Chemoselective oxidation of phenoxathiin-based thiacalix[4]arene and the stereoselective alkylation of products
Landovský, T.; Dvořáková, H.; Eigner, V.; Babor, M.; Krupička, M.; Kohout, M.; Lhoták, P.; New Journal of Chemistry 42 (2018) 20074–; doi:10.1039/C8NJ04690E

data_7057927
_publ_section_title
;
 Chemoselective oxidation of phenoxathiin-based thiacalix[4]arene and the
 stereoselective alkylation of products
;
_journal_issue                   24
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              20074
_journal_paper_doi               10.1039/C8NJ04690E
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C49 H63 O12 S4, C H Cl3'
_chemical_formula_sum            'C50 H64 Cl3 O12 S4'
_chemical_formula_weight         1091.67
_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
_audit_update_record
;
2018-05-22 deposited with the CCDC.
2018-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                89.772(3)
_cell_angle_beta                 81.452(3)
_cell_angle_gamma                68.198(3)
_cell_formula_units_Z            2
_cell_length_a                   11.9033(13)
_cell_length_b                   13.7880(15)
_cell_length_c                   17.6831(18)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    180
_cell_measurement_theta_max      72
_cell_measurement_theta_min      3
_cell_volume                     2660.5(5)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.064
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            77043
_diffrn_reflns_theta_full        68.238
_diffrn_reflns_theta_max         68.238
_diffrn_reflns_theta_min         2.531
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.517
_exptl_absorpt_correction_T_max  0.50
_exptl_absorpt_correction_T_min  0.45
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1150
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Chloroform; Methanol'
_exptl_crystal_size_max          0.339
_exptl_crystal_size_mid          0.228
_exptl_crystal_size_min          0.199
_refine_diff_density_max         0.81
_refine_diff_density_min         -0.94
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9918
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     661
_refine_ls_number_reflns         9724
_refine_ls_number_restraints     51
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0766
_refine_ls_shift/su_max          0.0051676
_refine_ls_shift/su_mean         0.0002393
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.13P)^2^ + 4.92P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2211
_refine_ls_wR_factor_gt          0.2176
_refine_ls_wR_factor_ref         0.2211
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                8874
_reflns_number_total             9726
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.29
_oxford_diffrn_Wilson_scale      170.30
_oxford_refine_ls_r_factor_ref   0.0800
_oxford_refine_ls_scale          0.12524(9)
_oxford_reflns_number_all        9724
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c8nj04690e2.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7057927--7057931.cif.
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7057927