Photocatalytic and electrocatalytic hydrogen production using nickel complexes supported by hemilabile and non-innocent ligands.
Inoue, Satoshi; Yan, Yin-Nan; Yamanishi, Katsunori; Kataoka, Yusuke; Kawamoto, Tatsuya; Chemical communications (Cambridge, England) 56 (2020) 2829–2832; doi:10.1039/c9cc09568c

data_7125991
_publ_section_title
;
 Photocatalytic and electrocatalytic hydrogen production using nickel
 complexes supported by hemilabile and non-innocent ligands.
;
_journal_issue                   19
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2829
_journal_page_last               2832
_journal_paper_doi               10.1039/c9cc09568c
_journal_volume                  56
_journal_year                    2020
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C30 H28 Cl2 N6 Ni O8 S2'
_chemical_formula_sum            'C30 H28 Cl2 N6 Ni O8 S2'
_chemical_formula_weight         794.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2019-12-07 deposited with the CCDC.	2020-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 115.404(5)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
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_cell_length_b                   8.33062(19)
_cell_length_c                   20.7006(8)
_cell_measurement_reflns_used    10689
_cell_measurement_temperature    296
_cell_measurement_theta_max      31.25
_cell_measurement_theta_min      2.67
_cell_volume                     3418.9(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2.2'
_computing_publication_material  'CrystalStructure 4.2.2 (Rigaku, 2016)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean 28.626
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.000
_diffrn_reflns_Laue_measured_fraction_max 0.000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10487
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_theta_full        25.350
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.178
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.904
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1632.00
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.53
_refine_diff_density_min         -0.35
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  2435 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.014(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     453
_refine_ls_number_reflns         5494
_refine_ls_number_restraints     29
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0703P)^2^+0.4539P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.0941
_reflns_number_gt                5345
_reflns_number_total             5494
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c9cc09568c2.cif
_cod_data_source_block           xcalibur
_cod_depositor_comments
'Adding full bibliography for 7125991--7125997.cif.'
_cod_original_cell_volume        3419.0(4)
_cod_database_code               7125991