Synthesis and Electrochemical Studies of Cobalt(III) Monohydride Complexes Containing Pendant Amines
Eric S. Wiedner; John A. S. Roberts; William G. Dougherty; W. Scott Kassel; Daniel L. DuBois; R. Morris Bullock; Inorganic Chemistry 52 (2013) 9975–9988; doi:10.1021/ic401232g

data_4335863
_publ_section_title
;
 Synthesis and Electrochemical Studies of Cobalt(III) Monohydride
 Complexes Containing Pendant Amines
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9975
_journal_page_last               9988
_journal_paper_doi               10.1021/ic401232g
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C52 H59 B2 Co F8 N5 P4'
_chemical_formula_weight         1110.47
_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                77.462(3)
_cell_angle_beta                 89.678(3)
_cell_angle_gamma                77.980(4)
_cell_formula_units_Z            2
_cell_length_a                   10.8932(11)
_cell_length_b                   15.0777(15)
_cell_length_c                   16.3551(16)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.03
_cell_measurement_theta_min      2.55
_cell_volume                     2562.5(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0424
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            75557
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         33.19
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.531
_exptl_absorpt_correction_T_max  0.9587
_exptl_absorpt_correction_T_min  0.9012
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       block
_exptl_crystal_F_000             1150
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.893
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     727
_refine_ls_number_reflns         19474
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0605
_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^)+(0.0535P)^2^+1.1555P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1123
_reflns_number_gt                15088
_reflns_number_total             19474
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401232g_si_002_2.cif
_cod_data_source_block           '[Co(L3)(CH3CN)][BF4]2'
_cod_database_code               4335863