Highly Selective Separation of Isopropylbenzene and α-Methylstyrene by Nonporous Adaptive Crystals of Perbromoethylated Pillararene via Vapor- and Liquid-Phase Adsorptions.
Zhu, Weijie; Li, Errui; Huang, Feihe; ACS applied materials & interfaces 13 (2021) 7370–7376; doi:10.1021/acsami.0c23059

data_4518488
_publ_section_title
;
 Highly Selective Separation of Isopropylbenzene and \a-Methylstyrene by
 Nonporous Adaptive Crystals of Perbromoethylated Pillararene via Vapor-
 and Liquid-Phase Adsorptions.
;
_journal_issue                   6
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              7370
_journal_page_last               7376
_journal_paper_doi               10.1021/acsami.0c23059
_journal_volume                  13
_journal_year                    2021
_chemical_formula_moiety         'C66 H84 O12, C9 H12'
_chemical_formula_sum            'C75 H96 O12'
_chemical_formula_weight         1189.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 113.997(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.5513(10)
_cell_length_b                   22.9120(19)
_cell_length_c                   14.5522(12)
_cell_measurement_reflns_used    1464
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      55.456
_cell_measurement_theta_min      3.858
_cell_volume                     3823.1(6)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.0748
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14919
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.150
_diffrn_reflns_theta_min         1.928
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.547
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.6235
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0780 before and 0.0515 after correction. The Ratio of minimum to maximum transmission is 0.8277. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.033
_exptl_crystal_description       block
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.863
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     428
_refine_ls_number_reflns         7029
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      0.861
_refine_ls_R_factor_all          0.1973
_refine_ls_R_factor_gt           0.1173
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2695
_refine_ls_wR_factor_ref         0.3276
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2987
_reflns_number_total             7029
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am0c23059_si_002.cif
_cod_data_source_block           cu_191130zwj_0m
_cod_depositor_comments
'Adding full bibliography for 4518485--4518488.cif.'
_cod_database_code               4518488
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.908
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C41-C40
 1.53 with sigma of 0.02
 C42-C41 = C41-C43
 1.53 with sigma of 0.02
 C42-C43
 2.44 with sigma of 0.02
 C42-C40
 2.35 with sigma of 0.02
 C43-C40
 2.35 with sigma of 0.02
 C35-C41 \\sim C41-C39
 with sigma of 0.02
3. Restrained planarity
 C35, C36, C37, C38, C39, C40, C41
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
O2 \\sim O4 \\sim O6 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim
C40 \\sim C41: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim
C43: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: H1A(0.5) H1B(0.5) H22A(0.5) H22B(0.5) C40(0.5) C35(0.5) H35(0.5)
 C36(0.5) H36(0.5) C37(0.5) H37(0.5) C38(0.5) H38(0.5) C39(0.5) H39(0.5)
 C41(0.5) H41(0.5) C42(0.5) H42A(0.5) H42B(0.5) H42C(0.5) C43(0.5) H43A(0.5)
 H43B(0.5) H43C(0.5)
6.a Ternary CH refined with riding coordinates:
 C41(H41)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C15(H15A,H15B), C22(H22A,H22B), C23(H23A,H23B),
 C25(H25A,H25B), C27(H27A,H27B), C29(H29A,H29B), C31(H31A,H31B), C33(H33A,H33B)
6.c Me refined with riding coordinates:
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C)
6.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C10(H10), C13(H13), C17(H17), C20(H20), C35(H35), C36(H36),
 C37(H37), C38(H38), C39(H39)
6.e Fitted hexagon refined as free rotating group:
 C40(C35,C36,C37,C38,C39)
6.f Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C30(H30A,H30B,
 H30C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              31408
_shelx_hkl_checksum              24813
_olex2_submission_special_instructions 'No special instructions were received'