Mechanical Stabilization of Helical Chirality in a Macrocyclic Oligothiophene.
Weiland, Kevin J.; Brandl, Thomas; Atz, Kenneth; Prescimone, Alessandro; Häussinger, Daniel; Šolomek, Tomáš; Mayor, Marcel; Journal of the American Chemical Society 141 (2019) 2104–2110; doi:10.1021/jacs.8b11797

data_4127939
_publ_section_title
;
 Mechanical Stabilization of Helical Chirality in a Macrocyclic
 Oligothiophene.
;
_journal_issue                   5
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2104
_journal_page_last               2110
_journal_paper_doi               10.1021/jacs.8b11797
_journal_volume                  141
_journal_year                    2019
_chemical_compound_source        'Kevin Weiland'
_chemical_formula_moiety         'C48 H52 O4 S4'
_chemical_formula_sum            'C48 H52 O4 S4'
_chemical_formula_weight         821.20
_chemical_melting_point          ?
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2018-05-22
_audit_creation_method           CRYSTALS_ver_14.61_build_6949
_cell_angle_alpha                95.895(3)
_cell_angle_beta                 91.044(3)
_cell_angle_gamma                117.920(3)
_cell_formula_units_Z            1
_cell_length_a                   7.6438(6)
_cell_length_b                   7.7858(6)
_cell_length_c                   19.8762(16)
_cell_measurement_reflns_used    9923
_cell_measurement_temperature    123
_cell_measurement_theta_max      71
_cell_measurement_theta_min      5
_cell_volume                     1036.72(14)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_av_unetI/netI     0.058
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12231
_diffrn_reflns_theta_full        68.000
_diffrn_reflns_theta_max         70.616
_diffrn_reflns_theta_min         2.241
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.454
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             436
_exptl_crystal_recrystallization_method
; 
DCM / EtOH
;
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.71
_refine_diff_density_min         -0.82
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0297
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3615
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0751
_refine_ls_shift/su_max          0.0008247
_refine_ls_shift/su_mean         0.0000447
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= 
 SQRT(W) = 1/(Data with the key SIGMA(/FO/) in list 6) 
;
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0587
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0586
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              9
_reflns_limit_k_min              -9
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                3432
_reflns_number_total             3671
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0722
_oxford_refine_ls_scale          0.18399(9)
_oxford_reflns_number_all        3653
_oxford_structure_analysis_title 'KW_W6_123K_0m in P-1'
_cod_data_source_file            ja8b11797_si_002.cif
_cod_data_source_block           KW_W6_123K
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        1036.71(14)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4127939
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)