Direct Assembly of Polyarenes via C-C Coupling Using PIFA/BF3.Et2O
Enrico Faggi; Rosa M. Sebastián; Roser Pleixats; Adelina Vallribera; Alexandr Shafir; Alejandra Rodríguez-Gimeno; Carmen Ramírez de Arellano; Journal of the American Chemical Society 132 (2010) 17980–17982; doi:10.1021/ja107467c

data_4103712
_publ_contact_author_address
;
Departamento de Qu\'imica Org\'anica
Universidad de Valencia
46100 Valencia Spain
;
_publ_contact_author_email       Carmen.ramirezdearellano@uv.es
_publ_contact_author_fax         '+34 963544939'
_publ_contact_author_name        'C. Ram\'irez de Arellano'
_publ_contact_author_phone       '+34 963543046'
_publ_section_title
;
 Direct Assembly of Polyarenes via C-C Coupling Using PIFA/BF3.Et2O
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17980
_journal_page_last               17982
_journal_paper_doi               10.1021/ja107467c
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C38 H34'
_chemical_formula_weight         490.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 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                 106.87(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.806(2)
_cell_length_b                   9.6651(8)
_cell_length_c                   24.423(2)
_cell_measurement_reflns_used    14923
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      30.8013
_cell_measurement_theta_min      2.2634
_cell_volume                     5603.5(10)
_computing_cell_refinement       'CrysAlisPro (Oxford Diff., 2009)'
_computing_data_collection       'CrysAlisPro (Oxford Diff., 2009)'
_computing_data_reduction        'CrysAlisPro (Oxford Diff., 2009)'
_computing_molecular_graphics    'CrystalMaker 2.1.5 (1994-2009)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 16.0267
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\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  0.1170
_diffrn_reflns_av_sigmaI/netI    0.0830
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            118667
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.146
_refine_diff_density_min         -0.168
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.802
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         11450
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.802
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0440P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0900
_reflns_number_gt                6102
_reflns_number_total             11450
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja107467c_si_002.cif
_cod_data_source_block           ef203_Compund_2a
_cod_database_code               4103712