Rh(iii)-catalyzed synthesis of tetracyclic isoquinolinium salts via C‒H activation and [4+2] annulation of 1-phenyl-3,4-dihydroisoquinolines and alkynes in ethanol
Dang, Xinxin; He, Yu; Liu, Yingtian; Chen, Xuehong; Li, Jun-Long; Zhou, Xian-Li; Jiang, Hezhong; Li, Jiahong; RSC Advances 8 (2018) 30050–; doi:10.1039/C8RA05443F

data_7231435
_publ_section_title
;
 Rh(iii)-catalyzed synthesis of tetracyclic isoquinolinium salts via C--H
 activation and [4+2] annulation of 1-phenyl-3,4-dihydroisoquinolines and
 alkynes in ethanol
;
_journal_issue                   52
_journal_name_full               'RSC Advances'
_journal_page_first              30050
_journal_paper_doi               10.1039/C8RA05443F
_journal_volume                  8
_journal_year                    2018
_chemical_formula_sum            'C34 H28 F3 N O5'
_chemical_formula_weight         587.57
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-03-12 deposited with the CCDC.
2018-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                87.958(5)
_cell_angle_beta                 74.654(5)
_cell_angle_gamma                70.533(5)
_cell_formula_units_Z            2
_cell_length_a                   10.8707(6)
_cell_length_b                   12.3194(7)
_cell_length_c                   13.1341(8)
_cell_measurement_reflns_used    3115
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.4330
_cell_measurement_theta_min      3.4900
_cell_volume                     1596.57(17)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11669
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.020
_diffrn_reflns_theta_max         25.020
_diffrn_reflns_theta_min         2.993
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93467
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            WHITE
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         5615
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0952
_refine_ls_R_factor_gt           0.0619
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1199P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1870
_refine_ls_wR_factor_ref         0.2164
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3642
_reflns_number_total             5615
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra05443f2.cif
_cod_data_source_block           171216_s1_dxx_sq
_cod_original_cell_volume        1596.56(17)
_cod_database_code               7231435
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.968
_shelx_estimated_absorpt_t_max   0.977
_shelx_res_checksum              69723
_shelx_fab_checksum              32636