Targeted design of porous materials without strong, directional interactions
O'Shaughnessy, Megan; Spackman, Peter A.; Little, Marc; Catalano, Luca; James, Alex Michael; Day, Graeme Matthew; Cooper, Andrew; Chemical Communications  (2022) –; doi:10.1039/D2CC04682B

data_7130835
_publ_section_title
;
 Targeted design of porous materials without strong, directional
 interactions
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC04682B
_journal_year                    2022
_chemical_formula_moiety         'C25 H16 Cl4 O8 S4'
_chemical_formula_sum            'C25 H16 Cl4 O8 S4'
_chemical_formula_weight         714.42
_chemical_name_common            TSCl
_chemical_name_systematic        Tetrakis(4-sulfonylchloridephenyl)methane
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-11-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-07-25 deposited with the CCDC.	2022-10-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.6104(8)
_cell_length_b                   13.6104(8)
_cell_length_c                   9.8000(5)
_cell_measurement_reflns_used    4246
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.895
_cell_measurement_theta_min      2.561
_cell_volume                     1815.38(18)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      200
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            10185
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.362
_diffrn_reflns_theta_min         2.561
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.595
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5326
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0868 before and 0.0628 after correction.
The Ratio of minimum to maximum transmission is 0.7145.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       block
_exptl_crystal_F_000             724
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: 1,1,2,2-Hexafluoro-2-propanol'
_exptl_crystal_size_max          0.127
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Flack x determined using 708 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.26(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         1842
_refine_ls_number_restraints     209
_refine_ls_restrained_S_all      1.242
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0954P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1293
_refine_ls_wR_factor_ref         0.1345
_reflns_Friedel_coverage         0.893
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                1647
_reflns_number_total             1842
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04682b2.cif
_cod_data_source_block           TSCl_200k
_cod_original_cell_volume        1815.4(2)
_cod_database_code               7130835
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.928
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.495(10)
 0.505(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Shared sites
{C1B, C1A}
4. Restrained distances
 Cl1B-S1B = Cl1A-S1A
 2.04 with sigma of 0.02
 S1B-O4A = S1A-O2A = S1B-O3A = S1A-O1A
 1.42 with sigma of 0.02
 C1B-C1 = C1A-C1
 1.49 with sigma of 0.005
 C6A-C1A = C6B-C1B = C6A-C5A = C6B-C5B = C5A-C4A = C5B-C4B = C4A-C3A = C4B-C3B
 = C3B-C2B = C3A-C2A = C2A-C1A = C2B-C1B
 1.39 with sigma of 0.01
 O2A-O1A
 2.48 with sigma of 0.02
 Cl1A-O1A \\sim Cl1A-O4A
 with sigma of 0.02
 Cl1B-O3A \\sim Cl1B-O4A
 with sigma of 0.02
5. Restrained planarity
 C1A, C2A, C3A, C4A, C5A, C6A
 with sigma of 0.001
 C1B, C2B, C3B, C4B, C5B, C6B
 with sigma of 0.001
6. Uiso/Uaniso restraints and constraints
Uanis(C1A) \\sim Ueq, Uanis(C1B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Cl1A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1A) = Uanis(C1B)
Uanis(C1B) = Uanis(C1A)
7. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
8. Others
 Fixed Sof: C1A(0.5) C6A(0.5) H6A(0.5) C5A(0.5) H5A(0.5) C4A(0.5) C3A(0.5)
 H3A(0.5) C2A(0.5) H2A(0.5) Cl1A(0.5) O1A(0.5) O2A(0.5) S1A(0.5) C1B(0.5)
 C6B(0.5) H6B(0.5) C5B(0.5) H5B(0.5) C4B(0.5) C3B(0.5) H3B(0.5) C2B(0.5)
 H2B(0.5) Cl1B(0.5) O3A(0.5) O4A(0.5) S1B(0.5)
9.a Aromatic/amide H refined with riding coordinates:
 C6A(H6A), C5A(H5A), C3A(H3A), C2A(H2A), C6B(H6B), C5B(H5B), C3B(H3B), C2B(H2B)
;
_shelx_res_checksum              96885
_shelx_hkl_checksum              48574
_olex2_submission_special_instructions 'No special instructions were received'