Electronic and Steric Tuning of Catalytic H<sub>2</sub> Evolution by Cobalt Complexes with Pentadentate Polypyridyl-Amine Ligands.
Wang, Ping; Liang, Guangchao; Reddy, M. Ramana; Long, Melissa; Driskill, Kandria; Lyons, Christian; Donnadieu, Bruno; Bollinger, John C.; Webster, Charles Edwin; Zhao, Xuan; Journal of the American Chemical Society 140 (2018) 9219–9229; doi:10.1021/jacs.8b05108

data_4132616
_publ_section_title
;
 Electronic and Steric Tuning of Catalytic H<sub>2</sub> Evolution by
 Cobalt Complexes with Pentadentate Polypyridyl-Amine Ligands.
;
_journal_issue                   29
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9219
_journal_page_last               9229
_journal_paper_doi               10.1021/jacs.8b05108
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C54 H57 Co2 F30 N10 O6 P5'
_chemical_formula_sum            'C54 H57 Co2 F30 N10 O6 P5'
_chemical_formula_weight         1784.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 100.363(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6956(19)
_cell_length_b                   17.882(3)
_cell_length_c                   25.751(3)
_cell_measurement_reflns_used    1486
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.044
_cell_measurement_theta_min      2.082
_cell_volume                     6656.6(16)
_computing_cell_refinement
'SHELXTL, Acta Cryst., Sect. A 2008, 64, 112-122.'
_computing_data_collection       'APEX3 v2017.3.0'
_computing_data_reduction        'Saint, APEX v2017.3.0.'
_computing_molecular_graphics    Ortep3
_computing_publication_material  'APEX3 v2017.3.0'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2014)'
_computing_structure_solution
'SHELXT, Acta Cryst., Sect. A 2015, A71, 3-8.'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker AXS D8 Venture '
_diffrn_measurement_method       'profile data from \q/2\q scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            92223
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.044
_diffrn_reflns_theta_min         2.082
_exptl_absorpt_coefficient_mu    0.761
_exptl_absorpt_correction_T_max  0.888
_exptl_absorpt_correction_T_min  0.642
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_description       'prism frag'
_exptl_crystal_F_000             3592
_exptl_crystal_size_max          0.639
_exptl_crystal_size_mid          0.326
_exptl_crystal_size_min          0.160
_refine_diff_density_max         1.689
_refine_diff_density_min         -1.625
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1028
_refine_ls_number_reflns         26645
_refine_ls_number_restraints     304
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0933P)^2^+12.3862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1626
_refine_ls_wR_factor_ref         0.1902
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20101
_reflns_number_total             26645
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b05108_si_002.cif
_cod_data_source_block           1h2o1
_cod_original_cell_volume        6656.7(15)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4132616
_shelx_estimated_absorpt_t_min   0.642
_shelx_estimated_absorpt_t_max   0.888
_shelx_res_checksum              98100
_shelx_hkl_checksum              69256