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_7248541
_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         'C38 H36 O3 S'
_chemical_formula_sum            'C38 H36 O3 S'
_chemical_formula_weight         572.77
_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
_audit_update_record
;
2024-02-29 deposited with the CCDC.	2024-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.9341(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.99070(12)
_cell_length_b                   11.76474(11)
_cell_length_c                   21.9240(3)
_cell_measurement_reflns_used    11049
_cell_measurement_temperature    120
_cell_measurement_theta_max      67.62
_cell_measurement_theta_min      3.76
_cell_volume                     3014.29(6)
_computing_cell_refinement
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_collection       'Gemini, (Oxford Diffraction, 2006)'
_computing_data_reduction
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_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      120
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.022
_diffrn_reflns_av_unetI/netI     0.033
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            16840
_diffrn_reflns_theta_full        66.235
_diffrn_reflns_theta_max         67.587
_diffrn_reflns_theta_min         3.782
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.237
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.502
_exptl_crystal_size_mid          0.385
_exptl_crystal_size_min          0.135
_refine_diff_density_max         0.34
_refine_diff_density_min         -0.38
_refine_ls_extinction_coef       71(8)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9799
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         5403
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.0010493
_refine_ls_shift/su_mean         0.0000608
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 1.21P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0923
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.0923
_reflns_limit_h_max              13
_reflns_limit_h_min              -14
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                5036
_reflns_number_total             5403
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.60
_oxford_diffrn_Wilson_scale      0.06
_oxford_refine_ls_r_factor_ref   0.0348
_oxford_refine_ls_scale          4.30(6)
_oxford_reflns_number_all        5403
_cod_data_source_file            d4ra02524e2.cif
_cod_data_source_block           12_KM129_16
_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_cell_volume        3014.30(6)
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               7248541
_oxford_refine_reflns_threshold_expression I>-3.0\s(I)
_oxford_refine_ls_r_factor_all   0.0348
_oxford_refine_ls_wr_factor_all  0.0923