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_7248538
_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         'C29 H42 O2'
_chemical_formula_sum            'C29 H42 O2'
_chemical_formula_weight         422.65
_chemical_name_systematic        1,3,6,8-Tetra-tert-butyl-4-methoxydibenzofuran
_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_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2024-02-27 deposited with the CCDC.	2024-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.059(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.9326(3)
_cell_length_b                   16.6120(9)
_cell_length_c                   26.1176(14)
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    180
_cell_measurement_theta_max      74.20
_cell_measurement_theta_min      4.31
_cell_volume                     2573.5(2)
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.046
_diffrn_reflns_av_unetI/netI     0.065
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            47694
_diffrn_reflns_theta_full        68.000
_diffrn_reflns_theta_max         70.064
_diffrn_reflns_theta_min         3.153
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.504
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.091
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.421
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.038
_refine_diff_density_max         0.37
_refine_diff_density_min         -0.32
_refine_ls_extinction_coef       40(10)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4867
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          0.0003998
_refine_ls_shift/su_mean         0.0000463
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.07P)^2^ + 2.02P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1486
_refine_ls_wR_factor_gt          0.1394
_refine_ls_wR_factor_ref         0.1486
_reflns_limit_h_max              7
_reflns_limit_h_min              -7
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              0
_reflns_number_gt                4131
_reflns_number_total             4868
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.79
_oxford_diffrn_Wilson_scale      40.42
_oxford_refine_ls_scale          0.15809(12)
_cod_data_source_file            d4ra02524e2.cif
_cod_data_source_block           KM303_3_8
_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 1 21/c 1 '
_cod_database_code               7248538
_oxford_refine_reflns_threshold_expression I>-3.0\s(I)
_refine_ls_r_factor_ref          0.0605
_reflns_number_all               4867