Rh(iii)-catalyzed highly site- and regio-selective alkenyl C-H activation/annulation of 4-amino-2-quinolones with alkynes <i>via</i> reversible alkyne insertion.
Hirako, Naohiro; Yasui, Takeshi; Yamamoto, Yoshihiko; Chemical science 14 (2023) 10971–10978; doi:10.1039/d3sc03987k

data_1569879
_publ_section_title
;
 Rh(iii)-catalyzed highly site- and regio-selective alkenyl C-H
 activation/annulation of 4-amino-2-quinolones with alkynes <i>via</i>
 reversible alkyne insertion.
;
_journal_issue                   39
_journal_name_full               'Chemical science'
_journal_page_first              10971
_journal_page_last               10978
_journal_paper_doi               10.1039/d3sc03987k
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C45 H27 Cl3 F12 N2 O2'
_chemical_formula_sum            'C45 H27 Cl3 F12 N2 O2'
_chemical_formula_weight         962.06
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2023-06-30 deposited with the CCDC.	2023-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                85.453(6)
_cell_angle_beta                 83.081(6)
_cell_angle_gamma                74.047(5)
_cell_formula_units_Z            2
_cell_length_a                   10.1061(11)
_cell_length_b                   14.1090(14)
_cell_length_c                   14.8443(15)
_cell_measurement_reflns_used    13523
_cell_measurement_temperature    123
_cell_measurement_theta_max      68.07
_cell_measurement_theta_min      3.00
_cell_volume                     2017.9(4)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2019)'
_computing_structure_refinement  'CRYSTALS (Carruthers, et al., 1999)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.1528
_diffrn_reflns_av_unetI/netI     0.1702
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23137
_diffrn_reflns_theta_full        67.68
_diffrn_reflns_theta_max         68.18
_diffrn_reflns_theta_min         3.002
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.946
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_correction_T_min  0.329
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             972.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.968
_refine_diff_density_min         -0.757
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     604
_refine_ls_number_reflns         4507
_refine_ls_R_factor_gt           0.1132
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0091Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.3232
_reflns_number_gt                2461
_reflns_number_total             7190
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d3sc03987k2.cif
_cod_data_source_block           NH-690-2
_cod_depositor_comments
'Adding full bibliography for 1569877--1569882.cif.'
_cod_database_code               1569879