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_1568079
_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, 4(C5 H5 N)'
_chemical_formula_sum            'C68 H36 F16 N4 S8'
_chemical_formula_weight         1469.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-05-25
_audit_creation_method
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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                90.0
_cell_angle_beta                 95.0947(16)
_cell_angle_gamma                90.0
_cell_formula_units_Z            2
_cell_length_a                   5.89701(12)
_cell_length_b                   32.2682(3)
_cell_length_c                   16.4767(3)
_cell_measurement_reflns_used    14876
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.92536400161465
_cell_measurement_theta_min      1.2171085816981666
_cell_volume                     3122.90(9)
_computing_data_collection       'GDA - generic data acquisition software'
_computing_data_reduction
;
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_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 0.998
_diffrn_measured_fraction_theta_max 0.925
_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  0.0513
_diffrn_reflns_av_unetI/netI     0.0593
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            62385
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         35.972
_diffrn_reflns_theta_min         1.223
_diffrn_source                   Synchrotron
_diffrn_source_details           'Allan et al. (2017)'
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_exptl_absorpt_coefficient_mu    0.353
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9796951000161046
_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    1.563
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pyridine'
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.709
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         14951
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0669P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1295
_refine_ls_wR_factor_ref         0.1390
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9446
_reflns_number_total             14951
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc05348a4.cif
_cod_data_source_block           1a-Pyridine
_cod_depositor_comments
'Adding full bibliography for 1568074--1568079.cif.'
_cod_original_cell_volume        3122.89(7)
_cod_database_code               1568079
_nottingham_internal_coll_name   OATSWO
_nottingham_internal_coll_number 19186
_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 19/05/2022
_nottingham_internal_refinement_user pczspa
_nottingham_internal_validation_date 19/05/2022
_nottingham_internal_validation_user pczspa
_nottingham_internal_archive_date 19/05/2022
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.979
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C22(H22), C23(H23), C25(H25), C26(H26), C42(H42), C43(H43), C45(H45),
 C46(H46), C2B(H2B), C3B(H3B), C4B(H4B), C5B(H5B), C6B(H6B), C2A(H2A), C3A(H3A),
  C4A(H4A), C5A(H5A), C6A(H6A)
;
_shelx_res_checksum              90137
_olex2_submission_special_instructions 'No special instructions were received'