A fluorine-functionalized microporous In-MOF with high physicochemical stability for light hydrocarbon storage and separation
Fan, Weidong; Liu, Xiuping; Wang, Xia; Li, Yue; Xing, Chengyong; Wang, Yutong; Guo, Wenyue; Zhang, Liangliang; Sun, Daofeng; Inorganic Chemistry Frontiers 5 (2018) 2445–; doi:10.1039/C8QI00652K

data_4349878
_publ_section_title
;
 A fluorine-functionalized microporous In-MOF with high physicochemical
 stability for light hydrocarbon storage and separation
;
_journal_issue                   10
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              2445
_journal_paper_doi               10.1039/C8QI00652K
_journal_volume                  5
_journal_year                    2018
_chemical_formula_moiety         'C20.5 H11.83 F In1.5 O7.67'
_chemical_formula_sum            'C20.5 H11.83 F In1.5 O7.67'
_chemical_formula_weight         572.03
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-04-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-04-17 deposited with the CCDC.
2018-08-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            36
_cell_length_a                   27.3963(13)
_cell_length_b                   27.3963(13)
_cell_length_c                   75.861(3)
_cell_measurement_reflns_used    12474
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      70.4330
_cell_measurement_theta_min      4.3950
_cell_volume                     49310(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28e (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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_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    -32.00  70.00   0.75    9.23    --    0.00  77.00-150.00  136
  2  \w     22.00 124.00   0.75   36.94    --   54.00  77.00 -90.00  136
  3  \w     33.00 123.00   0.75   36.94    --   54.00  77.00 150.00  120
  4  \w    116.00 169.25   0.75   36.94    --  108.00  77.00  30.00   71
  5  \w    109.00 175.00   0.75   36.94    --  108.00  77.00 -90.00   88
  6  \w     77.00 171.50   0.75   36.94    --  108.00  77.00 150.00  126
  7  \w    113.00 177.50   0.75   36.94    --  108.00  77.00  60.00   86
  8  \w     81.00 108.00   0.75   36.94    --  108.00  77.00  30.00   36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0603554000
_diffrn_orient_matrix_UB_12      -0.0155290000
_diffrn_orient_matrix_UB_13      0.0054767000
_diffrn_orient_matrix_UB_21      -0.0244253000
_diffrn_orient_matrix_UB_22      -0.0477635000
_diffrn_orient_matrix_UB_23      -0.0137316000
_diffrn_orient_matrix_UB_31      -0.0001907000
_diffrn_orient_matrix_UB_32      -0.0409454000
_diffrn_orient_matrix_UB_33      0.0139067000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       91
_diffrn_reflns_limit_l_min       -87
_diffrn_reflns_number            37141
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.779
_diffrn_reflns_theta_min         3.670
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.270
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56306
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.693
_exptl_crystal_description       block
_exptl_crystal_F_000             10032
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
;
_refine_diff_density_max         1.368
_refine_diff_density_min         -1.161
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         10368
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.1080
_refine_ls_R_factor_gt           0.0843
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1596P)^2^+689.9177P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2674
_refine_ls_wR_factor_ref         0.2989
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7892
_reflns_number_total             10368
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi00652k2.cif
_cod_data_source_block           wx-304
_cod_original_cell_volume        49310(5)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_original_formula_sum        'C20.50 H11.83 F In1.50 O7.67'
_cod_database_code               4349878
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         ' C H O F In'
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: C29(0.5) H29(0.5) O30(0.66667) H30A(0.66667) H30B(0.66667)
 H8A(0.5) H8B(0.5)
3.a Rotating group:
 O30(H30A,H30B), O8(H8A,H8B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C9(H9), C11(H11), C12(H12), C13(H13), C19(H19), C20(H20), C25(H25),
 C29(H29), C10(H10)
;
_shelx_res_checksum              17448
_shelx_hkl_checksum              27410
_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 1.757
_oxdiff_exptl_absorpt_empirical_full_min 0.713