A one-pot Garratt‒Braverman cyclization and Scholl oxidation route to acene‒helicene hybrids
Mitra, Tapobrata; Das, Joyee; Maji, Manasi; Das, Ranjita; Das, Uttam Kumar; Chattaraj, Pratim K.; Basak, Amit; RSC Advances 3 (2013) 19844–; doi:10.1039/c3ra42696c

data_7239130
_publ_section_title
;
 A one-pot Garratt--Braverman cyclization and Scholl oxidation route to
 acene--helicene hybrids
;
_journal_issue                   43
_journal_name_full               'RSC Advances'
_journal_page_first              19844
_journal_paper_doi               10.1039/c3ra42696c
_journal_volume                  3
_journal_year                    2013
_chemical_formula_sum            'C45.33 H26.67 O2.67 S1.33'
_chemical_formula_weight         656.75
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        '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                83.409(9)
_cell_angle_beta                 64.951(9)
_cell_angle_gamma                65.669(8)
_cell_formula_units_Z            3
_cell_length_a                   14.159(4)
_cell_length_b                   14.219(4)
_cell_length_c                   15.690(4)
_cell_measurement_temperature    293(2)
_cell_volume                     2600.7(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.926
_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  0.2394
_diffrn_reflns_av_sigmaI/netI    0.4396
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35608
_diffrn_reflns_theta_full        28.58
_diffrn_reflns_theta_max         28.58
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    0.154
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.752
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         12282
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.933
_refine_ls_R_factor_all          0.4118
_refine_ls_R_factor_gt           0.1252
_refine_ls_shift/su_max          0.303
_refine_ls_shift/su_mean         0.033
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1380P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2441
_refine_ls_wR_factor_ref         0.3794
_reflns_number_gt                2739
_reflns_number_total             12282
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ra42696c.txt
_cod_data_source_block           shelxl
_cod_original_cell_volume        2600.7(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7239130