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_7239131
_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            'C22 H16 N0 O2 S'
_chemical_formula_weight         344.41
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        '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                82.653(6)
_cell_angle_beta                 67.803(5)
_cell_angle_gamma                73.719(5)
_cell_formula_units_Z            4
_cell_length_a                   11.693(2)
_cell_length_b                   12.779(2)
_cell_length_c                   12.838(2)
_cell_measurement_temperature    293(2)
_cell_volume                     1704.4(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0813
_diffrn_reflns_av_sigmaI/netI    0.0903
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20319
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.202
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             720
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         5983
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1374
_refine_ls_R_factor_gt           0.0729
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0917P)^2^+0.4358P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1641
_refine_ls_wR_factor_ref         0.1990
_reflns_number_gt                3362
_reflns_number_total             5983
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ra42696c.txt
_cod_data_source_block           shelxl
_cod_database_code               7239131