Highly Chemo- and Regioselective Construction of Spirocarbocycles by a Pd(0)-Catalyzed Dearomatization of Phenol-Based Biaryls with 1,3-Dienes.
Luo, Lei; Zheng, Huayu; Liu, Jingjing; Wang, Hui; Wang, Yaoyu; Luan, Xinjun; Organic letters 18 (2016) 2082–2085; doi:10.1021/acs.orglett.6b00710

data_1543160
_publ_section_title
;
 Highly Chemo- and Regioselective Construction of Spirocarbocycles by a
 Pd(0)-Catalyzed Dearomatization of Phenol-Based Biaryls with 1,3-Dienes.
;
_journal_issue                   9
_journal_name_full               'Organic letters'
_journal_page_first              2082
_journal_page_last               2085
_journal_paper_doi               10.1021/acs.orglett.6b00710
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C26 H20 O'
_chemical_formula_weight         348.42
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.156(12)
_cell_angle_beta                 93.240(12)
_cell_angle_gamma                91.754(12)
_cell_formula_units_Z            4
_cell_length_a                   8.800(6)
_cell_length_b                   10.295(7)
_cell_length_c                   21.034(14)
_cell_measurement_reflns_used    1880
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.77
_cell_measurement_theta_min      2.22
_cell_volume                     1902(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_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  0.0548
_diffrn_reflns_av_sigmaI/netI    0.1234
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9323
_diffrn_reflns_theta_full        25.51
_diffrn_reflns_theta_max         25.51
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  0.9928
_exptl_absorpt_correction_T_min  0.9899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         6752
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.1769
_refine_ls_R_factor_gt           0.1107
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2980
_refine_ls_wR_factor_ref         0.3445
_reflns_number_gt                3218
_reflns_number_total             6752
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol6b00710_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 1543160.cif.

2019-02-17
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C52 H40 O2'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     696.84
_cod_database_code               1543160