Selective adsorption of fluorinated super greenhouse gases within a metal-organic framework with dynamic corrugated ultramicropores.
Whitehead, Bevan S.; Brennessel, William W.; Michtavy, Shane S.; Silva, Hope A.; Kim, Jaehwan; Milner, Phillip J.; Porosoff, Marc D.; Barnett, Brandon R.; Chemical science 15 (2024) 5964–5972; doi:10.1039/d3sc07007g

data_1571271
_publ_section_title
;
 Selective adsorption of fluorinated super greenhouse gases within a
 metal-organic framework with dynamic corrugated ultramicropores.
;
_journal_issue                   16
_journal_name_full               'Chemical science'
_journal_page_first              5964
_journal_page_last               5972
_journal_paper_doi               10.1039/d3sc07007g
_journal_volume                  15
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C17 H8 F6 O4 Zn'
_chemical_formula_sum            'C17 H8 F6 O4 Zn'
_chemical_formula_weight         455.60
_space_group_crystal_system      hexagonal
_space_group_IT_number           180
_space_group_name_Hall           'P 62 2 (0 0 4)'
_space_group_name_H-M_alt        'P 62 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-12-21
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-12-21 deposited with the CCDC.	2024-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   21.2076(5)
_cell_length_b                   21.2076(5)
_cell_length_c                   7.7012(2)
_cell_measurement_reflns_used    4723
_cell_measurement_temperature    298.00(10)
_cell_measurement_theta_max      73.5620
_cell_measurement_theta_min      2.3920
_cell_volume                     2999.66(13)
_computing_cell_refinement       'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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    -89.00 -15.00   0.50   20.00    --  -47.30 129.00-134.00  148
  2  \w     89.00 178.00   0.50   35.00    --  113.25 134.00-156.00  178
  3  \w     -9.00  28.00   0.50   20.00    --  -47.30  19.00-150.00   74
  4  \w     -9.00  28.00   0.50   20.00    --  -47.30  19.00-120.00   74
  5  \w     42.00 106.00   0.50   35.00    --  113.25 -94.00-180.00  128
  6  \w     41.00 178.00   0.50   35.00    --  113.25   0.00  90.00  274
  7  \w     42.00 106.00   0.50   35.00    --  113.25 -94.00-150.00  128
  8  \w     42.00  83.00   0.50   35.00    --  113.25 -61.00-180.00   82
  9  \w     42.00  83.00   0.50   35.00    --  113.25 -61.00  90.00   82
 10  \w     35.00 120.00   0.50   20.00    --   47.30  38.00 -60.00  170
 11  \w    -26.00  18.00   0.50   20.00    --   47.30  -8.00 -11.00   88
 12  \w   -163.00-105.00   0.50   35.00    --  -91.75 -77.00-120.00  116
 13  \w    115.00 178.00   0.50   35.00    --  113.25   0.00 150.00  126
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0828627000
_diffrn_orient_matrix_UB_12      0.0526429000
_diffrn_orient_matrix_UB_13      0.0052840000
_diffrn_orient_matrix_UB_21      0.0126891000
_diffrn_orient_matrix_UB_22      -0.0650929000
_diffrn_orient_matrix_UB_23      0.0198744000
_diffrn_orient_matrix_UB_31      0.0034992000
_diffrn_orient_matrix_UB_32      -0.0050999000
_diffrn_orient_matrix_UB_33      -0.1989473000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1166
_diffrn_reflns_av_unetI/netI     0.0645
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            17349
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.370
_diffrn_reflns_theta_min         2.406
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.406
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.02411
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.101a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_description       needle
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.169
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.018
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 588 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         2182
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0268P)^2^+1.0813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0887
_reflns_Friedel_coverage         0.656
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                1716
_reflns_number_total             2182
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc07007g2.cif
_cod_data_source_block           brbbsw97
_cod_depositor_comments
'Adding full bibliography for 1571271--1571275.cif.'
_cod_original_cell_volume        2999.66(16)
_cod_original_sg_symbol_Hall     'P 62 2c (0 0 1)'
_cod_database_code               1571271
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_usercomment     'Fully evacuated xtal'
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.687
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7)
;
_shelx_res_checksum              1785
_olex2_submission_original_sample_id brbbsw97
_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 16.928
_oxdiff_exptl_absorpt_empirical_full_min 0.385