State- and water repellency-controllable molecular glass of pillar[5]arenes with fluoroalkyl groups by guest vapors
Onishi, Katsuto; Ohtani, Shunsuke; Kato, Kenichi; Fa, Shixin; Sakata, Yoko; Akine, Shigehisa; Ogasawara, Moe; Asakawa, Hitoshi; Nagano, Shusaku; Takashima, Yoshinori; Mizuno, Motohiro; Ogoshi, Tomoki; Chemical Science  (2022) –; doi:10.1039/D2SC00828A

data_1566627
_publ_section_title
;
 State- and water repellency-controllable molecular glass of
 pillar[5]arenes with fluoroalkyl groups by guest vapors
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC00828A
_journal_year                    2022
_chemical_formula_moiety         C91H94F50O10
_chemical_formula_sum            'C91 H94 F50 O10'
_chemical_formula_weight         2297.66
_chemical_name_common            pillar[5]arene-(C3H6C2F5)10_hex
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-11-10 deposited with the CCDC.	2022-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                98.976(2)
_cell_angle_beta                 98.951(2)
_cell_angle_gamma                114.0170(17)
_cell_formula_units_Z            4
_cell_length_a                   20.9282(12)
_cell_length_b                   22.7403(13)
_cell_length_c                   24.2682(14)
_cell_measurement_reflns_used    151621
_cell_measurement_temperature    90
_cell_measurement_theta_max      67.078
_cell_measurement_theta_min      2.193
_cell_volume                     10108.6(10)
_computing_cell_refinement       'SAINT V8.37A/APEX3 (Bruker AXS Inc., 2015)'
_computing_data_collection       'Bruker Instrument Service V4.2.9 '
_computing_data_reduction        'SAINT V8.37A/APEX3 (Bruker AXS Inc., 2015)'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  ORTEP-3
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_av_unetI/netI     0.0710
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            151621
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.078
_diffrn_reflns_theta_max         67.078
_diffrn_reflns_theta_min         2.193
_diffrn_source                   'fine-focus rotating anode'
_exptl_absorpt_coefficient_mu    1.432
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5275
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Sheldrick, 1996 / Bruker AXS)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             4680
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3378
_refine_ls_number_reflns         35639
_refine_ls_number_restraints     3622
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0784
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1076P)^2^+12.5996P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2190
_refine_ls_wR_factor_ref         0.2370
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27431
_reflns_number_total             35639
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00828a3.cif
_cod_data_source_block           ogoshi047
_cod_database_code               1566627
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.535
_shelx_estimated_absorpt_t_max   0.906
_shelx_res_checksum              53931
_shelx_hkl_checksum              69428