Adsorptive separation of para-xylene by nonporous adaptive crystals of phenanthrene[2]arene
Hou, Ying; Duan, Yin-Rong; Ding, Man-Hua; Tang, Lin-Li; Zeng, Fei; RSC Advances 12 (2022) 22060–22063; doi:10.1039/D2RA03773D

data_7245288
_publ_section_title
;
 Adsorptive separation of para-xylene by nonporous adaptive crystals of
 phenanthrene[2]arene
;
_journal_issue                   34
_journal_name_full               'RSC Advances'
_journal_page_first              22060
_journal_page_last               22063
_journal_paper_doi               10.1039/D2RA03773D
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C66 H60 O12, 2(C8 H10)'
_chemical_formula_sum            'C82 H80 O12'
_chemical_formula_weight         1257.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-30
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2021.06.29 svn.r12e2184c for OlexSys, GUI svn.r6374)
;
_audit_update_record
;
2022-05-30 deposited with the CCDC.	2022-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.893(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.879(5)
_cell_length_b                   12.427(4)
_cell_length_c                   19.765(7)
_cell_measurement_reflns_used    2784
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      20.40
_cell_measurement_theta_min      2.20
_cell_volume                     3401(2)
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_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  0.0952
_diffrn_reflns_av_unetI/netI     0.0959
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            37527
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.596
_diffrn_reflns_theta_min         1.739
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   0.99
_exptl_transmission_factor_min   0.98
_refine_diff_density_max         0.253
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         7753
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1630
_refine_ls_R_factor_gt           0.0691
_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^)+(0.1020P)^2^+0.0865P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1704
_refine_ls_wR_factor_ref         0.2268
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3416
_reflns_number_total             7753
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra03773d2.cif
_cod_data_source_block           33
_cod_original_cell_volume        3401.3(19)
_cod_database_code               7245288
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.986
_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.a Secondary CH2 refined with riding coordinates:
 C00N(H00A,H00B)
2.b Aromatic/amide H refined with riding coordinates:
 C00D(H00D), C00I(H00I), C00J(H00J), C00L(H00L), C00R(H00R), C00S(H00S),
 C00U(H00U), C00V(H00V), C00W(H00W), C00X(H00X), C015(H015), C017(H017),
 C018(H018), C019(H019)
2.c Idealised Me refined as rotating group:
 C00Y(H00C,H00E,H00F), C00Z(H00G,H00H,H00K), C010(H01A,H01B,H01C), C011(H01D,
 H01E,H01F), C012(H01G,H01H,H01I), C014(H01J,H01K,H01L), C01A(H01M,H01N,H01O),
 C01B(H01P,H01Q,H01R)
;
_shelx_res_checksum              29098
_olex2_submission_special_instructions 'No special instructions were received'