Nickel Pyridinethiolate Complexes as Catalysts for the Light-Driven Production of Hydrogen from Aqueous Solutions in Noble-Metal-Free Systems
Zhiji Han; Luxi Shen; William W. Brennessel; Patrick L. Holland; Richard Eisenberg; Journal of the American Chemical Society 135 (2013) 14659–14669; doi:10.1021/ja405257s

data_4120872
_publ_section_title
;
 Nickel Pyridinethiolate Complexes as Catalysts for the Light-Driven
 Production of Hydrogen from Aqueous Solutions in Noble-Metal-Free Systems
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14659
_journal_page_last               14669
_journal_paper_doi               10.1021/ja405257s
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C20 H16 N4 Ni S2'
_chemical_formula_sum            'C20 H16 N4 Ni S2'
_chemical_formula_weight         435.20
_chemical_name_common            eiszh26
_chemical_name_systematic
; 
 ? 
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 98.718(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.2210(14)
_cell_length_b                   15.822(3)
_cell_length_c                   16.582(3)
_cell_measurement_reflns_used    3892
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      37.79
_cell_measurement_theta_min      2.49
_cell_volume                     1872.6(6)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2012)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            83693
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        37.785
_diffrn_reflns_theta_max         37.783
_diffrn_reflns_theta_min         1.789
_exptl_absorpt_coefficient_mu    1.271
_exptl_absorpt_correction_T_max  0.7476
_exptl_absorpt_correction_T_min  0.5462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_refine_diff_density_max         1.261
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         10358
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0575P)^2^+0.4569P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1105
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8677
_reflns_number_total             10358
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja405257s_si_006.cif
_cod_data_source_block           eiszh26
_cod_database_code               4120872
_shelx_estimated_absorpt_t_min   0.702
_shelx_estimated_absorpt_t_max   0.803
_diffrn_reflns_sigmai/neti       0.0549
_shelxl_version_number           2012-4
_shelx_res_checksum              10951