Synthesis of Functionalized Dioxa-aza[7]helicenes Using Palladium Catalyzed Arylations.
Kelgtermans, Hans; Dobrzańska, Liliana; Meervelt, Luc Van; Dehaen, Wim; Organic letters 14 (2012) 1500–1503; doi:10.1021/ol300236t

data_1507172
_publ_section_title
;
 Synthesis of Functionalized Dioxa-aza[7]helicenes Using Palladium
 Catalyzed Arylations.
;
_journal_issue                   6
_journal_name_full               'Organic letters'
_journal_page_first              1500
_journal_page_last               1503
_journal_paper_doi               10.1021/ol300236t
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         'C30 H17 N O2'
_chemical_formula_sum            'C30 H17 N O2'
_chemical_formula_weight         423.45
_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                79.838(4)
_cell_angle_beta                 83.351(4)
_cell_angle_gamma                74.729(4)
_cell_formula_units_Z            2
_cell_length_a                   8.3210(5)
_cell_length_b                   9.3857(6)
_cell_length_c                   13.8217(7)
_cell_measurement_reflns_used    1753
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      70.73
_cell_measurement_theta_min      3.257
_cell_volume                     1022.27(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Bruker SMART 6000'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  'crossed G\"obel mirrors'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0596
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4530
_diffrn_reflns_theta_full        68.00
_diffrn_reflns_theta_max         70.84
_diffrn_reflns_theta_min         3.26
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.683
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.202
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.895
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         3753
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.895
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0624P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1140
_reflns_number_gt                2539
_reflns_number_total             3753
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol300236t_si_001.cif
_cod_data_source_block           I
_cod_original_cell_volume        1022.27(10)
_cod_database_code               1507172