Coumarin-Annelated Regioisomeric Heptahelicenes: Influence of Helicity on Excited-State Properties and Chiroptical Properties.
Mukhopadhyay, Arindam; Jana, Kanyashree; Hossen, Tousif; Sahu, Kalyanasis; Moorthy, Jarugu Narasimha; The Journal of organic chemistry 84 (2019) 10658–10668; doi:10.1021/acs.joc.9b01126

data_4033879
_publ_section_title
;
 Coumarin-Annelated Regioisomeric Heptahelicenes: Influence of Helicity on
 Excited-State Properties and Chiroptical Properties.
;
_journal_issue                   17
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              10658
_journal_page_last               10668
_journal_paper_doi               10.1021/acs.joc.9b01126
_journal_volume                  84
_journal_year                    2019
_chemical_formula_moiety         'C29 H16 O2, 0.5(C H Cl3)'
_chemical_formula_sum            'C29.5 H16.5 Cl1.5 O2'
_chemical_formula_weight         456.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 96.334(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.1609(10)
_cell_length_b                   9.9347(8)
_cell_length_c                   34.851(3)
_cell_measurement_reflns_used    5579
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.384
_cell_measurement_theta_min      2.133
_cell_volume                     4184.8(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1418
_diffrn_reflns_av_unetI/netI     0.1337
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            60581
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.384
_diffrn_reflns_theta_min         2.133
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.274
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.107
_refine_diff_density_min         -1.081
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         10453
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.2358
_refine_ls_R_factor_gt           0.1441
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0882P)^2^+44.2972P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3355
_refine_ls_wR_factor_ref         0.3741
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5579
_reflns_number_total             10453
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b01126_si_006.cif
_cod_data_source_block           7-out
_cod_depositor_comments
;

2020-04-04
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_moiety     '2(C29 H16 O2), C H Cl3'
_cod_original_formula_sum        'C59 H33 Cl3 O4'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     912.20
_cod_database_code               4033879
_shelx_shelxl_version_number     2014/7