Catalysis enabled synthesis, structures, and reactivities of fluorinated S<sub>8</sub>-corona[<i>n</i>]arenes (<i>n</i> = 8-12).
Turley, Andrew T.; Hanson-Heine, Magnus W D; Argent, Stephen P.; Hu, Yaoyang; Jones, Thomas A.; Fay, Michael; Woodward, Simon; Chemical science 14 (2022) 70–77; doi:10.1039/d2sc05348a

data_1568076
_publ_section_title
;
 Catalysis enabled synthesis, structures, and reactivities of fluorinated
 S<sub>8</sub>-corona[<i>n</i>]arenes (<i>n</i> = 8-12).
;
_journal_issue                   1
_journal_name_full               'Chemical science'
_journal_page_first              70
_journal_page_last               77
_journal_paper_doi               10.1039/d2sc05348a
_journal_volume                  14
_journal_year                    2022
_chemical_formula_moiety         'C56 H32 F16 S8'
_chemical_formula_sum            'C56 H32 F16 S8'
_chemical_formula_weight         1265.29
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-05-25
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Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
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_audit_update_record
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2022-05-26 deposited with the CCDC.	2022-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                75.540(2)
_cell_angle_beta                 89.177(2)
_cell_angle_gamma                73.340(2)
_cell_formula_units_Z            1
_cell_length_a                   9.5286(2)
_cell_length_b                   10.3554(2)
_cell_length_c                   14.2500(4)
_cell_measurement_reflns_used    5375
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.678120671249744
_cell_measurement_theta_min      1.4290450194019093
_cell_volume                     1301.90(6)
_computing_data_collection       'GDA - generic data acquisition software'
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_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      'N2 gas'
_diffrn_ambient_temperature      100(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_type            'Dectris PILATUS 2M'
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.861
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0782
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.861
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26997
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.861
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         35.968
_diffrn_reflns_theta_min         2.059
_diffrn_source                   Synchrotron
_diffrn_source_details           'Allan et al. (2017)'
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_exptl_absorpt_coefficient_mu    0.408
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9922883275879729
_exptl_absorpt_correction_type   empirical
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CCP4 7.1.018: AIMLESS, version 0.7.7 : 23/04/21
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
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_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       block
_exptl_crystal_F_000             640
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform'
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         11650
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0546P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1263
_refine_ls_wR_factor_ref         0.1370
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7278
_reflns_number_total             11650
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc05348a4.cif
_cod_data_source_block           1b
_cod_depositor_comments
'Adding full bibliography for 1568074--1568079.cif.'
_cod_original_cell_volume        1301.90(5)
_cod_database_code               1568076
_nottingham_internal_coll_name   OATSWI
_nottingham_internal_coll_number 19140
_nottingham_internal_coll_client AT/SW
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'fine \w scans'
_nottingham_internal_coll_frame_time 0.2
_nottingham_internal_coll_frame_width 0.01
_nottingham_internal_coll_user   pczspa
_nottingham_internal_coll_date   09/05/2022
_nottingham_internal_coll_location DLS
_nottingham_internal_coll_instrument i19-EH1
_nottingham_internal_process_date 09/05/2022
_nottingham_internal_process_user pczspa
_nottingham_internal_solution_date 09/05/2022
_nottingham_internal_solution_user pczspa
_nottingham_internal_refinement_date 25/05/2022
_nottingham_internal_refinement_user pczspa
_nottingham_internal_validation_date 25/05/2022
_nottingham_internal_validation_user pczspa
_nottingham_internal_archive_date 25/05/2022
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C23(H23), C26(H26), C43(H43), C46(H46)
2.b Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C47(H47A,H47B,H47C), C48(H48A,H48B,
 H48C)
;
_shelx_res_checksum              57350
_olex2_submission_special_instructions 'No special instructions were received'