Two-in-One Strategy for Fluorene-Based Spirocycles via Pd(0)-Catalyzed Spiroannulation of o-Iodobiaryls with Bromonaphthols
Tan, Bojun; Liu, Long; Zheng, Huayu; Cheng, Tianyi; Zhu, Dianhu; Yang, Xiaofeng; Luan, Xinjun; Chemical Science  (2020) –; doi:10.1039/D0SC04386A

data_1559008
_publ_section_title
;
 Two-in-One Strategy for Fluorene-Based Spirocycles via Pd(0)-Catalyzed
 Spiroannulation of o-Iodobiaryls with Bromonaphthols
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC04386A
_journal_year                    2020
_chemical_formula_sum            'C24 H18 O'
_chemical_formula_weight         322.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-06-17 deposited with the CCDC.	2020-09-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.729(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.083(12)
_cell_length_b                   9.001(4)
_cell_length_c                   13.882(6)
_cell_measurement_reflns_used    1640
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.40
_cell_measurement_theta_min      2.37
_cell_volume                     3530(3)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8583
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.096
_diffrn_reflns_theta_max         25.096
_diffrn_reflns_theta_min         1.442
_exptl_absorpt_coefficient_mu    0.072
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.367
_exptl_crystal_size_mid          0.285
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.191
_refine_diff_density_min         -0.192
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         3130
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0676P)^2^+1.0715P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1405
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2136
_reflns_number_total             3130
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc04386a2.cif
_cod_data_source_block           xb9728_0m
_cod_original_cell_volume        3530(2)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1559008
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.974
_shelx_estimated_absorpt_t_max   0.985
_shelx_res_checksum              8970