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_7057928
_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         'C40 H46 O11 S4, C H2 Cl2, C H4 O'
_chemical_formula_sum            'C42 H52 Cl2 O12 S4'
_chemical_formula_weight         948.02
_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
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2018-06-12 deposited with the CCDC.
2018-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.0627(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7527(5)
_cell_length_b                   13.3087(4)
_cell_length_c                   25.0148(8)
_cell_measurement_reflns_used    280
_cell_measurement_temperature    180
_cell_measurement_theta_max      69
_cell_measurement_theta_min      28
_cell_volume                     4742.6(3)
_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      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 Apex3'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.132
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            82323
_diffrn_reflns_theta_full        74.668
_diffrn_reflns_theta_max         74.668
_diffrn_reflns_theta_min         3.102
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.358
_exptl_absorpt_correction_T_max  0.28
_exptl_absorpt_correction_T_min  0.20
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1991.966
_exptl_crystal_size_max          0.592
_exptl_crystal_size_mid          0.454
_exptl_crystal_size_min          0.382
_refine_diff_density_max         0.60
_refine_diff_density_min         -0.51
_refine_ls_extinction_coef       164(14)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9364
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         9700
_refine_ls_number_restraints     202
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.0009376
_refine_ls_shift/su_mean         0.0000636
_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: 
 11.9 18.3 8.63 2.09 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1403
_refine_ls_wR_factor_gt          0.1402
_refine_ls_wR_factor_ref         0.1403
_reflns_limit_h_max              17
_reflns_limit_h_min              -18
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              0
_reflns_number_gt                9552
_reflns_number_total             9700
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.24
_oxford_diffrn_Wilson_scale      60.44
_oxford_refine_ls_r_factor_ref   0.0561
_oxford_refine_ls_scale          0.12103(6)
_oxford_reflns_number_all        9700
_cod_data_source_file            c8nj04690e2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7057927--7057931.cif.'
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               7057928
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)