Oxo-functionalised mesoionic NHC nickel complexes for selective electrocatalytic reduction of CO2 to formate
Bertini, Simone; Rahaman, Motiar; Dutta, Abhijit; Schollhammer, Philippe; Rudnev, Alexander V.; Gloaguen, Fredric; Broekmann, Peter; Albrecht, Martin; Green Chemistry 23 (2021) 3365–3373; doi:10.1039/D1GC00388G

data_7242644
_publ_section_title
;
 Oxo-functionalised mesoionic NHC nickel complexes for selective
 electrocatalytic reduction of CO2 to formate
;
_journal_issue                   9
_journal_name_full               'Green Chemistry'
_journal_page_first              3365
_journal_page_last               3373
_journal_paper_doi               10.1039/D1GC00388G
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C36 H36 N6 Ni O2'
_chemical_formula_sum            'C36 H36 N6 Ni O2'
_chemical_formula_weight         643.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-08-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_audit_update_record
;
2020-05-15 deposited with the CCDC.	2021-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.6340(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.11310(10)
_cell_length_b                   10.38960(10)
_cell_length_c                   14.69520(10)
_cell_measurement_reflns_used    14089
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      27.9970
_cell_measurement_theta_min      1.9880
_cell_volume                     1598.07(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0965
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_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    -28.00 109.00   1.00    4.97    --   27.49  38.00 -30.00  137
  2  \w    -54.00  83.00   1.00    4.97    --   27.49 -38.00  30.00  137
  3  \w    -10.00 103.00   1.00    4.97    --   27.49  57.00   0.00  113
  4  \w    -16.00 112.00   1.00    4.97    --   27.49  77.00-180.00  128
  5  \w    -49.00  65.00   1.00    4.97    --   27.49 -57.00-180.00  114
  6  \w    -20.00  28.00   1.00    4.97    --  -23.50 -99.00 -60.00   48
  7  \w    -20.00  83.00   1.00    4.97    --   27.49 -99.00  60.00  103
  8  \w    -54.00  83.00   1.00    4.97    --   27.49 -38.00-120.00  137
  9  \w    -10.00 103.00   1.00    4.97    --   27.49  57.00 120.00  113
 10  \w     35.00 122.00   1.00    4.97    --   27.49 178.00  60.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0256630000
_diffrn_orient_matrix_UB_12      -0.0576975000
_diffrn_orient_matrix_UB_13      -0.0247453000
_diffrn_orient_matrix_UB_21      0.0615510000
_diffrn_orient_matrix_UB_22      -0.0178503000
_diffrn_orient_matrix_UB_23      -0.0001198000
_diffrn_orient_matrix_UB_31      0.0120234000
_diffrn_orient_matrix_UB_32      -0.0318363000
_diffrn_orient_matrix_UB_33      0.0448803000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26452
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         2.007
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.649
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       prism
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.234
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3647
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0298
_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^)+(0.0433P)^2^+0.5772P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0844
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3269
_reflns_number_total             3647
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1gc00388g2.cif
_cod_data_source_block           17ma116_SB279
_cod_depositor_comments
'Adding full bibliography for 7242639--7242644.cif.'
_cod_database_code               7242644
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C36H36N6Ni1O2
_shelx_estimated_absorpt_t_max   0.854
_shelx_estimated_absorpt_t_min   0.829
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C16(H16), C10(H10), C12(H12), C18(H18), C11(H11)
2.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C)
;
_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 1.334
_oxdiff_exptl_absorpt_empirical_full_min 0.834