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_4335864
_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            'C48 H53 B2 Co F8 N4 P4'
_chemical_formula_weight         1042.37
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 102.536(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.6942(8)
_cell_length_b                   18.8403(7)
_cell_length_c                   12.7507(5)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.10
_cell_measurement_theta_min      2.55
_cell_volume                     4852.8(3)
_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 1.000
_diffrn_measured_fraction_theta_max 0.988
_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  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            83601
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         33.30
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.555
_exptl_absorpt_correction_T_max  0.9465
_exptl_absorpt_correction_T_min  0.8876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       block
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.823
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     610
_refine_ls_number_reflns         18512
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0470P)^2^+2.6280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.1093
_reflns_number_gt                13277
_reflns_number_total             18512
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401232g_si_002_3.cif
_cod_data_source_block           '[HCo(L2)(CH3CN)][BF4]2'
_cod_database_code               4335864