Palladium-Catalyzed Aryne Insertion/Arene Dearomatization Domino Reaction: A Highly Chemoselective Route to Spirofluorenes
Zuo, Zhijun; Wang, Hui; Diao, Yunxia; Ge, Yicong; Liu, Jingjing; Luan, Xinjun; ACS Catalysis 8 (2018) 11029–; doi:10.1021/acscatal.8b03655

data_4515773
_publ_section_title
;
 Palladium-Catalyzed Aryne Insertion/Arene Dearomatization Domino
 Reaction: A Highly Chemoselective Route to Spirofluorenes
;
_journal_issue                   12
_journal_name_full               'ACS Catalysis'
_journal_page_first              11029
_journal_paper_doi               10.1021/acscatal.8b03655
_journal_volume                  8
_journal_year                    2018
_chemical_formula_sum            'C30 H28 O4'
_chemical_formula_weight         452.52
_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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                114.466(6)
_cell_angle_beta                 95.343(7)
_cell_angle_gamma                108.732(7)
_cell_formula_units_Z            2
_cell_length_a                   9.097(4)
_cell_length_b                   12.191(5)
_cell_length_c                   13.111(5)
_cell_measurement_reflns_used    1343
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.66
_cell_measurement_theta_min      3.14
_cell_volume                     1209.5(9)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6069
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         25.099
_diffrn_reflns_theta_min         1.948
_exptl_absorpt_coefficient_mu    0.081
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_description       block
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.357
_exptl_crystal_size_mid          0.249
_exptl_crystal_size_min          0.133
_refine_diff_density_max         0.158
_refine_diff_density_min         -0.185
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         4259
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0508
_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^)+(0.0837P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1369
_refine_ls_wR_factor_ref         0.1579
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2725
_reflns_number_total             4259
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b03655_si_003.cif
_cod_data_source_block           xb8970_0m
_cod_original_cell_volume        1209.5(8)
_cod_database_code               4515773
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.972
_shelx_estimated_absorpt_t_max   0.989
_shelx_res_checksum              35605
_shelx_hkl_checksum              34917