Cobalt-Catalyzed [2π + 2π] Cycloadditions of Alkenes: Scope, Mechanism, and Elucidation of Electronic Structure of Catalytic Intermediates.
Schmidt, Valerie A.; Hoyt, Jordan M.; Margulieux, Grant W.; Chirik, Paul J.; Journal of the American Chemical Society 137 (2015) 7903–7914; doi:10.1021/jacs.5b04034

data_4123825
_publ_section_title
;
 Cobalt-Catalyzed [2\p + 2\p] Cycloadditions of Alkenes: Scope, Mechanism,
 and Elucidation of Electronic Structure of Catalytic Intermediates.
;
_journal_issue                   24
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7903
_journal_page_last               7914
_journal_paper_doi               10.1021/jacs.5b04034
_journal_volume                  137
_journal_year                    2015
_chemical_formula_sum            'C41 H55 Co N6'
_chemical_formula_weight         690.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 100.562(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1752(5)
_cell_length_b                   15.4059(5)
_cell_length_c                   17.8232(5)
_cell_measurement_reflns_used    9688
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.71
_cell_measurement_theta_min      4.00
_cell_volume                     4366.2(2)
_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-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            42248
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.934
_diffrn_reflns_theta_min         3.394
_exptl_absorpt_coefficient_mu    3.313
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.4991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2014/2 (Bruker AXS)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.051
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.041
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         7684
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0646
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0362P)^2^+9.6007P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1388
_refine_ls_wR_factor_ref         0.1485
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6493
_reflns_number_total             7684
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b04034_si_002.cif
_cod_data_source_block           vas5_4pyrriPrPDICoN2
_cod_depositor_comments
'Adding full bibliography for 4123821--4123825.cif.'
_cod_database_code               4123825
_shelxl_version_number           2014-3
_shelx_res_checksum              10649
_shelx_hkl_checksum              58985
_shelx_fab_checksum              38