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_4335862
_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            'C51 H56.5 B2 Co F8 N5.5 P4'
_chemical_formula_weight         1102.95
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 102.008(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.0596(16)
_cell_length_b                   12.7110(13)
_cell_length_c                   27.968(3)
_cell_measurement_reflns_used    9584
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.20
_cell_measurement_theta_min      2.42
_cell_volume                     5236.6(10)
_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 0.990
_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  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0350
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            89962
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         33.30
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    0.520
_exptl_absorpt_correction_T_max  0.9032
_exptl_absorpt_correction_T_min  0.8854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       block
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
The SQUEEZE results suggest 2.5 molecule of CH3CN solvent per asymmetric
unit.  The difference map suggests three separate sites in the asymmetric
unit for the acetonitrile.  One is fully occupied and refines well.  The
other two are likely disordered over those two positions in a ratio
that would lead to an average of 1.5 equivalents of solvent.  These
would not refine well and their structures were bent instead of linear.
Therefore, all 3 solvent molecules were removed using SQUEEZE.  

PLATON Reference : Spek, A.L. (2003). J. Appl. Cryst. 36, 7-13.
                     Spek, A.L. (2009). Acta Cryst. D65, 148-155.
;
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         20034
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0499P)^2^+0.6181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1020
_reflns_number_gt                15004
_reflns_number_total             20034
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401232g_si_002_1.cif
_cod_data_source_block           '[Co(L2)(CH3CN)][BF4}2'
_cod_original_formula_sum        'C51 H56.50 B2 Co F8 N5.50 P4'
_cod_database_code               4335862