Cobalt-Mediated η5-Pentadienyl/Alkyne [5 + 2] Cycloaddition. Synthesis and Characterization of Unbridged η2,η3-Coordinated Cycloheptadienyl Complexes
Ross D. Witherell; Kai E. O. Ylijoki; Jeffrey M. Stryker; Journal of the American Chemical Society 130 (2008) 2176–2177; doi:10.1021/ja710568d

data_4107447
_publ_section_title
;
 Cobalt-Mediated \h5-Pentadienyl/Alkyne [5 + 2] Cycloaddition. Synthesis
 and Characterization of Unbridged \h2,\h3-Coordinated Cycloheptadienyl
 Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2176
_journal_page_last               2177
_journal_paper_doi               10.1021/ja710568d
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C18 H26 Co, F6 P'
_chemical_formula_sum            'C18 H26 Co F6 P'
_chemical_formula_weight         446.29
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 91.863(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.3594(14)
_cell_length_b                   8.5903(10)
_cell_length_c                   17.871(2)
_cell_measurement_reflns_used    5143
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.87
_cell_measurement_theta_min      2.28
_cell_volume                     1896.4(4)
_computing_cell_refinement       'Bruker SAINT (Bruker, 1997)'
_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector'
_diffrn_measurement_method       '\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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21432
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.045
_exptl_absorpt_correction_T_max  0.8676
_exptl_absorpt_correction_T_min  0.7049
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2002)'
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_description       prism
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.975
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         21432
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0617
_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^)+(0.0959P)^2^+1.4884P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1809
_refine_ls_wR_factor_ref         0.1929
_reflns_number_gt                14851
_reflns_number_total             21432
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja710568d-file001_1.cif
_cod_data_source_block           jms0435
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4107447