Cobalt Fluorocarbenes: Cycloaddition Reactions with Tetrafluoroethylene and Reactivity of the Perfluorometallacyclic Products
Daniel J. Harrison; Graham M. Lee; Matthew C. Leclerc; Ilia Korobkov; R. Tom Baker; Journal of the American Chemical Society 135 (2013) 18296–18299; doi:10.1021/ja411503c

data_4121306
_publ_section_title
;
 Cobalt Fluorocarbenes: Cycloaddition Reactions with Tetrafluoroethylene
 and Reactivity of the Perfluorometallacyclic Products
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18296
_journal_page_last               18299
_journal_paper_doi               10.1021/ja411503c
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C36 H34 Co F8 P'
_chemical_formula_weight         708.53
_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                97.1850(10)
_cell_angle_beta                 95.6370(10)
_cell_angle_gamma                118.4360(10)
_cell_formula_units_Z            2
_cell_length_a                   11.8486(2)
_cell_length_b                   11.8713(2)
_cell_length_c                   13.5919(2)
_cell_measurement_reflns_used    9827
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      30.41
_cell_measurement_theta_min      2.50
_cell_volume                     1640.45(5)
_computing_cell_refinement       'APEX II, Bruker (2009)'
_computing_data_collection       'APEX II, Bruker (2009)'
_computing_data_reduction        'XPREP, Bruker (2009)'
_computing_molecular_graphics    'SHELXTL, Bruker (2004)'
_computing_publication_material  'SHELXTL, Bruker (2004)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0162
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            40888
_diffrn_reflns_theta_full        30.53
_diffrn_reflns_theta_max         30.53
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    0.642
_exptl_absorpt_correction_T_max  0.8987
_exptl_absorpt_correction_T_min  0.8611
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2003)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.139
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         9895
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0709P)^2^+0.6870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1230
_reflns_number_gt                8422
_reflns_number_total             9895
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja411503c_si_005.cif
_cod_data_source_block           tb038
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4121306