Breaking thiacalix[4]arene into pieces – a novel synthetic approach to higher calixarenes bearing mixed (–S–, –CH2–) bridges
Kaiser, Lukáš; Landovský, Tomáš; Salvadori, Karolína; Eigner, Václav; Dvořáková, Hana; Lhoták, Pavel; RSC Advances 11 (2021) 36934–36941; doi:10.1039/D1RA07464D

data_7243933
_publ_section_title
;
 Breaking thiacalix[4]arene into pieces -- a novel synthetic approach to
 higher calixarenes bearing mixed (--S--, --CH2--) bridges
;
_journal_issue                   58
_journal_name_full               'RSC Advances'
_journal_page_first              36934
_journal_page_last               36941
_journal_paper_doi               10.1039/D1RA07464D
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C62 H76 O6 S4, 2(C2 H6 O S)'
_chemical_formula_sum            'C66 H88 O8 S6'
_chemical_formula_weight         1201.81
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2021-09-17 deposited with the CCDC.	2021-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                81.0129(10)
_cell_angle_beta                 70.9839(9)
_cell_angle_gamma                80.0849(10)
_cell_formula_units_Z            1
_cell_length_a                   11.1603(3)
_cell_length_b                   11.9646(3)
_cell_length_c                   13.1785(3)
_cell_measurement_reflns_used    965
_cell_measurement_temperature    200
_cell_measurement_theta_max      24.40
_cell_measurement_theta_min      3.55
_cell_volume                     1629.33(7)
_computing_cell_refinement       'Apex3 (Bruker AXS, 2015)'
_computing_data_collection       'Apex3 (Bruker AXS, 2015)'
_computing_data_reduction        'Apex3 (Bruker AXS, 2015)'
_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      200
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex3'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_av_unetI/netI     0.040
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            53539
_diffrn_reflns_theta_full        68.403
_diffrn_reflns_theta_max         68.403
_diffrn_reflns_theta_min         3.568
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.347
_exptl_absorpt_correction_T_max  0.76
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             643.997
_exptl_crystal_size_max          0.181
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.118
_refine_diff_density_max         0.26
_refine_diff_density_min         -0.39
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9642
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         5978
_refine_ls_number_restraints     62
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.0008240
_refine_ls_shift/su_mean         0.0000645
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 1.15P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0822
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0822
_reflns_limit_h_max              13
_reflns_limit_h_min              -12
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                5552
_reflns_number_total             5978
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.30
_oxford_diffrn_Wilson_scale      23.41
_oxford_refine_ls_r_factor_ref   0.0361
_oxford_refine_ls_scale          0.19502(9)
_oxford_reflns_number_all        5978
_cod_data_source_file            d1ra07464d2.cif
_cod_data_source_block           9
_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 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7243933
_oxford_refine_reflns_threshold_expression I>-3.0\s(I)
_oxford_refine_ls_r_factor_all   0.0361
_oxford_refine_ls_wr_factor_all  0.0822