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_4120869
_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 H20 N4 Ni S4, 2(N O3), C2 H6 O'
_chemical_formula_sum            'C22 H26 N6 Ni O7 S4'
_chemical_formula_weight         673.44
_chemical_name_common            eiszh14
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
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_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                106.605(3)
_cell_angle_beta                 95.703(3)
_cell_angle_gamma                95.721(3)
_cell_formula_units_Z            2
_cell_length_a                   8.4139(13)
_cell_length_b                   11.1458(17)
_cell_length_c                   15.787(3)
_cell_measurement_reflns_used    4057
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      2.45
_cell_volume                     1398.9(4)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2011)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       'area detector, \w scans per \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0965
_diffrn_reflns_av_sigmaI/netI    0.0937
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            41044
_diffrn_reflns_theta_full        33.14
_diffrn_reflns_theta_max         33.14
_diffrn_reflns_theta_min         1.92
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.045
_exptl_absorpt_correction_T_max  0.9027
_exptl_absorpt_correction_T_min  0.8506
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_description       block
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.883
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         10608
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1232
_refine_ls_R_factor_gt           0.0533
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0463P)^2^+0.0910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1293
_reflns_number_gt                5736
_reflns_number_total             10608
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja405257s_si_003.cif
_cod_data_source_block           eiszh14
_cod_original_cell_volume        1399.0(4)
_cod_database_code               4120869