Regioselective S<sub>N</sub>Ar reaction of the phenoxathiin-based thiacalixarene as a route to a novel macrocyclic skeleton.
Landovský, Tomáš; Eigner, Václav; Babor, Martin; Tichotová, Markéta; Dvořáková, Hana; Lhoták, Pavel; Chemical communications (Cambridge, England) 56 (2019) 78–81; doi:10.1039/c9cc08335a

data_7124541
_publ_section_title
;
 Regioselective S<sub>N</sub>Ar reaction of the phenoxathiin-based
 thiacalixarene as a route to a novel macrocyclic skeleton.
;
_journal_issue                   1
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              78
_journal_page_last               81
_journal_paper_doi               10.1039/c9cc08335a
_journal_volume                  56
_journal_year                    2019
_chemical_formula_moiety         'C46 H60 O13 S4, C H3 N O2'
_chemical_formula_sum            'C47 H63 N O15 S4'
_chemical_formula_weight         1010.27
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_update_record
;
2019-07-29 deposited with the CCDC.	2019-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.8797(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.5665(5)
_cell_length_b                   21.0808(6)
_cell_length_c                   13.5866(4)
_cell_measurement_reflns_used    163
_cell_measurement_temperature    180
_cell_measurement_theta_max      58
_cell_measurement_theta_min      13
_cell_volume                     5162.5(3)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_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      180
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
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_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            94775
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_diffrn_reflns_theta_max         72.225
_diffrn_reflns_theta_min         2.451
_diffrn_standards_number         0
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2143.986
_exptl_crystal_size_max          0.510
_exptl_crystal_size_mid          0.357
_exptl_crystal_size_min          0.228
_refine_diff_density_max         0.55
_refine_diff_density_min         -0.36
_refine_ls_extinction_coef       89(7)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         10175
_refine_ls_number_restraints     46
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.0016695
_refine_ls_shift/su_mean         0.0001106
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 3.85P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0943
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0943
_reflns_limit_h_max              22
_reflns_limit_h_min              -22
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                9358
_reflns_number_total             10176
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.66
_oxford_diffrn_Wilson_scale      83.96
_oxford_refine_ls_r_factor_ref   0.0390
_oxford_refine_ls_scale          0.10970(3)
_oxford_reflns_number_all        10175
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c9cc08335a2.cif
_cod_data_source_block           TL430b
_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 6909 2019-04-08 15:41:33Z antanas 

 Adding full bibliography for 7124541--7124542.cif.
;
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               7124541