Cobalt-Catalyzed gem-Cross-Dimerization of Terminal Alkynes
Chen, Jia-Feng; Li, Changkun; ACS Catalysis  (2020) 3881–; doi:10.1021/acscatal.9b05078

data_4517483
_publ_section_title
;
 Cobalt-Catalyzed gem-Cross-Dimerization of Terminal Alkynes
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              3881
_journal_paper_doi               10.1021/acscatal.9b05078
_journal_year                    2020
_chemical_formula_moiety         'C54 H47 Co O4 P3, 0.5(C6 H14), C4 H4 O'
_chemical_formula_sum            'C61 H58 Co O5 P3'
_chemical_formula_weight         1022.91
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 109.52
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2940(8)
_cell_length_b                   15.9747(8)
_cell_length_c                   22.8893(12)
_cell_measurement_reflns_used    9708
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.76
_cell_measurement_theta_min      3.07
_cell_volume                     5270.8(5)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_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  0.0452
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            161641
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.787
_diffrn_reflns_theta_min         3.065
_exptl_absorpt_coefficient_mu    3.801
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       block
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_transmission_factor_max   0.7531
_exptl_transmission_factor_min   0.6457
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         9729
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0711P)^2^+2.2563P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1138
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8979
_reflns_number_total             9729
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs9b05078_si_002.cif
_cod_data_source_block           ta_a
_cod_original_cell_volume        5270.9(5)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4517483
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.517
_shelx_estimated_absorpt_t_max   0.517
_shelx_res_checksum              54655
_shelx_hkl_checksum              69367