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_7158259
_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         'C54 H66 O12 S5, 4(C H3 N O2)'
_chemical_formula_sum            'C58 H78 N4 O20 S5'
_chemical_formula_weight         1311.60
_chemical_melting_point          515(2)
_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_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2021-03-09 deposited with the CCDC.	2021-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                111.084(2)
_cell_angle_beta                 108.289(2)
_cell_angle_gamma                93.047(2)
_cell_formula_units_Z            2
_cell_length_a                   15.2602(10)
_cell_length_b                   15.3461(10)
_cell_length_c                   15.8961(10)
_cell_measurement_reflns_used    299
_cell_measurement_temperature    180
_cell_measurement_theta_max      28
_cell_measurement_theta_min      3
_cell_volume                     3239.5(4)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            232684
_diffrn_reflns_theta_full        26.372
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.218
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.253
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1387.991
_exptl_crystal_size_max          0.413
_exptl_crystal_size_mid          0.401
_exptl_crystal_size_min          0.216
_refine_diff_density_max         1.15
_refine_diff_density_min         -0.61
_refine_ls_extinction_coef       139.110
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     784
_refine_ls_number_reflns         13209
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.0008528
_refine_ls_shift/su_mean         0.0000429
_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: 
 2.50 3.24 0.860 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1083
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1083
_reflns_limit_h_max              17
_reflns_limit_h_min              -19
_reflns_limit_k_max              17
_reflns_limit_k_min              -19
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                11203
_reflns_number_total             13215
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.83
_oxford_diffrn_Wilson_scale      69.96
_oxford_refine_ls_r_factor_ref   0.0499
_oxford_refine_ls_scale          0.11731(2)
_oxford_reflns_number_all        13209
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            d1ob01487k2.cif
_cod_data_source_block           TL550
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_chemical_melting_point' value '513.0-517.5' was changed
to '515(2)' -- the average value was taken and precision was
estimated.

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_H-M      'P -1 '
_cod_original_formula_sum        'C58 H78.00 N4 O20 S5'
_cod_database_code               7158259