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_7011830
_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_moiety
'C39 H38 Co N3 O1 1+, C24 H20 B 1-, 1.5(C H2 CL2), C6 H12'
_chemical_formula_sum            'C70.5 H73 B Cl3 Co N3 O'
_chemical_formula_weight         1154.41
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_date             2000-03-08
_audit_creation_method           SHELXL-97
_audit_update_record
;
?
;
_cell_angle_alpha                98.97(4)
_cell_angle_beta                 92.61(7)
_cell_angle_gamma                67.78(5)
_cell_formula_units_Z            4
_cell_length_a                   18.31(3)
_cell_length_b                   22.022(11)
_cell_length_c                   17.219(6)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      5.4
_cell_measurement_theta_min      4.6
_cell_volume                     6348(11)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1992-1997)'
_computing_molecular_graphics    'teXsan (MSC, 1992-1997)'
_computing_publication_material  'ORTEPII (Johnson, 1976)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF92 (Beurskens, P.T., et al, 1992)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.721
_diffrn_measured_fraction_theta_max 0.721
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC6s'
_diffrn_measurement_method       \w--2\q
_diffrn_orient_matrix_UB_11      -0.00406
_diffrn_orient_matrix_UB_12      -0.04424
_diffrn_orient_matrix_UB_13      -0.01606
_diffrn_orient_matrix_UB_21      -0.02123
_diffrn_orient_matrix_UB_22      0.00263
_diffrn_orient_matrix_UB_23      0.05344
_diffrn_orient_matrix_UB_31      -0.05491
_diffrn_orient_matrix_UB_32      0.02231
_diffrn_orient_matrix_UB_33      -0.01855
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.10152
_diffrn_reflns_av_sigmaI/netI    0.130
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12510
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        22.49
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         1.92
_diffrn_source_current           30
_diffrn_source_voltage           50
_diffrn_standards_decay_%        3.024
_diffrn_standards_interval_count 3
_diffrn_standards_number         150
_exptl_absorpt_coefficient_mu    0.441
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.845
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1432
_refine_ls_number_reflns         11971
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1879
_refine_ls_R_factor_gt           0.0642
_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^)+(0.1213P)^2^+22.9267P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1652
_refine_ls_wR_factor_ref         0.2534
_reflns_number_gt                5773
_reflns_number_total             11978
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b204560e.txt
_cod_data_source_block           shelxl
_cod_depositor_comments
;

2025-09-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C141 H146 B2 Cl6 Co2 N6 O2'
_cod_original_formula_weight         2308.82
_cod_original_formula_moiety
;
2(C39 H38 Co N3 O1)1+, 2(C24 H20 B)1-, 
3(C H2 CL2), 2(C6 H12) 
;
_cod_original_formula_units_Z            2
_cod_original_cell_volume        6348(10)
_cod_database_code               7011830