C-I···π Halogen Bonding Driven Supramolecular Helix of Bilateral N-Amidothioureas Bearing β-Turns.
Cao, Jinlian; Yan, Xiaosheng; He, Wenbin; Li, Xiaorui; Li, Zhao; Mo, Yirong; Liu, Maili; Jiang, Yun-Bao; Journal of the American Chemical Society 139 (2017) 6605–6610; doi:10.1021/jacs.6b13171

data_4125563
_publ_section_title
;
 C-I&#x00B7;&#x00B7;&#x00B7;\p Halogen Bonding Driven Supramolecular Helix
 of Bilateral N-Amidothioureas Bearing \b-Turns.
;
_journal_issue                   19
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6605
_journal_page_last               6610
_journal_paper_doi               10.1021/jacs.6b13171
_journal_volume                  139
_journal_year                    2017
_chemical_formula_sum            'C34 H46 Cl2 N8 O7 S5'
_chemical_formula_weight         909.99
_space_group_IT_number           4
_symmetry_cell_setting           &#x00A1;&#x00AF;monoclinic&#x00A1;&#x00AF;
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.742(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.1847(4)
_cell_length_b                   26.7032(9)
_cell_length_c                   9.8011(4)
_cell_measurement_reflns_used    2021
_cell_measurement_temperature    176(2)
_cell_measurement_theta_max      22.5360
_cell_measurement_theta_min      3.4490
_cell_volume                     2401.07(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      176(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_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  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0745
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            9306
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    0.401
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_refine_diff_density_max         2.644
_refine_diff_density_min         -0.992
_refine_diff_density_rms         0.138
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.21(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.296
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         6976
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.296
_refine_ls_R_factor_all          0.1461
_refine_ls_R_factor_gt           0.1263
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3341
_refine_ls_wR_factor_ref         0.3549
_reflns_number_gt                5136
_reflns_number_total             6976
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja6b13171_si_003.cif
_cod_data_source_block           p-sr
_cod_depositor_comments
'Adding full bibliography for 4125563--4125564.cif.'
_cod_original_sg_symbol_H-M      &#x00A1;&#x00AF;P2(1)&#x00A1;&#x00AF;
_cod_database_code               4125563