Synthesis and Structural Features of Quadruple Helicenes: Highly Distorted π Systems Enabled by Accumulation of Helical Repulsions.
Fujikawa, Takao; Segawa, Yasutomo; Itami, Kenichiro; Journal of the American Chemical Society 138 (2016) 3587–3595; doi:10.1021/jacs.6b01303

data_4130212
_publ_section_title
;
 Synthesis and Structural Features of Quadruple Helicenes: Highly
 Distorted \p Systems Enabled by Accumulation of Helical Repulsions.
;
_journal_issue                   10
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3587
_journal_page_last               3595
_journal_paper_doi               10.1021/jacs.6b01303
_journal_volume                  138
_journal_year                    2016
_chemical_formula_sum            'C66 H56 S4'
_chemical_formula_weight         977.35
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.951(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.2313(19)
_cell_length_b                   12.0935(11)
_cell_length_c                   25.119(3)
_cell_measurement_reflns_used    8804
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_cell_volume                     5007.1(9)
_computing_cell_refinement       'RIGAKU CrystalClear'
_computing_data_collection       'RIGAKU CrystalClear'
_computing_data_reduction        'RIGAKU CrystalClear'
_computing_molecular_graphics    ORTEP-III
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
;
PILATUS 200K with MicroMax-007
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  graphite
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_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
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_diffrn_reflns_number            67832
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_exptl_absorpt_coefficient_mu    0.233
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_exptl_absorpt_correction_T_min  0.9548
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
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_refine_diff_density_max         1.065
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     680
_refine_ls_number_reflns         8788
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+6.7181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1275
_reflns_number_gt                6847
_reflns_number_total             8788
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja6b01303_si_002.cif
_cod_data_source_block           QH-B
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file
'/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/lists/replacement-tags.lst'.

Automatic conversion script
Id: cif_correct_tags 6909 2019-04-08 15:41:33Z antanas 

The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4130212