A mechanistic study of proton reduction catalyzed by a pentapyridine cobalt complex: evidence for involvement of an anation-based pathway
King, Amanda E.; Surendranath, Yogesh; Piro, Nicholas A.; Bigi, Julian P.; Long, Jeffrey R.; Chang, Christopher J.; Chemical Science 4 (2013) 1578–; doi:10.1039/c3sc22239j

data_1514477
_publ_section_title
;
 A mechanistic study of proton reduction catalyzed by a pentapyridine
 cobalt complex: evidence for involvement of an anation-based pathway
;
_journal_issue                   4
_journal_name_full               'Chemical Science'
_journal_page_first              1578
_journal_paper_doi               10.1039/c3sc22239j
_journal_volume                  4
_journal_year                    2013
_chemical_formula_sum            'C53 H45 B Co N5'
_chemical_formula_weight         821.68
_chemical_name_common            AEK1071_0m
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.458(5)
_cell_angle_beta                 107.971(5)
_cell_angle_gamma                101.250(5)
_cell_formula_units_Z            2
_cell_length_a                   10.9829(8)
_cell_length_b                   13.7142(9)
_cell_length_c                   17.0064(13)
_cell_measurement_temperature    373(2)
_cell_volume                     2282.8(3)
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      373(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'HELIOS multilayer mirrors'
_diffrn_radiation_source         'microfocus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0749
_diffrn_reflns_av_sigmaI/netI    0.0819
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20067
_diffrn_reflns_theta_full        63.68
_diffrn_reflns_theta_max         63.68
_diffrn_reflns_theta_min         2.86
_exptl_absorpt_coefficient_mu    3.250
_exptl_absorpt_correction_T_max  0.9378
_exptl_absorpt_correction_T_min  0.7370
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plates
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
;
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.00062(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         7242
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0885P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1524
_refine_ls_wR_factor_ref         0.1685
_reflns_number_gt                4707
_reflns_number_total             7242
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc22239j.txt
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C26.50 H22.50 B0.50 Co0.50 F0 N2.50 O0'
_cod_database_code               1514477