Cobalt Complexes Containing Pendant Amines in the Second Coordination Sphere as Electrocatalysts for H2Production
Fang, Ming; Wiedner, Eric S.; Dougherty, William G.; Kassel, W. Scott; Liu, Tianbiao; DuBois, Daniel L.; Bullock, R. Morris; Organometallics 33 (2014) 5820–; doi:10.1021/om5004607

data_4083853
_publ_section_title
;
 Cobalt Complexes Containing Pendant Amines in the Second Coordination
 Sphere as Electrocatalysts for H2Production
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              5820
_journal_paper_doi               10.1021/om5004607
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C34 H40 B Co F8 N3 P2'
_chemical_formula_sum            'C34 H40 B Co F8 N3 P2'
_chemical_formula_weight         774.37
_chemical_name_common            mf26
_chemical_properties_physical
'air-sensitive, moisture-sensitive, oxygen-sensitive'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 99.341(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.2542(4)
_cell_length_b                   38.544(2)
_cell_length_c                   10.5136(5)
_cell_measurement_reflns_used    5981
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.80
_cell_measurement_theta_min      2.50
_cell_volume                     3300.5(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_sigmaI/netI    0.0602
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            29550
_diffrn_reflns_theta_full        28.38
_diffrn_reflns_theta_max         28.38
_diffrn_reflns_theta_min         1.06
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.694
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.8667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS,(Sheldrick, 2006)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platy
_exptl_crystal_F_000             1596
_exptl_crystal_recrystallization_method 'THF, CH3CN, Et2O'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.827
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         8197
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+1.5430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0932
_reflns_number_gt                5995
_reflns_number_total             8197
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5004607_si_002.cif
_cod_data_source_block           mf26_Co(III)HCpC5F4N
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4083853