Electrocatalytic reduction of nitrite to ammonium ion using Ni(ii) complexes with redox-active di(imino)pyridine ligands
Norouzinyanlakvan, Somayeh; Ovens, Jeffrey; Richeson, Darrin; Catalysis Science & Technology 14 (2024) 5422–5429; doi:10.1039/D4CY00715H

data_1572204
_publ_section_title
;
 Electrocatalytic reduction of nitrite to ammonium ion using Ni(ii)
 complexes with redox-active di(imino)pyridine ligands
;
_journal_issue                   18
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              5422
_journal_page_last               5429
_journal_paper_doi               10.1039/D4CY00715H
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'C44 H49 Br2 Cl2 N3 Ni'
_chemical_formula_sum            'C44 H49 Br2 Cl2 N3 Ni'
_chemical_formula_weight         909.29
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_update_record
;
2024-07-22 deposited with the CCDC.	2024-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                93.325(2)
_cell_angle_beta                 107.464(2)
_cell_angle_gamma                114.272(2)
_cell_formula_units_Z            1
_cell_length_a                   9.5290(6)
_cell_length_b                   9.7708(6)
_cell_length_c                   13.6707(9)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      26.57
_cell_measurement_theta_min      2.34
_cell_volume                     1082.49(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution
; 
 SHELXT 2014/5 (Sheldrick, 2014)
;
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_unetI/netI     0.0609
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_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       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12372
_diffrn_reflns_point_group_measured_fraction_full 0.934
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.576
_diffrn_reflns_theta_min         1.597
_exptl_absorpt_coefficient_mu    2.450
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5368
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_description       plate
_exptl_crystal_F_000             466
_exptl_crystal_size_max          0.918
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.236
_refine_diff_density_max         0.743
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Flack x determined using 3246 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.034(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         8201
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0296
_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^)+(0.0170P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0732
_refine_ls_wR_factor_ref         0.0749
_reflns_Friedel_coverage         0.838
_reflns_Friedel_fraction_full    0.870
_reflns_Friedel_fraction_max     0.828
_reflns_number_gt                7740
_reflns_number_total             8201
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cy00715h2.cif
_cod_data_source_block           S0928
_cod_depositor_comments          'Adding full bibliography for 1572204.cif.'
_cod_database_code               1572204
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              66639
_shelx_hkl_checksum              98787