Band gap of carbon-sulfur [N]helicenes.
Miyasaka, Makoto; Pink, Maren; Olankitwanit, Arnon; Rajca, Suchada; Rajca, Andrzej; Organic letters 14 (2012) 3076–3079; doi:10.1021/ol3011437

data_1507823
_publ_section_title
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 Band gap of carbon-sulfur [N]helicenes.
;
_journal_issue                   12
_journal_name_full               'Organic letters'
_journal_page_first              3076
_journal_page_last               3079
_journal_paper_doi               10.1021/ol3011437
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         'C36 H34 S9'
_chemical_formula_sum            'C36 H34 S9'
_chemical_formula_weight         755.17
_chemical_name_systematic
; 
 ? 
;
_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                118.11
_cell_angle_beta                 94.13
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.315
_cell_length_b                   18.860
_cell_length_c                   20.017
_cell_measurement_reflns_used    9424
_cell_measurement_temperature    95(2)
_cell_measurement_theta_max      16.0
_cell_measurement_theta_min      2.2
_cell_volume                     3755.202
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2008)'
_computing_publication_material  'SHELXTL (Bruker, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      95(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.889
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measurement_details
'0.5 degree frames measured for 2 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'silicon  1 1 1 and 3 1 1'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.43321
_diffrn_reflns_av_R_equivalents  0.0958
_diffrn_reflns_av_sigmaI/netI    0.0966
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22633
_diffrn_reflns_theta_full        15.86
_diffrn_reflns_theta_max         15.86
_diffrn_reflns_theta_min         0.71
_exptl_absorpt_coefficient_mu    0.287
_exptl_absorpt_correction_T_max  0.9971
_exptl_absorpt_correction_T_min  0.9747
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing; 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.455
_refine_diff_density_min         -1.681
_refine_diff_density_rms         0.279
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     815
_refine_ls_number_reflns         14048
_refine_ls_number_restraints     328
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1463
_refine_ls_R_factor_gt           0.1158
_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^)+(0.1481P)^2^+122.7870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3485
_refine_ls_wR_factor_ref         0.3843
_reflns_number_gt                10581
_reflns_number_total             14048
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol3011437_si_002.cif
_cod_data_source_block
;cmc0586_
Explanation for Alert A:
PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.889
The coverage is low (88%) due to a substantial fall of in scattering at high resolution, which is likely due to crystal quality and size.  The remaining electron density is reasonable for the structure.  The R-values are high, yet the connectivity of the molecule is unambiguously established.
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_cod_depositor_comments          'Adding full bibliography for 1507823.cif.'
_cod_original_cell_volume        3755.3
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1507823