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

data_4517484
_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_absolute_configuration ad
_chemical_formula_moiety         'C57 H43 Co O6 P3'
_chemical_formula_sum            'C57 H43 Co O6 P3'
_chemical_formula_weight         975.75
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1714(3)
_cell_length_b                   19.5049(5)
_cell_length_c                   22.2984(6)
_cell_measurement_reflns_used    9604
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      68.44
_cell_measurement_theta_min      4.43
_cell_volume                     4858.8(2)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_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  0.0521
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            82120
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.624
_diffrn_reflns_theta_min         3.010
_exptl_absorpt_coefficient_mu    4.118
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       block
_exptl_crystal_F_000             2020
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.220
_exptl_transmission_factor_max   0.1665
_exptl_transmission_factor_min   0.0555
_refine_diff_density_max         1.346
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
 Flack x determined using 3235 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.031(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         8732
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0683
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1403P)^2^+2.6889P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2013
_refine_ls_wR_factor_ref         0.2036
_reflns_Friedel_coverage         0.762
_reflns_Friedel_fraction_full    0.952
_reflns_Friedel_fraction_max     0.947
_reflns_number_gt                8345
_reflns_number_total             8732
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs9b05078_si_003.cif
_cod_data_source_block           a_a
_cod_database_code               4517484
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.438
_shelx_estimated_absorpt_t_max   0.464
_shelx_res_checksum              82625
_shelx_hkl_checksum              38195