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_1568077
_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         'C48 H16 F16 S8'
_chemical_formula_sum            'C54 H30 F16 N2 O2 S8'
_chemical_formula_weight         1299.28
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n :2'
_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                90
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_cell_angle_gamma                90
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_cell_length_a                   19.8473(2)
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_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.88788643132704
_cell_measurement_theta_min      1.3988005227080926
_cell_volume                     5197.08(8)
_computing_data_collection       'GDA - generic data acquisition software'
_computing_data_reduction
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aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
DIALS 3.dev (Winter, G. et al., 2018)
pointless (Evans, P., 2006)
XIA2 3.10.dev0 (Winter, G., 2010)
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_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
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_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1140
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            73694
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         27.339
_diffrn_reflns_theta_min         1.406
_diffrn_source                   Synchrotron
_diffrn_source_details           'Allan et al. (2017)'
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_exptl_absorpt_coefficient_mu    0.406
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9854052353473588
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
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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
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_description       needle
_exptl_crystal_F_000             2624
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dimethylformamide'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.912
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         6454
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0858P)^2^+2.4346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1436
_refine_ls_wR_factor_ref         0.1490
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5194
_reflns_number_total             6454
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc05348a4.cif
_cod_data_source_block           1a-DMF
_cod_depositor_comments
'Adding full bibliography for 1568074--1568079.cif.'
_cod_original_cell_volume        5197.08(11)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               1568077
_nottingham_internal_coll_name   OATSWM
_nottingham_internal_coll_number 19184
_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 24/05/2022
_nottingham_internal_refinement_user pczspa
_nottingham_internal_validation_date 24/05/2022
_nottingham_internal_validation_user pczspa
_nottingham_internal_archive_date 24/05/2022
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.961
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C22A(H22A), C23A(H23A), C25A(H25A), C26A(H26A), C22B(H22B), C23B(H23B),
 C25B(H25B), C26B(H26B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              31469
_shelx_fab_checksum              9580
_olex2_submission_special_instructions 'No special instructions were received'