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_7248537
_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         'C25 H33.87 O4 S1'
_chemical_formula_sum            'C25 H33.87 O4 S'
_chemical_formula_weight         430.48
_chemical_name_systematic        'phenoxathiin derivative'
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_update_record
;
2024-02-27 deposited with the CCDC.	2024-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.4068(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1548(4)
_cell_length_b                   13.1857(5)
_cell_length_c                   17.8205(7)
_cell_measurement_reflns_used    9844
_cell_measurement_temperature    180
_cell_measurement_theta_max      72.02
_cell_measurement_theta_min      4.19
_cell_volume                     2354.05(16)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_collection       'Apex4 (Bruker AXS, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_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  0.031
_diffrn_reflns_av_unetI/netI     0.041
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            88168
_diffrn_reflns_theta_full        72.162
_diffrn_reflns_theta_max         72.162
_diffrn_reflns_theta_min         4.191
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.437
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             927.480
_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.053
_refine_diff_density_max         0.46
_refine_diff_density_min         -0.32
_refine_ls_extinction_coef       94(13)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         4640
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.0010976
_refine_ls_shift/su_mean         0.0000623
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 0.80P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1038
_refine_ls_wR_factor_gt          0.1032
_refine_ls_wR_factor_ref         0.1038
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                4482
_reflns_number_total             4640
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.64
_oxford_diffrn_Wilson_scale      25.94
_oxford_refine_ls_scale          0.21851(19)
_cod_data_source_file            d4ra02524e2.cif
_cod_data_source_block           KM301
_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_H-M      'P 21/n '
_cod_original_formula_sum        'C25 H33.87 O4 S1'
_cod_database_code               7248537
_oxford_refine_reflns_threshold_expression I>-3.0\s(I)
_refine_ls_r_factor_ref          0.0374
_reflns_number_all               4640