Ligand-based electronic effects on the electrocatalytic hydrogen production by thiosemicarbazone nickel complexes.
Papadakis, Michael; Barrozo, Alexandre; Straistari, Tatiana; Queyriaux, Nicolas; Putri, Anisa; Fize, Jennifer; Giorgi, Michel; Réglier, Marius; Massin, Julien; Hardré, Renaud; Orio, Maylis; Dalton transactions (Cambridge, England : 2003) 49 (2020) 5064–5073; doi:10.1039/c9dt04775a

data_7703713
_publ_section_title
;
 Ligand-based electronic effects on the electrocatalytic hydrogen
 production by thiosemicarbazone nickel complexes.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5064
_journal_page_last               5073
_journal_paper_doi               10.1039/c9dt04775a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C20 H22 N6 Pd S4, 2(C3 H7 N O)'
_chemical_formula_sum            'C26 H36 N8 O2 Pd S4'
_chemical_formula_weight         727.27
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-02-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-20 deposited with the CCDC.	2020-03-05 downloaded from the CCDC.
;
_cell_angle_alpha                70.595(2)
_cell_angle_beta                 70.544(2)
_cell_angle_gamma                82.812(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3380(3)
_cell_length_b                   12.5181(3)
_cell_length_c                   12.8599(3)
_cell_measurement_reflns_used    14869
_cell_measurement_temperature    293
_cell_measurement_theta_max      68.7500
_cell_measurement_theta_min      3.7370
_cell_volume                     1623.01(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3048
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_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   -101.00 -35.00   1.00    1.00    --    0.00-178.00 -60.00   66
  2  \w    -91.00  47.00   1.00    1.00    --    0.00 -38.00-120.00  138
  3  \w    -91.00  35.00   1.00    1.00    --    0.00 -57.00 -30.00  126
  4  \w    -42.00 -17.00   1.00    1.00    --   26.00 129.00   3.17   25
  5  \w      2.00  27.00   1.00    5.00    --   50.00  92.00  87.29   25
  6  \w   -106.00 -67.00   1.00    5.00    --  -52.94 -77.00 -90.00   39
  7  \w    -85.00 -16.00   1.00    5.00    --  -52.94 125.00-150.00   69
  8  \w    -94.00  -6.00   1.00    5.00    --  -52.94 125.00  30.00   88
  9  \w    106.00 145.00   1.00    5.00    --   52.94 125.00 -90.00   39
 10  \w      6.00  31.00   1.00    5.00    --   52.94  90.00-117.73   25
 11  \w      6.00  31.00   1.00    5.00    --   52.94  90.00   4.72   25
 12  \w     10.00  35.00   1.00    5.00    --   54.00  83.00-178.95   25
 13  \w     14.00  40.00   1.00    5.00    --   58.00  83.00 -74.09   26
 14  \w     55.00 132.00   1.00    5.00    --   58.00  71.00  48.42   77
 15  \w     18.00  45.00   1.00    5.00    --   62.00  77.00 -15.46   27
 16  \w     62.00 158.00   1.00    5.00    --   62.00  71.00 164.86   96
 17  \w     68.00 161.00   1.00    5.00    --   62.00  76.00 105.64   93
 18  \w     19.00  46.00   1.00    5.00    --   62.00  71.00 164.86   27
 19  \w     41.00 143.00   1.00    5.00    --   62.00  70.00 -71.83  102
 20  \w     19.00  67.00   1.00    5.00    --   62.00  76.00 105.64   48
 21  \w     18.00  43.00   1.00    5.00    --   62.00  82.00  11.29   25
 22  \w     18.00  43.00   1.00    5.00    --   62.00  80.00-100.71   25
 23  \w     18.00  45.00   1.00    5.00    --   62.00  79.00  61.61   27
 24  \w     53.00 152.00   1.00    5.00    --   62.00  77.00 -15.46   99
 25  \w     18.00  45.00   1.00    5.00    --   62.00  80.00-170.72   27
 26  \w     39.00  65.00   1.00   10.00    --   82.00  75.00-170.70   26
 27  \w     43.00  83.00   1.00   10.00    --   86.00  73.00-153.16   40
 28  \w     62.00 178.00   1.00   10.00    --  105.88  77.00   0.00  116
