Neutral nickel complexes with tetradentate N-heterocyclic carbene amidate ligands for electrocatalytic hydrogen evolution.
Si, Si; Song, Wenxun; Chen, Jie; Zhang, Weimin; Ji, Wenhua; Nam, Wonwoo; Wang, Bin; Dalton transactions (Cambridge, England : 2003) 53 (2024) 19088–19092; doi:10.1039/d4dt02746a

data_7717512
_publ_section_title
;
 Neutral nickel complexes with tetradentate N-heterocyclic carbene amidate
 ligands for electrocatalytic hydrogen evolution.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              19088
_journal_page_last               19092
_journal_paper_doi               10.1039/d4dt02746a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C18 H16 Cl2 N6 Ni O2, 2(C3 H7 N O)'
_chemical_formula_sum            'C24 H30 Cl2 N8 Ni O4'
_chemical_formula_weight         624.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-10-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-06-28 deposited with the CCDC.	2024-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.317(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0789(4)
_cell_length_b                   10.4388(3)
_cell_length_c                   17.9250(5)
_cell_measurement_reflns_used    5969
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.4190
_cell_measurement_theta_min      3.7930
_cell_volume                     2784.27(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0355
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.865
_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    -51.00  33.00   1.00   13.64    --   16.17 -57.00   0.00   84
  2  \w    -25.00  22.00   1.00   13.64    --  -16.64 -99.00 150.00   47
  3  \w    -84.00  10.00   1.00   13.64    --  -16.64 -77.00 -90.00   94
  4  \w    -13.00  33.00   1.00   13.64    --   16.17  19.00 120.00   46
  5  \w    -73.00 -22.00   1.00   13.64    --  -16.64 130.00 130.27   51
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0214375000
_diffrn_orient_matrix_UB_12      0.0264511000
_diffrn_orient_matrix_UB_13      -0.0288766000
_diffrn_orient_matrix_UB_21      0.0011256000
_diffrn_orient_matrix_UB_22      -0.0614861000
_diffrn_orient_matrix_UB_23      -0.0166907000
_diffrn_orient_matrix_UB_31      -0.0425361000
_diffrn_orient_matrix_UB_32      0.0117328000
_diffrn_orient_matrix_UB_33      -0.0222926000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.865
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18576
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.865
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.133
_diffrn_reflns_theta_min         3.157
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.935
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86577
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_description       prism
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.400
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         6494
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+1.0247P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0939
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4973
_reflns_number_total             6494
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02746a2.cif
_cod_data_source_block           20211023_wb1b
_cod_depositor_comments
'Adding full bibliography for 7717511--7717512.cif.'
_cod_database_code               7717512
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_usercomment     'Ni C H N O Cl'
_reflns_odcompleteness_completeness 99.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C14(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C8(H8), C11(H11), C16(H16), C17(H17), C21(H21), C24(H24)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C)
;
_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 1.240
_oxdiff_exptl_absorpt_empirical_full_min 0.914