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_7158258
_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         'C53 H65 N O12 S5, 2.302(C H3 N O2)'
_chemical_formula_sum            'C55.3 H71.91 N3.3 O16.6 S5'
_chemical_formula_weight         1208.96
_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                94.9881(10)
_cell_angle_beta                 105.9354(10)
_cell_angle_gamma                114.8298(12)
_cell_formula_units_Z            2
_cell_length_a                   13.12948(15)
_cell_length_b                   14.11541(19)
_cell_length_c                   19.1344(2)
_cell_measurement_reflns_used    32551
_cell_measurement_temperature    95
_cell_measurement_theta_max      73.99
_cell_measurement_theta_min      3.85
_cell_volume                     3010.41(8)
_computing_cell_refinement
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_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      95
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  'focussing mirrors'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.020
_diffrn_reflns_av_unetI/netI     0.030
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            52998
_diffrn_reflns_theta_full        69.729
_diffrn_reflns_theta_max         74.180
_diffrn_reflns_theta_min         2.469
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.358
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1279.342
_exptl_crystal_size_max          0.159
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.085
_refine_diff_density_max         0.39
_refine_diff_density_min         -0.38
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9678
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     786
_refine_ls_number_reflns         12048
_refine_ls_number_restraints     73
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.0007216
_refine_ls_shift/su_mean         0.0000462
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 1.91P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0761
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0761
_reflns_limit_h_max              15
_reflns_limit_h_min              -16
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                11299
_reflns_number_total             12050
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.22
_oxford_diffrn_Wilson_scale      0.06
_oxford_refine_ls_r_factor_ref   0.0299
_oxford_refine_ls_scale          4.16(3)
_oxford_reflns_number_all        12048
_cod_data_source_file            d1ob01487k2.cif
_cod_data_source_block           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 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        'C55.30 H71.91 N3.30 O16.60 S5'
_cod_database_code               7158258
_oxford_refine_reflns_threshold_expression I>-3.0\s(I)
_oxford_refine_ls_r_factor_all   0.0299
_oxford_refine_ls_wr_factor_all  0.0761