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_4132615
_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         'C27 H23 Cl Co N5, 2(F6 P)'
_chemical_formula_sum            'C27 H23 Cl Co F12 N5 P2'
_chemical_formula_weight         801.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-04-05
_audit_creation_method
;
Olex2 1.2
(compiled Mar 28 2017 19:34:44 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                90
_cell_angle_beta                 115.933(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.0129(15)
_cell_length_b                   17.2789(12)
_cell_length_c                   17.2384(11)
_cell_measurement_reflns_used    9993
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.43
_cell_measurement_theta_min      3.40
_cell_volume                     5896.5(7)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Apex2 (Bruker)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24483
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.496
_diffrn_reflns_theta_min         3.395
_exptl_absorpt_coefficient_mu    7.419
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.4788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1222 before and 0.0692 after correction.
The Ratio of minimum to maximum transmission is 0.6358.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_description       block
_exptl_crystal_F_000             3216
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.043
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         5392
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0714
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+63.9046P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1480
_refine_ls_wR_factor_ref         0.1584
_reflns_number_gt                4399
_reflns_number_total             5392
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b05108_si_003.cif
_cod_data_source_block           sj17_003
_cod_database_code               4132615
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.318
_shelx_estimated_absorpt_t_min   0.214
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C21(H21A,H21B), C28(H28A,H28B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13), C14(H14),
 C16(H16), C23(H23), C24(H24), C25(H25), C26(H26), C30(H30), C31(H31), C32(H32),
  C33(H33)
;
_shelx_res_checksum              65844
_shelx_hkl_checksum              70117
_olex2_submission_special_instructions 'No special instructions were received'