Fluorinated <i>vs.</i> non-fluorinated tetrahedral Tri<sup>4</sup>Tri<sup>4</sup> porous organic cages for H<sub>2</sub>, CO<sub>2</sub>, and CH<sub>4</sub> adsorption.
David, Tim; Oestreich, Robert; Pausch, Tobias; Wada, Yuki; Fleck-Kunde, Tom; Kawano, Masaki; Janiak, Christoph; Schmidt, Bernd M.; Chemical communications (Cambridge, England) 60 (2024) 14762–14765; doi:10.1039/d4cc05277c

data_7133946
_publ_section_title
;
 Fluorinated <i>vs.</i> non-fluorinated tetrahedral
 Tri<sup>4</sup>Tri<sup>4</sup> porous organic cages for H<sub>2</sub>,
 CO<sub>2</sub>, and CH<sub>4</sub> adsorption.
;
_journal_issue                   99
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              14762
_journal_page_last               14765
_journal_paper_doi               10.1039/d4cc05277c
_journal_volume                  60
_journal_year                    2024
_chemical_formula_sum            'C350.54 H326.54 Cl45 N24'
_chemical_formula_weight         6470.58
_space_group_crystal_system      cubic
_space_group_IT_number           219
_space_group_name_Hall           'F -4a 2 3'
_space_group_name_H-M_alt        'F -4 3 c'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-11-04 deposited with the CCDC.	2024-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.2652(8)
_cell_length_b                   35.2652(8)
_cell_length_c                   35.2652(8)
_cell_measurement_reflns_used    2961
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      68.9520
_cell_measurement_theta_min      4.3640
_cell_volume                     43857.0(17)
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            12329
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        66.959
_diffrn_reflns_theta_max         66.959
_diffrn_reflns_theta_min         2.506
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.889
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.490
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.980
_exptl_crystal_description       cube
_exptl_crystal_F_000             13452
_exptl_crystal_size_max          0.234
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.179
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
;
 Flack x determined using 741 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.11(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.334
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         3155
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.373
_refine_ls_R_factor_all          0.1420
_refine_ls_R_factor_gt           0.1258
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3244
_refine_ls_wR_factor_ref         0.3455
_reflns_Friedel_coverage         0.821
_reflns_Friedel_fraction_full    0.919
_reflns_Friedel_fraction_max     0.919
_reflns_number_gt                2092
_reflns_number_total             3155
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc05277c2.cif
_cod_data_source_block           Et4H4
_cod_depositor_comments
'Adding full bibliography for 7133945--7133946.cif.'
_cod_original_cell_volume        43857(3)
_cod_original_sg_symbol_Hall     'F -4c 2 3'
_cod_database_code               7133946
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.551
_shelx_estimated_absorpt_t_max   0.626
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H5 of C5, H20 of C20, H13 of C13, H8 of C8, H11 of C11,
  H4 of C4, H7 of C7, H10 of C10
 At 1.5 times of:
  All C(H,H,H) groups, H21 of C21
2. Restrained distances
 C21-H21
 1.1 with sigma of 0.02
 H21-C21
 1.1 with sigma of 0.02
3. Rigid bond restraints
 Cl1, Cl2, Cl3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C21, Cl4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl2 \\sim Cl3: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C21 \\sim Cl4: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C20) \\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(Cl3)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(C20)=Sof(H20)=Sof(Cl1)=Sof(Cl2)=Sof(Cl3)=FVAR(1)
 Sof(C21)=Sof(H21)=0.25*FVAR(3)
 Sof(Cl4)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C20(H20)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
6.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13)
6.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C)
;
_shelx_res_checksum              39104
_shelx_hkl_checksum              51513