pseudo[1]Catenane-Type Pillar[5]thiacrown Whose Planar Chiral Inversion is Triggered by Metal Cation and Controlled by Anion.
Lee, Eunji; Ju, Huiyeong; Park, In-Hyeok; Jung, Jong Hwa; Ikeda, Mari; Kuwahara, Shunsuke; Habata, Yoichi; Lee, Shim Sung; Journal of the American Chemical Society 140 (2018) 9669–9677; doi:10.1021/jacs.8b05751

data_4132707
_publ_section_title
;
 pseudo[1]Catenane-Type Pillar[5]thiacrown Whose Planar Chiral Inversion
 is Triggered by Metal Cation and Controlled by Anion.
;
_journal_issue                   30
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9669
_journal_page_last               9677
_journal_paper_doi               10.1021/jacs.8b05751
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C53 H64 Cl2 Hg O20 S2'
_chemical_formula_weight         1356.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 91.173(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.9151(9)
_cell_length_b                   9.0545(5)
_cell_length_c                   22.8476(13)
_cell_measurement_reflns_used    9911
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.87
_cell_measurement_theta_min      2.56
_cell_volume                     3291.7(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0466
_diffrn_reflns_av_unetI/netI     0.0752
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            35461
_diffrn_reflns_point_group_measured_fraction_full 0.889
_diffrn_reflns_point_group_measured_fraction_max 0.876
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.545
_exptl_absorpt_coefficient_mu    2.547
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.080
_exptl_transmission_factor_max   0.7457
_exptl_transmission_factor_min   0.5910
_refine_diff_density_max         1.076
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details
; 
 Flack x determined using 3215 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.031(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     662
_refine_ls_number_reflns         11338
_refine_ls_number_restraints     1066
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0826P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1305
_refine_ls_wR_factor_ref         0.1351
_reflns_Friedel_coverage         0.642
_reflns_Friedel_fraction_full    0.763
_reflns_Friedel_fraction_max     0.734
_reflns_number_gt                9761
_reflns_number_total             11338
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b05751_si_002.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4132707
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.429
_shelx_estimated_absorpt_t_max   0.822