Direct Access to Fluorene by Successive C–O/C–H Bond Activations of 2-Phenylbenzyl Ester
Hirano, Masafumi; Kawazu, Sosuke; Komine, Nobuyuki; Organometallics 33 (2014) 1921–; doi:10.1021/om5001869

data_4083032
_publ_section_title
;
 Direct Access to Fluorene by Successive C--O/C--H Bond Activations of
 2-Phenylbenzyl Ester
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1921
_journal_paper_doi               10.1021/om5001869
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C43 H40 F3 O2.50 P2 Pd'
_chemical_formula_sum            'C43 H40 F3 O2.5 P2 Pd'
_chemical_formula_weight         822.13
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_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
_cell_angle_alpha                90.0000
_cell_angle_beta                 93.720(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   13.5362(7)
_cell_length_b                   15.1262(6)
_cell_length_c                   18.9707(9)
_cell_measurement_reflns_used    11206
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.02
_cell_volume                     3876.1(3)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30571
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.613
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_correction_T_min  0.857
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1684.00
_exptl_crystal_size_max          0.396
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.106
_refine_diff_density_max         1.590
_refine_diff_density_min         -7.620
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     451
_refine_ls_number_reflns         8857
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0738
_refine_ls_shift/su_max          0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1093P)^2^+17.7762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2091
_reflns_number_gt                7509
_reflns_number_total             8857
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om5001869_si_002.cif
_cod_data_source_block           Complex_2
_cod_depositor_comments          'Adding full bibliography for 4083032.cif.'
_cod_original_cell_volume        3876.1(4)
_cod_original_formula_sum        'C43 H40 F3 O2.50 P2 Pd'
_cod_database_code               4083032