Nucleophile-induced transformation of phenoxathiin-based thiacalixarenes.
Landovský, Tomáš; Babor, Martin; Čejka, Jan; Eigner, Václav; Dvořáková, Hana; Krupička, Martin; Lhoták, Pavel; Organic & biomolecular chemistry 19 (2021) 8075–8085; doi:10.1039/d1ob01487k

data_7158257
_publ_section_title
;
 Nucleophile-induced transformation of phenoxathiin-based thiacalixarenes.
;
_journal_issue                   37
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              8075
_journal_page_last               8085
_journal_paper_doi               10.1039/d1ob01487k
_journal_volume                  19
_journal_year                    2021
_chemical_formula_moiety         'C58 H68 O12 S5, C H3 N O2'
_chemical_formula_sum            'C59 H71 N O14 S5'
_chemical_formula_weight         1178.54
_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
;
2021-03-12 deposited with the CCDC.	2021-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                103.5302(9)
_cell_angle_beta                 99.6156(9)
_cell_angle_gamma                105.3475(9)
_cell_formula_units_Z            2
_cell_length_a                   13.1197(4)
_cell_length_b                   15.7488(5)
_cell_length_c                   16.2572(5)
_cell_measurement_reflns_used    316
_cell_measurement_temperature    200
_cell_measurement_theta_max      57
_cell_measurement_theta_min      12
_cell_volume                     3054.01(17)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.028
_diffrn_reflns_av_unetI/netI     0.038
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            97564
_diffrn_reflns_theta_full        72.208
_diffrn_reflns_theta_max         72.208
_diffrn_reflns_theta_min         2.883
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.268
_exptl_absorpt_correction_T_max  0.47
_exptl_absorpt_correction_T_min  0.40
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1248.000
_exptl_crystal_size_max          0.396
_exptl_crystal_size_mid          0.346
_exptl_crystal_size_min          0.330
_refine_diff_density_max         0.50
_refine_diff_density_min         -0.50
_refine_ls_extinction_coef       208(11)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9754
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     771
_refine_ls_number_reflns         11988
_refine_ls_number_restraints     98
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.0013893
_refine_ls_shift/su_mean         0.0000627
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 2.07P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1041
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1038
_reflns_limit_h_max              15
_reflns_limit_h_min              -16
_reflns_limit_k_max              18
_reflns_limit_k_min              -19
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                11362
_reflns_number_total             11990
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.20
_oxford_diffrn_Wilson_scale      83.97
_oxford_refine_ls_r_factor_ref   0.0393
_oxford_refine_ls_scale          0.15490(6)
_oxford_reflns_number_all        11990
_cod_data_source_file            d1ob01487k2.cif
_cod_data_source_block           14
_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 

 Adding full bibliography for 7158257--7158261.cif.
;
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C59 H71 N1 O14 S5'
_cod_database_code               7158257
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)