Iridium(I)-Catalyzed Intramolecular Cycloisomerization of Enynes: Scope and Mechanistic Course
Fernández, David F.; Rodrigues, Catarina A. B.; Calvelo, Martín; Gulías, Moisés; Mascareñas, José L.; López, Fernando; ACS Catalysis 8 (2018) 7397–; doi:10.1021/acscatal.8b02139

data_4515561
_publ_section_title
;
 Iridium(I)-Catalyzed Intramolecular Cycloisomerization of Enynes: Scope
 and Mechanistic Course
;
_journal_issue                   8
_journal_name_full               'ACS Catalysis'
_journal_page_first              7397
_journal_paper_doi               10.1021/acscatal.8b02139
_journal_volume                  8
_journal_year                    2018
_chemical_formula_sum            'C22 H23 N O2'
_chemical_formula_weight         333.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 110.254(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2561(9)
_cell_length_b                   9.8925(7)
_cell_length_c                   15.8384(11)
_cell_measurement_temperature    100(2)
_cell_volume                     1801.6(2)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            72598
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.117
_diffrn_reflns_theta_min         1.771
_exptl_absorpt_coefficient_mu    0.078
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.494
_exptl_crystal_size_mid          0.189
_exptl_crystal_size_min          0.112
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         6310
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0498P)^2^+0.7052P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1271
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4516
_reflns_number_total             6310
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b02139_si_002.cif
_cod_data_source_block           18MCD004
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4515561
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.962
_shelx_estimated_absorpt_t_max   0.991
_shelx_res_checksum              98549
_shelx_hkl_checksum              82857