Preparation of cationic cobalt phenoxide and ethoxide complexes and their reversible reaction with carbon dioxide
Archibald, Stephen J.; Foxon, Simon P.; Freeman, Jonathan D.; Hobson, James E.; Perutz, Robin N.; Walton, Paul H.; Journal of the Chemical Society, Dalton Transactions  (2002) 2797–; doi:10.1039/b204560e

data_7011829
_publ_section_title
;
 Preparation of cationic cobalt phenoxide and ethoxide complexes and
 their reversible reaction with carbon dioxide
;
_journal_issue                   14
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2797
_journal_paper_doi               10.1039/b204560e
_journal_year                    2002
_chemical_formula_sum            'C60 H61 B Co N3 O1.5'
_chemical_formula_weight         917.86
_chemical_name_systematic
;
?
;
_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                65.866(12)
_cell_angle_beta                 86.349(14)
_cell_angle_gamma                72.640(14)
_cell_formula_units_Z            2
_cell_length_a                   11.053(2)
_cell_length_b                   15.812(3)
_cell_length_c                   16.503(3)
_cell_measurement_temperature    150(2)
_cell_volume                     2506.6(9)
_computing_cell_refinement       X-AREA
_computing_data_collection       X-AREA
_computing_data_reduction        X-RED
_computing_molecular_graphics    'ORTEP II (Johnson, 1976)'
_computing_publication_material  'SHELXL 97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Stoe IPDSII image plate'
_diffrn_measurement_method
'180 frames at 2^o intervals, exposure time 4 minutes'
_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  0.1698
_diffrn_reflns_av_sigmaI/netI    0.2413
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            47525
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    0.387
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.946
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lathe
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       0.0146(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         14596
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.2087
_refine_ls_R_factor_gt           0.0901
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0858P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2216
_refine_ls_wR_factor_ref         0.2510
_reflns_number_gt                5081
_reflns_number_total             14596
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b204560e.txt
_cod_data_source_block           sja60_01
_cod_original_cell_volume        2506.6(8)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C60 H61 B Co N3 O1.50'
_cod_database_code               7011829