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_7713560
_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         'C31 H33 Cu N5 O2, 2(H2 O), 2(Cl O4)'
_chemical_formula_sum            'C31 H37 Cl2 Cu N5 O12'
_chemical_formula_weight         806.09
_space_group_crystal_system      tetragonal
_space_group_IT_number           78
_space_group_name_Hall           'P 4cw'
_space_group_name_H-M_alt        'P 43'
_atom_sites_solution_hydrogens   mixed
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0835(5)
_cell_length_b                   9.0835(5)
_cell_length_c                   42.651(4)
_cell_measurement_reflns_used    6999
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.6190
_cell_measurement_theta_min      2.6560
_cell_volume                     3519.1(4)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     35.25 117.00   0.75   50.00    --   27.63  54.00 -90.00  109
  2  \w     12.75 117.00   0.75   50.00    --   27.63  54.00  30.00  139
  3  \w    -69.00  47.25   0.75   50.00    --   27.63  54.00 120.00  155
;
_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      0.0775242000
_diffrn_orient_matrix_UB_12      -0.0083112000
_diffrn_orient_matrix_UB_13      0.0012524000
_diffrn_orient_matrix_UB_21      0.0100823000
_diffrn_orient_matrix_UB_22      0.0606119000
_diffrn_orient_matrix_UB_23      -0.0102561000
_diffrn_orient_matrix_UB_31      0.0003456000
_diffrn_orient_matrix_UB_32      0.0484205000
_diffrn_orient_matrix_UB_33      0.0130159000
_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  0.0414
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            17810
_diffrn_reflns_point_group_measured_fraction_full 0.889
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.674
_diffrn_reflns_theta_min         2.437
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.842
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81338
_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 blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_description       block
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.117
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 1789 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         5928
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0425P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0887
_reflns_Friedel_coverage         0.753
_reflns_Friedel_fraction_full    0.776
_reflns_Friedel_fraction_max     0.775
_reflns_number_gt                5164
_reflns_number_total             5928
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01091k2.cif
_cod_data_source_block           complex8
_cod_original_cell_volume        3519.2(5)
_cod_database_code               7713560
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cu1 P3 C55 H44 O5 F8 '
_shelx_estimated_absorpt_t_max   0.908
_shelx_estimated_absorpt_t_min   0.862
_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 O(H,H) groups
2. Restrained distances
 O2-H2A = O2-H2B
 0.85 with sigma of 0.02
 O1-H1A = O1-H1B
 0.85 with sigma of 0.02
 H2B-H1SA
 2.2 with sigma of 0.002
 H2A-H2B
 1.34 with sigma of 0.04
 H1A-H1B
 1.34 with sigma of 0.04
 Cu01-H2A \\sim Cu01-H2B
 with sigma of 0.02
 Cu01-H1A \\sim Cu01-H1B
 with sigma of 0.02
3.a Free rotating group:
 O2S(H2SA,H2SB), O1S(H1SA,H1SB)
3.b Ternary CH refined with riding coordinates:
 C22(H22)
3.c Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C25(H25A,H25B), C23(H23A,H23B), C26(H26A,H26B)
3.d Aromatic/amide H refined with riding coordinates:
 C11(H11), C14(H14), C31(H31), C8(H8), C12(H12), C5(H5), C18(H18), C30(H30),
 C15(H15), C19(H19), C1(H1), C4(H4), C28(H28), C13(H13), C21(H21), C17(H17),
 C2(H2), C3(H3), C20(H20), C29(H29)
;
_shelx_res_checksum              39002
_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 1.190
_oxdiff_exptl_absorpt_empirical_full_min 0.842