Electrocatalytic Hydrogen Evolution at Low Overpotentials by Cobalt Macrocyclic Glyoxime and Tetraimine Complexes
Xile Hu; Bruce S. Brunschwig; Jonas C. Peters; Journal of the American Chemical Society 129 (2007) 8988–8998; doi:10.1021/ja067876b

data_4109675
_publ_section_title
;
 Electrocatalytic Hydrogen Evolution at Low Overpotentials by Cobalt
 Macrocyclic Glyoxime and Tetraimine Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8988
_journal_page_last               8998
_journal_paper_doi               10.1021/ja067876b
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum
'C40.44 H47.33 B1.6 Co0.8 F3.2 N4.6 Na0.8 O10.21'
_chemical_formula_weight         904.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.319(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            5
_cell_length_a                   12.444(2)
_cell_length_b                   14.709(3)
_cell_length_c                   29.884(6)
_cell_measurement_temperature    100(2)
_cell_volume                     5460.8(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_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  0.0830
_diffrn_reflns_av_sigmaI/netI    0.0751
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            79724
_diffrn_reflns_theta_full        28.55
_diffrn_reflns_theta_max         28.55
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    0.402
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_F_000             2355
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.374
_refine_diff_density_min         -0.980
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     682
_refine_ls_number_reflns         12962
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1016
_refine_ls_R_factor_gt           0.0554
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0962P)^2^+0.8521P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1489
_refine_ls_wR_factor_ref         0.1727
_reflns_number_gt                8189
_reflns_number_total             12962
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja067876bsi20070502_125837_2.cif
_cod_data_source_block           xh22
_cod_original_cell_volume        5461.0(19)
_cod_original_formula_sum
'C40.44 H47.33 B1.60 Co0.80 F3.20 N4.60 Na0.80 O10.21'
_cod_database_code               4109675