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_7243934
_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         'C52 H64 O5 S3, C2 H6 O, H2 O'
_chemical_formula_sum            'C54 H72 O7 S3'
_chemical_formula_weight         929.36
_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                71.9424(11)
_cell_angle_beta                 82.1907(11)
_cell_angle_gamma                89.1864(12)
_cell_formula_units_Z            2
_cell_length_a                   13.2330(3)
_cell_length_b                   14.4941(4)
_cell_length_c                   14.6750(4)
_cell_measurement_reflns_used    63
_cell_measurement_temperature    200
_cell_measurement_theta_max      56
_cell_measurement_theta_min      3
_cell_volume                     2650.05(12)
_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_temperature      200
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.030
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            30366
_diffrn_reflns_theta_full        68.218
_diffrn_reflns_theta_max         68.22
_diffrn_reflns_theta_min         3.198
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.656
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1000.001
_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.093
_refine_diff_density_max         0.44
_refine_diff_density_min         -0.47
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9751
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         9625
_refine_ls_number_restraints     94
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.0013557
_refine_ls_shift/su_mean         0.0000378
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 10.8 17.1 9.06 3.14 0.548 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1527
_refine_ls_wR_factor_gt          0.1417
_refine_ls_wR_factor_ref         0.1527
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              17
_reflns_limit_k_min              -16
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                8101
_reflns_number_total             9633
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.91
_oxford_diffrn_Wilson_scale      85.99
_oxford_refine_ls_r_factor_ref   0.0632
_oxford_refine_ls_scale          0.13743(7)
_oxford_reflns_number_all        9633
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            d1ra07464d2.cif
_cod_data_source_block           8
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'Other' was changed to
'other' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

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               7243934