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_4518487
_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 H10'
_chemical_formula_sum            'C75 H82 Br12 O12'
_chemical_formula_weight         2134.20
_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                78.5090(10)
_cell_angle_beta                 76.4470(10)
_cell_angle_gamma                74.6900(10)
_cell_formula_units_Z            2
_cell_length_a                   13.7487(3)
_cell_length_b                   14.2271(3)
_cell_length_c                   21.6029(6)
_cell_measurement_reflns_used    9699
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      54.974
_cell_measurement_theta_min      2.955
_cell_volume                     3919.43(16)
_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 0.989
_diffrn_measured_fraction_theta_max 0.987
_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  0.0524
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            49990
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.957
_diffrn_reflns_theta_min         2.832
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.358
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.4858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1102 before and 0.0799 after correction. The Ratio of minimum to maximum transmission is 0.6470. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.808
_exptl_crystal_description       block
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.333
_refine_diff_density_min         -2.013
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     935
_refine_ls_number_reflns         14758
_refine_ls_number_restraints     124
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0824
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0778P)^2^+40.0117P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2105
_refine_ls_wR_factor_ref         0.2139
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13300
_reflns_number_total             14758
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am0c23059_si_003.cif
_cod_data_source_block           191101zwj_21_0m_pl
_cod_depositor_comments
'Adding full bibliography for 4518485--4518488.cif.'
_cod_database_code               4518487
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.481
_shelx_estimated_absorpt_t_min   0.446
_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
 1.53 with sigma of 0.02
 Br3A-C64
 1.85 with sigma of 0.02
 C58-C59
 1.53 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C75 \\sim C67 \\sim C72 \\sim C71 \\sim C69 \\sim C68 \\sim C73 \\sim C74:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C58 \\sim C59 \\sim Br11: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C64 \\sim Br12 \\sim Br3A \\sim C63: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C1 \\sim Br1 \\sim Br4A \\sim C2: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C58 \\sim C0AA \\sim Br2A \\sim C59 \\sim Br11: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: Br1(0.75) Br4(0.75) Br7(0.75) Br11(0.75) Br12(0.75) H1AA(0.75)
 H1AB(0.75) H1BC(0.25) H1BD(0.25) H20A(0.75) H20B(0.75) H20C(0.25) H20D(0.25)
 H37A(0.75) H37B(0.75) H37C(0.25) H37D(0.25) H58A(0.75) H58B(0.75) H58C(0.25)
 H58D(0.25) C59(0.75) H59A(0.75) H59B(0.75) H64A(0.75) H64B(0.75) H64C(0.25)
 H64D(0.25) Br0A(0.25) Br1A(0.25) Br3A(0.25) Br4A(0.25) Br2A(0.25) C0AA(0.25)
 H0AA(0.25) H0AB(0.25)
5.a 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),
 C20(H20C,H20D), C22(H22A,H22B), C25(H25A,H25B), C26(H26A,H26B), C30(H30A,H30B),
  C31(H31A,H31B), C33(H33A,H33B), C36(H36A,H36B), C37(H37A,H37B), C37(H37C,
 H37D), C41(H41A,H41B), C42(H42A,H42B), C44(H44A,H44B), C47(H47A,H47B),
 C48(H48A,H48B), C52(H52A,H52B), C53(H53A,H53B), C55(H55A,H55B), C58(H58A,H58B),
  C58(H58C,H58D), C59(H59A,H59B), C63(H63A,H63B), C64(H64A,H64B), C64(H64C,
 H64D), C66(H66A,H66B), C0AA(H0AA,H0AB)
5.b 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), C72(H72), C71(H71), C70(H70), C69(H69),
  C68(H68)
5.c Fitted hexagon refined as free rotating group:
 C67(C72,C71,C70,C69,C68)
5.d X=CH2 refined with riding coordinates:
 C74(H74A,H74B)
5.e Idealised Me refined as rotating group:
 C75(H75A,H75B,H75C)
;
_shelx_res_checksum              77039
_shelx_hkl_checksum              29862
_olex2_submission_special_instructions 'No special instructions were received'