 29  \w     96.00 178.00   1.00   10.00    --  105.88  77.00  30.00   82
 30  \w     62.00 145.00   1.00   10.00    --  105.88  77.00 -90.00   83
 31  \w     62.00  88.00   1.00   10.00    --  105.88  77.00  30.00   26
 32  \w     81.00 148.00   1.00   10.00    --  105.88 -91.00 -60.00   67
 33  \w     27.00 115.00   1.00   10.00    --  105.88-111.00-180.00   88
 34  \w      9.00  61.00   1.00   10.00    --  105.88 -91.00 -60.00   52
 35  \w     62.00 169.00   1.00   10.00    --  105.88  77.00-180.00  107
 36  \w     10.00 143.00   1.00   10.00    --  105.88 -91.00-150.00  133
 37  \w     62.00 178.00   1.00   10.00    --  105.88  77.00 120.00  116
 38  \w     62.00  92.00   1.00   10.00    --  105.88  77.00-150.00   30
 39  \w     64.00  92.00   1.00   10.00    --  105.88  63.00 -30.00   28
 40  \w     99.00 177.00   1.00   10.00    --  105.88  77.00 -60.00   78
 41  \w     62.00  89.00   1.00   10.00    --  105.88  63.00  60.00   27
 42  \w     62.00  88.00   1.00   10.00    --  105.88  77.00 -60.00   26
 43  \w     63.00 131.00   1.00   10.00    --  105.88  77.00 -30.00   68
 44  \w     86.00 149.00   1.00   10.00    --  105.88 178.00-150.00   63
 45  \w     95.00 178.00   1.00   10.00    --  105.88  77.00-150.00   83
 46  \w     62.00  89.00   1.00   10.00    --  105.88  63.00-120.00   27
 47  \w     62.00 167.00   1.00   10.00    --  105.88  77.00  90.00  105
 48  \w     62.00 152.00   1.00   10.00    --  105.88  77.00-120.00   90
 49  \w    100.00 127.00   1.00   10.00    --  105.88  77.00  60.00   27
 50  \w     62.00  88.00   1.00   10.00    --  105.88  77.00  60.00   26
 51  \w     62.00 178.00   1.00   10.00    --  105.88  76.00 147.00  116
 52  \w     62.00 132.00   1.00   10.00    --  105.88  63.00  90.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1395000000
_diffrn_orient_matrix_UB_12      -0.0114509000
_diffrn_orient_matrix_UB_13      0.0172422000
_diffrn_orient_matrix_UB_21      -0.0065210000
_diffrn_orient_matrix_UB_22      -0.1074886000
_diffrn_orient_matrix_UB_23      0.1042421000
_diffrn_orient_matrix_UB_31      -0.0356214000
_diffrn_orient_matrix_UB_32      0.0731049000
_diffrn_orient_matrix_UB_33      0.0818648000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0847
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21621
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.843
_diffrn_reflns_theta_min         3.744
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.324
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.44a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       needle
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.020
_refine_diff_density_min         -0.844
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         5954
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0597P)^2^+0.7526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1123
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5619
_reflns_number_total             5954
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04775a2.cif
_cod_data_source_block           ap22pdl2
_cod_depositor_comments          'Adding full bibliography for 7703713.cif.'
_cod_database_code               7703713
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'c20 h22 n6 s4 Pd1'
_shelx_estimated_absorpt_t_max   0.592
_shelx_estimated_absorpt_t_min   0.178
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N6(H6), C3(H3), C4(H4), C6(H6A), C7(H7), C13(H13), C14(H14), C16(H16),
  C17(H17), C23(H23), C26(H26)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,
 H25B,H25C)
;
_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 2.369
_oxdiff_exptl_absorpt_empirical_full_min 0.580