_diffrn_orient_matrix_UB_22      0.0760646000
_diffrn_orient_matrix_UB_23      0.0009478000
_diffrn_orient_matrix_UB_31      -0.0653502000
_diffrn_orient_matrix_UB_32      0.0358545000
_diffrn_orient_matrix_UB_33      -0.0021519000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26267
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.645
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79435
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_description       block
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.427
_exptl_crystal_size_mid          0.291
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.130
_refine_diff_density_min         -0.131
_refine_diff_density_rms         0.027
_refine_ls_abs_structure_details
;
 Flack x determined using 1947 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.3(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         5199
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0369
_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^)+(0.0551P)^2^+0.0890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.0995
_reflns_Friedel_coverage         0.867
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                4591
_reflns_number_total             5199
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01091k2.cif
_cod_data_source_block           ligand6
_cod_database_code               7713559
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C33 H44 O3 S2'
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.970
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H,H,H,H) groups
2. Others
 Fixed Sof: H1AA(0.7) H1AB(0.7) H1AC(0.7) H1BD(0.3) H1BE(0.3) H1BF(0.3)
 C2A(0.7) H2AA(0.7) H2AB(0.7) C2B(0.3) H2BA(0.3) H2BB(0.3) C3A(0.7) H3AA(0.7)
 H3AB(0.7) C3B(0.3) H3BA(0.3) H3BB(0.3) H4AA(0.7) H4AB(0.7) H4BC(0.3) H4BD(0.3)
 H9AA(0.5) H9AB(0.5) H9BC(0.5) H9BD(0.5) C10A(0.45553) H10A(0.45553)
 H10B(0.45553) C10B(0.54447) H10C(0.54447) H10D(0.54447) H11A(0.5) H11B(0.5)
 H11C(0.5) H11D(0.5)
3.a Ternary CH refined with riding coordinates:
 C8(H8)
3.b Secondary CH2 refined with riding coordinates:
 C2A(H2AA,H2AB), C2B(H2BA,H2BB), C3A(H3AA,H3AB), C3B(H3BA,H3BB), C4(H4AA,H4AB),
  C4(H4BC,H4BD), C9(H9AA,H9AB), C9(H9BC,H9BD), C10A(H10A,H10B), C10B(H10C,H10D),
  C11(H11A,H11B), C11(H11C,H11D), C12(H12A,H12B)
3.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21),
 C22(H22), C23(H23), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29)
3.d Idealised Me refined as rotating group:
 C1(H1AA,H1AB,H1AC), C1(H1BD,H1BE,H1BF)
;
_shelx_res_checksum              47550
_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 1.353
_oxdiff_exptl_absorpt_empirical_full_min 0.885