Reactivity of phenoxathiin-based thiacalixarenes towards C-nucleophiles
Mamleev, Kamil; Čejka, Jan; Eigner, Václav; Krupička, Martin; Dvořáková, Hana; Lhoták, Pavel; RSC Advances 14 (2024) 13463–13473; doi:10.1039/D4RA02524E

data_7248543
_publ_section_title
;
 Reactivity of phenoxathiin-based thiacalixarenes towards C-nucleophiles
;
_journal_issue                   19
_journal_name_full               'RSC Advances'
_journal_page_first              13463
_journal_page_last               13473
_journal_paper_doi               10.1039/D4RA02524E
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'C47 H62 O12 S4, C H2 Cl2'
_chemical_formula_sum            'C48 H64 Cl2 O12 S4'
_chemical_formula_weight         1032.20
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2024-02-29 deposited with the CCDC.	2024-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.165(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.3670(13)
_cell_length_b                   9.5552(6)
_cell_length_c                   25.7750(15)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    180
_cell_measurement_theta_max      68.50
_cell_measurement_theta_min      2.96
_cell_volume                     5179.8(5)
_computing_cell_refinement       'Apex4 (Bruker AXS, 2021)'
_computing_data_collection       'Apex4 (Bruker AXS, 2021)'
_computing_data_reduction        'Apex4 (Bruker AXS, 2021)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_pressure         101
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex4'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.054
_diffrn_reflns_av_unetI/netI     0.073
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            95073
_diffrn_reflns_theta_full        67.339
_diffrn_reflns_theta_max         68.714
_diffrn_reflns_theta_min         3.484
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.117
_exptl_absorpt_correction_T_max  0.62
_exptl_absorpt_correction_T_min  0.53
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.195
_exptl_crystal_size_mid          0.159
_exptl_crystal_size_min          0.155
_refine_diff_density_max         1.17
_refine_diff_density_min         -1.12
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         9530
_refine_ls_number_restraints     80
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0901
_refine_ls_shift/su_max          0.0020267
_refine_ls_shift/su_mean         0.0000717
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.16P)^2^ +15.48P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2637
_refine_ls_wR_factor_gt          0.2577
_refine_ls_wR_factor_ref         0.2637
_reflns_limit_h_max              25
_reflns_limit_h_min              -25
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                8644
_reflns_number_total             9531
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.00
_oxford_diffrn_Wilson_scale      160.99
_oxford_refine_ls_r_factor_ref   0.0945
_oxford_refine_ls_scale          0.08011(4)
_oxford_reflns_number_all        9531
_cod_data_source_file            d4ra02524e2.cif
_cod_data_source_block           13_KM_253_3B_1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               7248543
_oxford_refine_reflns_threshold_expression I>-3.0\s(I)
_oxford_refine_ls_r_factor_all   0.0945
_oxford_refine_ls_wr_factor_all  0.2637