Cobalt Schiff-Base Complexes for Electrocatalytic Hydrogen Generation
DiRisio, Ryan J.; Armstrong, Jessica E.; Frank, Mariah A.; Lake, William R.; McNamara, William Robert; Dalton Trans.  (2017) –; doi:10.1039/C7DT01750B

data_7043714
_publ_section_title
;
 Cobalt Schiff-Base Complexes for Electrocatalytic Hydrogen Generation
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01750B
_journal_year                    2017
_chemical_formula_moiety
'C18 H20 Co N6 O6, 0.70(F6 P), 2(C7 H8), 0.30(B F4)'
_chemical_formula_sum            'C32 H36 B0.3 Co F5.39 N6 O6 P0.7'
_chemical_formula_weight         786.97
_chemical_name_common            cwmwm10
_chemical_properties_physical    ', Moisture-sensitive'
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/4
_audit_update_record
;
2017-05-12 deposited with the CCDC.
2017-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.4907(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6579(11)
_cell_length_b                   18.1377(15)
_cell_length_c                   13.7492(11)
_cell_measurement_reflns_used    3983
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      35.63
_cell_measurement_theta_min      2.39
_cell_volume                     3405.9(5)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016b)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0754
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            118185
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        36.319
_diffrn_reflns_theta_max         36.406
_diffrn_reflns_theta_min         1.867
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.620
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.6514
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2016a)'
_exptl_crystal_colour            pink-red
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_description       needle
_exptl_crystal_F_000             1622
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol/toluene'
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.832
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         8288
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0478P)^2^+2.7873P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1093
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6153
_reflns_number_total             8288
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01750b2.cif
_cod_data_source_block           cwmwm10
_cod_original_formula_sum        'C32 H36 B0.30 Co F5.39 N6 O6 P0.70'
_cod_database_code               7043714
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.755
_shelx_estimated_absorpt_t_max   0.929
_shelx_res_checksum              76680