Chemoselective, Practical Synthesis of Cobaltocenium Carboxylic Acid Hexafluorophosphate
Vanicek, Stefan; Kopacka, Holger; Wurst, Klaus; Müller, Thomas; Schottenberger, Herwig; Bildstein, Benno; Organometallics 33 (2014) 1152–; doi:10.1021/om401120h

data_4082689
_publ_contact_author
;
      Benno Bildstein
      Institute of General, Inorganic and Theoretical Chemistry
      University of Innsbruck
      Innrain 80/82
      A-6020 Innsbruck
      Austria
;
_publ_section_title
;
 Chemoselective, Practical Synthesis of Cobaltocenium Carboxylic Acid
 Hexafluorophosphate
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1152
_journal_paper_doi               10.1021/om401120h
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C11 H10 Co O2, F6 P'
_chemical_formula_sum            'C11 H10 Co F6 O2 P'
_chemical_formula_weight         378.09
_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                98.896(2)
_cell_angle_beta                 100.238(2)
_cell_angle_gamma                92.907(2)
_cell_formula_units_Z            2
_cell_length_a                   7.0403(2)
_cell_length_b                   7.7380(2)
_cell_length_c                   12.3152(4)
_cell_measurement_reflns_used    7692
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.0
_cell_volume                     650.17(3)
_computing_data_collection       COLLECT
_computing_data_reduction        'DENZO and SCALEPACK'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      243(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi- and omega 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  0.0209
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4915
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         1.70
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.516
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.931
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.012(3)
_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   1.076
_refine_ls_hydrogen_treatment    'refined isotropically with bond restraints'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         2939
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0406P)^2^+0.3482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0878
_reflns_number_gt                2598
_reflns_number_total             2939
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om401120h_si_002.cif
_cod_data_source_block           5
_cod_database_code               4082689