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_4515774
_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            'C26 H20 O2'
_chemical_formula_weight         364.42
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.141(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.157(3)
_cell_length_b                   12.525(2)
_cell_length_c                   12.945(3)
_cell_measurement_reflns_used    646
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      17.37
_cell_measurement_theta_min      2.28
_cell_volume                     1970.7(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0712
_diffrn_reflns_av_sigmaI/netI    0.0925
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9830
_diffrn_reflns_theta_full        25.09
_diffrn_reflns_theta_max         25.09
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_T_max  0.9899
_exptl_absorpt_correction_T_min  0.9740
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_density_meas      1.220
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.193
_refine_diff_density_min         -0.160
_refine_diff_density_rms         0.036
_refine_ls_extinction_coef       0.0069(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         3515
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.1588
_refine_ls_R_factor_gt           0.0614
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0587P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1272
_refine_ls_wR_factor_ref         0.1691
_reflns_number_gt                1536
_reflns_number_total             3515
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs8b03655_si_002.cif
_cod_data_source_block           xb0554_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        1970.8(7)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4515774