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_7717511
_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_absolute_configuration ad
_chemical_formula_moiety         '3(C18 H24 N6 Ni O2), 2(C3 H7 N O)'
_chemical_formula_sum            'C60 H86 N20 Ni3 O8'
_chemical_formula_weight         1391.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_space_group_name_H-M_alt        'I 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-11-11
_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                 91.7110(17)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.4069(2)
_cell_length_b                   11.1844(2)
_cell_length_c                   27.0255(6)
_cell_measurement_reflns_used    11278
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8150
_cell_measurement_theta_min      3.9070
_cell_volume                     3446.36(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_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 0.995
_diffrn_measured_fraction_theta_max 0.996
_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   18.07    --   15.86 -57.00 -90.00   84
  2  \w    -51.00  33.00   1.00   18.07    --   15.86 -57.00  30.00   84
  3  \w    -25.00  55.00   1.00   18.07    --   15.86 -99.00   0.00   80
  4  \w    -25.00  22.00   1.00   18.07    --  -17.03 -99.00 150.00   47
  5  \w    -14.00  87.00   1.00   18.07    --   15.86  19.00  30.00  101
  6  \w    -78.00 -47.00   1.00   18.07    --  -17.03 138.00  77.38   31
  7  \w    -21.00   6.00   1.00   18.07    --   15.70 -37.00 120.00   27
  8  \w     27.00  52.00   1.00   18.07    --   15.70 -94.00 174.00   25
  9  \w     39.00  75.00   1.00   18.07    --   15.70 178.00 -60.00   36
 10  \w    -38.00   1.00   1.00   18.07    --  -16.79 -37.00  30.00   39
 11  \w    -42.00 -15.00   1.00   18.07    --  -16.79  94.00 -74.00   27
 12  \w    -74.00 -48.00   1.00   18.07    --  -16.79 -77.00-180.00   26
 13  \w     -1.00  83.00   1.00   18.07    --   15.70  57.00  60.00   84
 14  \w    -36.00  34.00   1.00   18.07    --  -16.79  37.00 120.00   70
 15  \w    -25.00  22.00   1.00   18.07    --  -16.79 -99.00-150.00   47
;
_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      0.0452834000
_diffrn_orient_matrix_UB_12      0.0238946000
_diffrn_orient_matrix_UB_13      0.0156143000
_diffrn_orient_matrix_UB_21      -0.0411660000
_diffrn_orient_matrix_UB_22      0.0105752000
_diffrn_orient_matrix_UB_23      0.0186653000
_diffrn_orient_matrix_UB_31      0.0111722000
_diffrn_orient_matrix_UB_32      -0.0577744000
_diffrn_orient_matrix_UB_33      0.0098714000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_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       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            27789
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.936
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.877
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77953
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1468
_exptl_crystal_size_max          0.025
_exptl_crystal_size_mid          0.024
_exptl_crystal_size_min          0.023
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.185
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 2928 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         7020
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0260
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+1.1878P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0649
_reflns_Friedel_coverage         0.900
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                6532
_reflns_number_total             7020
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02746a2.cif
_cod_data_source_block           180403_wb_1_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7717511--7717512.cif.
;
_cod_database_code               7717511
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N O Cl'
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.978
_reflns_odcompleteness_completeness 99.76
_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 Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C19(H19)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3B,H3A), C4(H4B,H4A), C5(H5A,H5B), C6(H6A,H6B), C8(H8B,H8A), C14(H14A,
 H14B), C20(H20A,H20B), C21(H21A,H21B), C23(H23B,H23A)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C15(H15), C16(H16), C24(H24), C25(H25), C28(H28)
2.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C17(H17A,H17B,H17C), C27(H27C,H27B,H27A), C29(H29C,H29B,
 H29A), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              27924
_shelx_hkl_checksum              25651
_shelx_fab_checksum              14289
_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 1.267
_oxdiff_exptl_absorpt_empirical_full_min 0.797