Electrocatalytic Hydrogen Evolution in Acidic Water with Molecular Cobalt Tetraazamacrocycles
Charles C. L. McCrory; Christopher Uyeda; Jonas C. Peters; Journal of the American Chemical Society 134 (2012) 3164–3170; doi:10.1021/ja210661k

data_4117458
_publ_section_title
;
 Electrocatalytic Hydrogen Evolution in Acidic Water with Molecular Cobalt
 Tetraazamacrocycles
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3164
_journal_page_last               3170
_journal_paper_doi               10.1021/ja210661k
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C11 H23 Cl2 Co N4 O12'
_chemical_formula_weight         533.16
_chemical_name_common            '[Co(DO)(DOH)pn(OH2)2](ClO4)2'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 109.992(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6993(5)
_cell_length_b                   15.4039(6)
_cell_length_c                   12.9476(6)
_cell_measurement_reflns_used    9673
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      45.20
_cell_measurement_theta_min      2.52
_cell_volume                     2005.32(16)
_computing_cell_refinement       'SAINT-Plus v7.66A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 v2010.7-0 (Bruker-AXS, 2010)'
_computing_data_reduction        'SAINT-Plus v7.66A (Bruker-AXS, 2009)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_measurement_method       '\w and \f scans'
_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  0.0355
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            120857
_diffrn_reflns_theta_full        45.36
_diffrn_reflns_theta_max         45.36
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    1.192
_exptl_absorpt_correction_T_max  0.9107
_exptl_absorpt_correction_T_min  0.5816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1 (Bruker-AXS, 2008)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_description       plate
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.982
_refine_diff_density_min         -1.004
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         16778
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0288
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+0.3529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0809
_reflns_number_gt                13461
_reflns_number_total             16778
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja210661k_si_002.cif
_cod_data_source_block           chu13
_cod_original_cell_volume        2005.32(15)
_cod_database_code               4117458