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_7057931
_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         'C61 H64 O11 S4, 2(C H Cl3), 0.392(H2 O) '
_chemical_formula_sum            'C63 H66.78 Cl6 O11.39 S4'
_chemical_formula_weight         1347.22
_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                99.2830(16)
_cell_angle_beta                 96.0609(15)
_cell_angle_gamma                107.4553(15)
_cell_formula_units_Z            2
_cell_length_a                   12.1853(5)
_cell_length_b                   13.2193(5)
_cell_length_c                   21.7629(9)
_cell_measurement_reflns_used    1363
_cell_measurement_temperature    180
_cell_measurement_theta_max      71
_cell_measurement_theta_min      4
_cell_volume                     3255.9(2)
_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 0.996
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.051
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            86869
_diffrn_reflns_theta_full        71.257
_diffrn_reflns_theta_max         72.711
_diffrn_reflns_theta_min         2.085
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.084
_exptl_absorpt_correction_T_max  0.59
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1403.80
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Chloroform; Methanol'
_exptl_crystal_size_max          0.333
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.98
_refine_diff_density_min         -0.92
_refine_ls_extinction_coef       29.4(14)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9765
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     800
_refine_ls_number_reflns         12852
_refine_ls_number_restraints     43
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.0023419
_refine_ls_shift/su_mean         0.0000734
_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: 
 2.84 3.64 0.910 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1330
_refine_ls_wR_factor_gt          0.1290
_refine_ls_wR_factor_ref         0.1330
_reflns_limit_h_max              14
_reflns_limit_h_min              -15
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                10974
_reflns_number_total             12853
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.82
_oxford_diffrn_Wilson_scale      91.25
_oxford_refine_ls_r_factor_ref   0.0602
_oxford_refine_ls_scale          0.10433(3)
_oxford_reflns_number_all        12852
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c8nj04690e2.cif
_cod_data_source_block           I_CCDC1
_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               7057931