Novel Hierarchical Meso-Microporous Hydrogen-Bonded Organic Framework for Selective Separation of Acetylene and Ethylene versus Methane.
Yin, Qi; Li, Yu-Lin; Li, Lan; Lü, Jian; Liu, Tian-Fu; Cao, Rong; ACS applied materials & interfaces 11 (2019) 17823–17827; doi:10.1021/acsami.9b03696

data_4514514
_publ_section_title
;
 Novel Hierarchical Meso-Microporous Hydrogen-Bonded Organic Framework for
 Selective Separation of Acetylene and Ethylene versus Methane.
;
_journal_issue                   19
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              17823
_journal_page_last               17827
_journal_paper_doi               10.1021/acsami.9b03696
_journal_volume                  11
_journal_year                    2019
_chemical_formula_moiety         'C44 H26 O8'
_chemical_formula_sum            'C44 H26 O8'
_chemical_formula_weight         682.65
_chemical_name_systematic        PFC-1
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-I 2y'
_space_group_name_H-M_alt        'I 1 2/m 1'
_symmetry_space_group_name_Hall  '-I 2y'
_symmetry_space_group_name_H-M   'I 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-10-17
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.841(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   3.7703(2)
_cell_length_b                   27.5034(16)
_cell_length_c                   29.3675(16)
_cell_measurement_reflns_used    1368
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      70.8120
_cell_measurement_theta_min      4.3730
_cell_volume                     3041.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5594
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -30.00  69.00   1.00    7.46    --   41.20 -57.00 -30.00   99
  2  \w     33.00 118.00   1.00    7.50    --  105.23 -45.00   0.00   85
  3  \w    125.00 178.00   1.00    7.50    --  105.23  45.00 -90.00   53
  4  \w    147.00 174.00   1.00    7.50    --  105.23 125.00   0.00   27
  5  \w    151.00 178.00   1.00    7.50    --  105.23 125.00 -60.00   27
  6  \w    106.00 170.00   1.00    7.50    --  105.23 125.00 -90.00   64
  7  \w    101.00 176.00   1.00    7.50    --  105.23 125.00  90.00   75
  8  \w     80.00 158.00   1.00    7.50    --  105.23  45.00-120.00   78
  9  \w    -79.00 -37.00   1.00    7.46    --  -41.20 -57.00  90.00   42
 10  \w    -89.00  -3.00   1.00    7.46    --  -41.20 125.00 150.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0478362000
_diffrn_orient_matrix_UB_12      0.0305702000
_diffrn_orient_matrix_UB_13      -0.0432112000
_diffrn_orient_matrix_UB_21      -0.2200024000
_diffrn_orient_matrix_UB_22      0.0412533000
_diffrn_orient_matrix_UB_23      0.0200865000
_diffrn_orient_matrix_UB_31      0.3415888000
_diffrn_orient_matrix_UB_32      0.0224165000
_diffrn_orient_matrix_UB_33      0.0220611000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            5872
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.249
_diffrn_reflns_theta_min         4.408
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.421
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58512
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.741
_exptl_crystal_description       needle
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.253
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         3042
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0549
_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^)+(0.1061P)^2^+0.1545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1750
_refine_ls_wR_factor_ref         0.1931
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2037
_reflns_number_total             3042
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am9b03696_si_003.cif
_cod_data_source_block           PFC-1
_cod_original_cell_volume        3041.5(3)
_cod_database_code               4514514
_chemical_oxdiff_usercomment     'C O H '
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C11(H11), C3(H3), C10(H10), C7(H7), C8(H8)
;
_shelx_fab_checksum              90052
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.819
_oxdiff_exptl_absorpt_empirical_full_min 0.626