Protonation of Cobalt−Allene Constitutional Isomers: Highly Selective Formation of Cobalt−Allyl and Oxacobaltacyclopentadiene Complexes
O’Connor, Joseph M.; Chen, Ming-Chou; Holland, Ryan L.; Organometallics 29 (2010) 6161–; doi:10.1021/om100701e

data_4066903
_publ_section_title
;
 Protonation of Cobalt&#x2212;Allene Constitutional Isomers: Highly
 Selective Formation of Cobalt&#x2212;Allyl and Oxacobaltacyclopentadiene
 Complexes
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6161
_journal_paper_doi               10.1021/om100701e
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C38 H37 Co F3 O7 P S'
_chemical_formula_weight         784.64
_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                 105.16
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.805
_cell_length_b                   16.209
_cell_length_c                   15.207
_cell_measurement_temperature    100(2)
_cell_volume                     3522.291
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'Bruker APEX 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  0.0208
_diffrn_reflns_av_sigmaI/netI    0.0194
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6443
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.67
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.658
_exptl_absorpt_correction_T_max  0.8907
_exptl_absorpt_correction_T_min  0.7561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.0002(2)
_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   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         6195
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0473P)^2^+3.9600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.0985
_reflns_number_gt                5417
_reflns_number_total             6195
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100701e_si_003.cif
_cod_data_source_block           Chen4
_cod_original_cell_volume        3522.3
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4066903