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_4518486
_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 H72 Br12 O12, C9 H12'
_chemical_formula_sum            'C75 H84 Br12 O12'
_chemical_formula_weight         2136.34
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                83.9386(8)
_cell_angle_beta                 75.6551(8)
_cell_angle_gamma                76.0824(7)
_cell_formula_units_Z            2
_cell_length_a                   13.9241(2)
_cell_length_b                   17.2403(2)
_cell_length_c                   17.6750(2)
_cell_measurement_reflns_used    9875
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      54.87
_cell_measurement_theta_min      3.29
_cell_volume                     3985.24(9)
_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      170.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            38865
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.876
_diffrn_reflns_theta_min         2.923
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.270
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.4944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0953 before and 0.0489 after correction. The Ratio of minimum to maximum transmission is 0.6585. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_description       block
_exptl_crystal_F_000             2100
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         3.088
_refine_diff_density_min         -2.306
_refine_diff_density_rms         0.138
_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     921
_refine_ls_number_reflns         14982
_refine_ls_number_restraints     104
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0677
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0823P)^2^+25.7344P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1727
_refine_ls_wR_factor_ref         0.1836
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12459
_reflns_number_total             14982
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am0c23059_si_004.cif
_cod_data_source_block           191102zwj_1_0m
_cod_depositor_comments
'Adding full bibliography for 4518485--4518488.cif.'
_cod_database_code               4518486
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.486
_shelx_estimated_absorpt_t_min   0.451
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C73-C67 = C75-C73 = C74-C73
 1.53 with sigma of 0.02
 H72-H74A
 2 with sigma of 0.02
 Br6-Br0A = Br0A-C31
 3 with sigma of 0.02
 Br0A-C31
 1.8 with sigma of 0.02
 Br1A-C53
 1.8 with sigma of 0.02
 Br0A-C30
 2.9 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C70 \\sim C67 \\sim C68 \\sim C72 \\sim C73 \\sim C69 \\sim C71 \\sim C74 \\sim
C75: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C53 \\sim Br1A \\sim Br10 \\sim C31 \\sim Br0A \\sim Br6: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
O6 \\sim C30 \\sim C31: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Others
 Fixed Sof: Br1(0.75) Br6(0.75) Br10(0.75) H1AA(0.75) H1AB(0.75) H1BC(0.25)
 H1BD(0.25) H31A(0.75) H31B(0.75) H31C(0.25) H31D(0.25) H53A(0.75) H53B(0.75)
 H53C(0.25) H53D(0.25) Br0A(0.25) Br2A(0.25) Br1A(0.25)
5.a Ternary CH refined with riding coordinates:
 C73(H73)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1AA,H1AB), C1(H1BC,H1BD), C2(H2A,H2B), C7(H7A,H7B), C8(H8A,H8B), C11(H11A,
 H11B), C14(H14A,H14B), C15(H15A,H15B), C19(H19A,H19B), C20(H20A,H20B),
 C22(H22A,H22B), C25(H25A,H25B), C26(H26A,H26B), C30(H30A,H30B), C31(H31A,H31B),
  C31(H31C,H31D), C33(H33A,H33B), C36(H36A,H36B), C37(H37A,H37B), C41(H41A,
 H41B), C42(H42A,H42B), C44(H44A,H44B), C47(H47A,H47B), C48(H48A,H48B),
 C52(H52A,H52B), C53(H53A,H53B), C53(H53C,H53D), C55(H55A,H55B), C58(H58A,H58B),
  C59(H59A,H59B), C63(H63A,H63B), C64(H64A,H64B), C66(H66A,H66B)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C9(H9), C16(H16), C21(H21), C27(H27), C32(H32), C38(H38), C43(H43),
 C49(H49), C54(H54), C60(H60), C65(H65), C68(H68), C69(H69), C70(H70), C71(H71),
  C72(H72)
5.d Idealised Me refined as rotating group:
 C74(H74A,H74B,H74C), C75(H75A,H75B,H75C)
;
_shelx_res_checksum              19344
_shelx_hkl_checksum              88505
_olex2_submission_special_instructions 'No special instructions were received'